[Synthesis and characteristics of porous hydroxyapatite bioceramics].

Science.gov (United States)

Niu, Jinlong; Zhang, Zhenxi; Jiang, Dazong

2002-06-01

The macroporous structure of human bone allows the ingrowth of the soft tissues and organic cells into the bone matrix, profits the development and metabolism of bone tissue, and adapts the bone to the change of load. There is great requirement for artificial biomimic porous bioactive ceramics with the similar structure of bone tissue that can be used clinically for repairing lost bone. Fine hydroxyapatite (HAp) powder produced by wet chemical reaction was mixed with hydrogen peroxide (H2O2), polyvinyl alcohol, methyl cellulose or other pores-making materials to form green cake. After drying at low temperature (below 100 degrees C) and decarbonizing at about 300 degrees C-400 degrees C, the spongy ceramic block was sintered at high temperature, thus, macroporous HAp bioceramic with interconnected pores and reasonable porosity and pore-diameter was manufactured. This kind of porous HAp bioceramics were intrinsically osteoinductive to a certain degree, but its outstanding property was that they can absorb human bone morphogenetic proteins and other bone growth factors to form composites, so that the macroporous HAp bioactive ceramic has appropriate feasibility for clinical application. From the point of biomedical application, the recent developments in synthesis and characteristics investigation of macroporous HAp are reviewed in this paper.

Characterization of x-ray diffraction and electron spin resonance: Effects of sintering time and temperature on bovine hydroxyapatite

International Nuclear Information System (INIS)

Kusrini, Eny; Sontang, Muhammad

2012-01-01

The physical and chemical properties of a hydroxyapatite produced by the sintering of bovine bone were investigated by powder x-ray diffraction (PXRD), electron spin resonance (ESR), energy dispersive x-ray spectroscopy (EDX), scanning electron microscopy (SEM), Fourier transform infrared (FTIR), and differential thermal analysis (DTA). A bovine bone powder was sintered at different temperatures ranging from 500 to 1400 °C. The influences of post-irradiation storage on the radiation ESR response of the bovine bone powder before and after sintering were also studied. The results indicate that the sintered bovine bone powder contained hydroxyapatite. Diffraction patterns were sharp and clear based on the (211), (300), and (202) reflections corresponding to bovine hydroxyapatite (BHA), which confirmed the phase purity and high crystalline grade of the BHA produced. The PXRD profile of BHA was dependent on sintering temperatures and times. The molecular formula of BHA was determined by Rietveld analysis showed a similar structure and composition to calcium hydroxyapatite in hexagonal P6 3 /m space group a=b=9.435 Å and c=6.895 Å. ESR data showed that the sintering process can decrease the number of free radicals in BHA; it also revealed that the number of free radicals is constant during long storage periods (75 days). The sintering technique described in this study may be used to extract hydroxyapatite from biowaste bovine bone, leading to its application as a bone filler. - Highlights: ► Natural hydroxyapatite was produced from the bio-wasting bovine bones by sintering method. ► PXRD profile of BHA is dependent on the different temperatures and times in sintering process. ► ESR data is useful to study the typical of free radicals formed in the samples after irradiation. ► Stability and physicochemical properties of BHA is dependent on the different storage times. ► Technique is able to be used to find the natural hydroxyapatite applicable for bone filler.

Influence of spark plasma sintering and baghdadite powder on mechanical properties of hydroxyapatite

NARCIS (Netherlands)

Khandan, A.; Karamian, E.; Mehdikhani-Nahrkhalaji, M.; Mirmohammadi, H.; Farzadi, A.; Ozada, N.; Heidarshenas, B.; Zamani, K.

2015-01-01

Since hydroxyapatite-based materials have similar composition and crystallinity as natural calcified tissues, can be used for bone/tissue engineering. In the present study a novel nanocomposite based on bioceramics such as Natural Hydroxyapatite (NHA) and Baghdadite (BAG), was sintered by spark

Hydroxyapatite-silver nanoparticles coatings on porous polyurethane scaffold.

Science.gov (United States)

Ciobanu, Gabriela; Ilisei, Simona; Luca, Constantin

2014-02-01

The present paper is focused on a study regarding the possibility of obtaining hydroxyapatite-silver nanoparticle coatings on porous polyurethane scaffold. The method applied is based on a combined strategy involving hydroxyapatite biomimetic deposition on polyurethane surface using a Supersaturated Calcification Solution (SCS), combined with silver ions reduction and in-situ crystallization processes on hydroxyapatite-polyurethane surface by sample immersing in AgNO3 solution. The morphology, composition and phase structure of the prepared samples were characterized by scanning electron microscopy coupled with energy dispersive X-ray spectroscopy (SEM-EDX), X-ray diffraction (XRD), UV-Vis spectroscopy and X-ray photoelectron spectroscopy (XPS) measurements. The data obtained show that a layer of hydroxyapatite was deposited on porous polyurethane support and the silver nanoparticles (average size 34.71 nm) were dispersed among and even on the hydroxyapatite crystals. Hydroxyapatite/polyurethane surface acts as a reducer and a stabilizing agent for silver ions. The surface plasmon resonance peak in UV-Vis absorption spectra showed an absorption maximum at 415 nm, indicating formation of silver nanoparticles. The hydroxyapatite-silver polyurethane scaffolds were tested against Staphylococcus aureus and Escherichia coli and the obtained data were indicative of good antibacterial properties of the materials. © 2013.

Zirconia-hydroxyapatite composite material with micro porous structure.

Science.gov (United States)

Matsumoto, Takuya Junior; An, Sang-Hyun; Ishimoto, Takuya; Nakano, Takayoshi; Matsumoto, Takuya; Imazato, Satoshi

2011-11-01

Titanium plates and apatite blocks are commonly used for restoring large osseous defects in dental and orthopedic surgery. However, several cases of allergies against titanium have been recently reported. Also, sintered apatite block does not possess sufficient mechanical strength. In this study, we attempted to fabricate a composite material that has mechanical properties similar to biocortical bone and high bioaffinity by compounding hydroxyapatite (HAp) with the base material zirconia (ZrO(2)), which possesses high mechanical properties and low toxicity toward living organisms. After mixing the raw material powders at several different ZrO(2)/HAp mixing ratios, the material was compressed in a metal mold (8 mm in diameter) at 5 MPa. Subsequently, it was sintered for 5 h at 1500°C to obtain the ZrO(2)/HAp composite. The mechanical property and biocompatibility of materials were investigated. Furthermore, osteoconductivity of materials was investigated by animal studies. A composite material with a minute porous structure was successfully created using ZrO(2)/HAp powders, having different particle sizes, as the starting material. The material also showed high protein adsorption and a favorable cellular affinity. When the mixing ratio was ZrO(2)/HAp=70/30, the strength was equal to cortical bone. Furthermore, in vivo experiments confirmed its high osteoconductivity. The composite material had strength similar to biocortical bones with high cell and tissue affinities by compounding ZrO(2) and HAp. The ZrO(2)/HAp composite material having micro porous structure would be a promising bone restorative material. Copyright © 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Hydroxyapatite-silver nanoparticles coatings on porous polyurethane scaffold

International Nuclear Information System (INIS)

Ciobanu, Gabriela; Ilisei, Simona; Luca, Constantin

2014-01-01

The present paper is focused on a study regarding the possibility of obtaining hydroxyapatite-silver nanoparticle coatings on porous polyurethane scaffold. The method applied is based on a combined strategy involving hydroxyapatite biomimetic deposition on polyurethane surface using a Supersaturated Calcification Solution (SCS), combined with silver ions reduction and in-situ crystallization processes on hydroxyapatite-polyurethane surface by sample immersing in AgNO 3 solution. The morphology, composition and phase structure of the prepared samples were characterized by scanning electron microscopy coupled with energy dispersive X-ray spectroscopy (SEM-EDX), X-ray diffraction (XRD), UV-Vis spectroscopy and X-ray photoelectron spectroscopy (XPS) measurements. The data obtained show that a layer of hydroxyapatite was deposited on porous polyurethane support and the silver nanoparticles (average size 34.71 nm) were dispersed among and even on the hydroxyapatite crystals. Hydroxyapatite/polyurethane surface acts as a reducer and a stabilizing agent for silver ions. The surface plasmon resonance peak in UV-Vis absorption spectra showed an absorption maximum at 415 nm, indicating formation of silver nanoparticles. The hydroxyapatite-silver polyurethane scaffolds were tested against Staphylococcus aureus and Escherichia coli and the obtained data were indicative of good antibacterial properties of the materials. - Highlights: • The hydroxyapatite and silver nanoparticles were grown on the polyurethane scaffold • The hydroxyapatite/polyurethane acts as reducing agent, stabilizer and matrix for Ag • The samples were well characterized by SEM-EDX, XRD, XPS, UV-visible spectroscopy • The hydroxyapatite/silver polyurethane scaffold shows antibacterial property

Preparation Of Porous And Dense Bodies From Hydroxyapatite Powders Prepared Via Sol-Gel Technique

International Nuclear Information System (INIS)

Sopyan, Lis

2001-01-01

Hydroxyapatite (HA) ceramics is clinically proven and, thus, a reliable material for medical applications, that is, for use in dental and orthopedical surgery to fill cavities in bones. In this paper, we report a preliminary study on development of HA porous and dense materials manufactured using fine HA powders prepared via a sol-gel technique. In the preparation of HA porous bodies, slurries of the as-prepared powder were prepared with an adjusted loading ofHA, using Duramax of 0-3021 type as dispersant. After soaking cellulosic sponges into the slurry, the sponges were dried and then subjected to heat-treatment at 600 o C, followed by sintering at 1250 o C for I h. The apparent density of the porous bodies is 1.290 g/cm 3 , with a porosity of 59%. The sintering shrinkage is about 20% (in respect of dimension) and 44 % (in respect of volume). Morphological evaluation of the porous bodies showed that the samples contained macropores of 1-2 mm diameter and micropores of 1-2 μm diameter. The measurement of mechanical strength provided 1.31 ± 0.30 MPa. Subsequently, dense samples were prepared from the as-prepared powder. In this case, the powder was mixed with poly(vinyl alcohol) and distilled water to make a slurry. The mixture was mixed using Zirconia balls as the crusher for 2h. The suspension was then spray-dried, and well-dispersed powder was obtained. The powder was compressed uniaxially using cold pressing technique at 800 kglcm2 and the pellets obtained were sintered in air at : 250 o C for I h. The sintered dense bodies have apparent density of 2.855 g/cm 3 , with a 10% porosity. The flexural strength of the dense bodies measured on the specimens of riimension 2 mm x 2.5 mm gave rise to the considerable value of 57.7 MPa

Thermally stable sintered porous metal articles

International Nuclear Information System (INIS)

Gombach, A.L.; Thellmann, E.L.

1980-01-01

A sintered porous metal article is provided which is essentially thermally stable at elevated temperatures. In addition, a method for producing such an article is also provided which method comprises preparing a blend of base metal particles and active dispersoid particles, forming the mixture into an article of the desired shape, and heating the so-formed article at sintering temperatures

Hydroxyapatite and zirconia composites: Effect of MgO and MgF2 on the stability of phases and sinterability

International Nuclear Information System (INIS)

Evis, Zafer; Usta, Metin; Kutbay, Isil

2008-01-01

Composites of hydroxyapatite with cubic zirconia with MgO or MgF 2 were pressureless sintered at temperatures from 1000 to 1300 deg. C. The reactions and transformations of phases were monitored with X-ray diffraction. For the hydroxyapatite and zirconia composites with MgO, calcium diffused from hydroxyapatite into the zirconia, and hydroxyapatite decomposed to tri-calcium phosphate at sintering temperatures higher than 1000 deg. C. Above about 1200 deg. C, CaZrO 3 was formed. Composites containing the MgF 2 decomposed slower than the composites with MgO which was verified by the changes in the lattice volume of the hydroxyapatite left in the composites. Fluorine ions in MgF 2 diffused into hydroxyapatite which resulted in thermal stability at high sintering temperatures. Composites with MgF 2 had higher hardness than those with MgO. The lowest porosity was found in a composite initially containing 10 wt% cubic zirconia and 5 wt% MgF 2

Superior sealing effect of hydroxyapatite in porous-coated implants

DEFF Research Database (Denmark)

Rahbek, Ole; Kold, Søren; Bendix, Knud

2005-01-01

Migration of wear debris to the periprosthetic bone is a major cause of osteolysis and implant failure. Both closed-pore porous coatings and hydroxyapatite (HA) coatings have been claimed to prevent the migration of wear debris. We investigated whether HA could augment the sealing effect of a por......Migration of wear debris to the periprosthetic bone is a major cause of osteolysis and implant failure. Both closed-pore porous coatings and hydroxyapatite (HA) coatings have been claimed to prevent the migration of wear debris. We investigated whether HA could augment the sealing effect...

Microwave sintering and in vitro study of defect-free stable porous multilayered HAp–ZrO2 artificial bone scaffold

Directory of Open Access Journals (Sweden)

Dong-Woo Jang, Thi-Hiep Nguyen, Swapan Kumar Sarkar and Byong-Taek Lee

2012-01-01

Full Text Available Continuously porous hydroxyapatite (HAp/t-ZrO2 composites containing concentric laminated frames and microchanneled bodies were fabricated by an extrusion process. To investigate the mechanical properties of HAp/t-ZrO2 composites, the porous composites were sintered at different temperatures using a microwave furnace. The microstructure was designed to imitate that of natural bone, particularly small bone, with both cortical and spongy bone sections. Each microchannel was separated by alternating lamina of HAp, HAp–(t-ZrO2 and t-ZrO2. HAp and ZrO2 phases existed on the surface of the microchannel and the core zone to increase the biocompatibility and mechanical properties of the HAp-ZrO2 artificial bone. The sintering behavior was evaluated and the optimum sintering temperature was found to be 1400 °C, which produced a stable scaffold. The material characteristics, such as the microstructure, crystal structure and compressive strength, were evaluated in detail for different sintering temperatures. A detailed in vitro study was carried out using MTT assay, western blot analysis, gene expression by polymerase chain reaction and laser confocal image analysis of cell proliferation. The results confirmed that HAp-ZrO2 performs as an artificial bone, showing excellent cell growth, attachment and proliferation behavior using osteoblast-like MG63 cells.

Fabrication and study of double sintered TiNi-based porous alloys

Science.gov (United States)

Sergey, Anikeev; Valentina, Hodorenko; Timofey, Chekalkin; Victor, Gunther; Ji-hoon, Kang; Ji-soon, Kim

2017-05-01

Double-sintered porous TiNi-based alloys were fabricated and their structural characteristics and physico-mechanical properties were investigated. A fabrication technology of powder mixtures is elaborated in this article. Sintering conditions were chosen experimentally to ensure good structure and properties. The porous alloys were synthesized by solid-state double diffusion sintering (DDS) of Ti-Ni powder and prepare to obtain dense, crack-free, and homogeneous samples. The Ti-Ni compound sintered at various temperatures was investigated by scanning electron microscopy. Phase composition of the sintered alloys was determined by x-ray diffraction. Analysis of the data confirmed the morphology and structural parameters. Mechanical and physical properties of the sintered alloys were evaluated. DDS at 1250 °C was found to be optimal to produce porous samples with a porosity of 56% and mean pore size of 90 μm. Pore size distribution was unimodal within the narrow range of values. The alloys present enhanced strength and ductility, owing to both the homogeneity of the macrostructure and relative elasticity of the bulk, which is hardened by the Ni-rich precipitates. These results suggest the possibility to manufacture porous TiNi-based alloys for application as a new class of dental implants.

Production of sintered porous metal fluoride pellets

Science.gov (United States)

Anderson, L.W.; Stephenson, M.J.

1973-12-25

Porous pellets characterized by a moderately reactive crust and a softer core of higher reactivity are produced by forming agglomerates containing a metal fluoride powder and a selected amount ofwater. The metal fluoride is selected to be sinterable and essentially non-reactive with gaseous fluorinating agents. The agglomerates are contacted with a gaseous fluorinating agent under controlled conditions whereby the heat generated by localized reaction of the agent and water is limited to values effccting bonding by localized sintering. Porous pellets composed of cryolite (Na/sub 3/AlF/sub 6/) can be used to selectively remove trace quantities of niobium pentafluoride from a feed gas consisting predominantly of uranium hexafluoride. (Official Gazette)

Characteristics Of The Porous Body Sintered By Nano-Sized Fe-Cr-Al Alloy Powder

Directory of Open Access Journals (Sweden)

Lee Su-In

2015-06-01

Full Text Available Porous metal with uniform honeycomb structure was successfully produced by sintering using Fe-Cr-Al nano powder, which was prepared by the pulsed wire evaporation (PWE in ethanol. Its process consisted of the several steps; 1 coating on the surface of polyurethane sponge with the liquid droplets generated from the ethanol-based slurry where the Fe-Cr-Al nano powders were uniformly dispersed, 2 heat treatment of debinding to remove the polyurethane sponge and 3 sintering of the porous green body formed by Fe-Cr-Al nano powders. The strut thickness of porous Fe-Cr-Al was increased by the increase of spraying times in ESP step. Also, The shrinkages and the oxidation resistance of the sintered porous body was increased with increase of sintering temperature. The optimal sintering temperature was shown to 1450°C in views to maximize the oxidation resistance and sinterability.

Sintering of Multilayered Porous Structures: Part I-Constitutive Models

DEFF Research Database (Denmark)

Olevsky, Eugene; Tadesse Molla, Tesfaye; Frandsen, Henrik Lund

2013-01-01

Theoretical analyses of shrinkage and distortion kinetics during sintering of bilayered porous structures are carried out. The developed modeling framework is based on the continuum theory of sintering; it enables the direct assessment of the cofiring process outcomes and of the impact of process...

Effect of the quantity of carbonate components and sintering parameters on the quality of hydrothermally synthesized carbonate hydroxyapatite

Science.gov (United States)

Ruddyard, A. A.; Soejoko, D. S.; Nurlely

2017-07-01

Carbonated hydroxyapatite is a biomaterial with high biocompatibility with human bone, moreso than regular hydroxyapatite, making it an acceptable synthetic bone graft material. The purpose of this research is to study the effect of sintering temperature and time on carbonated hydroxyapatite samples synthesized using a hydrothermal method with CaCO3 as one of its components. The samples are then characterized using Fourier-Transform Infrared Spectroscopy, X-Ray Diffraction, and Scanning Electron Microscope. Infrared (IR) spectra showed that the CO3 content in each sample is proportional to the amount of CaCO3 used during synthesis. X-Ray Diffraction (XRD) patterns showed an increase in apatite content and a decrease in calcite content as sintering temperature and time increases, with temperature increases having a stronger effect on the samples than time increases. Calcite disappears completely after sintering at 900 °C for 2 hours.

Influence of preparation method on hydroxyapatite porous scaffolds

Indian Academy of Sciences (India)

Administrator

Hydroxyapatite (HA) is extensively used in medical applications as an artificial bone because of its similarity to ... system, have been applied to fabricate HA porous scaffolds. In this work .... ceramic structured by the colloidal processing was.

Synthesis and release of trace elements from hollow and porous hydroxyapatite spheres

International Nuclear Information System (INIS)

Xia Wei; Grandfield, Kathryn; Schwenke, Almut; Engqvist, Haakan

2011-01-01

It is known that organic species regulate fabrication of hierarchical biological forms via solution methods. However, in this study, we observed that the presence of inorganic ions plays an important role in the formation and regulation of biological spherical hydroxyapatite formation. We present a mineralization method to prepare ion-doped hydroxyapatite spheres with a hierarchical structure that is free of organic surfactants and biological additives. Porous and hollow strontium-doped hydroxyapatite spheres were synthesized via controlling the concentration of strontium ions in a calcium and phosphate buffer solution. Similarly, fluoride and silicon-doped hydroxyapatite spheres were synthesized. While spherical particle formation was attainable at low and high temperature for Sr-doped hydroxyapatite, it was only possible at high temperature in the F/Si-doped system. The presence of inorganic ions not only plays an important role in the formation and regulation of biological spherical hydroxyapatite, but also could introduce pharmaceutical effects as a result of trace element release. Such ion release results showed a sustained release with pH responsive behavior, and significantly influenced the hydroxyapatite re-precipitation. These ion-doped hydroxyapatite spheres with hollow and porous structure could have promising applications as bone/tooth materials, drug delivery systems, and chromatography supports.

Hydroxyapatite coatings deposited by liquid precursor plasma spraying: controlled dense and porous microstructures and osteoblastic cell responses

International Nuclear Information System (INIS)

Huang Yi; Song Lei; Liu Xiaoguang; Xiao Yanfeng; Wu Yao; Chen Jiyong; Wu Fang; Gu Zhongwei

2010-01-01

Hydroxyapatite coatings were deposited on Ti-6Al-4V substrates by a novel plasma spraying process, the liquid precursor plasma spraying (LPPS) process. X-ray diffraction results showed that the coatings obtained by the LPPS process were mainly composed of hydroxyapatite. The LPPS process also showed excellent control on the coating microstructure, and both nearly fully dense and highly porous hydroxyapatite coatings were obtained by simply adjusting the solid content of the hydroxyapatite liquid precursor. Scanning electron microscope observations indicated that the porous hydroxyapatite coatings had pore size in the range of 10-200 μm and an average porosity of 48.26 ± 0.10%. The osteoblastic cell responses to the dense and porous hydroxyapatite coatings were evaluated with human osteoblastic cell MG-63, in respect of the cell morphology, proliferation and differentiation, with the hydroxyapatite coatings deposited by the atmospheric plasma spraying (APS) process as control. The cell experiment results indicated that the heat-treated LPPS coatings with a porous structure showed the best cell proliferation and differentiation among all the hydroxyapatite coatings. Our results suggest that the LPPS process is a promising plasma spraying technique for fabricating hydroxyapatite coatings with a controllable microstructure, which has great potential in bone repair and replacement applications.

The evaluation of hydroxyapatite (HA) coated and uncoated porous tantalum for biomedical material applications

International Nuclear Information System (INIS)

Safuan, Nadia; Sukmana, Irza; Kadir, Mohammed Rafiq Abdul; Noviana, Deni

2014-01-01

Porous tantalum has been used as an orthopedic implant for bone defects as it has a good corrosion resistance and fatigue behaviour properties. However, there are some reports on the rejection of porous Ta after the implantation. Those clinical cases refer to the less bioactivity of metallic-based materials. This study aims to evaluate hydroxyapatite coated and uncoated porous Tantalum in order to improve the biocompatibility of porous tantalum implant and osseointegration. Porous tantalum was used as metallic-base substrate and hydroxyapatite coating has been done using plasma-spraying technique. Scanning Electron Microscopy (SEM) and Field Emission Scanning Electron Microscopy (FESEM) techniques were utilizes to investigate the coating characteristics while Confocal Raman Microscopy to investigate the interface and image. The effect of coating to the corrosion behaviour was assessed by employing potentiodynamic polarization tests in simulated body fluid at 37±1 °C. Based on SEM and FESEM results, the morphologies as well the weight element consists in the uncoated and hydroxyapatite coated porous tantalum were revealed. The results indicated that the decrease in corrosion current density for HA coated porous Ta compared to the uncoated porous Ta. This study concluded that by coating porous tantalum with HA supports to decrease the corrosion rate of pure porous.

The Evaluation of Hydroxyapatite (HA) Coated and Uncoated Porous Tantalum for Biomedical Material Applications

Science.gov (United States)

Safuan, Nadia; Sukmana, Irza; Kadir, Mohammed Rafiq Abdul; Noviana, Deni

2014-04-01

Porous tantalum has been used as an orthopedic implant for bone defects as it has a good corrosion resistance and fatigue behaviour properties. However, there are some reports on the rejection of porous Ta after the implantation. Those clinical cases refer to the less bioactivity of metallic-based materials. This study aims to evaluate hydroxyapatite coated and uncoated porous Tantalum in order to improve the biocompatibility of porous tantalum implant and osseointegration. Porous tantalum was used as metallic-base substrate and hydroxyapatite coating has been done using plasma-spraying technique. Scanning Electron Microscopy (SEM) and Field Emission Scanning Electron Microscopy (FESEM) techniques were utilizes to investigate the coating characteristics while Confocal Raman Microscopy to investigate the interface and image. The effect of coating to the corrosion behaviour was assessed by employing potentiodynamic polarization tests in simulated body fluid at 37±1 °C. Based on SEM and FESEM results, the morphologies as well the weight element consists in the uncoated and hydroxyapatite coated porous tantalum were revealed. The results indicated that the decrease in corrosion current density for HA coated porous Ta compared to the uncoated porous Ta. This study concluded that by coating porous tantalum with HA supports to decrease the corrosion rate of pure porous.

Porous copper template from partially spark plasma-sintered Cu–Zn ...

Indian Academy of Sciences (India)

Administrator

analysis. Keywords. Metal; corrosion; porous structure; sintering; powder metallurgy. 1. Introduction ... well as in the case, when the overall electrode potential of the final ... at 100 °C/min to reach sintering temperature and load was applied ...

Accurate Fabrication of Hydroxyapatite Bone Models with Porous Scaffold Structures by Using Stereolithography

Energy Technology Data Exchange (ETDEWEB)

Maeda, Chiaki; Tasaki, Satoko; Kirihara, Soshu, E-mail: c-maeda@jwri.osaka-u.ac.jp [Joining and Welding Research Institute, Osaka University, 11-1 Mihogaoka, Ibaraki City, Osaka 567-0047 (Japan)

2011-05-15

Computer graphic models of bioscaffolds with four-coordinate lattice structures of solid rods in artificial bones were designed by using a computer aided design. The scaffold models composed of acryl resin with hydroxyapatite particles at 45vol. % were fabricated by using stereolithography of a computer aided manufacturing. After dewaxing and sintering heat treatment processes, the ceramics scaffold models with four-coordinate lattices and fine hydroxyapatite microstructures were obtained successfully. By using a computer aided analysis, it was found that bio-fluids could flow extensively inside the sintered scaffolds. This result shows that the lattice structures will realize appropriate bio-fluid circulations and promote regenerations of new bones.

Accurate Fabrication of Hydroxyapatite Bone Models with Porous Scaffold Structures by Using Stereolithography

International Nuclear Information System (INIS)

Maeda, Chiaki; Tasaki, Satoko; Kirihara, Soshu

2011-01-01

Computer graphic models of bioscaffolds with four-coordinate lattice structures of solid rods in artificial bones were designed by using a computer aided design. The scaffold models composed of acryl resin with hydroxyapatite particles at 45vol. % were fabricated by using stereolithography of a computer aided manufacturing. After dewaxing and sintering heat treatment processes, the ceramics scaffold models with four-coordinate lattices and fine hydroxyapatite microstructures were obtained successfully. By using a computer aided analysis, it was found that bio-fluids could flow extensively inside the sintered scaffolds. This result shows that the lattice structures will realize appropriate bio-fluid circulations and promote regenerations of new bones.

XANES analysis of calcium and sodium phosphates and silicates and hydroxyapatite-Bioglass (registered) 45S5 co-sintered bioceramics

Energy Technology Data Exchange (ETDEWEB)

Demirkiran, Hande [Graduate Student, Materials Science and Engineering Department, University of Texas at Arlington, Arlington, TX (United States); Hu Yongfeng; Zuin, Lucia [Beamline Scientist, Canadian Light Source, Saskatoon, SK (Canada); Appathurai, Narayana [Beamline Scientist, Synchrotron Radiation Center, Madison, WI (United States); Aswath, Pranesh B., E-mail: aswath@uta.edu [Materials Science and Engineering Department, University of Texas at Arlington, Arlington, TX (United States)

2011-03-12

Bioglass (registered) 45S5 was co-sintered with hydroxyapatite at 1200 deg. C. When small amounts (< 5 wt.%) of Bioglass (registered) 45S5 was added it behaved as a sintering aid and also enhanced the decomposition of hydroxyapatite to {beta}-tricalcium phosphate. However when 10 wt.% and 25 wt.% Bioglass (registered) 45S5 was used it resulted in the formation of Ca{sub 5}(PO{sub 4}){sub 2}SiO{sub 4} and Na{sub 3}Ca{sub 6}(PO{sub 4}){sub 5} in an amorphous silicate matrix respectively. These chemistries show improved bioactivity compared to hydroxyapatite and are the subject of this study. The structure of several crystalline calcium and sodium phosphates and silicates as well as the co-sintered hydroxyapatite-Bioglass (registered) 45S5 bioceramics were examined using XANES spectroscopy. The nature of the crystalline and amorphous phases were studied using silicon (Si) and phosphorus (P) K- and L{sub 2,3}-edge and calcium (Ca) K-edge XANES. Si L{sub 2,3}-edge spectra of sintered bioceramic compositions indicates that the primary silicates present in these compositions are sodium silicates in the amorphous state. From Si K-edge spectra, it is shown that the silicates are in a similar structural environment in all the sintered bioceramic compositions with 4-fold coordination. Using P L{sub 2,3}-edge it is clearly shown that there is no evidence of sodium phosphate present in the sintered bioceramic compositions. In the P K-edge spectra, the post-edge shoulder peak at around 2155 eV indicates that this shoulder to be more defined for calcium phosphate compounds with decreasing solubility and increasing thermodynamic stability. This shoulder peak is more noticeable in hydroxyapatite and {beta}-TCP indicating greater stability of the phosphate phase. The only spectra that does not show a noticeable peak is the composition with Na{sub 3}Ca{sub 6}(PO{sub 4}){sub 5} in a silicate matrix indicating that it is more soluble compared to the other compositions.

Porous HA-Al2O3 composite characterization using corn starch as a porogen agent

International Nuclear Information System (INIS)

Silva, L.A.J. da; Galdino, A.G.S.; Cardoso, G.B.C.; Zavaglia, C.A.C.

2011-01-01

The porous ceramics based on hydroxyapatite have great potential for application in bone grafts due to its chemical similarity with the mineral phase of bone tissue, but have poor biomechanical properties, which cause limitations in its applications. This work aims to analyze the structural characteristics of porous ceramics obtained by addition of hydroxyapatite (HA, sintered in the laboratory), Corn Starch (CS, commercial) and Al 2 O 3 (ALCOA), at different temperatures. Samples were made of dense HA (100% HA), porous (70% HA - 30% CS) and with addition of 2.5%, 5% and 7.5% Al 2 O 3 porous composition. The samples were sintered at 1250°C, 1300 deg C and 135 0°C and characterized by: XRF, XRD, SEM and density by the Archimedes method. Concludes It is the possibility of obtaining samples porous HA / Al 2 O 3 using starch as porogenic agent. The temperature and concentration of Al 2 O 3 most appropriate were: 1250°C and 7.5%. (author)

The effects of sintering behavior on piezoelectric properties of porous PZT ceramics for hydrophone application

International Nuclear Information System (INIS)

Zeng Tao; Dong Xianlin; Chen Heng; Wang Yonglin

2006-01-01

Porous lead zirconate titanate (PZT) ceramics were fabricated by adding polymethyl methacrylate (PMMA) and the effects of sintering behavior on their microstructure and piezoelectric properties were investigated. The porosity of PZT ceramics decreased with an increase in the sintering temperature at a fixed PMMA addition. The dielectric constant (ε), longitudinal piezoelectric coefficient (d 33 ) and hydrostatic figures of merit (d h g h ) of 34% porous PZT ceramics increased with an increase in sintering temperature from 1050 to 1300 deg. C. When sintered at 1300 deg. C, longitudinal piezoelectric coefficient of 34% porous PZT ceramic was very close to that of 95% dense PZT ceramics, while the hydrostatic figures of merit of 34% porous PZT ceramics is about fifteen times more than that of 95% dense PZT ceramics. Compared with PZT-polymer composites, the dielectric constant of 34% porous PZT sintered at 1300 deg. C is much higher, which can be more efficient to resist the interference in receiving sensitivities caused by loading effect of the cable

Does hydroxyapatite coating have no advantage over porous coating in primary total hip arthroplasty? A meta-analysis.

Science.gov (United States)

Chen, Yun-Lin; Lin, Tiao; Liu, An; Shi, Ming-Min; Hu, Bin; Shi, Zhong-Li; Yan, Shi-Gui

2015-01-28

There are some arguments between the use of hydroxyapatite and porous coating. Some studies have shown that there is no difference between these two coatings in total hip arthroplasty (THA), while several other studies have shown that hydroxyapatite has advantages over the porous one. We have collected the studies in Pubmed, MEDLINE, EMBASE, and the Cochrane library from the earliest possible years to present, with the search strategy of "(HA OR hydroxyapatite) AND ((total hip arthroplasty) OR (total hip replacement)) AND (RCT* OR randomiz* OR control* OR compar* OR trial*)". The randomized controlled trials and comparative observation trials that evaluated the clinical and radiographic effects between hydroxyapatite coating and porous coating were included. Our main outcome measurements were Harris hip score (HHS) and survival, while the secondary outcome measurements were osteolysis, radiolucent lines, and polyethylene wear. Twelve RCTs and 9 comparative observation trials were included. Hydroxyapatite coating could improve the HHS (p hydroxyapatite coating had no advantages on survival (p = 0.32), polyethylene wear (p = 0.08), and radiolucent lines (p = 0.78). Hydroxyapatite coating has shown to have an advantage over porous coating. The HHS and survival was duration-dependent-if given the sufficient duration of follow-up, hydroxyapatite coating would be better than porous coating for the survival. The properties of hydroxyapatite and the implant design had influence on thigh pain incidence, femoral osteolysis, and polyethylene wear. Thickness of 50 to 80 μm and purity larger than 90% increased the thigh pain incidence. Anatomic design had less polyethylene wear.

Permeability model of sintered porous media: analysis and experiments

Science.gov (United States)

Flórez Mera, Juan Pablo; Chiamulera, Maria E.; Mantelli, Marcia B. H.

2017-11-01

In this paper, the permeability of porous media fabricated from copper powder sintering process was modeled and measured, aiming the use of the porosity as input parameter for the prediction of the permeability of sintering porous media. An expression relating the powder particle mean diameter with the permeability was obtained, based on an elementary porous media cell, which is physically represented by a duct formed by the arrangement of spherical particles forming a simple or orthorhombic packing. A circular duct with variable section was used to model the fluid flow within the porous media, where the concept of the hydraulic diameter was applied. Thus, the porous is modeled as a converging-diverging duct. The electrical circuit analogy was employed to determine two hydraulic resistances of the cell: based on the Navier-Stokes equation and on the Darcýs law. The hydraulic resistances are compared between themselves and an expression to determine the permeability as function of average particle diameter is obtained. The atomized copper powder was sifted to reduce the size dispersion of the particles. The porosities and permeabilities of sintered media fabricated from powders with particle mean diameters ranging from 20 to 200 microns were measured, by means of the image analysis method and using an experimental apparatus. The permeability data of a porous media, made of copper powder and saturated with distilled water, was used to compare with the permeability model. Permeability literature models, which considers that powder particles have the same diameter and include porosity data as input parameter, were compared with the present model and experimental data. This comparison showed to be quite good.

XANES analysis of calcium and sodium phosphates and silicates and hydroxyapatite-Bioglass (registered) 45S5 co-sintered bioceramics

International Nuclear Information System (INIS)

Demirkiran, Hande; Hu Yongfeng; Zuin, Lucia; Appathurai, Narayana; Aswath, Pranesh B.

2011-01-01

Bioglass (registered) 45S5 was co-sintered with hydroxyapatite at 1200 deg. C. When small amounts ( 5 (PO 4 ) 2 SiO 4 and Na 3 Ca 6 (PO 4 ) 5 in an amorphous silicate matrix respectively. These chemistries show improved bioactivity compared to hydroxyapatite and are the subject of this study. The structure of several crystalline calcium and sodium phosphates and silicates as well as the co-sintered hydroxyapatite-Bioglass (registered) 45S5 bioceramics were examined using XANES spectroscopy. The nature of the crystalline and amorphous phases were studied using silicon (Si) and phosphorus (P) K- and L 2,3 -edge and calcium (Ca) K-edge XANES. Si L 2,3 -edge spectra of sintered bioceramic compositions indicates that the primary silicates present in these compositions are sodium silicates in the amorphous state. From Si K-edge spectra, it is shown that the silicates are in a similar structural environment in all the sintered bioceramic compositions with 4-fold coordination. Using P L 2,3 -edge it is clearly shown that there is no evidence of sodium phosphate present in the sintered bioceramic compositions. In the P K-edge spectra, the post-edge shoulder peak at around 2155 eV indicates that this shoulder to be more defined for calcium phosphate compounds with decreasing solubility and increasing thermodynamic stability. This shoulder peak is more noticeable in hydroxyapatite and β-TCP indicating greater stability of the phosphate phase. The only spectra that does not show a noticeable peak is the composition with Na 3 Ca 6 (PO 4 ) 5 in a silicate matrix indicating that it is more soluble compared to the other compositions.

Biomorphous porous hydroxyapatite-ceramics from rattan (Calamus Rotang).

Science.gov (United States)

Eichenseer, Christiane; Will, Julia; Rampf, Markus; Wend, Süsen; Greil, Peter

2010-01-01

The three-dimensional, highly oriented pore channel anatomy of native rattan (Calamus rotang) was used as a template to fabricate biomorphous hydroxyapatite (Ca(5)(PO(4))(3)OH) ceramics designed for bone regeneration scaffolds. A low viscous hydroxyapatite-sol was prepared from triethyl phosphite and calcium nitrate tetrahydrate and repeatedly vacuum infiltrated into the native template. The template was subsequently pyrolysed at 800 degrees C to form a biocarbon replica of the native tissue. Heat treatment at 1,300 degrees C in air atmosphere caused oxidation of the carbon skeleton and sintering of the hydroxyapatite. SEM analysis confirmed detailed replication of rattan anatomy. Porosity of the samples measured by mercury porosimetry showed a multimodal pore size distribution in the range of 300 nm to 300 microm. Phase composition was determined by XRD and FT-IR revealing hydroxyapatite as the dominant phase with minimum fractions of CaO and Ca(3)(PO(4))(2). The biomorphous scaffolds with a total porosity of 70-80% obtained a compressive strength of 3-5 MPa in axial direction and 1-2 MPa in radial direction of the pore channel orientation. Bending strength was determined in a coaxial double ring test resulting in a maximum bending strength of approximately 2 MPa.

Reaction-sintered porous mineral-based mullite ceramic membrane supports made from recycled materials.

Science.gov (United States)

Dong, Yingchao; Zhou, Jian-Er; Lin, Bin; Wang, Yongqing; Wang, Songlin; Miao, Lifeng; Lang, Ying; Liu, Xingqin; Meng, Guangyao

2009-12-15

Bulk porous mullite supports for ceramic membranes were prepared directly using a mixture of industrial waste fly ash and bauxite by dry-pressing, followed by sintering between 1200 and 1550 degrees C. The effects of sintering temperature on the phase composition and shrinkage percent of porous mullite were studied. The XRD results indicate that secondary mullitization reaction took place above 1200 degrees C, and completed at 1450 degrees C. During sintering, the mixture samples first shrunk, then expanded abnormally between 1326 and 1477 degrees C, and finally shrunk again above 1477 degrees C. This unique volume self-expansion is ascribed to the secondary mullitization reaction between bauxite and fly ash. More especially, the micro-structural variations induced by this self-expansion sintering were verified by SEM, porosity, pore size distribution and nitrogen gas permeation flux. During self-expansion sintering, with increasing temperature, an abnormal increase in both open porosity and pore size is observed, which also results in the increase of nitrogen gas flux. The mineral-based mullite supports with increased open porosity were obtained. Furthermore, the sintered porous mullite membrane supports were characterized in terms of thermal expansion co-efficient and mechanical strength.

Improved Modeling Approaches for Constrained Sintering of Bi-Layered Porous Structures

DEFF Research Database (Denmark)

Tadesse Molla, Tesfaye; Frandsen, Henrik Lund; Esposito, Vincenzo

2012-01-01

Shape instabilities during constrained sintering experiment of bi-layer porous and dense cerium gadolinium oxide (CGO) structures have been analyzed. An analytical and a numerical model based on the continuum theory of sintering has been implemented to describe the evolution of bow and densificat...

Tunable Degradation Rate and Favorable Bioactivity of Porous Calcium Sulfate Scaffolds by Introducing Nano-Hydroxyapatite

Directory of Open Access Journals (Sweden)

Jianhua Zhou

2016-12-01

Full Text Available The bone scaffolds should possess suitable physicochemical properties and osteogenic activities. In this study, porous calcium sulfate (CaSO4 scaffolds were fabricated successfully via selected laser sintering (SLS. Nano-hydroxyapatite (nHAp, a bioactive material with a low degradation rate, was introduced into CaSO4 scaffolds to overcome the overquick absorption. The results demonstrated that nHAp could not only control the degradation rate of scaffolds by adjusting their content, but also improve the pH environment by alleviating the acidification progress during the degradation of CaSO4 scaffolds. Moreover, the improved scaffolds were covered completely with the apatite spherulites in simulated body fluid (SBF, showing their favorable bioactivity. In addition, the compression strength and fracture toughness were distinctly enhanced, which could be ascribed to large specific area of nHAp and the corresponding stress transfer.

HAp physical investigation - the effect of sintering temperature

International Nuclear Information System (INIS)

Mohd Reusmaazran Yusof; Idris Besar; Rusnah Mustaffa; Cik Rohaida Che Hak

2004-01-01

The paper presents the effect of sintering temperature on the physical properties of porous hydroxyapatite (HAp). In this study, the HAp was prepared using polymeric sponge techniques with different binder concentration. The sintering process was carried out in air for temperature ranging from 1200 degree C to 1600 degree C. Different physical properties namely density and porosity were observed at different sintering temperatures. The HAp prepared with higher PVP binder showed a slightly decreased in apparent density with increasing sintering temperature, while those HAp prepared with lower PVP showed a slightly increase in apparent density with increasing sintering temperature. The total porosity was found to be approximately constant in the whole sintering temperature range. However, closed porosity decreases with increasing sintering temperature for HAp prepared by lower binder concentration. On the other hand, the HAp prepared by higher binder concentration HAp showed increasing closed porosity with increasing sintering temperature. Other features such as the influence of sintering temperatures on grain and strut also be presented in this paper. (Author)

Gradient porous hydroxyapatite ceramics fabricated by freeze casting method

International Nuclear Information System (INIS)

Zuo Kaihui; Zhang Yuan; Jiang Dongliang; Zeng Yuping

2011-01-01

By controlling the cooling rates and the composition of slurries, the gradient porous hydroxyapatite ceramics are fabricated by the freeze casting method. According to the different cooling rate, the pores of HAP ceramics fabricated by gradient freeze casting are divided into three parts: one is lamellar pores, another is column pore and the last one is fine round pores. The laminated freeze casting is in favour of obtaining the gradient porous ceramics composed of different materials and the ceramics have unclear interfaces.

Fabrication of porous Al-Cu sintered body and its permeability property

Energy Technology Data Exchange (ETDEWEB)

Kim, Se-Hoon; Sung, Si-Young; Noh, Sang Ho; Kim, Sang Min [Korea Automotive Technology Institute, Cheonan (Korea, Republic of); Jin, Kwang Jin; Kim, Sang Min [Dongwon Technology Co., Kimhae (Korea, Republic of)

2014-01-15

In this study, porous Al-Cu sintered body was fabricated without any space-holder material and its properties, such as porosity, compressive yield strength, shore hardness, and permeability, were evaluated. Al-Cu powder mixtures were prepared by low-energy ball milling. The ball-milled powders were granulated and classified into size with <150 µm and 150-300 µm, and then they were compacted and sintered at 600 ℃ for 1 h in a vacuum and N{sub 2} atmosphere. The porosities of sintered bodies could be controlled in range of 15-48% by controlling the compaction pressure. The compressive yield strength and hardness were increased with a decreasing porosity. As a result, the mechanical properties and permeability of the optimized porous body were superior to that of commercial one.

Quantification of iodine in porous hydroxyapatite matrices for application as radioactive sources in brachytherapy

Energy Technology Data Exchange (ETDEWEB)

Lacerda, Kassio Andre; Lameiras, Fernando Soares [Centro de Desenvolvimento da Tecnologia Nuclear, (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil); Silva, Viviane Viana [Centro de Desenvolvimento da Tecnologia Nuclear, (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil); Universidade Vale do Rio Verde de Tres Coracoes, MG (Brazil)

2007-07-15

In this study, non-radioactive iodine was incorporated in two types of biodegradable hydroxyapatite-based porous matrices (HA and HACL) through impregnation process from sodium iodine aqueous solutions with varying concentrations (0.5 and 1.0 mol/L) . The results revealed that both systems presented a high capacity of incorporating iodine into their matrices. The quantity of incorporated iodine was measured through Neutron Activation Analysis (NAA). The porous ceramic matrices based on hydroxyapatite demonstrated a great potential for uses in low dose rate (LDR) brachytherapy. (author)

Effects of talc and clay addition on pressureless sintering of porous ...

Indian Academy of Sciences (India)

Porous Si3N4 ceramics were successfully synthesized using cheaper talc and clay as sintering additives by pressureless sintering technology and the microstructure and mechanical properties of the ceramics were also investigated. The results indicated that the ceramics consisted of elongated -Si3N4 and small Si2N2O ...

Improvement of the electrochromic response of a low-temperature sintered dye-modified porous electrode using low-resistivity indium tin oxide nanoparticles

International Nuclear Information System (INIS)

Watanabe, Yuichi; Suemori, Kouji; Hoshino, Satoshi

2016-01-01

An indium tin oxide (ITO) nanoparticle-based porous electrode sintered at low temperatures was investigated as a transparent electrode for electrochromic displays (ECDs). The electrochromic (EC) response of the dye-modified ITO porous electrode sintered at 150 °C, which exhibited a generally low resistivity, was markedly superior to that of a conventional dye-modified TiO 2 porous electrode sintered at the same temperature. Moreover, the EC characteristics of the dye-modified ITO porous electrode sintered at 150 °C were better than those of the high-temperature (450 °C) sintered conventional dye-modified TiO 2 porous electrode. These improvements in the EC characteristics of the dye-modified ITO porous electrode are attributed to its lower resistivity than that of the TiO 2 porous electrodes. In addition to its sufficiently low resistivity attained under the sintering conditions required for flexible ECD applications, the ITO porous film had superior visible-light transparency and dye adsorption capabilities. We conclude that the process temperature, resistivity, optical transmittance, and dye adsorption capability of the ITO porous electrode make it a promising transparent porous electrode for flexible ECD applications.

Finite Element Simulation of Diametral Strength Test of Hydroxyapatite

International Nuclear Information System (INIS)

Ozturk, Fahrettin; Toros, Serkan; Evis, Zafer

2011-01-01

In this study, the diametral strength test of sintered hydroxyapatite was simulated by the finite element software, ABAQUS/Standard. Stress distributions on diametral test sample were determined. The effect of sintering temperature on stress distribution of hydroxyapatite was studied. It was concluded that high sintering temperatures did not reduce the stress on hydroxyapatite. It had a negative effect on stress distribution of hydroxyapatite after 1300 deg. C. In addition to the porosity, other factors (sintering temperature, presence of phases and the degree of crystallinity) affect the diametral strength of the hydroxyapatite.

Sintering behavior of porous wall tile bodies during fast single-firing process

Directory of Open Access Journals (Sweden)

Sidnei José Gomes Sousa

2005-06-01

Full Text Available In ceramic wall tile processing, fast single-firing cycles have been widely used. In this investigation a fast single-firing porous wall tile mixture was prepared using raw materials from the North Fluminense region.Specimens were obtained by uniaxial pressing and sintered in air at various temperatures (1080 - 1200 °C using a fast-firing cycle (60 minutes. Evolution of the microstructure was followed by XRD and SEM. The results revealed that the main phases formed during the sintering step are anorthite, gehlenite and hematite. It appears that the sintering process is characterized by the presence of a small amount of a liquid phase below 1140 °C. As a result, the microstructure of the ceramic bodies showed a network of small dense zones interconnected with a porous phase. In addition, the strength of the material below 1140 °C appeared to be related to the type and quantity of crystalline phases in the sintered bodies.

A study on improving mechanical properties of porous HA tissue engineering scaffolds by hot isostatic pressing

International Nuclear Information System (INIS)

Zhao Jing; Xiao Suguang; Lu Xiong; Wang Jianxin; Weng Jie

2006-01-01

Various interconnected porous hydroxyapatite (HA) ceramic scaffolds are universally used to induct the tissue growth for bone repair and replacement, and serve to support the adhesion, transfer, proliferation and differentiation of cells. Impregnation of polyurethane sponges with a ceramic slurry is adopted to produce highly porous HA ceramic scaffolds with a 3D interconnected structure. However, high porosity always accompanies a decrease in the strength of the HA ceramic scaffolds. Therefore, it is significant to improve the strength of the HA ceramic scaffolds with highly interconnected porosity so that they are more suitable in clinical applications. In this work, highly porous HA ceramic scaffolds are first produced by the polymer impregnation approach, and subsequently further sintered by hot isostatic pressing (HIP). The phase composition, macro- and micro-porous structure, sintering and mechanical properties of the porous HA scaffolds are investigated by x-ray diffraction (XRD), scanning electron microscopy (SEM), nanoindentation analysis and compressive test. The experimental results show that the nanohardness and compressive strength of HIP-sintered porous HA ceramics are higher than those of commonly sintered HA scaffolds. The HIP technique can effectively improve the sintering property and densification of porous HA ceramic scaffolds, so inducing an increase in the compression strength

Synthesis of calcium phosphates and porous hydroxyapatite beads prepared by emulsion method

Energy Technology Data Exchange (ETDEWEB)

Chen, B.-H. [Faculty of Biotechnology, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 807, Taiwan (China); Chen, K.-I [Department of Electronics Engineering and Computer Science, Tung-Fang Institute of Technology, 100 Dungfang Road, Hunei, Kaohsiung, Taiwan (China); Ho, M.-L. [Department of Physiology, Kaohsiung Medical University, Kaohsiung 807, Taiwan (China); Chen, H.-N. [Faculty of Medicinal and Applied Chemistry, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 807, Taiwan (China); Chen, W.-C. [Faculty of Dentistry, Kaohsiung Medical University, Kaohsiung 807, Taiwan (China); Wang, C.-K. [Faculty of Medicinal and Applied Chemistry, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 807, Taiwan (China)], E-mail: ckwang@kmu.edu.tw

2009-01-15

Raw calcium phosphates were synthesized via a chemical reaction between 0.5 M orthophosphoric acid and 0.5 M calcium hydroxide. Hydroxyapatite (HAp), {beta}-tricalcium phosphate ({beta}-TCP) or biphase calcium phosphate (BCP) comprising HAp and {beta}-TCP were obtained by changing pH value, Ca/P ratio, and the addition of glycerol. The as-synthesized and heat-treated powders were analyzed by X-ray diffraction (XRD) and Fourier transformation infrared spectrometry (FTIR). Thermal stability of the pure apatite phase was obtained to be 1300 deg. C, while synthesis was done at the pH value of 10.0 with a Ca/P ratio of 2.0 and a temperature of 37 deg. C. Besides, the {beta}-TCP phase (with higher purity) was achieved at 800 deg. C, whose synthesis was done at pH 6.4 with a Ca/P ratio of 1.5 and a temperature of 37 deg. C. Therefore, the biphase bioceramics comprising of HAp and {beta}-TCP could be obtained, since it was manipulated suitably. The HAp raw material was subjected to a simple emulsion method for the preparation of porous beads. They should have the advantage of exhibiting higher adsorptive ability and osteoconductivity in comparison with the sintered dense apatite. Additionally, the porous beads of apatite were demonstrated to be non-toxic to cells, and should be suitable for the use as a scaffold of cultured bone and bone graft material, as well as for drug delivery systems.

Porous hydroxyapatite and biphasic calcium phosphate ceramics promote ectopic osteoblast differentiation from mesenchymal stem cells

Energy Technology Data Exchange (ETDEWEB)

Zhang Lingli; Fan Hongsong; Zhang Xingdong [National Engineering Research Center for Biomaterials, Sichuan University, Chengdu, Sichuan 610064 (China); Hanagata, Nobutaka; Ikoma, Toshiyuki [Biomaterials Center, National Institute for Materials Science, Tsukuba, Ibaraki 305-0047 (Japan); Maeda, Megumi; Minowa, Takashi, E-mail: HANAGATA.Nobutaka@nims.go.j [Nanotechnology Innovation Center, National Institute for Materials Science, Tsukuba, Ibaraki 305-0047 (Japan)

2009-04-15

Because calcium phosphate (Ca-P) ceramics have been used as bone substitutes, it is necessary to investigate what effects the ceramics have on osteoblast maturation. We prepared three types of Ca-P ceramics with different Ca-P ratios, i.e. hydroxyapatite (HA), beta-tricalcium phosphate ({beta}-TCP), and biphasic calcium phosphate (BCP) ceramics with dense-smooth and porous structures. Comprehensive gene expression microarray analysis of mouse osteoblast-like cells cultured on these ceramics revealed that porous Ca-P ceramics considerably affected the gene expression profiles, having a higher potential for osteoblast maturation. In the in vivo study that followed, porous Ca-P ceramics were implanted into rat skeletal muscle. Sixteen weeks after the implantation, more alkaline-phosphatase-positive cells were observed in the pores of hydroxyapatite and BCP, and the expression of the osteocalcin gene (an osteoblast-specific marker) in tissue grown in pores was also higher in hydroxyapatite and BCP than in {beta}-TCP. In the pores of any Ca-P ceramics, 16 weeks after the implantation, we detected the expressions of marker genes of the early differentiation stage of chondrocytes and the complete differentiation stage of adipocytes, which originate from mesenchymal stem cells, as well as osteoblasts. These marker gene expressions were not observed in the muscle tissue surrounding the implanted Ca-P ceramics. These observations indicate that porous hydroxyapatite and BCP had a greater potential for promoting the differentiation of mesenchymal stem cells into osteoblasts than {beta}-TCP.

CAD-CAM-generated hydroxyapatite scaffold to replace the mandibular condyle in sheep: preliminary results.

Science.gov (United States)

Ciocca, Leonardo; Donati, Davide; Fantini, Massimiliano; Landi, Elena; Piattelli, Adriano; Iezzi, Giovanna; Tampieri, Anna; Spadari, Alessandro; Romagnoli, Noemi; Scotti, Roberto

2013-08-01

In this study, rapid CAD-CAM prototyping of pure hydroxyapatite to replace temporomandibular joint condyles was tested in sheep. Three adult animals were implanted with CAD-CAM-designed porous hydroxyapatite scaffolds as condyle substitutes. The desired scaffold shape was achieved by subtractive automated milling machining (block reduction). Custom-made surgical guides were created by direct metal laser sintering and were used to export the virtual planning of the bone cut lines into the surgical environment. Using the same technique, fixation plates were created and applied to the scaffold pre-operatively to firmly secure the condyles to the bone and to assure primary stability of the hydroxyapatite scaffolds during masticatory function. Four months post-surgery, the sheep were sacrificed. The hydroxyapatite scaffolds were explanted, and histological specimens were prepared. Different histological tissues penetrating the scaffold macropores, the sequence of bone remodeling, new apposition of bone and/or cartilage as a consequence of the different functional anatomic role, and osseointegration at the interface between the scaffold and bone were documented. This animal model was found to be appropriate for testing CAD-CAM customization and the biomechanical properties of porous, pure hydroxyapatite scaffolds used as joint prostheses.

In vitro electromagnetically stimulated SAOS-2 osteoblasts inside porous hydroxyapatite

Science.gov (United States)

Fassina, Lorenzo; Saino, Enrica; Sbarra, Maria Sonia; Visai, Livia; De Angelis, Maria Gabriella Cusella; Magenes, Giovanni; Benazzo, Francesco

2009-01-01

One of the key challenges in reconstructive bone surgery is to provide living constructs that possess the ability to integrate in the surrounding tissue. Bone graft substitutes, such as autografts, allografts, xenografts, and biomaterials have been widely used to heal critical-size long bone defects due to trauma, tumor resection, congenital deformity, and tissue degeneration. In particular, porous hydroxyapatite is widely used in reconstructive bone surgery owing to its biocompatibility. In addition, the in vitro modification of hydroxyapatite with osteogenic signals enhances the tissue regeneration in vivo, suggesting that the biomaterial modification could play an important role in tissue engineering. In this study we have followed a biomimetic strategy where electromagnetically stimulated SAOS-2 human osteoblasts proliferated and built their extracellular matrix inside a porous hydroxyapatite scaffold. The electromagnetic stimulus had the following parameters: intensity of the magnetic field equal to 2 mT, amplitude of the induced electric tension equal to 5 mV, frequency of 75 Hz, and pulse duration of 1.3 ms. In comparison with control conditions, the electromagnetic stimulus increased the cell proliferation and the surface coating with bone proteins (decorin, osteocalcin, osteopontin, type-I collagen, and type-III collagen). The physical stimulus aimed at obtaining a better modification of the biomaterial internal surface in terms of cell colonization and coating with bone matrix. PMID:19827111

Influence of the starch content and sintering temperature on the processing of porous zirconia substrates

International Nuclear Information System (INIS)

Albano, Maria P; Garrido, Liliana B

2008-01-01

Porous ceramics are used as electrodes in fuel cells, separators in batteries, filters, etc. Thin porous substrates of zirconium stabilized with yttrium oxide (ZSY) are used as anodes in solid oxide fuel cells. One way to obtain a porous band is to mix starch particles during the preparation stage of the ZSY suspension. The starch burns during the removal of the binder and leaves stable pores that are not eliminated in the subsequent sintering stage. This work used the band pouring process to produce porous bands of ZSY with porosities of 29% to 53% using starch as a transitory additive. Concentrated aqueous suspensions of ZSY were prepared with different contents of starch and of an acrylic latex binder. The influence of the fraction of starch volume and of the temperature on the sintering behavior and on the final micro structure of the bands was studied. The total porosity of the bands was higher than the fractions in volume of added starch, due to the presence of closed porosity in the matrix. The deviations compared to the porosity predicted based on the fractions in the volume of starch, were greater as the starch content increased. The percentage of open porosity in the sintered bands depended on the fraction in the volume of added starch and on the sintering temperature. When the fraction in volume of starch increased from 17.6% to 37.8% a gradual increase occurred in the opening of the porous structure. The contraction of the bands during sintering at a given temperature correlated with the density of the packing of ZSY (au)

Hydroxyapatite-based porous aggregates: physico-chemical nature, structure, texture and architecture.

Science.gov (United States)

Fabbri, M; Celotti, G C; Ravaglioli, A

1995-02-01

At the request of medical teams from the maxillofacial sector, a highly porous ceramic support based on hydroxyapatite of around 70-80% porosity was produced with a pore size distribution similar to bone texture ( 150 microns, approximately 86 vol%). The ceramic substrates were conceived not only as a fillers for bone cavities, but also for use as drug dispensers and as supports to host cells to produce particular therapeutic agents. A method is suggested to obtain a substrate of high porosity, exploiting the impregnation of spongy substrate with hydroxyapatite ceramic particles. X-ray and scanning electron microscopy analyses were carried out to evaluate the nature of the new ceramic support in comparison with the most common commercial product; pore size distribution and porosity were controlled to known hydroxyapatite ceramic architecture for the different possible uses.

Effect of sintering conditions on the microstructural and mechanical characteristics of porous magnesium materials prepared by powder metallurgy.

Science.gov (United States)

Čapek, Jaroslav; Vojtěch, Dalibor

2014-02-01

There has recently been an increased demand for porous magnesium materials in many applications, especially in the medical field. Powder metallurgy appears to be a promising approach for the preparation of such materials. Many works have dealt with the preparation of porous magnesium; however, the effect of sintering conditions on material properties has rarely been investigated. In this work, we investigated porous magnesium samples that were prepared by powder metallurgy using ammonium bicarbonate spacer particles. The effects of the purity of the argon atmosphere and sintering time on the microstructure (SEM, EDX and XRD) and mechanical behaviour (universal loading machine and Vickers hardness tester) of porous magnesium were studied. The porosities of the prepared samples ranged from 24 to 29 vol.% depending on the sintering conditions. The purity of atmosphere played a significant role when the sintering time exceeded 6h. Under a gettered argon atmosphere, a prolonged sintering time enhanced diffusion connections between magnesium particles and improved the mechanical properties of the samples, whereas under a technical argon atmosphere, oxidation at the particle surfaces caused deterioration in the mechanical properties of the samples. These results suggest that a refined atmosphere is required to improve the mechanical properties of porous magnesium. © 2013.

Porous SiC ceramics fabricated by quick freeze casting and solid state sintering

Directory of Open Access Journals (Sweden)

Feng Wang

2017-06-01

Full Text Available Porous SiC ceramics with uniform microstructure were fabricated by quick freezing in liquid nitrogen and solid state sintering. Poly (vinyl alcohol (PVA was added as binder and pore morphology controller in this work. The microstructure and mechanical properties of porous SiC ceramics could be controlled by the composition of the aqueous slurries. Both solid content of the slurries and PVA content impacted on the pore structures and mechanical properties of the porous SiC ceramics. The solid content of slurries and PVA content varied from 60 to 67.5 wt% and 2–6 wt%, respectively. Besides, the grain morphology of ceramics was also tailored by changing the sintering temperature from 2050 to 2150 °C. Porous SiC ceramics with an average porosity of 42.72%, flexural strength of 59.28 MPa were obtained at 2150 °C from 67.5 wt% slurries with 2 wt% PVA.

Calcination of Rod-like Hydroxyapatite Nanocrystals with an Anti-sintering Agent Surrounding the Crystals

International Nuclear Information System (INIS)

Okada, M.; Furuzono, T.

2007-01-01

Sintering-free nanocrystals of calcined hydroxyapatite (HAp) having a rod-like morphology were fabricated by calcination at 800 deg. C for 1 h with an anti-sintering agent surrounding original HAp particles and the agent was subsequently removed after calcination. The original HAp particles having a rod-like morphology with a size ranging from 30 to 80 nm (short axis) and 300 to 500 nm (long axis) were prepared by wet chemical process, and poly(acrylic acid, calcium salt) (PAA-Ca) was used as the anti-sintering agent. In the case of calcination without additives, the mean size of HAp crystals dispersed in an ethanol medium increased by about 4 times and the specific surface area of the crystals exhibited a 25% decrease compared to those of the original HAp particles because of calcination-induced sintering among the crystals. On the other hand, the HAp crystals calcined with the anti-sintering agent, PAA-Ca, could be dispersed in an ethanol medium at the same size as the original particles, and they preserved the specific surface area after calcination. These results indicate that PAA-Ca and/or its thermally decomposed product, CaO, surrounded the HAp particles and protected them against calcination-induced sintering during calcination. The HAp crystals calcined with PAA-Ca showed high crystallinity, and no other calcium phosphate phases could be detected after washing with water

Characterisation and sintering of nanophase hydroxyapatite synthesised by a species of Serratia

Science.gov (United States)

LSammons, R.; Thackray, A. C.; Medina Ledo, H.; Marquis, P. M.; Jones, I. P.; Yong, P.; Macaskie, L. E.

2007-12-01

The bacterium Serratia sp. NCIMB40259, which grows as a biofilm on polymeric, glass and metal substrates, produces extracellular crystals of hydroxyapatite (HA) by enzymatic cleavage of β-glycerophosphate in the presence of calcium chloride. Following growth on polyurethane foam, biomineralisation and subsequent sintering, an HA scaffold is formed whose three-dimensional architecture replicates that of the foam and the biofilm. Serratia HA was characterised using X-ray diffraction (XRD), Fourier Transform Infra-Red Spectroscopy (FTIR), energy dispersive X-ray analysis (EDX) scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron diffraction (ED). The nascent, unsintered material consisted mainly of calcium-deficient HA (CDHA) with a Ca/P ratio of 1.61+/- 0.06 and crystal size (TEM) of 50 +/- 10nm length. ED of unsintered crystals and crystals sintered at 600° C showed resolvable ring (unsintered) or dot (600° C) patterns ascribed to (0002), (1122) and (0006) planes of crystalline HA. Material sintered at 1200° C consisted of needle-like crystals of length range 54-111nm (XRD) with lattice parameters of a = 9.441 Å and c = 6.875 Å, consistent with HA.

Characterisation and sintering of nanophase hydroxyapatite synthesised by a species of Serratia

International Nuclear Information System (INIS)

LSammons, R; Thackray, A C; Ledo, H Medina; Marquis, P M; Jones, I P; Yong, P; Macaskie, L E

2007-01-01

The bacterium Serratia sp. NCIMB40259, which grows as a biofilm on polymeric, glass and metal substrates, produces extracellular crystals of hydroxyapatite (HA) by enzymatic cleavage of β-glycerophosphate in the presence of calcium chloride. Following growth on polyurethane foam, biomineralisation and subsequent sintering, an HA scaffold is formed whose three-dimensional architecture replicates that of the foam and the biofilm. Serratia HA was characterised using X-ray diffraction (XRD), Fourier Transform Infra-Red Spectroscopy (FTIR), energy dispersive X-ray analysis (EDX) scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron diffraction (ED). The nascent, unsintered material consisted mainly of calcium-deficient HA (CDHA) with a Ca/P ratio of 1.61+/- 0.06 and crystal size (TEM) of 50 +/- 10nm length. ED of unsintered crystals and crystals sintered at 600 0 C showed resolvable ring (unsintered) or dot (600 0 C) patterns ascribed to (0002), (1122) and (0006) planes of crystalline HA. Material sintered at 1200 0 C consisted of needle-like crystals of length range 54-111nm (XRD) with lattice parameters of a = 9.441 A and c = 6.875 A, consistent with HA

Characterisation and sintering of nanophase hydroxyapatite synthesised by a species of Serratia

Energy Technology Data Exchange (ETDEWEB)

LSammons, R [University of Birmingham School of Dentistry, St Chad' s Queensway, Birmingham, B4 6NN (United Kingdom); Thackray, A C [University of Birmingham School of Dentistry, St Chad' s Queensway, Birmingham, B4 6NN (United Kingdom); Ledo, H Medina [University of Birmingham School of Engineering, Metallurgy and Materials, Birmingham B15 2TT (United Kingdom); Marquis, P M [University of Birmingham School of Dentistry, St Chad' s Queensway, Birmingham, B4 6NN (United Kingdom); Jones, I P [University of Birmingham School of Engineering, Metallurgy and Materials, Birmingham B15 2TT (United Kingdom); Yong, P [University of Birmingham, School of Biosciences, Birmingham B15 2TT (United Kingdom); Macaskie, L E [University of Birmingham, School of Biosciences, Birmingham B15 2TT (United Kingdom)

2007-12-15

The bacterium Serratia sp. NCIMB40259, which grows as a biofilm on polymeric, glass and metal substrates, produces extracellular crystals of hydroxyapatite (HA) by enzymatic cleavage of {beta}-glycerophosphate in the presence of calcium chloride. Following growth on polyurethane foam, biomineralisation and subsequent sintering, an HA scaffold is formed whose three-dimensional architecture replicates that of the foam and the biofilm. Serratia HA was characterised using X-ray diffraction (XRD), Fourier Transform Infra-Red Spectroscopy (FTIR), energy dispersive X-ray analysis (EDX) scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron diffraction (ED). The nascent, unsintered material consisted mainly of calcium-deficient HA (CDHA) with a Ca/P ratio of 1.61+/- 0.06 and crystal size (TEM) of 50 +/- 10nm length. ED of unsintered crystals and crystals sintered at 600{sup 0} C showed resolvable ring (unsintered) or dot (600{sup 0} C) patterns ascribed to (0002), (1122) and (0006) planes of crystalline HA. Material sintered at 1200{sup 0} C consisted of needle-like crystals of length range 54-111nm (XRD) with lattice parameters of a = 9.441 A and c = 6.875 A, consistent with HA.

Sintering process of Eu doped luminescent glass prepared from porous glass

International Nuclear Information System (INIS)

Akai, T; Murakami, M; Yamashita, M; Okajima, T; Umesaki, N

2011-01-01

Eu doped high silica glass prepared by sintering porous glass exhibits blue luminescence with high quantum efficiency. In this work, we studied effects of sintering temperature on valance state of europium ion. To investigate a change of valance state of Eu, X-ray absorption near edge structure (XANES) spectroscopy measurements were carried out. Intensity of blue emission at around 430nm drastically increases when the sintering temperature is above 1000 deg. C. From XANES spectra, it is found that almost all the Eu exist as Eu 3+ in a samples sintered below 900 deg. C, while more than 70% of Eu exist as Eu 2+ in the sample sintered at 1050 deg. C and 1100 deg. C. The drastic change of oxidation state of europium ion between 900 and 1050 deg. C is discussed in relation to the structural change probed by infrared (IR) spectroscopy.

Preparation of micro-porous bioceramic containing silicon-substituted hydroxyapatite and beta-tricalcium phosphate.

Science.gov (United States)

Fuh, Lih-Jyh; Huang, Ya-Jing; Chen, Wen-Cheng; Lin, Dan-Jae

2017-06-01

Dimensional instability caused by sintering shrinkage is an inevitable drawback for conventional processing of hydroxyapatite (HA). A new preparation method for biphasic calcium phosphates was developed to increase micro pores and biodegradation without significant dimensional change. Powder pressed HA discs, under 100MPa, were immersed in a colloidal mixture of tetraethoxysilane (TEOS) and ammonium hydroxide for 10min, followed by drying, and then were sintered at 900°C, 1050°C, and 1200°C, respectively. Comparing with pure HA discs, the newly prepared product sintered up to 1200°C contained silicon substituted HA, beta-tricalcium phosphate, and calcium silicate with better micro-porosity, high specific surface area, less sintering shrinkage and the strength maintained. The cytocompatibility test demonstrated a better viability for D1 mice stem cells cultured on TEOS treated HA for 14days compared to the pure HA. This simple TEOS sol-gel pretreatment has the potential to be applied to any existing manufacturing process of HA scaffold for better control of sintering shrinkage, create micropores, and increase biodegradation. Copyright © 2017 Elsevier B.V. All rights reserved.

Modeling of the effective thermal conductivity of sintered porous pastes

NARCIS (Netherlands)

Ordonez-Miranda, J.; Hermens, M.; Nikitin, I.; Kouznetsova, V.G.; Volz, S.

2014-01-01

The thermal conductivity of sintered porous pastes of metals is modelled, based on an analytical and a numerical approach. The first method arises from the differential effective medium theory and considers the air voids as ellipsoidal pores of different sizes, while second one is based on the

The Production of Porous Hydroxyapatite Scaffolds with Graded Porosity by Sequential Freeze-Casting.

Science.gov (United States)

Lee, Hyun; Jang, Tae-Sik; Song, Juha; Kim, Hyoun-Ee; Jung, Hyun-Do

2017-03-31

Porous hydroxyapatite (HA) scaffolds with porosity-graded structures were fabricated by sequential freeze-casting. The pore structures, compressive strengths, and biocompatibilities of the fabricated porous HA scaffolds were evaluated. The porosities of the inner and outer layers of the graded HA scaffolds were controlled by adjusting the initial HA contents of the casting slurries. The interface between the dense and porous parts was compact and tightly adherent. The porosity and compressive strengths of the scaffold were controlled by the relative thicknesses of the dense/porous parts. In addition, the porous HA scaffolds showed good biocompatibility in terms of preosteoblast cell attachment and proliferation. The results suggest that porous HA scaffolds with load-bearing parts have potential as bone grafts in hard-tissue engineering.

Characterization of the porous structures of the green body and sintered biomedical titanium scaffolds with micro-computed tomography

Energy Technology Data Exchange (ETDEWEB)

Arifvianto, B., E-mail: b.arifvianto@tudelft.nl; Leeflang, M.A.; Zhou, J.

2016-11-15

The present research was aimed at gaining an understanding of the porous structure changes from the green body through water leaching and sintering to titanium scaffolds. Micro-computed tomography (micro-CT) was performed to generate 3D models of titanium scaffold preforms containing carbamide space-holding particles and sintered scaffolds containing macro- and micro-pores. The porosity values and structural parameters were determined by means of image analysis. The result showed that the porosity values, macro-pore sizes, connectivity densities and specific surface areas of the titanium scaffolds sintered at 1200 °C for 3 h did not significantly deviate from those of the green structures with various volume fractions of the space holder. Titanium scaffolds with a maximum specific surface area could be produced with an addition of 60–65 vol% carbamide particles to the matrix powder. The connectivity of pores inside the scaffold increased with rising volume fraction of the space holder. The shrinkage of the scaffolds prepared with > 50 vol% carbamide space holder, occurring during sintering, was caused by the reductions of macro-pore sizes and micro-pore sizes as well as the thickness of struts. In conclusion, the final porous structural characteristics of titanium scaffolds could be estimated from those of the green body. - Highlights: •Porous structures of green body and sintered titanium scaffolds was studied. •Porous structures of both samples were quantitatively characterized with micro-CT. •Porous structures of scaffolds could be controlled from the green body. •Shrinkage mechanisms of titanium scaffolds during sintering was established.

Development of membrane filters with nanostructured porous layer by coating of metal nanoparticles sintered onto a micro-filter

International Nuclear Information System (INIS)

Park, Seok Joo; Park, Young Ok; Lee, Dong Geun; Ryu, Jeong In

2008-01-01

The membrane filter adhered with nanostructured porous layer was made by heat treatment after deposition of nanoparticle-agglomerates sintered in aerosol phase onto a conventional micron-fibrous metal filter as a substrate filter. The Sintered-Nanoparticle-Agglomerates-coated NanoStructured porous layer Membrane Filter (SNA-NSMF), whose the filtration performance was improved compared with the conventional metal membrane filters, was developed by adhesion of nanoparticle-agglomerates of dendrite structure sintered onto the micron-fibrous metal filter. The size of nanoparticle-agglomerates of dendrite structure decreased with increasing the sintering temperature because nanoparticle-agglomerates shrank. When shrinking nanoparticle-agglomerates were deposited and treated with heat onto the conventional micron-fibrous metal filter, pore size of nanostructured porous layer decreased. Therefore, pressure drops of SNA-NSMFs increased from 0.3 to 0.516 KPa and filtration efficiencies remarkably increased from 95.612 to 99.9993%

Electrochemical corrosion and bioactivity of Ti-Nb-Sn-hydroxyapatite composites fabricated by pulse current activated sintering.

Science.gov (United States)

Xiaopeng, Wang; Fantao, Kong; Biqing, Han; Yuyong, Chen

2017-11-01

Ti-Nb-Sn-hydroxyapatite (HA) composites were prepared by mechanical alloying for different times (unmilled, 4, 8 and 12h), followed by pulse current activated sintering. The effects of the milling time on the electrochemical corrosion resistance and bioactivity of the sintered Ti-35Nb-2.5Sn-15HA composites were investigated. Potentiodynamic polarization test results indicated that the sintered Ti-35Nb-2.5Sn-15HA composites exhibited higher corrosion resistance with increasing milling time. The corrosion potential and current of the Ti-35Nb-2.5Sn-15HA composite sintered by 12h milled powders were - 0.261V and 0.18μA/cm 2 , respectively, and this sintered composite showed a stable and wide passivation region. The hemolysis rate of the sintered Ti-35Nb-2.5Sn-15HA composites reduced with increasing milling time and the lowest hemolytic rate of the composites was 0.87%. In addition, the in vitro cell culture results indicated that the composite sintered by 12h milled powders had good biocompatibility. These results indicate the significant potential of Ti-35Nb-2.5Sn/xHA composites for biomedical implant applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

Synthesis and Characterization of Hydroxyapatite Powder by Wet Precipitation Method

Science.gov (United States)

Cahyaningrum, S. E.; Herdyastuty, N.; Devina, B.; Supangat, D.

2018-01-01

Hydroxyapatite is main inorganic component of the bone with formula Ca10(PO4)6(OH)2. Hydroxyapatite can be used as substituted bone biomaterial because biocompatible, non toxic, and osteoconductive. In this study, hydroxyapatite is synthesized using wet precipitation method from egg shell. The product was sintered at different temperatures of 800°C to 1000°C to improve its crystallinity. The hydroxyapatite was characterized by X-ray analysis, Scanning Electron Microscopy (SEM) and Fourier Transform Infrared Spectroscopy (FTIR) to reveal its phase content, morphology and types of bond present within it. The analytical results showed hydroxyapatite had range in crystallinity from 85.527 to 98.753%. The analytical functional groups showed that presence of functional groups such as OH, (PO4)3 2-, and CO3 2- that indicated as hydroxyapatite. The result of characterization SEM indicated that hydroxyapatite without sintering and HAp sintering at 800 °C were irregular shape without pore. The best hydroxyapatite with temperature sintering at 900 °C showed oval shaped with pores without agglomerated.

Hydroxyapatite nanorod-assembled porous hollow polyhedra as drug/protein carriers.

Science.gov (United States)

Yu, Ya-Dong; Zhu, Ying-Jie; Qi, Chao; Jiang, Ying-Ying; Li, Heng; Wu, Jin

2017-06-15

Hydroxyapatite (HAP) with a porous hollow structure is an ideal biomaterial owing to its excellent biocompatibility and unique architecture. In this study, HAP nanorod-assembled porous hollow polyhedra, consisting of nanorod building blocks, have been successfully prepared at room temperature or under hydrothermal circumstances using a self-sacrificing Ca(OH) 2 template strategy. The hydrothermal treatment (at 180°C for 1h) can promote the HAP nanorods to be arranged with their axial direction normal to the polyhedron surface. The HAP nanorod-assembled porous hollow polyhedra have been explored for the potential application in drug/protein delivery, using ibuprofen (IBU) as a model drug and hemoglobin (Hb) as a model protein. The experimental results indicate that the HAP nanorod-assembled porous hollow polyhedra have a relatively high drug loading capacity and protein adsorption ability, and sustained drug and protein release. The HAP nanorod-assembled porous hollow polyhedra have promising applications in various biomedical fields such as the drug and protein delivery. Copyright © 2017 Elsevier Inc. All rights reserved.

Porous poly (lactic-co-glycolide) microsphere sintered scaffolds for tissue repair applications

International Nuclear Information System (INIS)

Wang Yingjun; Shi Xuetao; Ren Li; Wang Chunming; Wang Dongan

2009-01-01

In this paper, a new route to preparing porous poly (lactic-co-glycolide) (PLGA) scaffolds for bone tissue repair applications was developed. Novel porous PLGA scaffolds were fabricated via microsphere sintered technique and gas forming technique. Ammonium bicarbonate was used to regulate porosity of these porous scaffolds. Porosity of the scaffolds, and cell attachment, viability and proliferation on the scaffolds were evaluated. The results indicated that PLGA porous scaffolds were with the porosity from around 30% to 95% by regulating ammonium bicarbonate content from 0 to 10%. We also found that PLGA porous microsphere scaffolds benefited cell attachment and viability. Taken together, the achieved porous scaffolds have controlled porosity and also support mesenchymal stem cell proliferation, which could serve as potential scaffolds for bone repair applications.

Preparation of Porous Stainless Steel Hollow-Fibers through Multi-Modal Particle Size Sintering towards Pore Engineering

Directory of Open Access Journals (Sweden)

Francois-Marie Allioux

2017-08-01

Full Text Available The sintering of metal powders is an efficient and versatile technique to fabricate porous metal elements such as filters, diffusers, and membranes. Neck formation between particles is, however, critical to tune the porosity and optimize mass transfer in order to minimize the densification process. In this work, macro-porous stainless steel (SS hollow-fibers (HFs were fabricated by the extrusion and sintering of a dope comprised, for the first time, of a bimodal mixture of SS powders. The SS particles of different sizes and shapes were mixed to increase the neck formation between the particles and control the densification process of the structure during sintering. The sintered HFs from particles of two different sizes were shown to be more mechanically stable at lower sintering temperature due to the increased neck area of the small particles sintered to the large ones. In addition, the sintered HFs made from particles of 10 and 44 μm showed a smaller average pore size (<1 μm as compared to the micron-size pores of sintered HFs made from particles of 10 μm only and those of 10 and 20 μm. The novel HFs could be used in a range of applications, from filtration modules to electrochemical membrane reactors.

Bioactivity and mineralization of hydroxyapatite with bioglass as sintering aid and bioceramics with Na3Ca6(PO4)5 and Ca5(PO4)2SiO4 in a silicate matrix

International Nuclear Information System (INIS)

Demirkiran, Hande; Mohandas, Arunesh; Dohi, Motokazi; Fuentes, Alonso; Nguyen, Kytai; Aswath, Pranesh

2010-01-01

Hydroxyapatite and Bioglass-45S5 were sintered together creating new ceramic compositions that yielded increased apatite deposition and osteoblast differentiation and proliferation in vitro compared to hydroxyapatite. The sintered products characterized by X-ray diffraction, revealed hydroxyapatite as the main phase when small quantities (1, 2.5 and 5 wt.%) of bioglass was added. Bioglass behaved as a sintering aid with β-TCP (Ca 3 (PO 4 ) 2 ) being the minor phase. The amount of β-TCP increased with the amount of bioglass added. In compositions with larger additions of bioglass (10 and 25 wt.%), new phases with compositions of calcium phosphate silicate (Ca 5 (PO 4 ) 2 SiO 4 ) and sodium calcium phosphate (Na 3 Ca 6 (PO 4 ) 5 ) were formed respectively within amorphous silicate matrices. In vitro cell culture studies of the ceramic compositions were examined using bone marrow stromal cell (BMSC). Cell proliferation and differentiation of bone marrow stromal cells into osteoblasts were determined by Pico Green DNA assays and alkaline phosphatase (ALP) activity, respectively. All hydroxyapatite-bioglass co-sintered ceramics exhibited larger cell proliferation compared to pure hydroxyapatite samples. After 6 days in cell culture, the ceramic with Ca 5 (PO 4 ) 3 SiO 4 in a silicate matrix formed by reacting hydroxyapatite with 10 wt.% bioglass exhibited the maximum proliferation of the BMSC's. The ALP activity was found to be largest in the ceramic with Na 3 Ca 6 (PO 4 ) 5 embedded in a silicate matrix synthesized by reacting hydroxyapatite with 25 wt.% bioglass.

Determination of the Darcy permeability of porous media including sintered metal plugs

Science.gov (United States)

Frederking, T. H. K.; Hepler, W. A.; Yuan, S. W. K.; Feng, W. F.

1986-01-01

Sintered-metal porous plugs with a normal size of the order of 1-10 microns are used to evaluate the Darcy permeability of laminar flow at very small velocities in laminar fluids. Porous media experiment results and data adduced from the literature are noted to support the Darcy law analog for normal fluid convection in the laminar regime. Low temperature results suggest the importance of collecting room temperature data prior to runs at liquid He(4) temperatures. The characteristic length diagram gives a useful picture of the tolerance range encountered with a particular class of porous media.

Biocompatibility of hydroxyapatite scaffolds processed by lithography-based additive manufacturing.

Science.gov (United States)

Tesavibul, Passakorn; Chantaweroad, Surapol; Laohaprapanon, Apinya; Channasanon, Somruethai; Uppanan, Paweena; Tanodekaew, Siriporn; Chalermkarnnon, Prasert; Sitthiseripratip, Kriskrai

2015-01-01

The fabrication of hydroxyapatite scaffolds for bone tissue engineering applications by using lithography-based additive manufacturing techniques has been introduced due to the abilities to control porous structures with suitable resolutions. In this research, the use of hydroxyapatite cellular structures, which are processed by lithography-based additive manufacturing machine, as a bone tissue engineering scaffold was investigated. The utilization of digital light processing system for additive manufacturing machine in laboratory scale was performed in order to fabricate the hydroxyapatite scaffold, of which biocompatibilities were eventually evaluated by direct contact and cell-culturing tests. In addition, the density and compressive strength of the scaffolds were also characterized. The results show that the hydroxyapatite scaffold at 77% of porosity with 91% of theoretical density and 0.36 MPa of the compressive strength are able to be processed. In comparison with a conventionally sintered hydroxyapatite, the scaffold did not present any cytotoxic signs while the viability of cells at 95.1% was reported. After 14 days of cell-culturing tests, the scaffold was able to be attached by pre-osteoblasts (MC3T3-E1) leading to cell proliferation and differentiation. The hydroxyapatite scaffold for bone tissue engineering was able to be processed by the lithography-based additive manufacturing machine while the biocompatibilities were also confirmed.

Quantification of iodine in porous hydroxyapatite matrices for application as radioactive sources in brachytherapy

OpenAIRE

Lacerda, Kássio André; Lameiras, Fernando Soares; Silva, Viviane Viana

2007-01-01

In this study, non-radioactive iodine was incorporated in two types of biodegradable hydroxyapatite-based porous matrices (HA and HACL) through impregnation process from sodium iodine aqueous solutions with varying concentrations (0.5 and 1.0 mol/L) . The results revealed that both systems presented a high capacity of incorporating iodine into their matrices. The quantity of incorporated iodine was measured through Neutron Activation Analysis (NAA). The porous ceramic matrices based on hydrox...

[Construction of porous hydroxyapatite (HA) block loaded with cultured chondrocytes].

Science.gov (United States)

Yan, M; Dang, G

1999-07-01

To construct a kind of bone healing enhancing implant with cultured chondrocytes bound to hydroxyapatite (HA). Chondrocytes were obtained from the costicartilage of rat and were cultured on the porous HA blocks, 3 mm x 3 mm x 4 mm size, for three and seven days. Scanning electron micrograph was taken to show whether the cells grew outside and inside the pore of HA block. The cells cultured on tiny glass sheet for 2 days were used to prove where the cells come from by in situ hybridization technique with alpha1 (II) cDNA probe. Scanning electron micrographs showed that the pores of the HA surface and inside of the blocks are filled with cultured cells, especially the longer cultured block. The cells were chondrocytes confirmed by in situ hybridization. The porous HA can be used as cell cultured substrate and chondrocyte can adhere and proliferate inside the porous HA block.

Interconnected porous hydroxyapatite ceramics for bone tissue engineering

Science.gov (United States)

Yoshikawa, Hideki; Tamai, Noriyuki; Murase, Tsuyoshi; Myoui, Akira

2008-01-01

Several porous calcium hydroxyapatite (HA) ceramics have been used clinically as bone substitutes, but most of them possessed few interpore connections, resulting in pathological fracture probably due to poor bone formation within the substitute. We recently developed a fully interconnected porous HA ceramic (IP-CHA) by adopting the ‘foam-gel’ technique. The IP-CHA had a three-dimensional structure with spherical pores of uniform size (average 150 μm, porosity 75%), which were interconnected by window-like holes (average diameter 40 μm), and also demonstrated adequate compression strength (10–12 MPa). In animal experiments, the IP-CHA showed superior osteoconduction, with the majority of pores filled with newly formed bone. The interconnected porous structure facilitates bone tissue engineering by allowing the introduction of mesenchymal cells, osteotropic agents such as bone morphogenetic protein or vasculature into the pores. Clinically, we have applied the IP-CHA to treat various bony defects in orthopaedic surgery, and radiographic examinations demonstrated that grafted IP-CHA gained radiopacity more quickly than the synthetic HA in clinical use previously. We review the accumulated data on bone tissue engineering using the novel scaffold and on clinical application in the orthopaedic field. PMID:19106069

Porous calcium polyphosphate bone substitutes: additive manufacturing versus conventional gravity sinter processing-effect on structure and mechanical properties.

Science.gov (United States)

Hu, Youxin; Shanjani, Yaser; Toyserkani, Ehsan; Grynpas, Marc; Wang, Rizhi; Pilliar, Robert

2014-02-01

Porous calcium polyphosphate (CPP) structures proposed as bone-substitute implants and made by sintering CPP powders to form bending test samples of approximately 35 vol % porosity were machined from preformed blocks made either by additive manufacturing (AM) or conventional gravity sintering (CS) methods and the structure and mechanical characteristics of samples so made were compared. AM-made samples displayed higher bending strengths (≈1.2-1.4 times greater than CS-made samples), whereas elastic constant (i.e., effective elastic modulus of the porous structures) that is determined by material elastic modulus and structural geometry of the samples was ≈1.9-2.3 times greater for AM-made samples. X-ray diffraction analysis showed that samples made by either method displayed the same crystal structure forming β-CPP after sinter annealing. The material elastic modulus, E, determined using nanoindentation tests also showed the same value for both sample types (i.e., E ≈ 64 GPa). Examination of the porous structures indicated that significantly larger sinter necks resulted in the AM-made samples which presumably resulted in the higher mechanical properties. The development of mechanical properties was attributed to the different sinter anneal procedures required to make 35 vol % porous samples by the two methods. A primary objective of the present study, in addition to reporting on bending strength and sample stiffness (elastic constant) characteristics, was to determine why the two processes resulted in the observed mechanical property differences for samples of equivalent volume percentage of porosity. An understanding of the fundamental reason(s) for the observed effect is considered important for developing improved processes for preparation of porous CPP implants as bone substitutes for use in high load-bearing skeletal sites. Copyright © 2013 Wiley Periodicals, Inc.

Surface free energy predominates in cell adhesion to hydroxyapatite through wettability.

Science.gov (United States)

Nakamura, Miho; Hori, Naoko; Ando, Hiroshi; Namba, Saki; Toyama, Takeshi; Nishimiya, Nobuyuki; Yamashita, Kimihiro

2016-05-01

The initial adhesion of cells to biomaterials is critical in the regulation of subsequent cell behaviors. The purpose of this study was to investigate a mechanism through which the surface wettability of biomaterials can be improved and determine the effects of biomaterial surface characteristics on cellular behaviors. We investigated the surface characteristics of various types of hydroxyapatite after sintering in different atmospheres and examined the effects of various surface characteristics on cell adhesion to study cell-biomaterial interactions. Sintering atmosphere affects the polarization capacity of hydroxyapatite by changing hydroxide ion content and grain size. Compared with hydroxyapatite sintered in air, hydroxyapatite sintered in saturated water vapor had a higher polarization capacity that increased surface free energy and improved wettability, which in turn accelerated cell adhesion. We determined the optimal conditions of hydroxyapatite polarization for the improvement of surface wettability and acceleration of cell adhesion. Copyright © 2016 Elsevier B.V. All rights reserved.

3D printing of porous hydroxyapatite scaffolds intended for use in bone tissue engineering applications

Energy Technology Data Exchange (ETDEWEB)

Cox, Sophie C.; Thornby, John A.; Gibbons, Gregory J., E-mail: G.J.Gibbons@warwick.ac.uk; Williams, Mark A.; Mallick, Kajal K.

2015-02-01

A systematic characterisation of bone tissue scaffolds fabricated via 3D printing from hydroxyapatite (HA) and poly(vinyl)alcohol (PVOH) composite powders is presented. Flowability of HA:PVOH precursor materials was observed to affect mechanical stability, microstructure and porosity of 3D printed scaffolds. Anisotropic behaviour of constructs and part failure at the boundaries of interlayer bonds was highlighted by compressive strength testing. A trade-off between the ability to facilitate removal of PVOH thermal degradation products during sintering and the compressive strength of green parts was revealed. The ultimate compressive strength of 55% porous green scaffolds printed along the Y-axis and dried in a vacuum oven for 6 h was 0.88 ± 0.02 MPa. Critically, the pores of 3D printed constructs could be user designed, ensuring bulk interconnectivity, and the imperfect packing of powder particles created an inherent surface roughness and non-designed porosity within the scaffold. These features are considered promising since they are known to facilitate osteoconduction and osteointegration in-vivo. Characterisation techniques utilised in this study include two funnel flow tests, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), compressive strength testing and computed tomography (CT). - Highlights: • Flowability of HA and PVOH powders corresponded to scaffold printability. • Anisotropic behaviour of 3D printed scaffolds was highlighted by compressive tests. • Maximum compressive strength of 3D printed 55% porous scaffolds was 0.88 MPa. • Imperfect packing of precursors resulted in a rough surface and microporosity. • A CT method was designed and used to quantify designed and non-designed porosity.

3D printing of porous hydroxyapatite scaffolds intended for use in bone tissue engineering applications

International Nuclear Information System (INIS)

Cox, Sophie C.; Thornby, John A.; Gibbons, Gregory J.; Williams, Mark A.; Mallick, Kajal K.

2015-01-01

A systematic characterisation of bone tissue scaffolds fabricated via 3D printing from hydroxyapatite (HA) and poly(vinyl)alcohol (PVOH) composite powders is presented. Flowability of HA:PVOH precursor materials was observed to affect mechanical stability, microstructure and porosity of 3D printed scaffolds. Anisotropic behaviour of constructs and part failure at the boundaries of interlayer bonds was highlighted by compressive strength testing. A trade-off between the ability to facilitate removal of PVOH thermal degradation products during sintering and the compressive strength of green parts was revealed. The ultimate compressive strength of 55% porous green scaffolds printed along the Y-axis and dried in a vacuum oven for 6 h was 0.88 ± 0.02 MPa. Critically, the pores of 3D printed constructs could be user designed, ensuring bulk interconnectivity, and the imperfect packing of powder particles created an inherent surface roughness and non-designed porosity within the scaffold. These features are considered promising since they are known to facilitate osteoconduction and osteointegration in-vivo. Characterisation techniques utilised in this study include two funnel flow tests, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), compressive strength testing and computed tomography (CT). - Highlights: • Flowability of HA and PVOH powders corresponded to scaffold printability. • Anisotropic behaviour of 3D printed scaffolds was highlighted by compressive tests. • Maximum compressive strength of 3D printed 55% porous scaffolds was 0.88 MPa. • Imperfect packing of precursors resulted in a rough surface and microporosity. • A CT method was designed and used to quantify designed and non-designed porosity

Microstructure Evolution and Mechanical Properties Improvement in Liquid-Phase-Sintered Hydroxyapatite by Laser Sintering

Directory of Open Access Journals (Sweden)

Songlin Duan

2015-03-01

Full Text Available CaO-Al2O3-SiO2 (CAS as a liquid phase was introduced into hydroxyapatite (HAp to prepare bone scaffolds. The effects of the CAS content (1, 2, 3, 4 and 5 wt% on microstructure and mechanical properties of HAp ceramics were investigated. The optimal compression strength, fracture toughness and Vickers hardness reached 22.22 MPa, 1.68 MPa·m1/2 and 4.47 GPa when 3 wt% CAS was added, which were increased by 105%, 63% and 11% compared with those of HAp ceramics without CAS, respectively. The improvement of the mechanical properties was attributed to the improved densification, which was caused by the solid particle to rearrange during liquid phase sintering. Moreover, simulated body fluid (SBF study indicated the HAp ceramics could maintain the mechanical properties and form a bone-like apatite layer when they were immersed in SBF. Cell culture was used to evaluate biocompatibility of the HAp ceramics. The results demonstrated MG-63 cells adhered and spread well.

Fabrication, Structural Characterization and Uniaxial Tensile Properties of Novel Sintered Multi-Layer Wire Mesh Porous Plates

Directory of Open Access Journals (Sweden)

Liuyang Duan

2018-01-01

Full Text Available There is an increasing interest in developing porous metals or metallic foams for functional and structural applications. The study of the physical and mechanical properties of porous metals is very important and helpful for their application. In this paper, a novel sintered multilayer wire mesh porous plate material (WMPPs with a thickness of 0.5 mm–3 mm and a porosity of 10–35% was prepared by winding, pressing, rolling, and subsequently vacuum sintering them. The pore size and total size distribution in the as-prepared samples were investigated using the bubble point method. The uniaxial tensile behavior of the WMPPs was investigated in terms of the sintering temperature, porosity, wire diameter, and manufacturing technology. The deformation process and the failure mechanism under the tensile press was also discussed based on the appearance of the fractures (SEM figures. The results indicated that the pore size and total size distribution were closely related to the raw material used and the sintering temperature. For the WMPPs prepared by the wire mesh, the pore structures were inerratic and the vast majority of pore size was less than 10 μm. On the other hand, for the WMPPs that were prepared by wire mesh and powder, the pore structures were irregular and the pore size ranged from 0 μm–50 μm. The experimental data showed that the tensile strength of WMPPs is much higher than any other porous metals or metallic foams. Higher sintering temperatures led to coarser joints between wires and resulted in higher tensile strength. The sintering temperature decreased from 1330 °C to 1130 °C and the tensile strength decreased from 296 MPa to 164 MPa. Lower porosity means that there are more metallurgical joints and metallic frameworks resisting deformation per unit volume. Therefore, lower porosities exhibit higher tensile strength. An increase of porosity from 17.14% to 32.5% led to the decrease of the tensile strength by 90 MPa. The

A Modified Porous Titanium Sheet Prepared by Plasma-Activated Sintering for Biomedical Applications

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Yukimichi Tamaki

2010-01-01

Full Text Available This study aimed to develop a contamination-free porous titanium scaffold by a plasma-activated sintering within an originally developed TiN-coated graphite mold. The surface of porous titanium sheet with or without a coated graphite mold was characterized. The cell adhesion property of porous titanium sheet was also evaluated in this study. The peak of TiC was detected on the titanium sheet processed with the graphite mold without a TiN coating. Since the titanium fiber elements were directly in contact with the carbon graphite mold during processing, surface contamination was unavoidable event in this condition. The TiC peak was not detectable on the titanium sheet processed within the TiN-coated carbon graphite mold. This modified plasma-activated sintering with the TiN-coated graphite mold would be useful to fabricate a contamination-free titanium sheet. The number of adherent cells on the modified titanium sheet was greater than that of the bare titanium plate. Stress fiber formation and the extension of the cells were observed on the titanium sheets. This modified titanium sheet is expected to be a new tissue engineering material in orthopedic bone repair.

Sintering of Multilayered Porous Structures: Part II – Experiments and Model Applications

DEFF Research Database (Denmark)

Ni, De Wei; Olevsky, Eugene; Esposito, Vincenzo

2013-01-01

Experimental analyses of shrinkage and distortion kinetics during sintering of bilayered porous and dense gadolinium-doped ceria Ce0.9Gd0.1O1.95d structures are carried out, and compared with the theoretical models developed in Part I of this work. A novel approach is developed for the determinat...

Hydroxyapatite additive influenced the bioactivity of bioactive nano-titania ceramics and new bone-forming capacity

Energy Technology Data Exchange (ETDEWEB)

Li Zhensheng [Third Military Medical University, College of Biomedical Engineering and Medical Imaging (China); Yang Xiaozhan [Chongqing University of Technology, School of Optoelectronic Information (China); Guo Hongfeng [Third Military Medical University, Tissue Engineering Research Center of Chongqing, Department of Anatomy, College of Basic Medical Sciences (China); Yang Xiaochao; Sun Lili [Third Military Medical University, College of Biomedical Engineering and Medical Imaging (China); Dong Shiwu, E-mail: shiwudong@gmail.com [Third Military Medical University, Tissue Engineering Research Center of Chongqing, Department of Anatomy, College of Basic Medical Sciences (China)

2012-09-15

Bioceramics plays an important role in bone-substitutes. In this study, titania porous ceramics with excellent bioactivity were prepared using hydroxyapatite (HA, 10 vol.% contents) as a grain growth inhibitor. The pure TiO{sub 2} porous ceramics were also prepared as a control. After sintered at 1,000 Degree-Sign C with a pressureless sintering method, the particle size of the pure TiO{sub 2} and TiO{sub 2}/HA (10 vol.%) porous ceramics were 450 and 310 nm, respectively. Each of the porous ceramics presented numerous pores, which were cross-connected. The size of the pores ranged from 100 to 300 {mu}m. There were also profuse micropores inside the pore wall and between the particles. A SBF soaking experiment demonstrated that the HA additive played an important role in promoting apatite formation. The cell proliferation demonstrated that osteoblasts on the TiO{sub 2}/HA (10 vol.%) porous ceramics proliferated faster than that on the pure TiO{sub 2} ceramics. The histological sections and EDX assay results of the two porous ceramics also illustrated that TiO{sub 2}/HA (10 vol.%) composite ceramics combined with Ca and P elements induced much better apatite formation than that of the pure TiO{sub 2} ceramics. These results indicated that titania ceramics combined with HA holds great promise for bone-substitutes.

Compressive deformation of liquid phase-sintered porous silicon carbide ceramics

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Taro Shimonosono

2014-12-01

Full Text Available Porous silicon carbide ceramics were fabricated by liquid phase sintering with 1 wt% Al2O3–1 wt% Y2O3 additives during hot-pressing at 1400–1900 °C. The longitudinal strain at compressive fracture increased at a higher porosity and was larger than the lateral strain. The compressive Young's modulus and the strain at fracture depended on the measured direction, and increased with the decreased specific surface area due to the formation of grain boundary. However, the compressive strength and the fracture energy were not sensitive to the measured direction. The compressive strength of a porous SiC compact increased with increasing grain boundary area. According to the theoretical modeling of the strength–grain boundary area relation, it is interpreted that the grain boundary of a porous SiC compact is fractured by shear deformation rather than by compressive deformation.

Development of porous ceramics by lycopodium using uniaxial pressing and sintering

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Rita Serzane

2010-12-01

Full Text Available In this work microporous hydroxyapatite (HAp ceramics were fabricated using lycopodium as a porosifier. The samples were produced by uniaxial pressing and then heating at high temperatures, 1100°C and 1200°C, to burn-out porogens and sintering. The obtained samples had porosity over the variable range of 12 to 45% with different pore size ranging from 0.2 to 25 µm. Chemical and physical characterization was determined by scanning electron microscopy (SEM, X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FTIR and bending strength measurements. The bending strength of the prepared samples was in the range of 1.97–21.81 MPa.

Novel porous graphene oxide and hydroxyapatite nanosheets-reinforced sodium alginate hybrid nanocomposites for medical applications

International Nuclear Information System (INIS)

Xiong, Guangyao; Luo, Honglin; Zuo, Guifu; Ren, Kaijing; Wan, Yizao

2015-01-01

Graphene oxide (GO) and hydroxyapatite (HAp) are frequently used as reinforcements in polymers to improve mechanical and biological properties. In this work, novel porous hybrid nanocomposites consisting of GO, HAp, and sodium alginate (SA) have been prepared by facile solution mixing and freeze drying in an attempt to obtain a scaffold with desirable mechanical and biological properties. The as-prepared porous GO/HAp/SA hybrid nanocomposites were characterized by SEM, XRD, FTIR, TGA, and mechanical testing. In addition, preliminary cell behavior was assessed by CCK8 assay. It is found that the GO/HAp/SA nanocomposites show improved compressive strength and modulus over neat SA and HAp/SA nanocomposites. CCK8 results reveal that the GO/HAp/SA nanocomposites show enhanced cell proliferation over neat SA and GO/SA nanocomposite. It has been demonstrated that GO/HAp20/SA holds promise in bone tissue engineering. - Graphical abstract: Display Omitted - Highlights: • Graphene oxide (GO), hydroxyapatite (HAp), and alginate (SA) nanocomposites were fabricated. • The novel porous composites were prepared by solution mixture and freeze drying. • The GO/HAp/SA had porous structure with porosity > 85% and pore size > 150 μm. • The GO/HAp/SA exhibited improved mechanical properties over HAp/SA counterparts. • The GO/HAp/SA showed enhanced cell proliferation over GO/SA counterparts

Novel porous graphene oxide and hydroxyapatite nanosheets-reinforced sodium alginate hybrid nanocomposites for medical applications

Energy Technology Data Exchange (ETDEWEB)

Xiong, Guangyao [School of Mechanical and Electrical Engineering, East China Jiaotong University, Nanchang 330013 (China); Luo, Honglin [Research Institute of Biomaterials and Transportation, East China Jiaotong University, Nanchang 330013 (China); School of Materials Science and Engineering, Tianjin Key Laboratory of Composite and Functional Materials, Key Laboratory of Advanced Ceramics and Machining Technology, Ministry of Education, Tianjin University, Tianjin 300072 (China); Zuo, Guifu [Hebei Provincial Key Laboratory of Inorganic Nonmetallic Materials, College of Materials Science and Engineering, Hebei United University, Tangshan 063009 (China); Ren, Kaijing [Department of Joint Surgery, Tianjin Hospital, Tianjin 300211 (China); Wan, Yizao, E-mail: yzwantju@126.com [Research Institute of Biomaterials and Transportation, East China Jiaotong University, Nanchang 330013 (China); School of Materials Science and Engineering, Tianjin Key Laboratory of Composite and Functional Materials, Key Laboratory of Advanced Ceramics and Machining Technology, Ministry of Education, Tianjin University, Tianjin 300072 (China)

2015-09-15

Graphene oxide (GO) and hydroxyapatite (HAp) are frequently used as reinforcements in polymers to improve mechanical and biological properties. In this work, novel porous hybrid nanocomposites consisting of GO, HAp, and sodium alginate (SA) have been prepared by facile solution mixing and freeze drying in an attempt to obtain a scaffold with desirable mechanical and biological properties. The as-prepared porous GO/HAp/SA hybrid nanocomposites were characterized by SEM, XRD, FTIR, TGA, and mechanical testing. In addition, preliminary cell behavior was assessed by CCK8 assay. It is found that the GO/HAp/SA nanocomposites show improved compressive strength and modulus over neat SA and HAp/SA nanocomposites. CCK8 results reveal that the GO/HAp/SA nanocomposites show enhanced cell proliferation over neat SA and GO/SA nanocomposite. It has been demonstrated that GO/HAp20/SA holds promise in bone tissue engineering. - Graphical abstract: Display Omitted - Highlights: • Graphene oxide (GO), hydroxyapatite (HAp), and alginate (SA) nanocomposites were fabricated. • The novel porous composites were prepared by solution mixture and freeze drying. • The GO/HAp/SA had porous structure with porosity > 85% and pore size > 150 μm. • The GO/HAp/SA exhibited improved mechanical properties over HAp/SA counterparts. • The GO/HAp/SA showed enhanced cell proliferation over GO/SA counterparts.

3D printing of porous hydroxyapatite scaffolds intended for use in bone tissue engineering applications.

Science.gov (United States)

Cox, Sophie C; Thornby, John A; Gibbons, Gregory J; Williams, Mark A; Mallick, Kajal K

2015-02-01

A systematic characterisation of bone tissue scaffolds fabricated via 3D printing from hydroxyapatite (HA) and poly(vinyl)alcohol (PVOH) composite powders is presented. Flowability of HA:PVOH precursor materials was observed to affect mechanical stability, microstructure and porosity of 3D printed scaffolds. Anisotropic behaviour of constructs and part failure at the boundaries of interlayer bonds was highlighted by compressive strength testing. A trade-off between the ability to facilitate removal of PVOH thermal degradation products during sintering and the compressive strength of green parts was revealed. The ultimate compressive strength of 55% porous green scaffolds printed along the Y-axis and dried in a vacuum oven for 6h was 0.88 ± 0.02 MPa. Critically, the pores of 3D printed constructs could be user designed, ensuring bulk interconnectivity, and the imperfect packing of powder particles created an inherent surface roughness and non-designed porosity within the scaffold. These features are considered promising since they are known to facilitate osteoconduction and osteointegration in-vivo. Characterisation techniques utilised in this study include two funnel flow tests, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), compressive strength testing and computed tomography (CT). Copyright © 2014 Elsevier B.V. All rights reserved.

Pore Formation Process of Porous Ti3SiC2 Fabricated by Reactive Sintering

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Huibin Zhang

2017-02-01

Full Text Available Porous Ti3SiC2 was fabricated with high purity, 99.4 vol %, through reactive sintering of titanium hydride (TiH2, silicon (Si and graphite (C elemental powders. The reaction procedures and the pore structure evolution during the sintering process were systematically studied by X-ray diffraction (XRD and scanning electron microscope (SEM. Our results show that the formation of Ti3SiC2 from TiH2/Si/C powders experienced the following steps: firstly, TiH2 decomposed into Ti; secondly, TiC and Ti5Si3 intermediate phases were generated; finally, Ti3SiC2 was produced through the reaction of TiC, Ti5Si3 and Si. The pores formed in the synthesis procedure of porous Ti3SiC2 ceramics are derived from the following aspects: interstitial pores left during the pressing procedure; pores formed because of the TiH2 decomposition; pores formed through the reactions between Ti and Si and Ti and C powders; and the pores produced accompanying the final phase synthesized during the high temperature sintering process.

Facile method of building hydroxyapatite 3D scaffolds assembled from porous hollow fibers enabling nutrient delivery

NARCIS (Netherlands)

Salamon, David; Da Silva Teixeira, Sandra; Dutczak, S.M.; Stamatialis, Dimitrios

2014-01-01

Nowadays, diffusion through scaffold and tissue usually limits transport, and forms potentially hypoxic regions. Several methods are used for preparation of 3D hydroxyapatite scaffolds, however, production of a scaffold including porous hollow fibers for nutrition delivery is difficult and

Microstructure, mechanical properties and superelasticity of biomedical porous NiTi alloy prepared by microwave sintering.

Science.gov (United States)

Xu, J L; Bao, L Z; Liu, A H; Jin, X J; Tong, Y X; Luo, J M; Zhong, Z C; Zheng, Y F

2015-01-01

Porous NiTi alloys were prepared by microwave sintering using ammonium hydrogen carbonate (NH4HCO3) as the space holder agent to adjust the porosity in the range of 22-62%. The effects of porosities on the microstructure, hardness, compressive strength, bending strength, elastic modulus, phase transformation temperature and superelasticity of the porous NiTi alloys were investigated. The results showed that the porosities and average pore sizes of the porous NiTi alloys increased with increasing the contents of NH4HCO3. The porous NiTi alloys consisted of nearly single NiTi phase, with a very small amount of two secondary phases (Ni3Ti, NiTi2) when the porosities are lower than 50%. The amount of Ni3Ti and NiTi2 phases increased with further increasing of the porosity proportion. The porosities had few effects on the phase transformation temperatures of the porous NiTi alloys. By increasing the porosities, all of the hardness, compressive strength, elastic modulus, bending strength and superelasticity of the porous NiTi alloys decreased. However, the compressive strength and bending strength were higher or close to those of natural bone and the elastic modulus was close to the natural bone. The superelastic recovery strain of the trained porous NiTi alloys could reach between 3.1 and 4.7% at the pre-strain of 5%, even if the porosity was up to 62%. Moreover, partial shape memory effect was observed for all porosity levels under the experiment conditions. Therefore, the microwave sintered porous NiTi alloys could be a promising candidate for bone implant. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis and sintering of nanocrystalline hydroxyapatite powders by citric acid sol-gel combustion method

International Nuclear Information System (INIS)

Han Yingchao; Li Shipu; Wang Xinyu; Chen Xiaoming

2004-01-01

The citric acid sol-gel combustion method has been used for the synthesis of nanocrystalline hydroxyapatite (HAP) powder from calcium nitrate, diammonium hydrogen phosphate and citric acid. The phase composition of HAP powder was characterized by X-ray powder diffraction analysis (XRD). The morphology of HAP powder was observed by transmission electron microscope (TEM). The HAP powder has been sintered into microporous ceramic in air at 1200 deg. C with 3 h soaking time. The microstructure and phase composition of the resulting HAP ceramic were characterized by scanning electron microscope (SEM) and XRD, respectively. The physical characterization of open porosity and flexural strength have also been carried out

Laser-Induced Breakdown Spectroscopy (LIBS) for Monitoring the Formation of Hydroxyapatite Porous Layers

OpenAIRE

Sola, Daniel; Paulés, Daniel; Grima, Lorena; Anzano, Jesús

2017-01-01

Laser-induced breakdown spectroscopy (LIBS) is applied to characterize the formation of porous hydroxyapatite layers on the surface of 0.8CaSiO3-0.2Ca3(PO4)2 biocompatible eutectic glass immersed in simulated body fluid (SBF). Compositional and structural characterization analyses were also conducted by field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDX), and micro-Raman spectroscopy.

Hydroxyapatite implants with designed internal architecture.

Science.gov (United States)

Chu, T M; Halloran, J W; Hollister, S J; Feinberg, S E

2001-06-01

Porous hydroxyapatite (HA) has been used as a bone graft material in the clinics for decades. Traditionally, the pores in these HAs are either obtained from the coralline exoskeletal patterns or from the embedded organic particles in the starting HA powder. Both processes offer very limited control on the pore structure. A new method for manufacturing porous HA with designed pore channels has been developed. This method is essentially a lost-mold technique with negative molds made with Stereolithography and a highly loaded curable HA suspension as the ceramic carrier. Implants with designed channels and connection patterns were first generated from a Computer-Aided-Design (CAD) software and Computer Tomography (CT) data. The negative images of the designs were used to build the molds on a stereolithography apparatus with epoxy resins. A 40 vol% HA suspension in propoxylated neopentyl glycol diacrylate (PNPGDA) and iso-bornyl acrylate (IBA) was formulated. HA suspension was cast into the epoxy molds and cured into solid at 85 degrees C. The molds and acrylate binders were removed by pyrolysis, followed by HA green body sintering. With this method, implants with six different channel designs were built successfully and the designed channels were reproduced in the sintered HA implants. The channels created in the sintered HA implants were between 366 microm and 968 microm in diameter with standard deviations of 50 microm or less. The porosity created by the channels were between 26% and 52%. The results show that HA implants with designed connection pattern and well controlled channel size can be built with the technique developed in this study. Copyright 2001 Kluwer Academic Publishers

Solvent/non-solvent sintering: a novel route to create porous microsphere scaffolds for tissue regeneration.

Science.gov (United States)

Brown, Justin L; Nair, Lakshmi S; Laurencin, Cato T

2008-08-01

Solvent/non-solvent sintering creates porous polymeric microsphere scaffolds suitable for tissue engineering purposes with control over the resulting porosity, average pore diameter, and mechanical properties. Five different biodegradable biocompatible polyphosphazenes exhibiting glass transition temperatures from -8 to 41 degrees C and poly (lactide-co-glycolide), (PLAGA) a degradable polymer used in a number of biomedical settings, were examined to study the versatility of the process and benchmark the process to heat sintering. Parameters such as: solvent/non-solvent sintering solution composition and submersion time effect the sintering process. PLAGA microsphere scaffolds fabricated with solvent/non-solvent sintering exhibited an interconnected porosity and pore size of 31.9% and 179.1 mum, respectively which was analogous to that of conventional heat sintered PLAGA microsphere scaffolds. Biodegradable polyphosphazene microsphere scaffolds exhibited a maximum interconnected porosity of 37.6% and a maximum compressive modulus of 94.3 MPa. Solvent/non-solvent sintering is an effective strategy for sintering polymeric microspheres, with a broad spectrum of glass transition temperatures, under ambient conditions making it an excellent fabrication route for developing tissue engineering scaffolds and drug delivery vehicles. (c) 2007 Wiley Periodicals, Inc.

Bone Regeneration of Hydroxyapatite with Granular Form or Porous Scaffold in Canine Alveolar Sockets

Science.gov (United States)

JANG, SEOK JIN; KIM, SE EUN; HAN, TAE SUNG; SON, JUN SIK; KANG, SEONG SOO; CHOI, SEOK HWA

2017-01-01

This study was undertaken to assess bone regeneration using hydroxyapatite (HA). The primary focus was comparison of bone regeneration between granular HA (gHA) forms and porous HA (pHA) scaffold. The extracted canine alveolar sockets were divided with three groups: control, gHA and pHA. Osteogenic effect in the gHA and pHA groups showed bone-specific surface and bone mineral density to be significantly higher than that of the control group (psocket healing. For new bone formation during 8 weeks' post-implantation, HA with porous scaffold was superior to the granular form of HA. PMID:28438860

Boric oxide or boric acid sintering aid for sintering ceramics

International Nuclear Information System (INIS)

Lawler, H.A.

1979-01-01

The invention described relates to the use of liquid sintering aid in processes involving sintering of ceramic materials to produce dense, hard articles having industrial uses. Although the invention is specifically discussed in regard to compositions containing silicon carbide as the ceramic material, other sinterable carbides, for example, titanium carbide, may be utilized as the ceramic material. A liquid sintering aid for densifying ceramic material is selected from solutions of H 3 BO 3 , B 2 O 3 and mixtures of these solutions. In sintering ceramic articles, e.g. silicon carbide, a shaped green body is formed from a particulate ceramic material and a resin binder, and the green body is baked at a temperature of 500 to 1000 0 C to form a porous body. The liquid sintering aid of B 2 O 3 and/or H 3 BO 3 is then dispersed through the porous body and the treated body is sintered at a temperature of 1900 to 2200 0 C to produce the sintered ceramic article. (U.K.)

Comparative evaluation of electrical conductivity of hydroxyapatite ceramics densified through ramp and hold, spark plasma and post sinter Hot Isostatic Pressing routes

Energy Technology Data Exchange (ETDEWEB)

Buchi Suresh, M., E-mail: suresh@arci.res.in; Biswas, P.; Mahender, V.; Johnson, Roy, E-mail: royjohnson@arci.res.in

2017-01-01

Hydroxyapatite ceramics synthesized through sonochemical route were processed and densified through ramp & hold (R&H) and Spark Plasma Sintering (SPS) routes. The effect of processing route on the relative density and electrical conductivity were studied. Further, the samples were Hot Isostatically Pressed (HIP) under argon pressure at elevated temperature to further densify the sample. All these samples processed under different conditions were characterized by X-ray diffraction, Scanning Electron Microscopy and AC Conductivity. The samples have exhibited hydroxyapatite phase; however, microstructures exhibited distinctly different grain morphologies and grain sizes. AC impedance spectroscopic measurement was carried out on hydroxyapatite samples processed through different routes and the corresponding spectra were analyzed by the analogy to equivalent circuit involving resistors and capacitors. SPS sintered sample after HIPing has exhibited the highest conductivity. This can be attributed to the higher density in combination with finer grain sizes. Activation energy based on Arrhenius equation is calculated and the prominent conduction mechanism is proposed. - Highlights: • Hot Isostatic Pressing (HIP) of SPS and R&H processed samples has resulted into densities near to theoretical densities • No change in the crystal structure is observed in SPS and R&H samples before and after HIP treatment • SPS processed and HIP treated samples resulted into higher conductivities with smaller grain sizes and grain boundary area.

Laser-Induced Breakdown Spectroscopy (LIBS for Monitoring the Formation of Hydroxyapatite Porous Layers

Directory of Open Access Journals (Sweden)

Daniel Sola

2017-12-01

Full Text Available Laser-induced breakdown spectroscopy (LIBS is applied to characterize the formation of porous hydroxyapatite layers on the surface of 0.8CaSiO3-0.2Ca3(PO42 biocompatible eutectic glass immersed in simulated body fluid (SBF. Compositional and structural characterization analyses were also conducted by field emission scanning electron microscopy (FESEM, energy dispersive X-ray spectroscopy (EDX, and micro-Raman spectroscopy.

Microstructural and Mechanical Properties of Porous 60NiTi Prepared by Conventional Press-and-sinter Method

Directory of Open Access Journals (Sweden)

Khanlari Khashayar

2017-01-01

Full Text Available An intermetallic nickel-titanium alloy, 60NiTi, comprised of approximately 60 wt.% Ni and 40 wt.% Ti, contains a broad combination of physical and mechanical properties such as high hardness, low elastic modulus, resistance to aqueous corrosion and good biocompatibility. These unique combinations make this alloy an attractive candidate for medical components such as implants and prosthesis, where biocompatible materials with high hardness and low stiffness are typically used. The conventional press-and-sinter method which represents the least complex, most flexible and economic powder metallurgy method was used to produce porous 60NiTi parts suitable for biomedical applications. The effect of sintering holding time on the microstructure and mechanical properties is investigated. The structure of the as sintered parts is quite porous which is beneficial based on the medical point of view. The ultimate compressive strength of the samples is higher than that of the compact human bone and can, therefore, meet the strength demand of implants for general bone replacement applications.

Hydrothermal synthesis of porous triphasic hydroxyapatite/(alpha and beta) tricalcium phosphate.

Science.gov (United States)

Vani, R; Girija, E K; Elayaraja, K; Prakash Parthiban, S; Kesavamoorthy, R; Narayana Kalkura, S

2009-12-01

A novel, porous triphasic calcium phosphate composed of nonresorbable hydroxyapatite (HAp) and resorbable tricalcium phosphate (alpha- and beta-TCP) has been synthesized hydrothermally at a relatively low temperature. The calcium phosphate precursor for hydrothermal treatment was prepared by gel method in the presence of ascorbic acid. XRD, FT-IR, Raman analyses confirmed the presence of HAp/TCP. The surface area and average pore size of the samples were found to be 28 m2/g and 20 nm, respectively. The samples were found to be bioactive in simulated body fluid (SBF).

Synthesis and synchrotron characterisation of novel dual-template of hydroxyapatite scaffolds with controlled size porous distribution

Energy Technology Data Exchange (ETDEWEB)

Lima, Thiago A. R. M.; Ilavsky, Jan; Hammons, Joshua; Sarmento, Victor H. V.; Rey, José F. Q.; Valerio, Mário E. G.

2017-03-01

Hydroxyapatite (HAP) scaffolds with a hierarchical porous architecture were prepared by a new dual-template (corn starch and cetyltrimethylammonium bromide (CTAB) surfactant) used to cast HAP nanoparticles and development scaffolds with size hierarchical porous distribution. The Powder X-Ray diffraction (XRD) results showed that only the HAP crystalline phase is present in the samples after calcination; the Scanning Electron Microscopy (SEM) combined with Small Angle (SAXS) and Ultra-Small Angle X-ray Scattering (USAXS) techniques showed that the porous arrangement is promoted by needle-like HAP nanoparticles, and that the pore size distributions depend on the drip-order of the calcium and the phosphate solutions during the template preparation stage.

Bioactivity and mineralization of hydroxyapatite with bioglass as sintering aid and bioceramics with Na{sub 3}Ca{sub 6}(PO{sub 4}){sub 5} and Ca{sub 5}(PO{sub 4}){sub 2}SiO{sub 4} in a silicate matrix

Energy Technology Data Exchange (ETDEWEB)

Demirkiran, Hande [Materials Science and Engineering Department, University of Texas at Arlington, Arlington, TX 76019 (United States); Mohandas, Arunesh; Dohi, Motokazi; Fuentes, Alonso; Nguyen, Kytai [Bioengineering Department, University of Texas at Arlington, Arlington, TX 76019 (United States); Aswath, Pranesh, E-mail: aswath@uta.edu [Materials Science and Engineering Department, University of Texas at Arlington, Arlington, TX 76019 (United States)

2010-01-30

Hydroxyapatite and Bioglass-45S5 were sintered together creating new ceramic compositions that yielded increased apatite deposition and osteoblast differentiation and proliferation in vitro compared to hydroxyapatite. The sintered products characterized by X-ray diffraction, revealed hydroxyapatite as the main phase when small quantities (1, 2.5 and 5 wt.%) of bioglass was added. Bioglass behaved as a sintering aid with {beta}-TCP (Ca{sub 3}(PO{sub 4}){sub 2}) being the minor phase. The amount of {beta}-TCP increased with the amount of bioglass added. In compositions with larger additions of bioglass (10 and 25 wt.%), new phases with compositions of calcium phosphate silicate (Ca{sub 5}(PO{sub 4}){sub 2}SiO{sub 4}) and sodium calcium phosphate (Na{sub 3}Ca{sub 6}(PO{sub 4}){sub 5}) were formed respectively within amorphous silicate matrices. In vitro cell culture studies of the ceramic compositions were examined using bone marrow stromal cell (BMSC). Cell proliferation and differentiation of bone marrow stromal cells into osteoblasts were determined by Pico Green DNA assays and alkaline phosphatase (ALP) activity, respectively. All hydroxyapatite-bioglass co-sintered ceramics exhibited larger cell proliferation compared to pure hydroxyapatite samples. After 6 days in cell culture, the ceramic with Ca{sub 5}(PO{sub 4}){sub 3}SiO{sub 4} in a silicate matrix formed by reacting hydroxyapatite with 10 wt.% bioglass exhibited the maximum proliferation of the BMSC's. The ALP activity was found to be largest in the ceramic with Na{sub 3}Ca{sub 6}(PO{sub 4}){sub 5} embedded in a silicate matrix synthesized by reacting hydroxyapatite with 25 wt.% bioglass.

Synthesis and characterization of porous silicon as hydroxyapatite host matrix of biomedical applications.

Directory of Open Access Journals (Sweden)

A Dussan

Full Text Available In this work, porous-silicon samples were prepared by electrochemical etching on p-type (B-doped Silicon (Si wafers. Hydrofluoric acid (HF-ethanol (C2H5OH [HF:Et] and Hydrofluoric acid (HF-dimethylformamide (DMF-C3H7NO [HF:DMF] solution concentrations were varied between [1:2]-[1:3] and [1:7]-[1:9], respectively. Effects of synthesis parameters, like current density, solution concentrations, reaction time, on morphological properties were studied by scanning electron microscopy (SEM and atomic force microscopy (AFM measurements. Pore sizes varying from 20 nm to micrometers were obtained for long reaction times and [HF:Et] [1:2] concentrations; while pore sizes in the same order were observed for [HF:DMF] [1:7], but for shorter reaction time. Greater surface uniformity and pore distribution was obtained for a current density of around 8 mA/cm2 using solutions with DMF. A correlation between reflectance measurements and pore size is presented. The porous-silicon samples were used as substrate for hydroxyapatite growth by sol-gel method. X-ray diffraction (XRD and SEM were used to characterize the layers grown. It was found that the layer topography obtained on PS samples was characterized by the evidence of Hydroxyapatite in the inter-pore regions and over the surface.

Synthesis and characterization of porous silicon as hydroxyapatite host matrix of biomedical applications.

Science.gov (United States)

Dussan, A; Bertel, S D; Melo, S F; Mesa, F

2017-01-01

In this work, porous-silicon samples were prepared by electrochemical etching on p-type (B-doped) Silicon (Si) wafers. Hydrofluoric acid (HF)-ethanol (C2H5OH) [HF:Et] and Hydrofluoric acid (HF)-dimethylformamide (DMF-C3H7NO) [HF:DMF] solution concentrations were varied between [1:2]-[1:3] and [1:7]-[1:9], respectively. Effects of synthesis parameters, like current density, solution concentrations, reaction time, on morphological properties were studied by scanning electron microscopy (SEM) and atomic force microscopy (AFM) measurements. Pore sizes varying from 20 nm to micrometers were obtained for long reaction times and [HF:Et] [1:2] concentrations; while pore sizes in the same order were observed for [HF:DMF] [1:7], but for shorter reaction time. Greater surface uniformity and pore distribution was obtained for a current density of around 8 mA/cm2 using solutions with DMF. A correlation between reflectance measurements and pore size is presented. The porous-silicon samples were used as substrate for hydroxyapatite growth by sol-gel method. X-ray diffraction (XRD) and SEM were used to characterize the layers grown. It was found that the layer topography obtained on PS samples was characterized by the evidence of Hydroxyapatite in the inter-pore regions and over the surface.

Enhanced osteoconductivity of sodium-substituted hydroxyapatite by system instability.

Science.gov (United States)

Sang Cho, Jung; Um, Seung-Hoon; Su Yoo, Dong; Chung, Yong-Chae; Hye Chung, Shin; Lee, Jeong-Cheol; Rhee, Sang-Hoon

2014-07-01

The effect of substituting sodium for calcium on enhanced osteoconductivity of hydroxyapatite was newly investigated. Sodium-substituted hydroxyapatite was synthesized by reacting calcium hydroxide and phosphoric acid with sodium nitrate followed by sintering. As a control, pure hydroxyapatite was prepared under identical conditions, but without the addition of sodium nitrate. Substitution of calcium with sodium in hydroxyapatite produced the structural vacancies for carbonate ion from phosphate site and hydrogen ion from hydroxide site of hydroxyapatite after sintering. The total system energy of sodium-substituted hydroxyapatite with structural defects calculated by ab initio methods based on quantum mechanics was much higher than that of hydroxyapatite, suggesting that the sodium-substituted hydroxyapatite was energetically less stable compared with hydroxyapatite. Indeed, sodium-substituted hydroxyapatite exhibited higher dissolution behavior of constituent elements of hydroxyapatite in simulated body fluid (SBF) and Tris-buffered deionized water compared with hydroxyapatite, which directly affected low-crystalline hydroxyl-carbonate apatite forming capacity by increasing the degree of apatite supersaturation in SBF. Actually, sodium-substituted hydroxyapatite exhibited markedly improved low-crystalline hydroxyl-carbonate apatite forming capacity in SBF and noticeably higher osteoconductivity 4 weeks after implantation in calvarial defects of New Zealand white rabbits compared with hydroxyapatite. In addition, there were no statistically significant differences between hydroxyapatite and sodium-substituted hydroxyapatite on cytotoxicity as determined by BCA assay. Taken together, these results indicate that sodium-substituted hydroxyapatite with structural defects has promising potential for use as a bone grafting material due to its enhanced osteoconductivity compared with hydroxyapatite. © 2013 Wiley Periodicals, Inc.

Hydroxyapatite in total hip arthroplasty. Our experience with a plasma spray porous titanium alloy/hydroxyapatite double-coated cementless stem.

Science.gov (United States)

Castellini, Iacopo; Andreani, Lorenzo; Parchi, Paolo Domenico; Bonicoli, Enrico; Piolanti, Nicola; Risoli, Francesca; Lisanti, Michele

2016-01-01

Total hip arthroplasty could fail due to many factors and one of the most common is the aseptic loosening. In order to achieve an effective osseointegration and reduce risk of lossening, the use of cemented implant, contact porous bearing surface and organic coating were developed. Aim of this study was to evaluate clinical and radiological mid-term outcomes of a porous titanium alloy/hydroxyapatite double coating manufactured cementless femoral stem applied with "plasma spray" technique and to demonstrate the possibility to use this stem in different types of femoral canals. Between January 2008 and December 2012, 240 consecutive primary total hip arthroplasties (THAs) were performed using a porous titanium alloy/hydroxyapatite double coating manufactured cementless femoral stem. 182 patients were examined: 136 were females (74.7%) and 46 males (25.2%); average age was 72 years old (ranging from 26 to 92 years old). For each patient, Harris Hip Scores (HHS) and Womac Scores were collected. All X-ray images were analyzed in order to demonstrate stem survival rate and subsidence. Harris Hip Score was good or excellent in 85% of the cases (average 90%) and mean WOMAC score was 97.5 (ranging from 73.4 to 100). No cases of early/late infection or periprosthetic fracture were noticed, with an excellent implant survival rate (100%) in a mean period of 40 months (ranging from 24 and 84 months). 5 cases presented acute implant dislocation, 2 due to wrong cup positioning in a dysplastic acetabulum and 3 after ground level fall. Dorr classification of femoral geometry was uses and the results were: 51 type A bone, 53 type B bone and 78 type C bone. Stem subsidence over 2 mm was considered as a risk factor of future implant loosening and was evidenced in 3 female patients with type C of Dorr classification. No radiolucencies signs around the proximally coated portion of stem or proximal reabsorption were visible during the radiographic follow-up. Concerning the use of porous

Dispersed hydroxyapatite and modified bioglass 45S5 composites: sintering behavior of glass matrix ranging from 20 to 30 wt% in calcium oxide investigation

Energy Technology Data Exchange (ETDEWEB)

Silva, A.C.; Parra-Silva, J.; Santos, S.C.; Mello-Castanho, S.R.H, E-mail: dasilva.ac@uol.com.br [Instituto de Pesquisas Enegeticas e Nucleares (IPEN/CNEN-SP), DP (Brazil); Braga, F.J.C. [Consulmat Materiais de Referencia, Solucoes e Servicos, Sao Carlos, SP (Brazil); Setz, L.F.G. [Universidade Federal do ABC (UFABC), Santo Andre, SP (Brazil)

2014-07-01

Biomaterial technology plays an important role in cell-based tissue proliferation environment creation. The hydroxyapatite (HA) bioceramics are reference materials to employment as a bone substitute, however, their slow rate of degradation and its low rate of bioactivity (Ib) are presented as limiting factors for application as bone graft. In contrast, the bioglass (BG) is a resorbable and osteoinductive material and can act as fluxing in HA/BG composites. The present work objective the development of HA/BG (40/70wt%) composites, Three compositions of the 45S5 bioglass derived ranging from 20-30wt% in CaO were used in order to study the sintering behavior of these materials with hydroxyapatite 30wt% dispersed. The composites were uniaxially pressed in the form of cylinders and sinterized at (1100°C/1h). The characterization was made employing scanning electron microscopy, Infra-Red Spectrometry, X-ray diffraction and hydrolytic resistance test. The results indicate the potential use of the materials developed for applications like bone graft.(author)

Dispersed hydroxyapatite and modified bioglass 45S5 composites: sintering behavior of glass matrix ranging from 20 to 30 wt% in calcium oxide investigation

International Nuclear Information System (INIS)

Silva, A.C.; Parra-Silva, J.; Santos, S.C.; Mello-Castanho, S.R.H; Braga, F.J.C.; Setz, L.F.G.

2014-01-01

Biomaterial technology plays an important role in cell-based tissue proliferation environment creation. The hydroxyapatite (HA) bioceramics are reference materials to employment as a bone substitute, however, their slow rate of degradation and its low rate of bioactivity (Ib) are presented as limiting factors for application as bone graft. In contrast, the bioglass (BG) is a resorbable and osteoinductive material and can act as fluxing in HA/BG composites. The present work objective the development of HA/BG (40/70wt%) composites, Three compositions of the 45S5 bioglass derived ranging from 20-30wt% in CaO were used in order to study the sintering behavior of these materials with hydroxyapatite 30wt% dispersed. The composites were uniaxially pressed in the form of cylinders and sinterized at (1100°C/1h). The characterization was made employing scanning electron microscopy, Infra-Red Spectrometry, X-ray diffraction and hydrolytic resistance test. The results indicate the potential use of the materials developed for applications like bone graft.(author)

Structure and properties of porous TiNi(Co, Mo)-based alloy produced by the reaction sintering

Science.gov (United States)

Artyukhova, Nadezda; Yasenchuk, Yuriy; Chekalkin, Timofey; Gunther, Victor; Kim, Ji-Soon; Kang, Ji-Hoon

2016-10-01

Modern medical technologies have developed many new devices that can be implanted into humans to repair, assist or take the place of diseased or defective bones, arteries and even organs. The materials, especially porous ones, used for these devices have evolved steadily over the past twenty years with TiNi-based alloys replacing stainless steels and titanium. The aim of the paper is to presents results for examination of porous TiNi(Co,Mo)-based alloys intended further to be used in clinical practice. The structure and properties of porous TiNi-based alloys obtained by reaction sintering of Ti and Ni powders with additions of Co and Mo have been studied. It has been shown that alloying additions both Co and Mo inhibit the compaction of nickel powders in the initial stage of sintering. The maximum irreversible strain of porous samples under loading in the austenitic state is fixed with the Co addition, and the minimum one is fixed with the Mo addition. The Co addition leads to the fact that the martensite transformation in the TiNi phase becomes close to a one-step, and the Mo addition leads to the fact that the martensite transformation becomes more uniform. Both Co and Mo lead to an increase in the maximum accumulated strain as a result of the formation of temperature martensite. The additional increase in the maximum accumulated strain of the Ti50Ni49Co1 alloy is caused by decreased resistance of the porous Ni γ -based mass during the load.

Titanium Powder Sintering in a Graphite Furnace and Mechanical Properties of Sintered Parts

Directory of Open Access Journals (Sweden)

Changzhou Yu

2017-02-01

Full Text Available Recent accreditation of titanium powder products for commercial aircraft applications marks a milestone in titanium powder metallurgy. Currently, powder metallurgical titanium production primarily relies on vacuum sintering. This work reported on the feasibility of powder sintering in a non-vacuum furnace and the tensile properties of the as-sintered Ti. Specifically, we investigated atmospheric sintering of commercially pure (C.P. titanium in a graphite furnace backfilled with argon and studied the effects of common contaminants (C, O, N on sintering densification of titanium. It is found that on the surface of the as-sintered titanium, a severely contaminated porous scale was formed and identified as titanium oxycarbonitride. Despite the porous surface, the sintered density in the sample interiors increased with increasing sintering temperature and holding time. Tensile specimens cut from different positions within a large sintered cylinder reveal different tensile properties, strongly dependent on the impurity level mainly carbon and oxygen. Depending on where the specimen is taken from the sintered compact, ultimate tensile strength varied from 300 to 580 MPa. An average tensile elongation of 5% to 7% was observed. Largely depending on the interstitial contents, the fracture modes from typical brittle intergranular fracture to typical ductile fracture.

Improvement of the stability of hydroxyapatite through glass ceramic reinforcement.

Science.gov (United States)

Ha, Na Ra; Yang, Zheng Xun; Hwang, Kyu Hong; Kim, Tae Suk; Lee, Jong Kook

2010-05-01

Hydroxyapatite has achieved significant application in orthopedic and dental implants due to its excellent biocompatibility. Sintered hydroxyapatites showed significant dissolution, however, after their immersion in water or simulated body fluid (SBF). This grain boundary dissolution, even in pure hydroxyapatites, resulted in grain separation at the surfaces, and finally, in fracture. In this study, hydroxyapatite ceramics containing apatite-wollastonite (AW) or calcium silicate (SG) glass ceramics as additives were prepared to prevent the dissolution. AW and SG glass ceramics were added at 0-7 wt% and powder-compacted uniaxially followed by firing at moisture conditions. The glass phase was incorporated into the hydroxyapatite to act as a sintering aid, followed by crystallization, to improve the mechanical properties without reducing the biocompatibility. As seen in the results of the dissolution test, a significant amount of damage was reduced even after more than 14 days. TEM and SEM showed no decomposition of HA to the secondary phase, and the fracture toughness increased, becoming even higher than that of the commercial hydroxyapatite.

Analysis of the sintering stresses and shape distortion produced in co-firing of CGO-LSM/CGO bi-layer porous structures

DEFF Research Database (Denmark)

Ni, De Wei; Esposito, Vincenzo; Schmidt, Cristine Grings

such as cracks, de-lamination and shape distortion can result as a consequence of sintering mismatch stresses caused by the strain rate difference between layers. This work seeks to understand the underlying mechanisms that occur during the co-firing of porous CGO-LSM/CGO bi-layer laminates, by evaluating...... the sintering mismatch stress and distortion development through modeling and experiments....

Nano-hydroxyapatite colloid suspension coated on chemically modified porous silicon by cathodic bias: a suitable surface for cell culture

Energy Technology Data Exchange (ETDEWEB)

Sanchez, Alejandra [Escuela de Quimica, Universidad de Costa Rica, 2060 (Costa Rica); Centro de Electroquimica y Energia Quimica de la Universidad de Costa Rica (CELEQ), Universidad de Costa Rica, 2060 (Costa Rica); Gonzalez, Jerson [Escuela de Quimica, Universidad de Costa Rica, 2060 (Costa Rica); Garcia-Pineres, Alfonso [Escuela de Quimica, Universidad de Costa Rica, 2060 (Costa Rica); Centro de Investigacion en Biologia Celular y Molecular (CIBCM), Universidad de Costa Rica, 2060 (Costa Rica); Montero, Mavis L. [Escuela de Quimica, Universidad de Costa Rica, 2060 (Costa Rica); Centro de Electroquimica y Energia Quimica de la Universidad de Costa Rica (CELEQ), Universidad de Costa Rica, 2060 (Costa Rica); Centro de Ciencia e Ingenieria en Materiales (CICIMA), Universidad de Costa Rica, 2060 (Costa Rica)

2011-06-15

The properties of porous silicon make it an interesting material for biological applications. However, porous silicon is not an appropriate surface for cell growth. Surface modification is an alternative that could afford a bioactive material. In this work, we report a method to yield materials by modification of the porous silicon surface with hydroxyapatite of nanometric dimensions, produced using an electrochemical process and coated on macroporous silicon substrates by cathodic bias. The chemical nature of the calcium phosphate deposited on the substrates after the experimental process and the amount of cell growth on these surfaces were characterized. (copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

Augmenting the osseointegration of endoprostheses using laser-sintered porous collars: an in vivo study.

Science.gov (United States)

Mumith, A; Coathup, M; Chimutengwende-Gordon, M; Aston, W; Briggs, T; Blunn, G

2017-02-01

Massive endoprostheses rely on extra-cortical bone bridging (ECBB) to enhance fixation. The aim of this study was to investigate the role of selective laser sintered (SLS) porous collars in augmenting the osseointegration of these prostheses. The two novel designs of porous SLS collars, one with small pores (Ø700 μm, SP) and one with large pores (Ø1500 μm, LP), were compared in an ovine tibial diaphyseal model. Osseointegration of these collars was compared with that of a clinically used solid, grooved design (G). At six months post-operatively, the ovine tibias were retrieved and underwent radiological and histological analysis. Porous collars provided a significantly greater surface (p direct ingrowth of more bone and are better than current designs which rely on surface ongrowth and ECBB. Cite this article: Bone Joint J 2017;99-B:276-82. ©2017 The British Editorial Society of Bone & Joint Surgery.

Structural characteristics of porous hydroxyapatite coating on CaO-SiO{sub 2} system glass

Energy Technology Data Exchange (ETDEWEB)

Zhang Hongquan; Yan Yuhua; Li Shipu [Wuhan Univ. of Technology (China). Biomedical and Engineering Research Center

2001-07-01

Hydroxyapatite(HA) coated CaO-SiO{sub 2} system glass composites were prepared successfully by the hydrothermal coating method at the temperature of 250 to 350 C and at pH of 7 to 9. The microstructure and phase composition were identified by XRD, FT-IR, SEM, EPMA and TEM. It is shown that HA coating possessed a porous gradient construction in the interface; HA coating and glass substrate were tightly bonded by an obvious transition. HA coating had a well-distributed porous construction on the surface layer. The interface structure, phase composition and the stability of HA coated glass composites were related with its forming process. These kinds of structure will benefit to the interface bonging strength and bone bonding strength. (orig.)

IR-spectroscopical investigations on the glass structure of porous and sintered compacts of colloidal silica gels

Science.gov (United States)

Clasen, Rolf; Hornfeck, M.; Theiss, Wolfgang

1991-08-01

The forming and sintering of fumed silica powders is an interesting route for the preparation of large, very pure or doped silica glasses with a precise geometry. The processing from the shaping of a porous compact to the sintering of transparent silica glass can be successfully investigated with optical spectroscopy. As only the dielectric function DF (a dielectric function is the square root of the complex refractive index) characterizes the material, the vibrational bands were calculated from reflectance measurements. In compacts of fine particles, the topology cannot be neglected. Therefore, the models describing topological effects are briefly reviewed. With these model calculations it could be proven that new bands in the compacts and the significant shifts in the reflectance spectra during sintering are mainly caused by topological effects and that changes in the glass structure play only a secondary role.

Calcium silicate ceramic scaffolds toughened with hydroxyapatite whiskers for bone tissue engineering

International Nuclear Information System (INIS)

Feng, Pei; Wei, Pingpin; Li, Pengjian; Gao, Chengde; Shuai, Cijun; Peng, Shuping

2014-01-01

Calcium silicate possessed excellent biocompatibility, bioactivity and degradability, while the high brittleness limited its application in load-bearing sites. Hydroxyapatite whiskers ranging from 0 to 30 wt.% were incorporated into the calcium silicate matrix to improve the strength and fracture resistance. Porous scaffolds were fabricated by selective laser sintering. The effects of hydroxyapatite whiskers on the mechanical properties and toughening mechanisms were investigated. The results showed that the scaffolds had a uniform and continuous inner network with the pore size ranging between 0.5 mm and 0.8 mm. The mechanical properties were enhanced with increasing hydroxyapatite whiskers, reached a maximum at 20 wt.% (compressive strength: 27.28 MPa, compressive Young's modulus: 156.2 MPa, flexural strength: 15.64 MPa and fracture toughness: 1.43 MPa·m 1/2 ) and then decreased by addition of more hydroxyapatite whiskers. The improvement of mechanical properties was due to whisker pull-out, crack deflection and crack bridging. Moreover, the degradation rate decreased with the increase of hydroxyapatite whisker content. A layer of bone-like apatite was formed on the scaffold surfaces after being soaked in simulated body fluid. Human osteoblast-like MG-63 cells spread well on the scaffolds and proliferated with increasing culture time. These findings suggested that the calcium silicate scaffolds reinforced with hydroxyapatite whiskers showed great potential for bone regeneration and tissue engineering applications. - Highlights: • HA whiskers were incorporated into CS to improve the properties. • The scaffolds were successfully fabricated by SLS. • Toughening mechanisms was whisker pull-out, crack deflection and bridging. • The scaffolds showed excellent apatite forming ability

Calcium silicate ceramic scaffolds toughened with hydroxyapatite whiskers for bone tissue engineering

Energy Technology Data Exchange (ETDEWEB)

Feng, Pei [State Key Laboratory of High Performance Complex Manufacturing, Central South University, Changsha 410083, PR China, (China); Wei, Pingpin [Cancer Research Institute, Central South University, Changsha 410078 (China); Li, Pengjian; Gao, Chengde [State Key Laboratory of High Performance Complex Manufacturing, Central South University, Changsha 410083, PR China, (China); Shuai, Cijun, E-mail: shuai@csu.edu.cn [State Key Laboratory of High Performance Complex Manufacturing, Central South University, Changsha 410083, PR China, (China); Department of Regenerative Medicine and Cell Biology, Medical University of South Carolina, Charleston, SC 29425 (United States); Peng, Shuping, E-mail: shuping@csu.edu.cn [Cancer Research Institute, Central South University, Changsha 410078 (China)

2014-11-15

Calcium silicate possessed excellent biocompatibility, bioactivity and degradability, while the high brittleness limited its application in load-bearing sites. Hydroxyapatite whiskers ranging from 0 to 30 wt.% were incorporated into the calcium silicate matrix to improve the strength and fracture resistance. Porous scaffolds were fabricated by selective laser sintering. The effects of hydroxyapatite whiskers on the mechanical properties and toughening mechanisms were investigated. The results showed that the scaffolds had a uniform and continuous inner network with the pore size ranging between 0.5 mm and 0.8 mm. The mechanical properties were enhanced with increasing hydroxyapatite whiskers, reached a maximum at 20 wt.% (compressive strength: 27.28 MPa, compressive Young's modulus: 156.2 MPa, flexural strength: 15.64 MPa and fracture toughness: 1.43 MPa·m{sup 1/2}) and then decreased by addition of more hydroxyapatite whiskers. The improvement of mechanical properties was due to whisker pull-out, crack deflection and crack bridging. Moreover, the degradation rate decreased with the increase of hydroxyapatite whisker content. A layer of bone-like apatite was formed on the scaffold surfaces after being soaked in simulated body fluid. Human osteoblast-like MG-63 cells spread well on the scaffolds and proliferated with increasing culture time. These findings suggested that the calcium silicate scaffolds reinforced with hydroxyapatite whiskers showed great potential for bone regeneration and tissue engineering applications. - Highlights: • HA whiskers were incorporated into CS to improve the properties. • The scaffolds were successfully fabricated by SLS. • Toughening mechanisms was whisker pull-out, crack deflection and bridging. • The scaffolds showed excellent apatite forming ability.

Densification and grain growth during sintering of porous Ce0.9Gd0.1O1.95tape cast layers: A comprehensive study on heuristic methods

DEFF Research Database (Denmark)

Ni, De Wei; Schmidt, Cristine Grings; Teocoli, Francesca

2013-01-01

The sintering behavior of porous Ce0.9Gd0.1O1.95(CGO10) tape cast layers was systematically investigated to establish fundamental kinetic parameters associated to densification and grain growth. Densification and grain growth were characterized by a set of different methods to determine the domin...... and grain boundary mobility in the porous body was estimated around 10−18–10−16m3N−1s−1 at the investigated temperature range.© 2013 Elsevier Ltd. All rights reserved.......The sintering behavior of porous Ce0.9Gd0.1O1.95(CGO10) tape cast layers was systematically investigated to establish fundamental kinetic parameters associated to densification and grain growth. Densification and grain growth were characterized by a set of different methods to determine...... the dominant sintering mechanisms and kinetics, both in isothermal and at constant heating rate (iso-rate) conditions. Densification of porous CGO10 tape is thermally activated with typical activation energy which was estimated around 440–470 kJ mol−1. Grain growth showed similar thermal activation energy...

In vitro degradation of porous nano-hydroxyapatite/collagen/PLLA scaffold reinforced by chitin fibres

International Nuclear Information System (INIS)

Li Xiaoming; Feng Qingling; Cui Fuzhai

2006-01-01

In this paper, a novel porous scaffold for bone tissue engineering was prepared with nano-hydroxyapatite/collagen/Poly-L-lactic acid (PLLA) composite reinforced by chitin fibres. To enhance the strength of the scaffold further, PLLA was linked with chitin fibres by Dicyclohexylcarbodimide (DCC). The structures of the reinforced scaffold with and without linking were characterized by Scanning Electron Microscopy (SEM). The chemical characteristics of the chitin fibres with and without linking were evaluated by Fourier-transformed infrared (FTIR) spectroscopy. The mechanical performance during degradation in vitro was investigated. The results indicated that the nano-hydroxyapatite/collagen/PLLA composite reinforced by chitin fibres with linking kept better mechanical properties than that of the composite without linking. These results denoted that the stronger interfacial bonding strength of the scaffold with linking could decrease the degradation rate in vitro. The reinforced composite with the link-treatment can be severed as a scaffold for bone tissue engineering

Degradation and biocompatibility of porous nano-hydroxyapatite/polyurethane composite scaffold for bone tissue engineering

Energy Technology Data Exchange (ETDEWEB)

Dong Zhihong [Research Center for Nano-Biomaterials, Analytical and Testing Center, Sichuan University, Chengdu 610064 (China); Shanghai Institute of Ceramics, Chinese Academy of Sciences, 1295 Dingxi Road, Shanghai 200050 (China); Li Yubao, E-mail: nic7504@scu.edu.cn [Research Center for Nano-Biomaterials, Analytical and Testing Center, Sichuan University, Chengdu 610064 (China); Zou Qin [Research Center for Nano-Biomaterials, Analytical and Testing Center, Sichuan University, Chengdu 610064 (China)

2009-04-01

Porous scaffold containing 30 wt% nano-hydroxyapatite (n-HA) and 70 wt% polyurethane (PU) from castor oil was prepared by a foaming method and investigated by X-ray diffraction (XRD), Fourier transform infrared absorption (FTIR), scanning electron microscopy (SEM) techniques. The results show that n-HA particles disperse homogeneously in the PU matrix. The porous scaffold has not only macropores of 100-800 {mu}m in size but also a lot of micropores on the walls of macropores. The porosity and compressive strength of scaffold are 80% and 271 kPa, respectively. After soaking in simulated body fluid (SBF), hydrolysis and deposition partly occur on the scaffold. The biological evaluation in vitro and in vivo shows that the n-HA/PU scaffold is non-cytotoxic and degradable. The porous structure provides a good microenvironment for cell adherence, growth and proliferation. The n-HA/PU composite scaffold can be satisfied with the basic requirement for tissue engineering, and has the potential to be applied in repair and substitute of human menisci of the knee-joint and articular cartilage.

Quantification of iodine in porous hydroxyapatite matrices for application as radioactive sources in brachytherapy

Directory of Open Access Journals (Sweden)

Kássio André Lacerda

2007-07-01

Full Text Available In this study, non-radioactive iodine was incorporated in two types of biodegradable hydroxyapatite-based porous matrices (HA and HACL through impregnation process from sodium iodine aqueous solutions with varying concentrations (0.5 and 1.0 mol/L . The results revealed that both systems presented a high capacity of incorporating iodine into their matrices. The quantity of incorporated iodine was measured through Neutron Activation Analysis (NAA. The porous ceramic matrices based on hydroxyapatite demonstrated a great potential for uses in low dose rate (LDR brachytherapy.Materiais cerâmicos porosos à base de compostos de fosfatos de cálcio (CFC vêm sendo estudados e desenvolvidos para várias aplicações biomédicas tais como implantes, sistemas para liberação de drogas e fontes radioativas para braquiterapia. Dois tipos de matrizes porosas biodegradáveis de hidroxiapatita (HA e HACL foram avaliadas em termos da capacidade de incorporação de iodo em suas estruturas. Resultados revelaram que as matrizes porosas a base de hidroxiapatita apresentaram alta capacidade de incorporar iodo em sua estrutura. A quantidade de iodo foi mensurada através da técnica de Análise por Ativação Nêutronica (AAN. As matrizes cerâmicas porosas à base de hidroxiapatita demostraram ter grande potencial para aplicação em braquiterapia de baixa taxa de dose (LDR - Low Dose Rate.

The affect of densification and dehydroxylation on the mechanical properties of stoichiometric hydroxyapatite bioceramics

International Nuclear Information System (INIS)

Laasri, S.; Taha, M.; Laghzizil, A.; Hlil, E.K.; Chevalier, J.

2010-01-01

This paper reports the effects of processing densification on the mechanical properties of hydroxyapatite bioceramics. Densification of synthetic hydroxyapatite is conducted in the range 1000-1300 o C. X-ray diffraction and SEM microscopy are used to check the microstructure transformations. Vickers hardness, toughness and Young's modulus are analyzed versus the density and grain size. The sintering temperature and the particle size influence strongly the densification and the resulting mechanical properties. In addition, the critical sintering temperature appears around 1200 o C and the declined strength at the temperature up to 1200 o C is found sensitive to the dehydroxylation process of hydroxyapatite.

Preparation and Microstructure of Porous ZrB2 Ceramics Using Reactive Spark Plasma Sintering Method

Institute of Scientific and Technical Information of China (English)

YUAN Huiping; LI Junguo; SHEN Qiang; ZHANG Lianmeng

2015-01-01

Zirconium oxide (ZrO2) and boron carbide (B4C) were added to ZrB2 raw powders to prepare ZrB2 porous ceramics by reactive spark plasma sintering (RSPS). The reactions between ZrO2 and B4C which produce ZrB2 and gas (such as CO and B2O3) result in pore formation. X-Ray Diffraction results indicated that the products phase was ZrB2 and the reaction was completed after the RSPS process. The porosity could be controlled by changing the ratio of synthesized ZrB2 to raw ZrB2 powders. The porosity of porous ceramics with 20 wt% and 40 wt% synthsized ZrB2 are 0.185 and 0.222, respectivly. And dense ZrB2-SiC ceramic with a porosity of 0.057 was prepared under the same conditions for comparison. The pores were homogeneously distributed within the microstructure of the porous ceramics. The results indicate a promising method for preparing porous ZrB2-based ceramics.

Fabrication of novel biodegradable porous bone scaffolds based on amphiphilic hydroxyapatite nanorods

Energy Technology Data Exchange (ETDEWEB)

Zheng, Xiaoyan; Hui, Junfeng [Shaanxi Key Laboratory of Degradable Biomedical Materials, Shaanxi R& D Center of Biomaterials and Fermentation Engineering, School of Chemical and Engineering, Northwest University, Xi' an 710069, Shaanxi, PR China2 (China); Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of the Ministry of Education, Shaanxi Key Laboratory of Physico-Inorganic Chemistry, College of Chemistry & Materials Science, Northwest University, Xi' an 710069, Shaanxi (China); Li, Hui; Zhu, Chenhui [Shaanxi Key Laboratory of Degradable Biomedical Materials, Shaanxi R& D Center of Biomaterials and Fermentation Engineering, School of Chemical and Engineering, Northwest University, Xi' an 710069, Shaanxi, PR China2 (China); Hua, Xiufu, E-mail: hua_xiufu@163.com [Department of Scientific Research and Development, Tsinghua University, Beijing 100084 (China); Ma, Haixia, E-mail: mahx@nwu.edu.cn [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of the Ministry of Education, Shaanxi Key Laboratory of Physico-Inorganic Chemistry, College of Chemistry & Materials Science, Northwest University, Xi' an 710069, Shaanxi (China); Fan, Daidi, E-mail: fandaidi@nwu.edu.cn [Shaanxi Key Laboratory of Degradable Biomedical Materials, Shaanxi R& D Center of Biomaterials and Fermentation Engineering, School of Chemical and Engineering, Northwest University, Xi' an 710069, Shaanxi, PR China2 (China)

2017-06-01

This paper describes a new synthetic strategy and biological application for novel amphiphilic hydroxyapatite (HAp) nanorods. The prepared HAp nanorods were able to be dispersed in water, ethyl alcohol and cyclohexane. The co-anchoring of the multidentate ligands of PEG 20000 and hydrophobic oleic acid (OA) on the rods' surfaces endowed them with excellent amphibious properties. Utilizing amphiphilic HAp nanorods with excellent biocompatibility as the inorganic phase, human-like collagen (HLC) as the organic phase and natural genipin as the cross-linker, optimal HLC/HAp porous scaffolds (HLC: HAp = 1:4, w/w) were fabricated. The compression stress and three-point bending strength of the scaffolds with pore diameters of 150 to 200 μm reached approximately 3.4 MPa and 5.4 MPa, respectively, and their porosity was 77.35 ± 3.75%. Cytological tests showed that HLC/HAp scaffolds could contribute to cell proliferation and differentiation. The results indicated that these novel amphiphilic HAp nanorods can be expected to become recognized as an excellent inorganic material for the porous scaffolds used in repairing bone and related applications. - Highlights: • A simple and effective hydrothermal method was developed for preparing uniform HAp nanorods with amphiphilic surfaces. • The synthesized amphiphilic HAp nanorods could be dispersed in water, ethyl alcohol or cyclohexane. • The prepared HLC/HAp porous scaffolds had good mechanical properties, biocompatibility and osteoconductive etc.

Fabrication of novel biodegradable porous bone scaffolds based on amphiphilic hydroxyapatite nanorods

International Nuclear Information System (INIS)

Zheng, Xiaoyan; Hui, Junfeng; Li, Hui; Zhu, Chenhui; Hua, Xiufu; Ma, Haixia; Fan, Daidi

2017-01-01

This paper describes a new synthetic strategy and biological application for novel amphiphilic hydroxyapatite (HAp) nanorods. The prepared HAp nanorods were able to be dispersed in water, ethyl alcohol and cyclohexane. The co-anchoring of the multidentate ligands of PEG 20000 and hydrophobic oleic acid (OA) on the rods' surfaces endowed them with excellent amphibious properties. Utilizing amphiphilic HAp nanorods with excellent biocompatibility as the inorganic phase, human-like collagen (HLC) as the organic phase and natural genipin as the cross-linker, optimal HLC/HAp porous scaffolds (HLC: HAp = 1:4, w/w) were fabricated. The compression stress and three-point bending strength of the scaffolds with pore diameters of 150 to 200 μm reached approximately 3.4 MPa and 5.4 MPa, respectively, and their porosity was 77.35 ± 3.75%. Cytological tests showed that HLC/HAp scaffolds could contribute to cell proliferation and differentiation. The results indicated that these novel amphiphilic HAp nanorods can be expected to become recognized as an excellent inorganic material for the porous scaffolds used in repairing bone and related applications. - Highlights: • A simple and effective hydrothermal method was developed for preparing uniform HAp nanorods with amphiphilic surfaces. • The synthesized amphiphilic HAp nanorods could be dispersed in water, ethyl alcohol or cyclohexane. • The prepared HLC/HAp porous scaffolds had good mechanical properties, biocompatibility and osteoconductive etc.

The affect of densification and dehydroxylation on the mechanical properties of stoichiometric hydroxyapatite bioceramics

Energy Technology Data Exchange (ETDEWEB)

Laasri, S.; Taha, M. [Laboratoire de Thermodynamique Metallurgie et Rheologie des Materiaux, Universite Ibn Zohr, Faculte des sciences, BP8106 Cite Dakhla, Agadir (Morocco); Laghzizil, A., E-mail: laghzizi@fsr.ac.ma [Laboratoire de Chimie Physique Generale, Universite Mohammed V Rabat BP1014 (Morocco); Hlil, E.K. [Institut Neel MCMF, CNRS, BP 166, 38042 Grenoble Cedex 9 (France); Chevalier, J. [Universite de Lyon, INSA-Lyon, MATEIS UMR CNRS 5510, 20 Avenue Albert Einstein, 69621 Villeurbanne Cedex (France)

2010-10-15

This paper reports the effects of processing densification on the mechanical properties of hydroxyapatite bioceramics. Densification of synthetic hydroxyapatite is conducted in the range 1000-1300 {sup o}C. X-ray diffraction and SEM microscopy are used to check the microstructure transformations. Vickers hardness, toughness and Young's modulus are analyzed versus the density and grain size. The sintering temperature and the particle size influence strongly the densification and the resulting mechanical properties. In addition, the critical sintering temperature appears around 1200 {sup o}C and the declined strength at the temperature up to 1200 {sup o}C is found sensitive to the dehydroxylation process of hydroxyapatite.

Hydroxyapatite scaffolds processed using a TBA-based freeze-gel casting/polymer sponge technique.

Science.gov (United States)

Yang, Tae Young; Lee, Jung Min; Yoon, Seog Young; Park, Hong Chae

2010-05-01

A novel freeze-gel casting/polymer sponge technique has been introduced to fabricate porous hydroxyapatite scaffolds with controlled "designer" pore structures and improved compressive strength for bone tissue engineering applications. Tertiary-butyl alcohol (TBA) was used as a solvent in this work. The merits of each production process, freeze casting, gel casting, and polymer sponge route were characterized by the sintered microstructure and mechanical strength. A reticulated structure with large pore size of 180-360 microm, which formed on burn-out of polyurethane foam, consisted of the strut with highly interconnected, unidirectional, long pore channels (approximately 4.5 microm in dia.) by evaporation of frozen TBA produced in freeze casting together with the dense inner walls with a few, isolated fine pores (<2 microm) by gel casting. The sintered porosity and pore size generally behaved in an opposite manner to the solid loading, i.e., a high solid loading gave low porosity and small pore size, and a thickening of the strut cross section, thus leading to higher compressive strengths.

Microstructure and Mechanical Properties of Graphene-Reinforced Titanium Matrix/Nano-Hydroxyapatite Nanocomposites.

Science.gov (United States)

Li, Feng; Jiang, Xiaosong; Shao, Zhenyi; Zhu, Degui; Zhu, Minhao

2018-04-16

Biomaterial composites made of titanium and hydroxyapatite (HA) powder are among the most important biomedicalmaterials due to their good mechanical properties and biocompatibility. In this work, graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites were prepared by vacuum hot-pressing sintering. The microstructure and mechanical properties of graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites with different graphene content were systematically investigated. Microstructures of the nanocomposites were examined by X-ray diffraction (XRD), back scattered electron imaging (BSE), scanning electron microscope (SEM) equipped with energy dispersive spectrometer (EDS), electron probe microanalyzer (EPMA), and transmission electron microscope (TEM). The mechanical properties were determined from microhardness, shear strength, and compressive strength. Results showed that during the high-temperature sintering process, complex chemical reactions occurred, resulting in new phases of nucleation such as Ca₃(PO₄)₂, Ti x P y , and Ti₃O.The new phases, which easily dropped off under the action of external force, could hinder the densification of sintering and increase the brittleness of the nanocomposites. Results demonstrated that graphene had an impact on the microstructure and mechanical properties of the nanocomposites. Based on the mechanical properties and microstructure of the nanocomposites, the strengthening and fracture mechanisms of the graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites with different graphene content were analyzed.

Microstructure and Mechanical Properties of Graphene-Reinforced Titanium Matrix/Nano-Hydroxyapatite Nanocomposites

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Feng Li

2018-04-01

Full Text Available Biomaterial composites made of titanium and hydroxyapatite (HA powder are among the most important biomedicalmaterials due to their good mechanical properties and biocompatibility. In this work, graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites were prepared by vacuum hot-pressing sintering. The microstructure and mechanical properties of graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites with different graphene content were systematically investigated. Microstructures of the nanocomposites were examined by X-ray diffraction (XRD, back scattered electron imaging (BSE, scanning electron microscope (SEM equipped with energy dispersive spectrometer (EDS, electron probe microanalyzer (EPMA, and transmission electron microscope (TEM. The mechanical properties were determined from microhardness, shear strength, and compressive strength. Results showed that during the high-temperature sintering process, complex chemical reactions occurred, resulting in new phases of nucleation such as Ca3(PO42, TixPy, and Ti3O.The new phases, which easily dropped off under the action of external force, could hinder the densification of sintering and increase the brittleness of the nanocomposites. Results demonstrated that graphene had an impact on the microstructure and mechanical properties of the nanocomposites. Based on the mechanical properties and microstructure of the nanocomposites, the strengthening and fracture mechanisms of the graphene-reinforced titanium matrix/nano-hydroxyapatite nanocomposites with different graphene content were analyzed.

Novel synthesis and characterization of an AB-type carbonate-substituted hydroxyapatite.

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Gibson, Iain R; Bonfield, William

2002-03-15

A novel synthesis route has been developed to produce a high-purity mixed AB-type carbonate-substituted hydroxyapatite (CHA) with a carbonate content that is comparable to the type and level observed in bone mineral. This method involves the aqueous precipitation in the presence of carbonate ions in solution of a calcium phosphate apatite with a Ca/P molar ratio greater than the stoichiometric value of 1.67 for hydroxyapatite (HA). The resulting calcium-rich carbonate-apatite is sintered/heat-treated in a carbon dioxide atmosphere to produce a single-phase, crystalline carbonate-substituted hydroxyapatite. In contrast to previous methods for producing B- or AB-type carbonate-substituted hydroxyapatites, no sodium or ammonium ions, which would be present in the reaction mixture from the sodium or ammonium carbonates commonly used as a source of carbonate ions, were present in the final product. The chemical and phase compositions of the carbonate-substituted hydroxyapatite was characterized by X-ray fluorescence and X-ray diffraction, respectively, and the level and nature of the carbonate substitution were studied using C-H-N analysis and Fourier transform infrared spectroscopy, respectively. The carbonate substitution improves the densification of hydroxyapatite and reduces the sintering temperature required to achieve near-full density by approximately 200 degrees C compared to stoichiometric HA. Initial studies have shown that these carbonate-substituted hydroxyapatites have improved mechanical and biologic properties compared to stoichiometric hydroxyapatite. Copyright 2001 John Wiley & Sons, Inc. J Biomed Mater Res 59: 697-708, 2002

Porous 45S5 Bioglass®-based scaffolds using stereolithography: Effect of partial pre-sintering on structural and mechanical properties of scaffolds.

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Thavornyutikarn, Boonlom; Tesavibul, Passakorn; Sitthiseripratip, Kriskrai; Chatarapanich, Nattapon; Feltis, Bryce; Wright, Paul F A; Turney, Terence W

2017-06-01

Scaffolds made from 45S5 Bioglass® ceramic (BG) show clinical potential in bone regeneration due to their excellent bioactivity and ability to bond to natural bone tissue. However, porous BG scaffolds are limited by their mechanical integrity and by the substantial volume contractions occurring upon sintering. This study examines stereolithographic (SLA) methods to fabricate mechanically robust and porous Bioglass®-based ceramic scaffolds, with regular and interconnected pore networks and using various computer-aided design architectures. It was found that a diamond-like (DM) architecture gave scaffolds the most controllable results without any observable closed porosity in the fired scaffolds. When the pore dimensions of the DM scaffolds of the same porosity (~60vol%) were decreased from 700 to 400μm, the compressive strength values increased from 3.5 to 6.7MPa. In addition, smaller dimensional shrinkage could be obtained by employing partially pre-sintered bioglass, compared to standard 45S5 Bioglass®. Scaffolds derived from pre-sintered bioglass also showed marginally improved compressive strength. Copyright © 2017 Elsevier B.V. All rights reserved.

Porous Polyethylene Coated with Functionalized Hydroxyapatite Particles as a Bone Reconstruction Material

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H. Fouad

2018-03-01

Full Text Available In this study, porous polyethylene scaffolds were examined as bone substitutes in vitro and in vivo in critical-sized calvarial bone defects in transgenic Sprague-Dawley rats. A microscopic examination revealed that the pores appeared to be interconnected across the material, making them suitable for cell growth. The creep recovery behavior of porous polyethylene at different loads indicated that the creep strain had two main portions. In both portions, strain increased with increased applied load and temperature. In terms of the thermographic behavior of the material, remarkable changes in melting temperature and heat fusion were revealed with increased the heating rates. The tensile strength results showed that the material was sensitive to the strain rate and that there was adequate mechanical strength to support cell growth. The in vitro cell culture results showed that human bone marrow mesenchymal stem cells attached to the porous polyethylene scaffold. Calcium sulfate–hydroxyapatite (CS–HA coating of the scaffold not only improved attachment but also increased the proliferation of human bone marrow mesenchymal stem cells. In vivo, histological analysis showed that the study groups had active bone remodeling at the border of the defect. Bone regeneration at the border was also evident, which confirmed that the polyethylene acted as an osteoconductive bone graft. Furthermore, bone formation inside the pores of the coated polyethylene was also noted, which would enhance the process of osteointegration.

Effect of precursor concentration and spray pyrolysis temperature upon hydroxyapatite particle size and density.

Science.gov (United States)

Cho, Jung Sang; Lee, Jeong-Cheol; Rhee, Sang-Hoon

2016-02-01

In the synthesis of hydroxyapatite powders by spray pyrolysis, control of the particle size was investigated by varying the initial concentration of the precursor solution and the pyrolysis temperature. Calcium phosphate solutions (Ca/P ratio of 1.67) with a range of concentrations from 0.1 to 2.0 mol/L were prepared by dissolving calcium nitrate tetrahydrate and diammonium hydrogen phosphate in deionized water and subsequently adding nitric acid. Hydroxyapatite powders were then synthesized by spray pyrolysis at 900°C and at 1500°C, using these calcium phosphate precursor solutions, under the fixed carrier gas flow rate of 10 L/min. The particle size decreased as the precursor concentration decreased and the spray pyrolysis temperature increased. Sinterability tests conducted at 1100°C for 1 h showed that the smaller and denser the particles were, the higher the relative densities were of sintered hydroxyapatite disks formed from these particles. The practical implication of these results is that highly sinterable small and dense hydroxyapatite particles can be synthesized by means of spray pyrolysis using a low-concentration precursor solution and a high pyrolysis temperature under a fixed carrier gas flow rate. © 2015 Wiley Periodicals, Inc.

Intrinsic Osteoinductivity of Porous Titanium Scaffold for Bone Tissue Engineering

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Maryam Tamaddon

2017-01-01

Full Text Available Large bone defects and nonunions are serious complications that are caused by extensive trauma or tumour. As traditional therapies fail to repair these critical-sized defects, tissue engineering scaffolds can be used to regenerate the damaged tissue. Highly porous titanium scaffolds, produced by selective laser sintering with mechanical properties in range of trabecular bone (compressive strength 35 MPa and modulus 73 MPa, can be used in these orthopaedic applications, if a stable mechanical fixation is provided. Hydroxyapatite coatings are generally considered essential and/or beneficial for bone formation; however, debonding of the coatings is one of the main concerns. We hypothesised that the titanium scaffolds have an intrinsic potential to induce bone formation without the need for a hydroxyapatite coating. In this paper, titanium scaffolds coated with hydroxyapatite using electrochemical method were fabricated and osteoinductivity of coated and noncoated scaffolds was compared in vitro. Alizarin Red quantification confirmed osteogenesis independent of coating. Bone formation and ingrowth into the titanium scaffolds were evaluated in sheep stifle joints. The examinations after 3 months revealed 70% bone ingrowth into the scaffold confirming its osteoinductive capacity. It is shown that the developed titanium scaffold has an intrinsic capacity for bone formation and is a suitable scaffold for bone tissue engineering.

Hyper-elastic modeling and mechanical behavior investigation of porous poly-D-L-lactide/nano-hydroxyapatite scaffold material.

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Han, Quan Feng; Wang, Ze Wu; Tang, Chak Yin; Chen, Ling; Tsui, Chi Pong; Law, Wing Cheung

2017-07-01

Poly-D-L-lactide/nano-hydroxyapatite (PDLLA/nano-HA) can be used as the biological scaffold material in bone tissue engineering as it can be readily made into a porous composite material with excellent performance. However, constitutive modeling for the mechanical response of porous PDLLA/nano-HA under various stress conditions has been very limited so far. In this work, four types of fundamental compressible hyper-elastic constitutive models were introduced for constitutive modeling and investigation of mechanical behaviors of porous PDLLA/nano-HA. Moreover, the unitary expressions of Cauchy stress tensor have been derived for the PDLLA/nano-HA under uniaxial compression (or stretch), biaxial compression (or stretch), pure shear and simple shear load by using the theory of continuum mechanics. The theoretical results determined from the approach based on the Ogden compressible hyper-elastic constitutive model were in good agreement with the experimental data from the uniaxial compression tests. Furthermore, this approach can also be used to predict the mechanical behaviors of the porous PDLLA/nano-HA material under the biaxial compression (or stretch), pure shear and simple shear. Copyright © 2017 Elsevier Ltd. All rights reserved.

Characterization of hydroxyapatite substituted with silicon

International Nuclear Information System (INIS)

Silva, H.M. da; Soares, G.A.; Mateescu, M.; Anselme, K.; Palard, M.; Champion, E.

2009-01-01

Incorporation of silicon (Si) ions into hydroxyapatite structure (HA) influences on physical, chemical and physiological properties. Some studies reported the improved bioactivity Si substitution, and it also accelerates the biomineralization process. The main objective of this work is to characterize stoichiometric hydroxyapatite and hydroxyapatite substituted with 1.13% in weight of Si (SiHA) using a wet precipitation method followed by a heat treatment. SEM/EDS, AFM, DRX and FTIR analyses were used to characterize the samples. EDS and FTIR results confirmed the presence of Si. Silicon induces small changes on crystal structure of HA, not detected on X-ray diffraction patterns of sintered tablets of SiHA and HA. No secondary phases were observed, that indicates the Si had entered the HA lattice. (author)

Obtention of hydroxyapatite submicrometric of bovine origin by vibratory grinding for rapid prototyping

International Nuclear Information System (INIS)

Meira, C.R.; Purquerio, B.M.; Fortulan, C.A.

2011-01-01

Submicron bovine hydroxyapatite was obtained for rapid prototyping. Hydroxyapatite structure originated from bovine mineral bone has great importance among the biomaterials and biocompatibility due to its great similarity with the human bone structure. This study aims to obtain powder for manufacture by rapid prototyping of scaffolds. This technique manufacture requires highly reactive powders to compensate for the absence of pressure forming. Hydroxyapatite was milled in a ball mill and vibratory mill, and analyzed for their average equivalent spherical diameter and surface area. Test specimens were isostatically pressed at 100 MPa and machined into cylindrical test specimens. These specimens were sintered at several temperatures to determine the optimal sintering temperature based on densification and chemistry stability. In grinding ball mill was obtained particles of equivalent diameter of 0.74 micron in vibratory mill of 0.46 micrometers. An average flexural strength of 100 MPa and 99,8% of real density was attained for the sample sintered at 1300 deg C/2h, signaling potential for use in rapid prototyping. (author)

In situ ring-opening polymerization of hydroxyapatite/poly (ethylene ...

Indian Academy of Sciences (India)

2016-08-26

Aug 26, 2016 ... Hydroxyapatite/poly(ethylene adipate)--poly(ethylene terephthalate) biomaterials (HAp/PEA--PET) have been prepared by ring opening polymerization (ROP) of cyclic oligo(ethylene adipate)--oligo(ethylene terephthalate) (C-OEA--C-OET) in the porous hydroxyapatite (HAp) scaffolds at 250 ...

Development of porous structure simulator for multi-scale simulation of irregular porous catalysts

International Nuclear Information System (INIS)

Koyama, Michihisa; Suzuki, Ai; Sahnoun, Riadh; Tsuboi, Hideyuki; Hatakeyama, Nozomu; Endou, Akira; Takaba, Hiromitsu; Kubo, Momoji; Del Carpio, Carlos A.; Miyamoto, Akira

2008-01-01

Efficient development of highly functional porous materials, used as catalysts in the automobile industry, demands a meticulous knowledge of the nano-scale interface at the electronic and atomistic scale. However, it is often difficult to correlate the microscopic interfacial interactions with macroscopic characteristics of the materials; for instance, the interaction between a precious metal and its support oxide with long-term sintering properties of the catalyst. Multi-scale computational chemistry approaches can contribute to bridge the gap between micro- and macroscopic characteristics of these materials; however this type of multi-scale simulations has been difficult to apply especially to porous materials. To overcome this problem, we have developed a novel mesoscopic approach based on a porous structure simulator. This simulator can construct automatically irregular porous structures on a computer, enabling simulations with complex meso-scale structures. Moreover, in this work we have developed a new method to simulate long-term sintering properties of metal particles on porous catalysts. Finally, we have applied the method to the simulation of sintering properties of Pt on alumina support. This newly developed method has enabled us to propose a multi-scale simulation approach for porous catalysts

Improved osteoblasts growth on osteomimetic hydroxyapatite/BaTiO_3 composites with aligned lamellar porous structure

International Nuclear Information System (INIS)

Liu, Beilei; Chen, Liangjian; Shao, Chunsheng; Zhang, Fuqiang; Zhou, Kechao; Cao, Jun; Zhang, Dou

2016-01-01

Osteoblasts growing into bone substitute is an important step of bone regeneration. This study prepared porous hydroxyapatite (HA)/BaTiO_3 piezoelectric composites with porosity of 40%, 50% and 60% by ice-templating method. Effects of HA/BaTiO_3 composites with different porosities, with and without polarizing treatment on adhesion, proliferation and differentiation of osteoblasts were investigated in vitro. Results revealed that cell densities of the porous groups were significantly higher than those of the dense group (p 0.05). The absence of mechanical loading on the polarized samples may account for this. The results indicated that hierarchically porous HA/BaTiO_3 played a favorable part in osteoblasts proliferation, differentiation and adhesion process and is a promising bone substitute material. - Graphical abstract: Aligned porous structure of HA/BaTiO_3 piezoelectric composites prepared by ice-templating method was similar to the lamellar Haversian system in bone tissue. When co-cultured with human osteosarcoma cells (MG63), porous HA/BaTiO_3 composites exhibited remarkable biological activity in promoting proliferation, differentiation and adhesion of MG63 cells. - Highlights: • The aligned porous structure of HA/BaTiO_3 composite was similar to the lamellar Haversian system in bone tissue. • The piezoelectric d_3_3 coefficient of HA/BaTiO_3 with porosity of 50% was 5.0 pC/N, much higher than that of natural bone. • HA/BaTiO_3 with porosity of 50% promoted proliferation, differentiation and adhesion of MG63 cells remarkably.

Synthesis, characterization and cell behavior of fluoridated hydroxyapatite

Science.gov (United States)

Qu, Haibo

Fluorine-containing hydroxyapatite (Ca5(PO4) 3(OH)1-xFx FHA), where F- partially replaces OH- in hydroxyapatite (HA), is recognized as a possible biomaterial for bone and tooth implants and gaining attention in the last several years as a possible alternative to HA. In this study, FHA powders were synthesized through a pH-cycling method. It was discovered that fluorine incorporation increased with the fluorine content in the initial solution and the number of pH cycles employed. A relatively low fluorine incorporation efficiency, ˜60%, was attained for most of the FHA samples. The short time of stay at each pH cycle and the limited number of cycles used are believed to be the main reasons of the low fluorine incorporation into the apatite structure. It was also revealed that the FHA particles produced by the pH-cycling method were inhomogeneous. They were a mixture of hydroxyapatite and F-rich apatite (or FA) particles. The mechanisms of incorporation of fluorine ions into hydroxyapatite by a pH cyclicing method were studied using TEM, XRD and fluorine measurement. Instead of forming laminated structures as reported by other research groups, a mixture of nano-sized F-rich apatite (FHA) and hydroxyapatite (HA) particles were obtained using the pH-cyclicing method. After calcination, these FHA particles were homogenized and became single phased FHA. The effect of fluorine content, preparing method, and sintering temperature on both the bulk density and biaxial flexural strength of sintered FHA was studied. Both uniaxially pressed un-milled (UPU) and cold isostatically pressed milled (IPM) FHA discs were sintered at temperatures between 1200˜400°C at an interval of 100°C. It was found that the fluorine content had a significant impact on the sintering behavior, densification, and mechanical properties of FHA discs. A close correlation between the sintered density and biaxial flexural strength of the specimens was revealed, where the biaxial flexural strength

In situ ring-opening polymerization of hydroxyapatite/poly (ethylene ...

Indian Academy of Sciences (India)

Hydroxyapatite/poly(ethylene adipate)--poly(ethylene terephthalate) biomaterials (HAp/PEA--PET) have been prepared by ring opening polymerization (ROP) of cyclic oligo(ethylene adipate)--oligo(ethylene terephthalate) (C-OEA--C-OET) in the porous hydroxyapatite (HAp) scaffolds at 250 °C for 24 h under ...

Synthesis of dense nano cobalt-hydroxyapatite by modified electroless deposition technique

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Mohd Zaheruddin, K., E-mail: zaheruddin@unimap.edu.my; Rahmat, A., E-mail: azmirahmat@unimap.edu.my; Shamsul, J. B., E-mail: sbaharin@unimap.edu.my; Mohd Nazree, B. D., E-mail: nazree@unimap.edu.my; Aimi Noorliyana, H., E-mail: aimiliyana@unimap.edu.my [School of Materials Engineering, Universiti Malaysia Perlis, Kompleks Pusat Pengajian Jejawi Universiti Malaysia Perlis, Taman Muhibbah, Jejawi 02600 Arau Perlis (Malaysia)

2016-07-19

Cobalt-hydroxyapatite (Co-HA) composites was successfully prepared by simple electroless deposition process of Co on the surface of hydroxyapatite (HA) particles. Co deposition was carried out in an alkaline bath with sodium hypophosphite as a reducing agent. The electroless process was carried out without sensitization and activation steps. The deposition of Co onto HA was characterized by scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). The Co-HA composite powder was compacted and sintered at 1250°C. The Co particles were homogeneously dispersed in the HA matrix after sintering and the mechanical properties of composites was enhanced to 100 % with 3 % wt Co and gradually decreased at higher Co content.

Development and Characterization of Sr-Containing Glass-Ceramic Composites Based on Biogenic Hydroxyapatite

Science.gov (United States)

Kuda, Oleksii; Pinchuk, Nataliia; Bykov, Oleksandr; Tomila, Tamara; Olifan, Olena; Golovkova, Maryna

2018-05-01

Composite materials based on hydroxyapatite are widely used for bone tissue engineering. There is evidence of a positive effect of the presence of strontium in osteoplastic materials in the case of a Ca/Sr certain ratio. To examine the effect of the addition of Sr2+, a study was made by introducing it into the material composition based on biogenic hydroxyapatite and sodium borosilicate glass (50/50% wt.). The strontium was introduced into the composition in an amount of 1% wt. Composite materials were obtained at final sintering temperatures of 780 °C and a sintering time of 1 h. The effect of additions of glass phase and strontium affect changes in the crystal lattice of biogenic hydroxyapatite was investigated with the help of X-ray phase analysis, IR spectroscopy. Also the behavior of composites in vitro in physiological solution was studied.

Pressureless sintering and gas flux properties of porous ceramic membranes for gas applications

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David O. Obada

Full Text Available The preparation and characterization of kaolin based ceramic membranes using styrofoam (STY and sawdust (SD as pore formers have been prepared by mechano-chemical synthesis using pressureless sintering technique with porogen content between (0–20 wt% by die pressing. Pellets were fired at 1150 °C and soaking time of 4 h. The membranes cast as circular disks were subjected to characterization studies to evaluate the effect of the sintering temperature and pore former content on porosity, density, water absorption and mechanical strength. Obtained membranes show effective porosity with maximum at about 43 and 47% respectively for membranes formulated with styrofoam and sawdust porogens but with a slightly low mechanical strength that does not exceed 19 MPa. The resultant ceramic bodies show a fine porous structure which is mainly caused by the volatilization of the porogens. The fabricated membrane exhibited high N2 gas flux, hence, these membranes can be considered as efficient for potential application for gas separation by reason of the results shown in the gas flux tests. Keywords: Porosity, Pore formers, Kaolin, Physico-mechanical properties, Gas separation, Gas flux

Development of revolutionizing biomaterials substituting various mammalian organs by means of sintered bioceramics

Energy Technology Data Exchange (ETDEWEB)

Ueda, T. [West Saitama National Central Hospital, Tokorozawa (Japan); Hirota, K. [National Inst. for Research in Inorganic Materials Tsukuba, Ibaraki (Japan); Nishihara, K. [Tokyo Univ. (Japan). Dept. of Oral Surgery

2001-07-01

Development of biomaterials substituting various mammalian organs can be carried out by means of experimental evolutionary studies using collagen -hydroxyapatite composite, derived from adult cattle. The revolution of the tissue-immune system can be studies by compound-ceramics of collagen-hydroxyapatite composite. Collagen-hydroxyapatite composite was sintered by high-pressure technique using collagen extracted from cattle skin, which had antigenicity. Artificial bone marrow chambers were fabricated with the sintered collagen-hydroxyapatite composite. Experimental evolutionary studies using mammals (dogs) and chondrichthyes (sharks) were carried out implanting the chambers into their muscles. The result showed that around the collagen composed chambers implanted into dorsal muscle of dogs, marked cell differentiation as well as dedifferentiation with atypia could be observed, which resembled a part the digestive tract of intestine histologically. Around the chambers implanted into dorsal muscle of sharks hemopoietic nests could be observed, which were quite similar to those induced by the chambers of conventionally sintered hydroxyapatite. Hemopoiesis and osteoid formation 4 months after surgery were observed around the collagen-apatite chamber implanted in the shark muscle as well as in upper site of vertebral cartilage of the spinal cord. No bone marrow in the cartilaginous tissue in upper site of the spinal cord is evident in control sharks. Xenotransplantation of skin, i.e., skin grafts between sharks of different kinds of species, as well as between sharks and xenopus (amphibian), sharks and mammals (rat) are carried out. All of them are successful and chimera placoids between them are developed. After that, the author successfully carried out xenotransplantation of various organs of chondrichthyes into those of dogs. (orig.)

Study of sintering on Mg-Zn-Ca alloy system

Science.gov (United States)

Annur, Dhyah; Lestari, Franciska P.; Erryani, Aprilia; Kartika, Ika

2018-05-01

Magnesium and its alloy have gained a lot of interest to be used in biomedical application due to its biodegradable and biocompatible properties. In this study, sintering process in powder metallurgy was chosen to fabricatenonporous Mg-6Zn-1Ca (in wt%) alloy and porous Mg-6Zn-1Ca-10 Carbamide alloy. For creating porous alloy, carbamide (CO(NH2)2 was added to alloy system as the space holder to create porous structure material. Effect of the space holder addition and sintering temperature on porosity, phase formation, mechanical properties, and corrosion properties was observed. Sintering process was done in a tube furnace under Argon atmosphere in for 5 hours. The heat treatment was done in two steps; heated up at 250 °C for 4 hours to decompose spacer particle, followed by heated up at 580 °C or 630 °C for 5 hours. The porous structure of the resulted alloys was examined using Scanning Electron Microscope (SEM), while the phase formation was characterized by X-ray diffraction (XRD) analysis. Mechanical properties were examined using compression testing. From this study, increasing sintering temperature up to 630 °C reduced the mechanical properties of Mg-Zn-Ca alloy.

Obtaining of ceramics biphasic dense and porous

International Nuclear Information System (INIS)

Pallone, E.M.J.A.; Rigo, E.C.S.; Fraga, A.F.

2010-01-01

Among the bioceramic hydroxyapatite (HAP) and beta-tricalcium phosphate (beta-TCP) are materials commonly used in biomedical field. Their combined properties result in a material with absorbable and at the same time with bioactive surface. Called biphasic ceramics such materials respond more quickly when exposed to physiological environment. In this work, powders of HAP/beta-TCP were obtained by chemical precipitation. After obtaining the post-phase was added at a ratio of 0, 15% and 30w% aqueous solutions of corn starch in order to obtain porous bodies. After mixing the resulting solutions were dried, resigned in tablet form and sintered at 1300 deg C. The initial powder was characterized by X-ray diffraction with Rietveld refinement to quantify the phases present. Bodies-of-evidence has been characterized by calculating the bulk density, X-ray diffraction (XRD), scanning electron microscopy and diametral compression. (author)

Processing and characterization of glass reinforced biogenic hydroxyapatite composites with ferromagnetic additives

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Nataliya Pinchuk

2008-06-01

Full Text Available Biogenic hydroxyapatite-glass composites, with addition of up to 2 wt.% of Fe or Fe3O4, were fabricated from biogenic hydroxyapatite powder and four types of reinforcing glasses by sintering under different conditions. It has been established that the relative density, mechanical and magnetic properties of the prepared composites depend on the composition and sintering conditions. The composites with 1 wt.% Fe or Fe3O4 sintered at 500°С in vacuum have a magnetic susceptibility of 2–3·10-3 cm3/g. This parameter decreases to 0.858·10-3 cm3/g for the specimens with 1 wt.% additives sintered at 800°С in vacuum and to 0.27–1.3·10-3cm3/g for the specimens with 2 wt.% additives sintered at 500°С under the usual atmospheric conditions. The magnetic susceptibility for the specimens with 2 wt.% additives sintered at 780°С under the same atmospheric conditions decreases to 0.24–1.25·10-6 cm3/g. These ferromagnetic additives influence the degradation rate in vitro within the first 40 min of the composite soaking. Short-term treatment of specimens by the magnetic field leads to an increase in the initial degradation rate, but insignificantly influences it within more prolonged soaking.

The usability of ark clam shell (Anadara granosa) as calcium precursor to produce hydroxyapatite nanoparticle via wet chemical precipitate method in various sintering temperature.

Science.gov (United States)

Khiri, Mohammad Zulhasif Ahmad; Matori, Khamirul Amin; Zainuddin, Norhazlin; Abdullah, Che Azurahanim Che; Alassan, Zarifah Nadakkavil; Baharuddin, Nur Fadilah; Zaid, Mohd Hafiz Mohd

2016-01-01

This paper reported the uses of ark clam shell calcium precursor in order to form hydroxyapatite (HA) via the wet chemical precipitation method. The main objective of this research is to acquire better understanding regarding the effect of sintering temperature in the fabrication of HA. Throughout experiment, the ratio of Ca:P were constantly controlled, between 1.67 and 2.00. The formation of HA at these ratio was confirmed by means of energy-dispersive X-ray spectroscopy analysis. In addition, the effect of sintering temperature on the formation of HA was observed using X-ray diffraction analysis, while the structural and morphology was determined by means of field emission scanning electron microscopy. The formation of HA nanoparticle was recorded (~35-69 nm) in the form of as-synthesize HA powder. The bonding compound appeared in the formation of HA was carried out using Fourier transform infrared spectroscopy such as biomaterials that are expected to find potential applications in orthopedic and biomedical industries .

Metrology of nanosize biopowders using porous silicon surface

International Nuclear Information System (INIS)

Zhuravel', L.V.; Latukhina, N.V.; Pisareva, E.V.; Vlasov, M.Yu.; Volkov, A.V.; Volodkin, B.O.

2008-01-01

Powders of hydroxyapatite deposited on porous silicon surface were investigated by TEM and STM methods. Thickness of porous lay was 1-100 micrometers; porous diameter was 0.01-10 micrometers. Images of porous silicon surface with deposited particles give possibility to estimate particles size and induce that only proportionate porous diameter particles have good adhesion to porous silicon surface.

MRI of orbital hydroxyapatite implants

International Nuclear Information System (INIS)

Flanders, A.E.; De Potter P.; Rao, V.M.; Tom, B.M.; Shields, C.L.; Shields, J.A.

1996-01-01

Our aim was to use MRI for the postsurgical assessment of a new form of integrated orbital implant composed of a porous calcium phosphate hydroxyapatite substrate. We studied ten patients 24-74 years of age who underwent enucleation and implantation of a hydroxyapatite ball; 5-13 months after surgery, each patient was examined by spin-echo MRI, with fat suppression and gadolinium enhancement. Fibrovascular ingrowth was demonstrated in all ten patients as areas of enhancement at the periphery of the hydroxyapatite sphere that extended to the center to a variable degree. The radiologist should aware of the MRI appearances of the coralline hydroxyapatite orbital implant since it is now widely used following enucleation. MRI is a useful means to determine successful incorporation of the substrate into the orbital tissues. The normal pattern of contrast enhancement should not be mistaken for recurrent tumor or infection. (orig.)

Joining of porous silicon carbide bodies

Science.gov (United States)

Bates, Carl H.; Couhig, John T.; Pelletier, Paul J.

1990-05-01

A method of joining two porous bodies of silicon carbide is disclosed. It entails utilizing an aqueous slip of a similar silicon carbide as was used to form the porous bodies, including the sintering aids, and a binder to initially join the porous bodies together. Then the composite structure is subjected to cold isostatic pressing to form a joint having good handling strength. Then the composite structure is subjected to pressureless sintering to form the final strong bond. Optionally, after the sintering the structure is subjected to hot isostatic pressing to further improve the joint and densify the structure. The result is a composite structure in which the joint is almost indistinguishable from the silicon carbide pieces which it joins.

Effect of highly dispersed yttria addition on thermal stability of hydroxyapatite

International Nuclear Information System (INIS)

Parente, P.; Savoini, B.; Ferrari, B.; Monge, M.A.; Pareja, R.; Sanchez-Herencia, A.J.

2013-01-01

The capability of the colloidal method to produce yttria (Y 2 O 3 ) dispersed hydroxyapatite (HA) has been investigated as an alternative method to the conventional method of mechanical mixing and sintering for developing HA-based materials that could exhibit controllable and enhanced functional properties. A water based colloidal route to produce HA materials with highly dispersed Y 2 O 3 has been applied, and the effect of 10 wt.% Y 2 O 3 addition to HA investigated by thermal analysis, X-ray diffraction and Fourier transform infrared spectroscopy. These measurements evidence a remarkable effect of this Y 2 O 3 addition on decomposition mechanisms of synthetic HA. Results show that incorporation of Y 2 O 3 as dispersed second phase is beneficial because it hinders the decomposition mechanisms of HA into calcium phosphates. This retardation will allow the control of the sintering conditions for developing HA implants with improved properties. Besides, substitution of Ca 2+ with Y 3+ ions appears to promote the formation of OH − vacancies, which could improve the conductive properties of HA favorable to osseointegration. - Highlights: ► We reveal the influence of Y 2 O 3 on thermal stability of hydroxyapatite. ► Incorporation of Y 2 O 3 delays decomposition of hydroxyapatite to calcium phosphates. ► Addition of Y 2 O 3 enables sintering conditions more favorable to the densification.

Injectable porous nano-hydroxyapatite/chitosan/tripolyphosphate scaffolds with improved compressive strength for bone regeneration

Energy Technology Data Exchange (ETDEWEB)

Uswatta, Suren P.; Okeke, Israel U. [Department of Bioengineering, The University of Toledo, Toledo, OH 43614 (United States); Jayasuriya, Ambalangodage C., E-mail: a.jayasuriya@utoledo.edu [Department of Bioengineering, The University of Toledo, Toledo, OH 43614 (United States); Department of Orthopaedic Surgery, The University of Toledo, Toledo, OH 43614 (United States)

2016-12-01

In this study we have fabricated porous injectable spherical scaffolds using chitosan biopolymer, sodium tripolyphosphate (TPP) and nano-hydroxyapatite (nHA). TPP was primarily used as an ionic crosslinker to crosslink nHA/chitosan droplets. We hypothesized that incorporating nHA into chitosan could support osteoconduction by emulating the mineralized cortical bone structure, and improve the Ultimate Compressive Strength (UCS) of the scaffolds. We prepared chitosan solutions with 0.5%, 1% and 2% (w/v) nHA concentration and used simple coacervation and lyophilization techniques to obtain spherical scaffolds. Lyophilized spherical scaffolds had a mean diameter of 1.33 mm (n = 25). Further, portion from each group lyophilized scaffolds were soaked and dried to obtain Lyophilized Soaked and Dried (LSD) scaffolds. LSD scaffolds had a mean diameter of 0.93 mm (n = 25) which is promising property for the injectability. Scanning Electron Microscopy images showed porous surface morphology and interconnected pore structures inside the scaffolds. Lyophilized and LSD scaffolds had surface pores < 10 and 2 μm, respectively. 2% nHA/chitosan LSD scaffolds exhibited UCS of 8.59 MPa compared to UCS of 2% nHA/chitosan lyophilized scaffolds at 3.93 MPa. Standardize UCS values were 79.98 MPa and 357 MPa for 2% nHA/chitosan lyophilized and LSD particles respectively. One-way ANOVA results showed a significant increase (p < 0.001) in UCS of 1% and 2% nHA/chitosan lyophilized scaffolds compared to 0% and 0.5% nHA/chitosan lyophilized scaffolds. Moreover, 2% nHA LSD scaffolds had significantly increased (p < 0.005) their mean UCS by 120% compared to 2% nHA lyophilized scaffolds. In a drawback, all scaffolds have lost their mechanical properties by 95% on the 2nd day when fully immersed in phosphate buffered saline. Additionally live and dead cell assay showed no cytotoxicity and excellent osteoblast attachment to both lyophilized and LSD scaffolds at the end of 14th day of in vitro

Injectable porous nano-hydroxyapatite/chitosan/tripolyphosphate scaffolds with improved compressive strength for bone regeneration

International Nuclear Information System (INIS)

Uswatta, Suren P.; Okeke, Israel U.; Jayasuriya, Ambalangodage C.

2016-01-01

In this study we have fabricated porous injectable spherical scaffolds using chitosan biopolymer, sodium tripolyphosphate (TPP) and nano-hydroxyapatite (nHA). TPP was primarily used as an ionic crosslinker to crosslink nHA/chitosan droplets. We hypothesized that incorporating nHA into chitosan could support osteoconduction by emulating the mineralized cortical bone structure, and improve the Ultimate Compressive Strength (UCS) of the scaffolds. We prepared chitosan solutions with 0.5%, 1% and 2% (w/v) nHA concentration and used simple coacervation and lyophilization techniques to obtain spherical scaffolds. Lyophilized spherical scaffolds had a mean diameter of 1.33 mm (n = 25). Further, portion from each group lyophilized scaffolds were soaked and dried to obtain Lyophilized Soaked and Dried (LSD) scaffolds. LSD scaffolds had a mean diameter of 0.93 mm (n = 25) which is promising property for the injectability. Scanning Electron Microscopy images showed porous surface morphology and interconnected pore structures inside the scaffolds. Lyophilized and LSD scaffolds had surface pores < 10 and 2 μm, respectively. 2% nHA/chitosan LSD scaffolds exhibited UCS of 8.59 MPa compared to UCS of 2% nHA/chitosan lyophilized scaffolds at 3.93 MPa. Standardize UCS values were 79.98 MPa and 357 MPa for 2% nHA/chitosan lyophilized and LSD particles respectively. One-way ANOVA results showed a significant increase (p < 0.001) in UCS of 1% and 2% nHA/chitosan lyophilized scaffolds compared to 0% and 0.5% nHA/chitosan lyophilized scaffolds. Moreover, 2% nHA LSD scaffolds had significantly increased (p < 0.005) their mean UCS by 120% compared to 2% nHA lyophilized scaffolds. In a drawback, all scaffolds have lost their mechanical properties by 95% on the 2nd day when fully immersed in phosphate buffered saline. Additionally live and dead cell assay showed no cytotoxicity and excellent osteoblast attachment to both lyophilized and LSD scaffolds at the end of 14th day of in vitro

Synthesis of hydroxyapatite coatings on metal substrates using a spincasting technique

International Nuclear Information System (INIS)

Yuan Qiuhua; Sahu, Laxmi Kumari; D'Souza, Nandika A.; Golden, Teresa Diane

2009-01-01

Hydroxyapatite coatings on stainless steel substrates were prepared by a simple spincasting technique. Nanosized hydroxyapatite powders were prepared by precipitating in an electrolytic suspension, and then added to a polylactic acid solution for spincasting. The polylactic acid gave enhanced protection from corrosion and inhibited decomposition of the hydroxyapatite coating during the sintering process in air, a significant advantage over other solution processing techniques. Characterization of the phase composition and morphology of the fabricated films on stainless steel was accomplished by X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, and Fourier transform infrared spectroscopy.

Fabrication and characterization of hydroxyapatite-coated forsterite ...

Indian Academy of Sciences (India)

... a novel hydroxyapatite (HA)-coated forsterite scaffold with a desired porous structure, high ... X-ray diffraction, scanning electron microscopy, transmission electron ... Dental Materials Research Center, Isfahan University of Medical Sciences, ...

Characterization of humidity-controlling porous ceramics produced from coal fly ash and waste catalyst by co-sintering

Science.gov (United States)

Lin, Kae-Long; Ma, Chih-Ming; Lo, Kang-Wei; Cheng, Ta-Wui

2018-04-01

In this study, the following operating conditions were applied to develop humidity-controlling porous ceramic (HCPC) products: sintering temperatures of 800-1000 °C and percentages of coal fly ash in waste catalyst of 0%-40%. The HCPC samples then underwent a flexural strength test, to determine their quality according to the Chinese National Standards (CNS 3298). Their microstructures, crystal structures, and pore volume were determined in terms of equilibrium moisture content, water vapor adsorption/desorption, and hygroscopic sorption properties over 48 h. Nitrogen adsorption/desorption isotherms showed a hydrophobic behavior (type H3 isotherm). The water vapor adsorption/desorption and hygroscopic sorption properties satisfied the JIS A1470 intensity specification for building materials (>29 g/m2). At sintering temperatures of 950-1000 °C, HCPC samples for coal fly ash containing 20%-30% waste catalyst met the JIS A1470 intensity specifications for building materials (<29 g/m2).

Synthesis and characterization of magnetite/hydroxyapatite tubes ...

Indian Academy of Sciences (India)

The first step is the formation of magnetite (Fe 3 O 4 ) tubes on natural template followed by hydroxyapatite (HAp) bioceramic coated on the Fe 3 O 4 tubes. HAp improves the biocompatibility and stability of the prepared tubes. Sintering at 900 ∘ C improves the crystalline stability of nanotubes and removes the natural ...

Preliminary biocompatible evaluation of nano-hydroxyapatite/polyamide 66 composite porous membrane

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Yili Qu

2010-06-01

Full Text Available Yili Qu1,3, Ping Wang1,3, Yi Man1, Yubao Li2, Yi Zuo2, Jidong Li21State Key Laboratory of Oral Diseases, Sichuan University, Chengdu 610064, China; 2Research Center for Nano-Biomaterials, Analytical and Testing Center, Sichuan University, Chengdu 610064, China; 3These authors contributed equally to this workAbstract: Nano-hydroxyapatite/polyamide 66 (nHA/PA66 composite with good bioactivity and osteoconductivity was employed to develop a novel porous membrane with asymmetric structure for guided bone regeneration (GBR. In order to test material cytotoxicity and to investigate surface-dependent responses of bone-forming cells, the morphology, proliferation, and cell cycle of bone marrow stromal cells (BMSCs of rats cultured on the prepared membrane were determined. The polygonal and fusiform shape of BMSCs was observed by scanning electronic microscopy (SEM. The proliferation of BMSCs cultured on nHA/PA66 membrane tested by the MTT method (MTT: [3-{4,5-dimethylthiazol-2yl}-2,5-diphenyl-2H-tetrazoliumbromide] was higher than that of negative control groups for 1 and 4 days’ incubation and had no significant difference for 7 and 11 days’ culture. The results of cell cycle also suggested that the membrane has no negative influence on cell division. The nHA/PA66 membranes were then implanted into subcutaneous sites of nine Sprague Dawley rats. The wounds and implant sites were free from suppuration and necrosis in all periods. All nHA/PA66 membranes were surrounded by a fibrous capsule with decreasing thickness 1 to 8 weeks postoperatively. In conclusion, the results of the in vitro and in vivo studies reveal that nHA/PA66 membrane has excellent biocompatibility and indicate its use in guided tissue regeneration (GTR or GBR.Keywords: hydroxyapatite/polyamide, barrier membrane, biocompatibility, guided bone regeneration

Low Temperature Two-Steps Sintering (LTTSS) - an innovative method for consolidating porous UO2 pellets

International Nuclear Information System (INIS)

Sanjay Kumar, D.; Ananthasivan, K.; Senapati, Abhiram; Venkata Krishnan, R.

2015-01-01

Metallic uranium and its alloys are an important fuel for fast reactors. Presently, metallic uranium is being prepared using expensive fluoro-metallothermic process. Recent reports suggest that metal oxide could be reduced to metal using a novel electrochemical de-oxidation method and this could serve as attractive alternate for expensive metallothermic process. In view of which, a research program is being pursued in our Centre to develop an optimum process parameter for the scaled up preparation of metallic uranium efficiently. One of the important process parameter is the size, nature and distribution of porosity in the urania pellet. Essentially the ceramic form of the urania should encompass interconnected porosity that would allow percolation of melts into the UO 2 . However, the matrix density of the pellet should be high to ensure that it possesses good handling strength and is electrically conducting. Hence preparation of high dense porous UO 2 pellets was required. In this study, we report the preparation of porous UO 2 pellets possessing a very high matrix density by using the citrate gel-combustion method. The 'as-prepared' powders were consolidated at various compaction pressures as such and these pellets were sintered in 8 mol %Ar+H 2 gas with a flow rate of 250 mL/min at 1073 K for 30 min followed by soaking at 1473 K for 4 h with heating rate of 5 K min -1 in a molybdenum furnace. X-ray diffraction studies revealed that these pellets contained UO 2 . The morphological analysis sintered pellets was carried out by using Scanning Electron Microscope (M/s. Philips model XL 30, Netherlands). All these pellets were gold coated

Facile fabrication of poly(L-lactic acid) microsphere-incorporated calcium alginate/hydroxyapatite porous scaffolds based on Pickering emulsion templates.

Science.gov (United States)

Hu, Yang; Ma, Shanshan; Yang, Zhuohong; Zhou, Wuyi; Du, Zhengshan; Huang, Jian; Yi, Huan; Wang, Chaoyang

2016-04-01

In this study, we develop a facile one-pot approach to the fabrication of poly(L-lactic acid) (PLLA) microsphere-incorporated calcium alginate (ALG-Ca)/hydroxyapatite (HAp) porous scaffolds based on HAp nanoparticle-stabilized oil-in-water Pickering emulsion templates, which contain alginate in the aqueous phase and PLLA in the oil phase. The emulsion aqueous phase is solidified by in situ gelation of alginate with Ca(2+) released from HAp by decreasing pH with slow hydrolysis of D-gluconic acid δ-lactone (GDL) to produce emulsion droplet-incorporated gels, followed by freeze-drying to form porous scaffolds containing microspheres. The pore structure of porous scaffolds can be adjusted by varying the HAp or GDL concentration. The compressive tests show that the increase of HAp or GDL concentration is beneficial to improve the compressive property of porous scaffolds, while the excessive HAp can lead to the decrease in compressive property. Moreover, the swelling behavior studies display that the swelling ratios of porous scaffolds reduce with increasing HAp or GDL concentration. Furthermore, hydrophobic drug ibuprofen (IBU) and hydrophilic drug bovine serum albumin (BSA) are loaded into the microspheres and scaffold matrix, respectively. In vitro drug release results indicate that BSA has a rapid release while IBU has a sustained release in the dual drug-loaded scaffolds. In vitro cell culture experiments verify that mouse bone mesenchymal stem cells can proliferate on the porous scaffolds well, indicating the good biocompatibility of porous scaffolds. All these results demonstrate that the PLLA microsphere-incorporated ALG-Ca/HAp porous scaffolds have a promising potential for tissue engineering and drug delivery applications. Copyright © 2016 Elsevier B.V. All rights reserved.

A clinical evaluation of a bioresorbable membrane and porous hydroxyapatite in the treatment of human molar class II furcations

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K Gita Malathi

2013-01-01

Full Text Available Background: The ultimate goal of periodontal therapy is predictable regeneration of a functional attachment apparatus destroyed as a result of periodontitis. Reconstructive procedures have been used with varying success during the past decades to accomplish this goal. Aim: To evaluate whether the use of porous hydroxyapatite alone or a bioresorbable membrane alone would enhance the clinical results in the treatment of class II furcation defects in human lower molars. Materials and Methods: Fifteen patients with chronic periodontitis, aged between 39 and 49 years, with a pair of similar bilateral class II furcation defects (classification of Hamp et al. in mandibular first molars were selected. A split-mouth design was incorporated and the selected 30 furcation defects were assigned to one of the two treatment groups, i.e., Group I treated with a bioresorbable membrane from bovine-derived collagen guided tissue regeneration membrane and Group II treated using porous hydroxyapatite bone graft material on the contralateral sides. Evaluation of clinical parameters, probing depths and attachment levels, and radiographs was done preoperatively and 6 months postoperatively. Results: Both the groups showed statistically significant mean reduction in probing depths and gain in clinical attachment levels and linear bone fill. Comparison between Group I and Group II showed insignificant difference. Conclusion: Within the limits of this study, both the treatment modalities are beneficial for the treatment of human mandibular class II furcation defects.

Mechanical behaviour of new zirconia-hydroxyapatite ceramic materials

Energy Technology Data Exchange (ETDEWEB)

Delgado, J.A.; Morejon, L. [La Habana Univ. (Cuba). Centro de Biomateriales; Martinez, S. [Barcelona Univ. (Spain). Dept. Cristallografia, Mineralogia; Ginebra, M.P.; Carlsson, N.; Fernandez, E.; Planell, J.A. [Universidad Politecnica de Cataluna, Barcelona (Spain). CREB; Clavaguera-Mora, M.T.; Rodriguez-Viejo, J. [Universitat Autonoma de Barcelona (Spain). Dept. de Fisica

2001-07-01

In this work a new zirconia-hydroxyapatite ceramic material was obtained by uniaxial pressing and sintering in humid environment. The powder X-ray diffraction (XRD) patterns and infrared spectra (FT-IR) showed that the hydroxyapatite (HA) is the only calcium phosphate phase present. The fracture toughness for HA with 20 wt.% of magnesia partially stabilised zirconia (Mg-PSZ) was around 2.5 times higher than those obtained for HA pure, also the highest value of bending strength (160 MPa) was obtained for material reinforced with Mg-PSZ. For the MgPSZ-HA (20%) the fracture mechanism seems to be less transgranular. (orig.)

Processing of hydroxyapatite obtained by combustion synthesis

International Nuclear Information System (INIS)

Canillas, M.; Rivero, R.; García-Carrodeguas, R.; Barba, F.; Rodríguez, M.A.

2017-01-01

One of the reasons of implants failure are the stress forces appearing in the material–tissue interface due to the differences between their mechanical properties. For this reason, similar mechanical properties to the surrounding tissue are desirable. The synthesis of hydroxyapatite by solution combustion method and its processing have been studied in order to obtain fully dense ceramic bodies with improved mechanical strength. Combustion synthesis provides nanostructured powders characterized by a high surface area to facilitate the following sintering. Moreover, synthesis was conducted in aqueous and oxidizing media. Oxidizing media improve homogenization and increase the energy released during combustion. It gives rise to particles whose morphology and size suggest lower surface energies compared with aqueous media. The obtained powders were sintered by using a controlled sintering rate schedule. Lower surfaces energies minimize the shrinkage during sintering and relative densities measurements and diametral compression test confirm improved densification and consequently mechanical properties. [es

Processing of hydroxyapatite obtained by combustion synthesis

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M. Canillas

2017-09-01

Full Text Available One of the reasons of implants failure are the stress forces appearing in the material–tissue interface due to the differences between their mechanical properties. For this reason, similar mechanical properties to the surrounding tissue are desirable. The synthesis of hydroxyapatite by solution combustion method and its processing have been studied in order to obtain fully dense ceramic bodies with improved mechanical strength. Combustion synthesis provides nanostructured powders characterized by a high surface area to facilitate the following sintering. Moreover, synthesis was conducted in aqueous and oxidizing media. Oxidizing media improve homogenization and increase the energy released during combustion. It gives rise to particles whose morphology and size suggest lower surface energies compared with aqueous media. The obtained powders were sintered by using a controlled sintering rate schedule. Lower surfaces energies minimize the shrinkage during sintering and relative densities measurements and diametral compression test confirm improved densification and consequently mechanical properties.

Surgical pitfalls with custom-made porous hydroxyapatite cranial implants

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Bruno Zanotti

2015-03-01

Full Text Available Aim: Cranioplasty implants are used primarily in cases of surgical cranial decompression following pathological elevations of intracranial pressure. Available bone substitutes include porous hydroxyapatite (HA and polymethylmethacrylate. Whichever material is used, however, prosthetic cranial implants are susceptible to intra- and postsurgical complications and even failure. The aim of this study was to investigate such occurrences in HA cranioplasty implants, seeking not only to determine the likely causes (whether correlated or not with the device itself but also, where possible, to suggest countermeasures. Methods: We analyzed information regarding failures or complications reported in postmarketing surveillance and clinical studies of patients treated worldwide with custom-made HA cranial implants (Custom Bone Service Fin-Ceramica Faenza, Italy in the period 1997-2013. Results: The two most common complications were implant fractures (84 cases, 2.9% of the total fitted and infections (51 cases, 1.77%. Conclusion: Although cranioplasties are superficial and not difficult types of surgery, and use of custom-made implants are often considered the "easy" option from a surgical perspective, these procedures are nonetheless plagued by potential pitfalls. If performed well they yield more than satisfactory results from the points of view of both the patient and surgeon, but lack of appropriate care can open the door to numerous potential sources of failure, which can compromise-even irreparably-the ability to heal.

Fabrication, Properties and Applications of Dense Hydroxyapatite: A Review

Science.gov (United States)

Prakasam, Mythili; Locs, Janis; Salma-Ancane, Kristine; Loca, Dagnija; Largeteau, Alain; Berzina-Cimdina, Liga

2015-01-01

In the last five decades, there have been vast advances in the field of biomaterials, including ceramics, glasses, glass-ceramics and metal alloys. Dense and porous ceramics have been widely used for various biomedical applications. Current applications of bioceramics include bone grafts, spinal fusion, bone repairs, bone fillers, maxillofacial reconstruction, etc. Amongst the various calcium phosphate compositions, hydroxyapatite, which has a composition similar to human bone, has attracted wide interest. Much emphasis is given to tissue engineering, both in porous and dense ceramic forms. The current review focusses on the various applications of dense hydroxyapatite and other dense biomaterials on the aspects of transparency and the mechanical and electrical behavior. Prospective future applications, established along the aforesaid applications of hydroxyapatite, appear to be promising regarding bone bonding, advanced medical treatment methods, improvement of the mechanical strength of artificial bone grafts and better in vitro/in vivo methodologies to afford more particular outcomes. PMID:26703750

Fabrication, Properties and Applications of Dense Hydroxyapatite: A Review

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Mythili Prakasam

2015-12-01

Full Text Available In the last five decades, there have been vast advances in the field of biomaterials, including ceramics, glasses, glass-ceramics and metal alloys. Dense and porous ceramics have been widely used for various biomedical applications. Current applications of bioceramics include bone grafts, spinal fusion, bone repairs, bone fillers, maxillofacial reconstruction, etc. Amongst the various calcium phosphate compositions, hydroxyapatite, which has a composition similar to human bone, has attracted wide interest. Much emphasis is given to tissue engineering, both in porous and dense ceramic forms. The current review focusses on the various applications of dense hydroxyapatite and other dense biomaterials on the aspects of transparency and the mechanical and electrical behavior. Prospective future applications, established along the aforesaid applications of hydroxyapatite, appear to be promising regarding bone bonding, advanced medical treatment methods, improvement of the mechanical strength of artificial bone grafts and better in vitro/in vivo methodologies to afford more particular outcomes.

Synthesis and characterization of natural hydroxyapatite (recycled) composites with titania

International Nuclear Information System (INIS)

Mendes Filho, Antonio Alves; Gouveia, Vitor Jose Pinto; Pereira, Renato Alves; Araujo, Fernando Gabriel da Silva; Sousa, Camila Mateus de

2010-01-01

Natural hydroxyapatite biphasic ceramics (recycled) with titania (TiO_2-Hap) were studied in this work. For the formation of such ceramic the powders were mixed natural hydroxyapatite obtained from veal bone by the hydrothermal method with titania (TiO_2), forming the composites H9T1. The powders, manually homogenized, were conformed in pellet and sintered at temperatures between 1200 and 1400 deg C The ceramic bodies were characterized by XRD and SEM/EDS. The initial results were not satisfactory and require new studies. (author)

Porous electrode preparation method

Science.gov (United States)

Arons, R.M.; Dusek, J.T.

1983-10-18

A porous sintered plaque is provided with a bimodal porosity that is especially well suited for use as an electrode within a molten carbonate fuel cell. The coarse porosity is sufficient for admitting gases into contact with the reaction surfaces while the fine porosity is wetted with and retains molten electrolyte on the reaction sites. The electrode structure is prepared by providing a very fine powder of such as nickel oxide and blending the powder with a suitable decomposable binder to form a solid mass. The mass is comminuted into agglomerate size particles substantially larger than the fine oxide particles and formed into a cohesive compact for subsequent sintering. Sintering is carried out at sufficient conditions to bind the agglomerates together into a porous structure having both coarse and fine porosity. Where lithiated nickel oxide cathodes are prepared, the sintering conditions can be moderate enough to retain substantial quantities of lithium within the electrode for adequate conductivity. 2 figs.

Hydroxyapatite hierarchically nanostructured porous hollow microspheres: rapid, sustainable microwave-hydrothermal synthesis by using creatine phosphate as an organic phosphorus source and application in drug delivery and protein adsorption.

Science.gov (United States)

Qi, Chao; Zhu, Ying-Jie; Lu, Bing-Qiang; Zhao, Xin-Yu; Zhao, Jing; Chen, Feng; Wu, Jin

2013-04-22

Hierarchically nanostructured porous hollow microspheres of hydroxyapatite (HAP) are a promising biomaterial, owing to their excellent biocompatibility and porous hollow structure. Traditionally, synthetic hydroxyapatite is prepared by using an inorganic phosphorus source. Herein, we report a new strategy for the rapid, sustainable synthesis of HAP hierarchically nanostructured porous hollow microspheres by using creatine phosphate disodium salt as an organic phosphorus source in aqueous solution through a microwave-assisted hydrothermal method. The as-obtained products are characterized by powder X-ray diffraction (XRD), Fourier-transform IR (FTIR) spectroscopy, SEM, TEM, Brunauer-Emmett-Teller (BET) nitrogen sorptometry, dynamic light scattering (DLS), and thermogravimetric analysis (TGA). SEM and TEM micrographs show that HAP hierarchically nanostructured porous hollow microspheres consist of HAP nanosheets or nanorods as the building blocks and DLS measurements show that the diameters of HAP hollow microspheres are within the range 0.8-1.5 μm. The specific surface area and average pore size of the HAP porous hollow microspheres are 87.3 m(2) g(-1) and 20.6 nm, respectively. The important role of creatine phosphate disodium salt and the influence of the experimental conditions on the products were systematically investigated. This method is facile, rapid, surfactant-free and environmentally friendly. The as-prepared HAP porous hollow microspheres show a relatively high drug-loading capacity and protein-adsorption ability, as well as sustained drug and protein release, by using ibuprofen as a model drug and hemoglobin (Hb) as a model protein, respectively. These experiments indicate that the as-prepared HAP porous hollow microspheres are promising for applications in biomedical fields, such as drug delivery and protein adsorption. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Porous stable poly(lactic acid)/ethyl cellulose/hydroxyapatite composite scaffolds prepared by a combined method for bone regeneration.

Science.gov (United States)

Mao, Daoyong; Li, Qing; Bai, Ningning; Dong, Hongzhou; Li, Daikun

2018-01-15

A major challenge in bone tissue engineering is the development of biomimetic scaffolds which should simultaneously meet mechanical strength and pore structure requirements. Herein, we combined technologies of high concentration solvent casting, particulate leaching, and room temperature compression molding to prepare a novel poly(lactic acid)/ethyl cellulose/hydroxyapatite (PLA/EC/HA) scaffold. The functional, structural and mechanical properties of the obtained porous scaffolds were characterized. The results indicated that the PLA/EC/HA scaffolds at the 20wt% HA loading level showed optimal mechanical properties and desired porous structure. Its porosity, contact angle, compressive yield strength and weight loss after 56days were 84.28±7.04%, 45.13±2.40°, 1.57±0.09MPa and 4.77±0.32%, respectively, which could satisfy the physiological demands to guide bone regeneration. Thus, the developed scaffolds have potential to be used as a bone substitute material for bone tissue engineering application. Copyright © 2017. Published by Elsevier Ltd.

Effect of material, process parameters, and simulated body fluids on mechanical properties of 13-93 bioactive glass porous constructs made by selective laser sintering.

Science.gov (United States)

Kolan, Krishna C R; Leu, Ming C; Hilmas, Gregory E; Velez, Mariano

2012-09-01

The effect of particle size distribution, binder content, processing parameters, and sintering schedule on the microstructure and mechanical properties of porous constructs was investigated. The porous constructs were produced by indirect selective laser sintering (SLS) of 13-93 bioactive glass using stearic acid as a polymeric binder. The binder content and d(50) particle size in the feedstock powders were simultaneously reduced from 22 to 12 wt% and from 20 to 11 μm, respectively, to identify the minimum binder content required for the SLS fabrication. An average particle size of ∼16 μm with a binder content of 15 wt% significantly reduced post-processing time and improved mechanical properties. Increasing the laser power and scan speed at the energy density of 1 cal/cm² maintained the feature sharpness of the parts during the fabrication of green parts and could almost double the mechanical properties of the sintered parts. Changes in the heating rates, ranging from 0.1 to 2 °C/min, during the post-processing of the fabricated "green" scaffolds showed that the heating rate significantly affects the densification and mechanical properties of the sintered scaffolds. The compressive strength of the scaffolds manufactured with the optimized parameters varied from 41 MPa, for a scaffold with a porosity of ∼50%, to 157 MPa, for a dense part. The bioactive scaffolds soaked in simulated body fluids for durations up to 6 weeks were used to evaluate the change in mechanical properties in vitro. Copyright © 2012 Elsevier Ltd. All rights reserved.

Hydroxyapatite Reinforced Coatings with Incorporated Detonationally Generated Nanodiamonds

International Nuclear Information System (INIS)

Pramatarova, L.; Pecheva, E.; Hikov, T.; Fingarova, D.; Dimitrova, R.; Spassov, T.; Krasteva, N.; Mitev, D.

2010-01-01

We studied the effect of the substrate chemistry on the morphology of hydroxyapatite-detonational nanodiamond composite coatings grown by a biomimetic approach (immersion in a supersaturated simulated body fluid). When detonational nanodiamond particles were added to the solution, the morphology of the grown for 2 h composite particles was porous but more compact then that of pure hydroxyapatite particles. The nanodiamond particles stimulated the hydroxyapatite growth with different morphology on the various substrates (Ti, Ti alloys, glasses, Si, opal). Biocompatibility assay with MG63 osteoblast cells revealed that the detonational nanodiamond water suspension with low and average concentration of the detonational nanodiamond powder is not toxic to living cells.

An in situ Study of NiTi Powder Sintering Using Neutron Diffraction

Directory of Open Access Journals (Sweden)

Gang Chen

2015-04-01

Full Text Available This study investigates phase transformation and mechanical properties of porous NiTi alloys using two different powder compacts (i.e., Ni/Ti and Ni/TiH2 by a conventional press-and-sinter means. The compacted powder mixtures were sintered in vacuum at a final temperature of 1373 K. The phase evolution was performed by in situ neutron diffraction upon sintering and cooling. The predominant phase identified in all the produced porous NiTi alloys after being sintered at 1373 K is B2 NiTi phase with the presence of other minor phases. It is found that dehydrogenation of TiH2 significantly affects the sintering behavior and resultant microstructure. In comparison to the Ni/Ti compact, dehydrogenation occurring in the Ni/TiH2 compact leads to less densification, yet higher chemical homogenization, after high temperature sintering but not in the case of low temperature sintering. Moreover, there is a direct evidence of the eutectoid decomposition of NiTi at ca. 847 and 823 K for Ni/Ti and Ni/TiH2, respectively, during furnace cooling. The static and cyclic stress-strain behaviors of the porous NiTi alloys made from the Ni/Ti and Ni/TiH2 compacts were also investigated. As compared with the Ni/Ti sintered samples, the samplessintered from the Ni/TiH2 compact exhibited a much higher porosity, a higher close-to-total porosity, a larger pore size and lower tensile and compressive fracture strength.

Micromechanical finite element modeling and experimental characterization of the compressive mechanical properties of polycaprolactone:hydroxyapatite composite scaffolds prepared by selective laser sintering for bone tissue engineering

Science.gov (United States)

Eshraghi, Shaun; Das, Suman

2012-01-01

Bioresorbable scaffolds with mechanical properties suitable for bone tissue engineering were fabricated from polycaprolactone (PCL) and hydroxyapatite (HA) by selective laser sintering (SLS) and modeled by finite element analysis (FEA). Both solid gage parts and scaffolds having 1-D, 2-D and 3-D orthogonal, periodic porous architectures were made with 0, 10, 20 and 30% HA by volume. PCL:HA scaffolds manufactured by SLS had nearly full density (99%) in the designed solid regions and had excellent geometric and dimensional control. Through optimization of the SLS process, the compressive moduli for our solid gage parts and scaffolds are the highest reported in the literature for additive manufacturing. The compressive moduli of solid gage parts were 299.3, 311.2, 415.5 and 498.3 MPa for PCL:HA loading at 100:0, 90:10, 80:20 and 70:30 respectively. The compressive effective stiffness tended to increase as the loading of HA was increased and the designed porosity was lowered. In the case of the most 3-D porous scaffold, the compressive modulus more than doubled from 14.9 MPa to 36.2 MPa when changing the material from 100:0 to 70:30 PCL:HA. A micromechanical finite element analysis (FEA) model was developed to investigate the reinforcement effect of HA loading on the compressive modulus of the bulk material. Using a first-principles based approach, the random distribution of HA particles in a solidified PCL matrix was modeled for any loading of HA to predict the bulk mechanical properties of the composites. The bulk mechanical properties were also used for FEA of the scaffold geometries. Results of the FEA were found to be in good agreement with experimental mechanical testing. The development of patient and site-specific composite tissue engineering constructs with tailored properties can be seen as a direct extension of this work on computational design, a priori modeling of mechanical properties and direct digital manufacturing. PMID:22522129

Micromechanical finite-element modeling and experimental characterization of the compressive mechanical properties of polycaprolactone-hydroxyapatite composite scaffolds prepared by selective laser sintering for bone tissue engineering.

Science.gov (United States)

Eshraghi, Shaun; Das, Suman

2012-08-01

Bioresorbable scaffolds with mechanical properties suitable for bone tissue engineering were fabricated from polycaprolactone (PCL) and hydroxyapatite (HA) by selective laser sintering (SLS) and modeled by finite-element analysis (FEA). Both solid gage parts and scaffolds having 1-D, 2-D and 3-D orthogonal, periodic porous architectures were made with 0, 10, 20 and 30 vol.% HA. PCL:HA scaffolds manufactured by SLS had nearly full density (99%) in the designed solid regions and had excellent geometric and dimensional control. Through optimization of the SLS process, the compressive moduli for our solid gage parts and scaffolds are the highest reported in the literature for additive manufacturing. The compressive moduli of solid gage parts were 299.3, 311.2, 415.5 and 498.3 MPa for PCL:HA loading at 100:0, 90:10, 80:20 and 70:30, respectively. The compressive effective stiffness tended to increase as the loading of HA was increased and the designed porosity was lowered. In the case of the most 3-D porous scaffold, the compressive modulus more than doubled from 14.9 to 36.2 MPa when changing the material from 100:0 to 70:30 PCL:HA. A micromechanical FEA model was developed to investigate the reinforcement effect of HA loading on the compressive modulus of the bulk material. Using a first-principles based approach, the random distribution of HA particles in a solidified PCL matrix was modeled for any HA loading to predict the bulk mechanical properties of the composites. The bulk mechanical properties were also used for FEA of the scaffold geometries. The results of the FEA were found to be in good agreement with experimental mechanical testing. The development of patient- and site-specific composite tissue-engineering constructs with tailored properties can be seen as a direct extension of this work on computational design, a priori modeling of mechanical properties and direct digital manufacturing. Copyright © 2012 Acta Materialia Inc. Published by Elsevier Ltd. All

Synthesis, structural properties and thermal stability of Mn-doped hydroxyapatite

Science.gov (United States)

Paluszkiewicz, Czesława; Ślósarczyk, Anna; Pijocha, Dawid; Sitarz, Maciej; Bućko, Mirosław; Zima, Aneta; Chróścicka, Anna; Lewandowska-Szumieł, Małgorzata

2010-07-01

Hydroxyapatite (HA) - Ca 10(PO 4) 6(OH) 2 is a basic inorganic model component of hard biological tissues, such as bones and teeth. The significant property of HA is its ability to exchange Ca 2+ ions, which influences crystallinity, physico-chemical and biological properties of modified hydroxyapatite materials. In this work, FTIR, Raman spectroscopy, XRD, SEM and EDS techniques were used to determine thermal stability, chemical and phase composition of Mn containing hydroxyapatite (MnHA). Described methods confirmed thermal decomposition and phase transformation of MnHA to αTCP, βTCP and formation of Mn 3O 4 depending on sintering temperature and manganese content. In vitro biological evaluation of Mn-modified HA ceramics was also performed using human osteoblast cells.

Evaluating morphology and mechanical properties of glass-reinforced natural hydroxyapatite composites.

Science.gov (United States)

Yazdanpanah, Z; Bahrololoom, M E; Hashemi, B

2015-01-01

Hydroxyapatite has been used in a wide variety of biomedical applications and it can be produced from natural resources such as bovine bone. This material does not have acceptable mechanical properties by itself. In the present work, hydroxyapatite composites with different weight percentages of sodalime glass were made and sintered at different temperatures (800-1200°C). Eventually the properties such as density, micro hardness, compressive strength and wear of specimens were evaluated. Specific percentages of glass additive increased the density and hardness of specimens due to increasing the sintering temperature. The hardness and density of specimens were decreased with higher percentage of glass additive. Moreover, the results of compressive test showed that increasing the glass addition increases the compressive performance. Furthermore, the SEM micrographs on worn specimens showed that the mechanism of wear was abrasive. Copyright © 2014 Elsevier Ltd. All rights reserved.

Effect of highly dispersed yttria addition on thermal stability of hydroxyapatite

Energy Technology Data Exchange (ETDEWEB)

Parente, P., E-mail: pparente@icv.csic.es [Instituto de Ceramica y Vidrio, CSIC, C/Kelsen 5, Madrid 28049 (Spain); Savoini, B. [Departamento de Fisica, Universidad Carlos III de Madrid, Avda. Universidad 30, Leganes 28911 (Spain); Ferrari, B. [Instituto de Ceramica y Vidrio, CSIC, C/Kelsen 5, Madrid 28049 (Spain); Monge, M.A.; Pareja, R. [Departamento de Fisica, Universidad Carlos III de Madrid, Avda. Universidad 30, Leganes 28911 (Spain); Sanchez-Herencia, A.J. [Instituto de Ceramica y Vidrio, CSIC, C/Kelsen 5, Madrid 28049 (Spain)

2013-03-01

The capability of the colloidal method to produce yttria (Y{sub 2}O{sub 3}) dispersed hydroxyapatite (HA) has been investigated as an alternative method to the conventional method of mechanical mixing and sintering for developing HA-based materials that could exhibit controllable and enhanced functional properties. A water based colloidal route to produce HA materials with highly dispersed Y{sub 2}O{sub 3} has been applied, and the effect of 10 wt.% Y{sub 2}O{sub 3} addition to HA investigated by thermal analysis, X-ray diffraction and Fourier transform infrared spectroscopy. These measurements evidence a remarkable effect of this Y{sub 2}O{sub 3} addition on decomposition mechanisms of synthetic HA. Results show that incorporation of Y{sub 2}O{sub 3} as dispersed second phase is beneficial because it hinders the decomposition mechanisms of HA into calcium phosphates. This retardation will allow the control of the sintering conditions for developing HA implants with improved properties. Besides, substitution of Ca{sup 2+} with Y{sup 3+} ions appears to promote the formation of OH{sup -} vacancies, which could improve the conductive properties of HA favorable to osseointegration. - Highlights: Black-Right-Pointing-Pointer We reveal the influence of Y{sub 2}O{sub 3} on thermal stability of hydroxyapatite. Black-Right-Pointing-Pointer Incorporation of Y{sub 2}O{sub 3} delays decomposition of hydroxyapatite to calcium phosphates. Black-Right-Pointing-Pointer Addition of Y{sub 2}O{sub 3} enables sintering conditions more favorable to the densification.

Suspension thermal spraying of hydroxyapatite: microstructure and in vitro behaviour.

Science.gov (United States)

Bolelli, Giovanni; Bellucci, Devis; Cannillo, Valeria; Lusvarghi, Luca; Sola, Antonella; Stiegler, Nico; Müller, Philipp; Killinger, Andreas; Gadow, Rainer; Altomare, Lina; De Nardo, Luigi

2014-01-01

In cementless fixation of metallic prostheses, bony ingrowth onto the implant surface is often promoted by osteoconductive plasma-sprayed hydroxyapatite coatings. The present work explores the use of the innovative High Velocity Suspension Flame Spraying (HVSFS) process to coat Ti substrates with thin homogeneous hydroxyapatite coatings. The HVSFS hydroxyapatite coatings studied were dense, 27-37μm thick, with some transverse microcracks. Lamellae were sintered together and nearly unidentifiable, unlike conventional plasma-sprayed hydroxyapatite. Crystallinities of 10%-70% were obtained, depending on the deposition parameters and the use of a TiO2 bond coat. The average hardness of layers with low (hydroxyapatite, with a Weibull modulus of ≈3.3. During soaking in simulated body fluid, glassy coatings were progressively resorbed and replaced by a new, precipitated hydroxyapatite layer, whereas coatings with 70% crystallinity were stable up to 14days of immersion. The interpretation of the precipitation behaviour was also assisted by surface charge assessments, performed through Z-potential measurements. During in vitro tests, HA coatings showed no cytotoxicity towards the SAOS-2 osteoblast cell line, and surface cell proliferation was comparable with proliferation on reference polystyrene culture plates. © 2013.

Preparation of hollow hydroxyapatite microspheres by the conversion of borate glass at near room temperature

International Nuclear Information System (INIS)

Yao, Aihua; Ai, Fanrong; Liu, Xin; Wang, Deping; Huang, Wenhai; Xu, Wei

2010-01-01

Hollow hydroxyapatite microspheres, consisting of a hollow core and a porous shell, were prepared by converting Li 2 O-CaO-B 2 O 3 glass microspheres in dilute phosphate solution at 37 o C. The results confirmed that Li 2 O-CaO-B 2 O 3 glass was transformed to hydroxyapatite without changing the external shape and dimension of the original glass object. Scanning electron microscopy images showed the shell wall of the microsphere was built from hydroxyapatite particles, and these particles spontaneously align with one another to form a porous sphere with an interior cavity. Increase in phosphate concentration resulted in an increase in the reaction rate, which in turn had an effect on shell wall structure of the hollow hydroxyapatite microsphere. For the Li 2 O-CaO-B 2 O 3 glass microspheres reacted in low-concentration K 2 HPO 4 solution, lower reaction rate and a multilayered microstructure were observed. On the other hand, the glass microspheres reacted in higher phosphate solution converted more rapidly and produced a single hydroxyapatite layer. Furthermore, the mechanism of forming hydroxyapatite hollow microsphere was described.

Immobilisation of hydroxyapatite-collagen on polydopamine grafted stainless steel 316L: Coating adhesion and in vitro cells evaluation.

Science.gov (United States)

Tapsir, Zafirah; Jamaludin, Farah H; Pingguan-Murphy, Belinda; Saidin, Syafiqah

2018-02-01

The utilisation of hydroxyapatite and collagen as bioactive coating materials could enhance cells attachment, proliferation and osseointegration. However, most methods to form crystal hydroxyapatite coating do not allow the incorporation of polymer/organic compound due to production phase of high sintering temperature. In this study, a polydopamine film was used as an intermediate layer to immobilise hydroxyapatite-collagen without the introduction of high sintering temperature. The surface roughness, coating adhesion, bioactivity and osteoblast attachment on the hydroxyapatite-collagen coating were assessed as these properties remains unknown on the polydopamine grafted film. The coating was developed by grafting stainless steel 316L disks with a polydopamine film. Collagen type I fibres were then immobilised on the grafted film, followed by the biomineralisation of hydroxyapatite. The surface roughness and coating adhesion analyses were later performed by using AFM instrument. An Alamar Blue assay was used to determine the cytotoxicity of the coating, while an alkaline phosphatase activity test was conducted to evaluate the osteogenic differentiation of human fetal osteoblasts on the coating. Finally, the morphology of cells attachment on the coating was visualised under FESEM. The highest RMS roughness and coating adhesion were observed on the hydroxyapatite-collagen coating (hydroxyapatite-coll-dopa). The hydroxyapatite-coll-dopa coating was non-toxic to the osteoblast cells with greater cells proliferation, greater level of alkaline phosphate production and more cells attachment. These results indicate that the immobilisation of hydroxyapatite and collagen using an intermediate polydopamine is identical to enhance coating adhesion, osteoblast cells attachment, proliferation and differentiation, and thus could be implemented as a coating material on orthopaedic and dental implants.

Characteristics of porous zirconia coated with hydroxyapatite as ...

Indian Academy of Sciences (India)

TECS

Zirconia; porosity; hydroxyapatite; coating; compressive strength. 1. Introduction. A lot of .... typically from 300–500 μm, estimated from the SEM images. Thus, the .... Kim H W, Georgiou F, Knowles J C, Koh Y H and Kim H E. 2004 Biomaterials ...

Improved osteoblasts growth on osteomimetic hydroxyapatite/BaTiO{sub 3} composites with aligned lamellar porous structure

Energy Technology Data Exchange (ETDEWEB)

Liu, Beilei [Department of Stomatology, Third Xiangya Hospital, Central South University, Changsha, Hunan 410013 (China); Chen, Liangjian, E-mail: jian007040@sina.com [Department of Stomatology, Third Xiangya Hospital, Central South University, Changsha, Hunan 410013 (China); State Key Laboratory of Powder Metallurgy, Central South University, Changsha, Hunan 410083 (China); Shao, Chunsheng [Department of Stomatology, Third Xiangya Hospital, Central South University, Changsha, Hunan 410013 (China); Zhang, Fuqiang; Zhou, Kechao [State Key Laboratory of Powder Metallurgy, Central South University, Changsha, Hunan 410083 (China); Cao, Jun [Department of Stomatology, Third Xiangya Hospital, Central South University, Changsha, Hunan 410013 (China); Zhang, Dou, E-mail: dzhang@csu.edu.cn [State Key Laboratory of Powder Metallurgy, Central South University, Changsha, Hunan 410083 (China)

2016-04-01

Osteoblasts growing into bone substitute is an important step of bone regeneration. This study prepared porous hydroxyapatite (HA)/BaTiO{sub 3} piezoelectric composites with porosity of 40%, 50% and 60% by ice-templating method. Effects of HA/BaTiO{sub 3} composites with different porosities, with and without polarizing treatment on adhesion, proliferation and differentiation of osteoblasts were investigated in vitro. Results revealed that cell densities of the porous groups were significantly higher than those of the dense group (p < 0.05), so did the alkaline phosphate (ALP) and bone gla protein (BGP) activities. Porosity of 50% group exhibited higher ALP activity and BGP activity than those of the 40% and 60% groups. Scanning electron microscopy (SEM) observations revealed that osteoblasts adhered and stretched better on porous HA/BaTiO{sub 3} than on the dense one, especially HA/BaTiO{sub 3} with porosity of 50% and 60%. However, there was no significant difference in the cell morphology, cell densities, ALP and BGP activities between the polarized group and the non-polarized group (p > 0.05). The absence of mechanical loading on the polarized samples may account for this. The results indicated that hierarchically porous HA/BaTiO{sub 3} played a favorable part in osteoblasts proliferation, differentiation and adhesion process and is a promising bone substitute material. - Graphical abstract: Aligned porous structure of HA/BaTiO{sub 3} piezoelectric composites prepared by ice-templating method was similar to the lamellar Haversian system in bone tissue. When co-cultured with human osteosarcoma cells (MG63), porous HA/BaTiO{sub 3} composites exhibited remarkable biological activity in promoting proliferation, differentiation and adhesion of MG63 cells. - Highlights: • The aligned porous structure of HA/BaTiO{sub 3} composite was similar to the lamellar Haversian system in bone tissue. • The piezoelectric d{sub 33} coefficient of HA/BaTiO{sub 3} with porosity

Degradation and in vitro cell–material interaction studies on hydroxyapatite-coated biodegradable porous iron for hard tissue scaffolds

Directory of Open Access Journals (Sweden)

Nurizzati Mohd Daud

2014-10-01

Full Text Available This paper describes degradation and cell–material interaction studies on hydroxyapatite (HA-coated biodegradable porous iron proposed for hard tissue scaffolds. Porous iron scaffolds are expected to serve as an ideal platform for bone regeneration. To couple their inherent mechanical strength, pure HA and HA/poly(ε-caprolactone (HA/PCL were coated onto porous iron using dip coating technique. The HA/PCL mixture was prepared to provide a more stable and flexible coating than HA alone. Degradation of the samples was evaluated by weight loss and potentiodynamic polarisation. Human skin fibroblast (HSF and human mesenchymal stem cells (hMSC were put in contact with the samples and their interaction was observed. Results showed that coated samples degraded ∼10 times slower (0.002 mm/year for HA/PCL-Fe, 0.003 mm/year for HA-Fe than the uncoated ones (0.031 mm/year, indicating an inhibition effect of the coating on degradation. Both HSF and hMSC maintained high viability when in contact with the coated samples (100–110% control for hMSC during 2–5 days of incubation, indicating the effect of HA in enhancing cytocompatibility of the surface. This study provided early evidence of the potential translation of biodegradable porous iron scaffolds for clinical use in orthopedic surgery. However, further studies including in vitro and in vivo tests are necessary.

Near net-shape fabrication of hydroxyapatite glass composites

NARCIS (Netherlands)

Zhu, Q.; With, de G.; Dortmans, L.; Feenstra, F.

2004-01-01

Near net-shape fabrication of hydroxyapatite (HA) glass composites has been attempted by infiltrating a glass into porous HA performs. Main efforts were put to develop glasses that are chemically compatible with HA at elevated temperatures. After extensive investigations in the phosphate and

[Characterization of alumina adobe and sintered body of GI-infiltrated ceramic].

Science.gov (United States)

Wang, H; Chao, Y; Liao, Y; Liang, X; Zhu, Z; Gao, W

2001-06-01

This study was conducted to elucidate the mechanism of formation of porous structure by investigating the porosity of the alumina adobe and sintered body of GI-II Infiltrate Ceramic, and its role in strengthening and toughening this kind of ceramic composite. The alumina powder size-mass distribution was obtained by BI-XDC powder size analysis device; the open pore parameters of alumina adobe and sintered body were analyzed using the mercury pressure method. Their fracture surfaces were observed under scanning electronic microscope. Fine powder had two main size groups of 0.09-0.1 micron and 0.2-0.5 micron, respectively, and coarse powder, with size between 1.5 to 4.5 microns, occupied the majority of powder mass. Alumina adobe's pores became larger after sintering. The median pore radii of adobe and sintered body were 0.2531 micron and 0.3081 micron, respectively; the average pore radii changed from 0.0956 micron to 0.1102 micron. Under scanning electronic microscope, fine alumina powders were fused partially together and their surfaces were blunted, but coarse powders did not show such phenomena. The alumina size distribution contributes to the formation of porous structure of alumina sintered body. This porous structure is not only the shape skeleton but also the mechanical skeleton of GI-II Infiltrated Ceramic. It plays an important role in raising the mechanical properties of this kind of ceramic composite.

Fabrication and Microstructure of Hydroxyapatite Coatings on Zirconia by Room Temperature Spray Process.

Science.gov (United States)

Seo, Dong Seok; Chae, Hak Cheol; Lee, Jong Kook

2015-08-01

Hydroxyapatite coatings were fabricated on zirconia substrates by a room temperature spray process and were investigated with regards to their microstructure, composition and dissolution in water. An initial hydroxyapatite powder was prepared by heat treatment of bovine-bone derived powder at 1100 °C for 2 h, while dense zirconia substrates were fabricated by pressing 3Y-TZP powder and sintering it at 1350 °C for 2 h. Room temperature spray coating was performed using a slit nozzle in a low pressure-chamber with a controlled coating time. The phase composition of the resultant hydroxyapatite coatings was similar to that of the starting powder, however, the grain size of the hydroxyapatite particles was reduced to about 100 nm due to their formation by particle impaction and fracture. All areas of the coating had a similar morphology, consisting of reticulated structure with a high surface roughness. The hydroxyapatite coating layer exhibited biostability in a stimulated body fluid, with no severe dissolution being observed during in vitro experimentation.

Investigating the addition of SiO₂-CaO-ZnO-Na₂O-TiO₂ bioactive glass to hydroxyapatite: Characterization, mechanical properties and bioactivity.

Science.gov (United States)

Yatongchai, Chokchai; Placek, Lana M; Curran, Declan J; Towler, Mark R; Wren, Anthony W

2015-11-01

Hydroxyapatite (Ca10(PO4)6(OH)2) is widely investigated as an implantable material for hard tissue restoration due to its osteoconductive properties. However, hydroxyapatite in bulk form is limited as its mechanical properties are insufficient for load-bearing orthopedic applications. Attempts have been made to improve the mechanical properties of hydroxyapatite, by incorporating ceramic fillers, but the resultant composite materials require high sintering temperatures to facilitate densification, leading to the decomposition of hydroxyapatite into tricalcium phosphate, tetra-calcium phosphate and CaO phases. One method of improving the properties of hydroxyapatite is to incorporate bioactive glass particles as a second phase. These typically have lower softening points which could possibly facilitate sintering at lower temperatures. In this work, a bioactive glass (SiO2-CaO-ZnO-Na2O-TiO2) is incorporated (10, 20 and 30 wt%) into hydroxyapatite as a reinforcing phase. X-ray diffraction confirmed that no additional phases (other than hydroxyapatite) were formed at a sintering temperature of 560 ℃ with up to 30 wt% glass addition. The addition of the glass phase increased the % crystallinity and the relative density of the composites. The biaxial flexural strength increased to 36 MPa with glass addition, and there was no significant change in hardness as a function of maturation. The pH of the incubation media increased to pH 10 or 11 through glass addition, and ion release profiles determined that Si, Na and P were released from the composites. Calcium phosphate precipitation was encouraged in simulated body fluid with the incorporation of the bioactive glass phase, and cell culture testing in MC-3T3 osteoblasts determined that the composite materials did not significantly reduce cell viability. © The Author(s) 2015.

Characterization of hydroxyapatite substituted with silicon; Caracterizacao de hiroxiapatita substituida com silicio

Energy Technology Data Exchange (ETDEWEB)

Silva, H.M. da; Soares, G.A., E-mail: helena@metalmat.ufrj.b [Universidade Federal do Rio de Janeiro (COPPE/UFRJ), RJ (Brazil). Coordenacao dos Programas de Pos-graduacao em Engenharia. Lab. de Biomateriais para Engenharia Ossea; Mateescu, M.; Anselme, K. [Universite de Haute-Alsace (UHA/IS2M), Mulhouse (France). Inst. de Science des Materiaux; Palard, M.; Champion, E. [Universite de Limoges (France). Fac. des Sciences et Techniques

2009-07-01

Incorporation of silicon (Si) ions into hydroxyapatite structure (HA) influences on physical, chemical and physiological properties. Some studies reported the improved bioactivity Si substitution, and it also accelerates the biomineralization process. The main objective of this work is to characterize stoichiometric hydroxyapatite and hydroxyapatite substituted with 1.13% in weight of Si (SiHA) using a wet precipitation method followed by a heat treatment. SEM/EDS, AFM, DRX and FTIR analyses were used to characterize the samples. EDS and FTIR results confirmed the presence of Si. Silicon induces small changes on crystal structure of HA, not detected on X-ray diffraction patterns of sintered tablets of SiHA and HA. No secondary phases were observed, that indicates the Si had entered the HA lattice. (author)

Three-dimensional printing of porous ceramic scaffolds for bone tissue engineering.

Science.gov (United States)

Seitz, Hermann; Rieder, Wolfgang; Irsen, Stephan; Leukers, Barbara; Tille, Carsten

2005-08-01

This article reports a new process chain for custom-made three-dimensional (3D) porous ceramic scaffolds for bone replacement with fully interconnected channel network for the repair of osseous defects from trauma or disease. Rapid prototyping and especially 3D printing is well suited to generate complex-shaped porous ceramic matrices directly from powder materials. Anatomical information obtained from a patient can be used to design the implant for a target defect. In the 3D printing technique, a box filled with ceramic powder is printed with a polymer-based binder solution layer by layer. Powder is bonded in wetted regions. Unglued powder can be removed and a ceramic green body remains. We use a modified hydroxyapatite (HA) powder for the fabrication of 3D printed scaffolds due to the safety of HA as biocompatible implantable material and efficacy for bone regeneration. The printed ceramic green bodies are consolidated at a temperature of 1250 degrees C in a high temperature furnace in ambient air. The polymeric binder is pyrolysed during sintering. The resulting scaffolds can be used in tissue engineering of bone implants using patient-derived cells that are seeded onto the scaffolds. This article describes the process chain, beginning from data preparation to 3D printing tests and finally sintering of the scaffold. Prototypes were successfully manufactured and characterized. It was demonstrated that it is possible to manufacture parts with inner channels with a dimension down to 450 microm and wall structures with a thickness down to 330 microm. The mechanical strength of dense test parts is up to 22 MPa. Copyright 2005 Wiley Periodicals, Inc.

Porous SiC/SiC composites development for industrial application

International Nuclear Information System (INIS)

Maeta, S.; Hinoki, T.

2014-01-01

Silicon carbide (SiC) is promising structural materials in nuclear fields due to an excellent irradiation resistance and low activation characteristics. Conventional SiC fibers reinforced SiC matrix (SiC/SiC composites) fabricated by liquid phase sintering (LPS-SiC/SiC composites) have been required high cost and long processing time. And microstructure and mechanical property data of finally obtained LPS-SiC/SiC composites are easily scattered, because quality of the composites depend on personal skill. Thus, conventional LPS-SiC/SiC composites are inadequate for industrial use. In order to overcome these issues, the novel “porous SiC/SiC composites” have been developed by means of liquid phase sintering fabrication process. The composites consist of porous SiC matrix and SiC fibers without conventional carbon interfacial layer. The composites don’t have concerns of the degradation interfacial layer at the severe accident. Porous SiC/SiC composites preform was prepared with a thin sheet shape of SiC, sintering additives and carbon powder mixture by tape casting process which was adopted because of productive and high yielding rate fabrication process. The preform was stacked with SiC fibers and sintered in hot-press at the high temperature in argon environment. The sintered preform was decarburized obtain porous matrix structure by heat-treatment in air. Moreover, mechanical property data scattering of the obtained porous SiC/SiC composites decreased. In the flexural test, the porous SiC/SiC composites showed pseudo-ductile behavior with sufficient strength even after heat treatment at high temperature in air. From these conclusions, it was proven that porous SiC/SiC composites were reliable material at severe environment such as high temperature in air, by introducing tape casting fabrication process that could produce reproducible materials with low cost and simple way. Therefore development of porous SiC/SiC composites for industrial application was

Production of porous sintered materials using wastes of manufacturing engineering in self-propagating high-temperature synthesis

Directory of Open Access Journals (Sweden)

Y. S. Povstyana

2016-06-01

Full Text Available The increasing amount of wastes produced by the manufacturing engineering, as well as their physical and mechanical properties and restorability provide a search for sphere of their application. The actual problem of modern science is the utilization of wastes and using them in further production that will minimize their harmful impact on the environment and reduce the cost of expensive raw materials. Wastes are ideally suitable for the manufacture of porous permeable materials (filters. Powder metallurgy allows obtaining products with controlled filtration, physical and mechanical properties. Such materials are good filters for regeneration of technical liquids, oils, cooling fluids, sewage etc. The article analyzes the methods and technologies for the manufacture of porous ceramic materials and a new technology for their manufacture, which is based on use of mill scale and natural mineral – saponite as the main components. Compression technology provides products at low pressures and sintering by passing high-temperature synthesis. The proposed technology is characterized by low cost and good physical and mechanical properties of the product that gives a reason to use them for filtering and regeneration of technical liquids.

Bioactive glass/hydroxyapatite composites: mechanical properties and biological evaluation.

Science.gov (United States)

Bellucci, Devis; Sola, Antonella; Anesi, Alexandre; Salvatori, Roberta; Chiarini, Luigi; Cannillo, Valeria

2015-06-01

Bioactive glass/hydroxyapatite composites for bone tissue repair and regeneration have been produced and discussed. The use of a recently developed glass, namely BG_Ca/Mix, with its low tendency to crystallize, allowed one to sinter the samples at a relatively low temperature thus avoiding several adverse effects usually reported in the literature, such as extensive crystallization of the glassy phase, hydroxyapatite (HA) decomposition and reaction between HA and glass. The mechanical properties of the composites with 80wt.% BG_Ca/Mix and 20wt.% HA are sensibly higher than those of Bioglass® 45S5 reference samples due to the presence of HA (mechanically stronger than the 45S5 glass) and to the thermal behaviour of the BG_Ca/Mix, which is able to favour the sintering process of the composites. Biocompatibility tests, performed with murine fibroblasts BALB/3T3 and osteocites MLO-Y4 throughout a multi-parametrical approach, allow one to look with optimism to the produced composites, since both the samples themselves and their extracts do not induce negative effects in cell viability and do not cause inhibition in cell growth. Copyright © 2015 Elsevier B.V. All rights reserved.

Porous Nb-Ti based alloy produced from plasma spheroidized powder

Directory of Open Access Journals (Sweden)

Qijun Li

Full Text Available Spherical Nb-Ti based alloy powder was prepared by the combination of plasma spheroidization and mechanical alloying. Phase constituents, microstructure and surface state of the powder, and pore characteristics of the resulting porous alloy were investigated. The results show that the undissolved W and V in the mechanically alloyed powder is fully alloyed after spheroidization, and single β phase is achieved. Particle size of the spheroidized powder is in the range of 20–110 μm. With the decrease of particle size, a transformation from typical dendrite solidification structure to fine cell microstructure occurs. The surface of the spheroidized powder is coated by a layer of oxides consisting mainly of TiO2 and Nb2O5. Probabilities of sinter-neck formation and particle coalescence increases with increasing sintering temperature. Porous skeleton with relatively homogeneous pore distribution and open pore channel is formed after vacuum sintering at 1700 °C, and the porosity is 32%. The sintering kinetic analysis indicates that grain boundary diffusion is the primary mass transport mechanism during sintering process. Keywords: Powder metallurgy, Nb-Ti based alloy, Porous material, Mechanical alloying, Plasma spheroidizing, Solidification microstructure

Studies on sintering additives for hydroxyapatite, and controlled porosity structures of calcium aluminates and polypropylene-tricalcium phosphate for bone graft applications

Science.gov (United States)

Kalita, Samar Jyoti

Tissue engineering has made a significant contribution in developing new biomaterials that can restore the structural features and physiological functions of natural tissues. Various materials, such as metals, ceramics, polymers and composites have been developed for their use in hard tissue engineering applications. Part A of this thesis describes my research on HAp ceramics. HAp, a bioactive ceramic, is known for its osteoconductivity, but shows poor mechanical performance. This program aimed at improving mechanical performance of synthetic HAp by introducing small quantities of various sintering additives. A range of oxide-based sintering additives were selected and prepared. Dense compacts were prepared using a uniaxial press with an average green density of 1.6 g/cc. Results showed that some of these sintering additives improved densification, hardness and compression strength of synthetic HAp compared to the pure composition. A maximum bulk density of 3.06 g/cc was achieved for 2.5 wt% addition of MgO. A Microhardness of 4.9 GPa (505 HV) was measured for 2.5 wt% addition of BaO, and the highest compression strength (220MPa) was reported for 2.5 wt% addition of CaO. Cytotoxicity and cell proliferation studies with a modified human osteoblast (HOB) cell-line (OPC1) proved most of these materials non-toxic and biocompatible. Microscopic observation revealed that bone cells were attached and grew well on most of these ceramic matrices. Part B describes my work on development of controlled porosity polypropylene-tricalcium phosphate composite scaffolds via the fused deposition modeling (FDM) process. Hg-porosimetry was performed to determine pore size and their distribution. Uniaxial compression testing performed on samples with 36 vol% porosity and pore size of 160 mum showed the best compressive strength of 12.7 MPa. Part C includes my research on development of "3-D honeycomb" porous calcium aluminate structures via the indirect FDM process. Samples of 29% and

Sintering process optimization for multi-layer CGO membranes by in situ techniques

DEFF Research Database (Denmark)

Kaiser, Andreas; Prasad, A.S.; Foghmoes, Søren Preben Vagn

2013-01-01

The sintering of asymmetric CGO bi-layers (thin dense membrane on a porous support; Ce0.9Gd0.1O1.95-delta = CGO) with Co3O4 as sintering additive has been optimized by combination of two in situ techniques. Optical dilatometry revealed that bi-layer shape and microstructure are dramatically...... changing in a narrow temperature range of less than 100 degrees C. Below 1030 degrees C, a higher densification rate in the dense membrane layer than in the porous support leads to concave shape, whereas the densification rate of the support is dominant above 1030 degrees C, leading to convex shape. A fiat...... bi-layer could be prepared at 1030 degrees C, when shrinkage rates were similar. In situ van der Pauw measurements on tape cast layers during sintering allowed following the conductivity during sintering. A strong increase in conductivity and in activation energy E-a for conduction was observed...

Self-Consolidation Mechanism Of Porous Ti-6Al-4V Implant Prototypes Produced By Electro-Discharge-Sintering Of Spherical Ti-6Al-4V Powders

Directory of Open Access Journals (Sweden)

Lee W.H.

2015-06-01

Full Text Available Electro-Discharge-Sintering (EDS was employed to fabricate Ti-6Al-4V porous implant prototypes from atomized powders (100 – 150 μm, that were subjected to discharges of 0.75 to 2.0 kJ/0.7g-powder from 150, 300, and 450 μF capacitors. Both fully porous and porous-surfaced Ti-6Al-4V compacts with various solid core sizes were self-consolidated in less than 86 – 155 μsec. It is known that EDS can simultaneously produce the pinch pressure to squeeze and deform powder particles and the heat to weld them together. The formation of a solid core in these prototypes depends on the amounts of both the pinch pressure and heat generated during a discharge. The size of the solid core and the thickness of the porous layer can be successfully controlled by manipulating the discharge conditions such as input energy and capacitance.

Advanced Microstructural Study of Suspension Plasma Sprayed Hydroxyapatite Coatings

Science.gov (United States)

Podlesak, Harry; Pawlowski, Lech; D'Haese, Romain; Laureyns, Jacky; Lampke, Thomas; Bellayer, Severine

2010-03-01

Fine, home-synthesized, hydroxyapatite powder was formulated with water and alcohol to obtain a suspension used to plasma spray coatings onto a titanium substrate. The deposition process was optimized using statistical design of 2 n experiments with two variables: spray distance and electric power input to plasma. X-ray diffraction (XRD) was used to determine quantitatively the phase composition of obtained deposits. Raman microscopy and electron probe microanalysis (EPMA) enabled localization of the phases in different positions of the coating cross sections. Transmission electron microscopic (TEM) study associated with energy-dispersive x-ray spectroscopy (EDS) enabled visualization and analysis of a two-zone microstructure. One zone contained crystals of hydroxyapatite, tetracalcium phosphate, and a phase rich in calcium oxide. This zone included lamellas, usually observed in thermally sprayed coatings. The other zone contained fine hydroxyapatite grains that correspond to nanometric and submicrometric solids from the suspension that were agglomerated and sintered in the cold regions of plasma jet and on the substrate.

Effect of low-level laser irradiation on osteoblast-like cells cultured on porous hydroxyapatite scaffolds

Directory of Open Access Journals (Sweden)

Serena Incerti Parenti

2013-09-01

Full Text Available OBJECTIVE: To determine the effect of laser irradiation at a low dose on human osteoblastlike cells. Materials and methods: 32 porous hydroxyapatite scaffolds currently used for bone tissue engineering were seeded with MG63 cells and irradiated or not with a GaAlAs diode laser (wavelength 915 nm, dose 2 J/cm² using different power density and exposure duration. RESULTS: After 72-h incubation, cells showed well spread morphology and good adhesion on both laser-treated and untreated scaffolds. Laser irradiation did not interfere in cell viability and proliferation as compared with the non-irradiated controls. CONCLUSION: This study suggests that there is no effect of 915 nm laser irradiation at a dose of 2 J/cm² on the proliferation rate of MG63 cells. Future investigations are needed to compare different dose and wavelength regimens in order to determine the optimal set of laser parameters for maximum cell yield and safe clinical application.

Macroporous hydroxyapatite bioceramics by solid freeform fabrication: towards custom implants

CSIR Research Space (South Africa)

Richter, PW

1999-08-01

Full Text Available structure that would be impossible to make by conventional manufacturing methods. Application of this technology to the manufacture of macro porous hydroxyapatite bio ceramics for bone substitute applications is discussed. A new design is described...

Sol-gel auto-combustion synthesis of hydroxyapatite nanotubes array in porous alumina template

International Nuclear Information System (INIS)

Yuan Yuan; Liu Changsheng; Zhang Yuan; Shan Xiaoqian

2008-01-01

In this paper, an array of highly ordered hydroxyapatite (HAP) nanotubes was synthesized by sol-gel auto-combustion method with porous anodic aluminum oxide (AAO) template for the first time. Based on thermogravimetry (DTA/TG), Fourier transform infrared (FTIR) and X-ray diffraction (XRD), the dried gel, derived from the sol solution with Ca(NO 3 ) 2 .4H 2 O and PO(CH 3 O) 3 as precursors and ethylene glycol as the polymeric matrix, exhibited a typical self-propagating combustion behavior at low temperature, directly resulting in hexagonal crystalline HAP materials. The resultant HAP arrays fabricated from the above sol-gel in the AAO template were uniformly distributed, highly ordered nanotubes with uniform length and diameter according to the observations of scanning electron microscopy (SEM) and transmission electron microscope (TEM). The electron diffraction (ED), XRD and X-ray photoelectron spectroscopy (XPS) survey proved the formation of HAP phase with polycrystalline structure in the AAO template. Based on these results, a potential mechanism of 'an auto-combustion from dried gel to nanoparticles and a subsequent in situ reaction from nanoparticles to nanotubes' was proposed

Obtention of hydroxyapatite submicrometric of bovine origin by vibratory grinding for rapid prototyping; Obtencao de hidroxiapatita submicrometrica de origem bovina por moagem vibratoria visando prototipagem rapida

Energy Technology Data Exchange (ETDEWEB)

Meira, C.R.; Purquerio, B.M.; Fortulan, C.A., E-mail: camilameira@sc.usp.br [Universidade de Sao Paulo (USP), Sao Carlos, SP (Brazil). Escola de Engenharia; Braga, F.J.C. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

2011-07-01

Submicron bovine hydroxyapatite was obtained for rapid prototyping. Hydroxyapatite structure originated from bovine mineral bone has great importance among the biomaterials and biocompatibility due to its great similarity with the human bone structure. This study aims to obtain powder for manufacture by rapid prototyping of scaffolds. This technique manufacture requires highly reactive powders to compensate for the absence of pressure forming. Hydroxyapatite was milled in a ball mill and vibratory mill, and analyzed for their average equivalent spherical diameter and surface area. Test specimens were isostatically pressed at 100 MPa and machined into cylindrical test specimens. These specimens were sintered at several temperatures to determine the optimal sintering temperature based on densification and chemistry stability. In grinding ball mill was obtained particles of equivalent diameter of 0.74 micron in vibratory mill of 0.46 micrometers. An average flexural strength of 100 MPa and 99,8% of real density was attained for the sample sintered at 1300 deg C/2h, signaling potential for use in rapid prototyping. (author)

Obtaining of ceramics biphasic dense and porous; Obtencao de ceramicas bifasicas densas e porosas

Energy Technology Data Exchange (ETDEWEB)

Pallone, E.M.J.A.; Rigo, E.C.S., E-mail: eliria@usp.b [Universidade de Sao Paulo (FZEA/USP), Pirassununga, SP (Brazil). Dept. de Ciencias Basicas; Silva, K.L. [Universidade Estadual de Campinas (FEM/UNICAMP), SP (Brazil). Faculdade de Engenharia Mecanica; Rezende, M.E. [Universidade Sao Francisco, Itatiba, SP (Brazil); Fraga, A.F. [Universidade Federal de Sao Carlos (DEMa/UFSCar), SP (Brazil). Dept. de Engenharia de Materiais; Marques, R.F.C. [Universidade Federal de Alfenas (UNIFAL), Pocos de Caldas, MG (Brazil)

2010-07-01

Among the bioceramic hydroxyapatite (HAP) and beta-tricalcium phosphate (beta-TCP) are materials commonly used in biomedical field. Their combined properties result in a material with absorbable and at the same time with bioactive surface. Called biphasic ceramics such materials respond more quickly when exposed to physiological environment. In this work, powders of HAP/beta-TCP were obtained by chemical precipitation. After obtaining the post-phase was added at a ratio of 0, 15% and 30w% aqueous solutions of corn starch in order to obtain porous bodies. After mixing the resulting solutions were dried, resigned in tablet form and sintered at 1300 deg C. The initial powder was characterized by X-ray diffraction with Rietveld refinement to quantify the phases present. Bodies-of-evidence has been characterized by calculating the bulk density, X-ray diffraction (XRD), scanning electron microscopy and diametral compression. (author)

The influences of target properties and deposition times on pulsed laser deposited hydroxyapatite films

International Nuclear Information System (INIS)

Bao Quanhe; Chen Chuanzhong; Wang Diangang; Liu Junming

2008-01-01

Hydroxyapatite films were produced by pulsed laser deposition from three kinds of hydroxyapatite targets and with different deposition times. A JXA-8800R electron probe microanalyzer (EPMA) with a Link ISIS300 energy spectrum analyzer was used to give the secondary electron image (SE) and determine the element composition of the films. The phases of thin film were analyzed by a D/max-γc X-ray diffractometer (XRD). The Fourier-transform infrared spectroscopy (FT-IR) was used to characterize the hydroxyl, phosphate and other functional groups. The results show that deposited films were amorphous which mainly composed of droplet-like particles and vibration of PO 4 3- groups. With the target sintering temperature deposition times increasing, the density of droplets is decreased. While with deposition times increasing, the density of droplets is increased. With the target sintering temperature and deposition time increasing, the ratio of Ca/P is increasing and higher than that of theoretical value of HA

Induced wettability and surface-volume correlation of composition for bovine bone derived hydroxyapatite particles

Science.gov (United States)

Maidaniuc, Andreea; Miculescu, Florin; Voicu, Stefan Ioan; Andronescu, Corina; Miculescu, Marian; Matei, Ecaterina; Mocanu, Aura Catalina; Pencea, Ion; Csaki, Ioana; Machedon-Pisu, Teodor; Ciocan, Lucian Toma

2018-04-01

Hydroxyapatite powders characteristics need to be determined both for quality control purposes and for a proper control of microstructural features of bone reconstruction products. This study combines bulk morphological and compositional analysis methods (XRF, SEM-EDS, FT-IR) with surface-related methods (XPS, contact angle measurements) in order to correlate the characteristics of hydroxyapatite powders derived from bovine bone for its use in medical applications. An experimental approach for correlating the surface and volume composition was designed based on the analysis depth of each spectral method involved in the study. Next, the influences of powder particle size and forming method on the contact angle between water drops and ceramic surface were evaluated for identifying suitable strategies of tuning hydroxyapatite's wettability. The results revealed a preferential arrangement of chemical elements at the surface of hydroxyapatite particles which could induce a favourable material behaviour in terms of sinterability and biological performance.

Amorphous hydroxyapatite-sintered polymeric scaffolds for bone tissue regeneration: physical characterization studies.

Science.gov (United States)

Cushnie, Emily K; Khan, Yusuf M; Laurencin, Cato T

2008-01-01

Given the inherent shortcomings of autografts and allografts, donor-site morbidity and risk of disease transmission, respectively, alternatives to traditional bone grafting options are warranted. To this end, poly(lactide-co-glycolide) (PLAGA) and in situ-synthesized amorphous hydroxyapatite (HA) were used to construct three-dimensional microsphere-based composite scaffolds of varying HA content for bone regeneration. In the current study, the effect of adding amorphous HA to the PLAGA scaffolds on their physical characteristics and in vitro degradation mechanism was investigated. Porosimetry and uniaxial compression testing were used to analyze the internal structure and elastic modulus of the scaffolds, respectively. Additionally, gel permeation chromatography (GPC) was performed to assess the polymer molecular weight over the course of an 8-week degradation study. HA content (17% or 27%) of the composite scaffolds was found to increase scaffold pore volume from 33.86% for pure polymer scaffolds, to 40.49% or 46.29%, depending on the amount of incorporated HA. This increased pore volume provided the composite scaffolds with a greater surface area and a corresponding decrease in elastic modulus. Scaffold degradation studies conducted over 8 weeks showed PLAGA to degrade in a first-order mechanism, with the rate of polymer degradation for the 27% HA composite scaffold being significantly slower than that of the pure PLAGA scaffold (degradation constants of 0.0324 and 0.0232 week(-1), respectively). These results suggest that the addition of amorphous HA to PLAGA microspheres resulted in porous, bioactive scaffolds that offer potential as alternative bone grafting materials for the field of regenerative medicine. (c) 2007 Wiley Periodicals, Inc. J Biomed Mater Res, 2008.

Topography, wetting, and corrosion responses of electrodeposited hydroxyapatite and fluoridated hydroxyapatite on magnesium.

Science.gov (United States)

Assadian, Mahtab; Jafari, Hassan; Ghaffari Shahri, Seyed Morteza; Idris, Mohd Hasbullah; Almasi, Davood

2016-08-12

In this study, different types of calcium-phosphate phases were coated on NaOH pre-treated pure magnesium. The coating was applied by electrodeposition method in order to provide higher corrosion resistance and improve biocompatibility for magnesium. Thickness, surface morphology and topography of the coatings were analyzed using optical, scanning electron and atomic-force microscopies, respectively. Composition and chemical bonding, crystalline structures and wettability of the coatings were characterized using energy-dispersive and attenuated total reflectance-Fourier transform infrared spectroscopies, grazing incidence X-ray diffraction and contact angle measurement, respectively. Degradation behavior of the coated specimens was also investigated by potentiodynamic polarization and immersion tests. The experiments proved the presence of a porous coating dominated by dicalcium-phosphate dehydrate on the specimens. It was also verified that the developed hydroxyapatite was crystallized by alkali post-treatment. Addition of supplemental fluoride to the coating electrolyte resulted in stable and highly crystallized structures of fluoridated hydroxyapatite. The coatings were found effective to improve biocompatibility combined with corrosion resistance of the specimens. Noticeably, the fluoride supplemented layer was efficient in lowering corrosion rate and increasing surface roughness of the specimens compared to hydroxyapatite and dicalcium-phosphate dehydrates layers.

Silk as a biocohesive sacrificial binder in the fabrication of hydroxyapatite load bearing scaffolds.

Science.gov (United States)

McNamara, Stephanie L; Rnjak-Kovacina, Jelena; Schmidt, Daniel F; Lo, Tim J; Kaplan, David L

2014-08-01

Limitations of current clinical methods for bone repair continue to fuel the demand for a high strength, bioactive bone replacement material. Recent attempts to produce porous scaffolds for bone regeneration have been limited by the intrinsic weakness associated with high porosity materials. In this study, ceramic scaffold fabrication techniques for potential use in load-bearing bone repairs have been developed using naturally derived silk from Bombyx mori. Silk was first employed for ceramic grain consolidation during green body formation, and later as a sacrificial polymer to impart porosity during sintering. These techniques allowed preparation of hydroxyapatite (HA) scaffolds that exhibited a wide range of mechanical and porosity profiles, with some displaying unusually high compressive strength up to 152.4 ± 9.1 MPa. Results showed that the scaffolds exhibited a wide range of compressive strengths and moduli (8.7 ± 2.7 MPa to 152.4 ± 9.1 MPa and 0.3 ± 0.1 GPa to 8.6 ± 0.3 GPa) with total porosities of up to 62.9 ± 2.7% depending on the parameters used for fabrication. Moreover, HA-silk scaffolds could be molded into large, complex shapes, and further machined post-sinter to generate specific three-dimensional geometries. Scaffolds supported bone marrow-derived mesenchymal stem cell attachment and proliferation, with no signs of cytotoxicity. Therefore, silk-fabricated HA scaffolds show promise for load bearing bone repair and regeneration needs. Copyright © 2014 Elsevier Ltd. All rights reserved.

Improving osteointegration and osteogenesis of three-dimensional porous Ti6Al4V scaffolds by polydopamine-assisted biomimetic hydroxyapatite coating.

Science.gov (United States)

Li, Yong; Yang, Wei; Li, Xiaokang; Zhang, Xing; Wang, Cairu; Meng, Xiangfei; Pei, Yifeng; Fan, Xiangli; Lan, Pingheng; Wang, Chunhui; Li, Xiaojie; Guo, Zheng

2015-03-18

Titanium alloys with various porous structures can be fabricated by advanced additive manufacturing techniques, which are attractive for use as scaffolds for bone defect repair. However, modification of the scaffold surfaces, particularly inner surfaces, is critical to improve the osteointegration of these scaffolds. In this study, a biomimetic approach was employed to construct polydopamine-assisted hydroxyapatite coating (HA/pDA) onto porous Ti6Al4V scaffolds fabricated by the electron beam melting method. The surface modification was characterized with the field emission scanning electron microscopy, energy dispersive spectroscopy, water contact angle measurement, and confocal laser scanning microscopy. Attachment and proliferation of MC3T3-E1 cells on the scaffold surface were significantly enhanced by the HA/pDA coating compared to the unmodified surfaces. Additionally, MC3T3-E1 cells grown on the HA/pDA-coated Ti6Al4V scaffolds displayed significantly higher expression of runt-related transcription factor-2, alkaline phosphatase, osteocalcin, osteopontin, and collagen type-1 compared with bare Ti6Al4V scaffolds after culture for 14 days. Moreover, microcomputed tomography analysis and Van-Gieson staining of histological sections showed that HA/pDA coating on surfaces of porous Ti6Al4V scaffolds enhanced osteointegration and significantly promoted bone regeneration after implantation in rabbit femoral condylar defects for 4 and 12 weeks. Therefore, this study provides an alternative to biofunctionalized porous Ti6Al4V scaffolds with improved osteointegration and osteogenesis functions for orthopedic applications.

In vitro and in vivo study to the biocompatibility and biodegradation of hydroxyapatite/poly(vinyl alcohol)/gelatin composite.

NARCIS (Netherlands)

Wang, M.; Li, Y.; Wu, J.; Xu, F.; Zuo, Y.; Jansen, J.A.

2008-01-01

A novel porous composite material composed of hydroxyapatite, poly(vinyl alcohol) (PVA), and gelatin (Gel) was fabricated by emulsification. Scanning electron microscopy showed that the material had a well-interconnected porous structure including many macropores (100-500 microm) and micropores

Processing conditions and microstructural features of porous 316L stainless steel components by DMLS

Energy Technology Data Exchange (ETDEWEB)

Gu Dongdong [College of Materials Science and Technology, Nanjing University of Aeronautics and Astronautics, 29 Yudao Street, 210016 Nanjing (China)], E-mail: dongdonggu@nuaa.edu.cn; Shen Yifu [College of Materials Science and Technology, Nanjing University of Aeronautics and Astronautics, 29 Yudao Street, 210016 Nanjing (China)

2008-12-30

Direct metal laser sintering (DMLS), due to its flexibility in materials and shapes, would be especially interesting to produce complex shaped porous metallic components. In the present work, processing conditions and microstructural characteristics of direct laser sintered porous 316L stainless steel components were studied. It was found that a partial melting mechanism of powders gave a high feasibility in obtaining porous sintered structures possessing porosities of {approx}21-{approx}55%. Linear energy density (LED), which was defined by the ratio of laser power to scan speed, was used to tailor the laser sintering mechanism. A moderate LED of {approx}3400-{approx}6000 J/m and a lower scan speed less than 0.06 m/s proved to be feasible. With the favorable sintering mechanism prevailed, lowering laser power or increasing scan speed, scan line spacing, and powder layer thickness generally led to a higher porosity. Metallurgical mechanisms of pore formation during DMLS were addressed. It showed that the presence of pores was through: (i) the formation of liquid bridges between partially melted particles during laser irradiation; and (ii) the growth of sintering necks during solidification, leaving residual pores between solidified metallic agglomerates.

Processing conditions and microstructural features of porous 316L stainless steel components by DMLS

Science.gov (United States)

Gu, Dongdong; Shen, Yifu

2008-12-01

Direct metal laser sintering (DMLS), due to its flexibility in materials and shapes, would be especially interesting to produce complex shaped porous metallic components. In the present work, processing conditions and microstructural characteristics of direct laser sintered porous 316L stainless steel components were studied. It was found that a partial melting mechanism of powders gave a high feasibility in obtaining porous sintered structures possessing porosities of ˜21-˜55%. Linear energy density (LED), which was defined by the ratio of laser power to scan speed, was used to tailor the laser sintering mechanism. A moderate LED of ˜3400-˜6000 J/m and a lower scan speed less than 0.06 m/s proved to be feasible. With the favorable sintering mechanism prevailed, lowering laser power or increasing scan speed, scan line spacing, and powder layer thickness generally led to a higher porosity. Metallurgical mechanisms of pore formation during DMLS were addressed. It showed that the presence of pores was through: (i) the formation of liquid bridges between partially melted particles during laser irradiation; and (ii) the growth of sintering necks during solidification, leaving residual pores between solidified metallic agglomerates.

Processing conditions and microstructural features of porous 316L stainless steel components by DMLS

International Nuclear Information System (INIS)

Gu Dongdong; Shen Yifu

2008-01-01

Direct metal laser sintering (DMLS), due to its flexibility in materials and shapes, would be especially interesting to produce complex shaped porous metallic components. In the present work, processing conditions and microstructural characteristics of direct laser sintered porous 316L stainless steel components were studied. It was found that a partial melting mechanism of powders gave a high feasibility in obtaining porous sintered structures possessing porosities of ∼21-∼55%. Linear energy density (LED), which was defined by the ratio of laser power to scan speed, was used to tailor the laser sintering mechanism. A moderate LED of ∼3400-∼6000 J/m and a lower scan speed less than 0.06 m/s proved to be feasible. With the favorable sintering mechanism prevailed, lowering laser power or increasing scan speed, scan line spacing, and powder layer thickness generally led to a higher porosity. Metallurgical mechanisms of pore formation during DMLS were addressed. It showed that the presence of pores was through: (i) the formation of liquid bridges between partially melted particles during laser irradiation; and (ii) the growth of sintering necks during solidification, leaving residual pores between solidified metallic agglomerates.

The Properties of Sintered Calcium Phosphate with [Ca]/[P] = 1.50

Directory of Open Access Journals (Sweden)

Moo-Chin Wang

2012-10-01

Full Text Available In order to obtain the properties of the sintered as-dried calcium phosphate with [Ca]/[P] = 1.50, the characteristics of sintered pellets have been investigated using X-ray diffraction (XRD, inductively coupled plasma-mass spectrometry (ICP-MS, Fourier-transform infrared (FT-IR spectra, Vickers hardness indentation and scanning electron microscopy (SEM. When the pellet samples were sintered between 700 °C and 1200 °C for 4 h, the hydroxyapatite (Ca10(PO46(OH2, HA still maintained the major phase, accompanied with the rhenanite (NaCaPO4 as the secondary phase and β-tricalcium phosphate (β-Ca3(PO42, β-TCP as the minor phases. In addition, the HA partially transformed to α-tricalcium phosphate (α-Ca3(PO42, α-TCP and tetracalcium phosphate (Ca4(PO42O, TTCP, when the pellet samples were sintered at 1300 °C and 1400 °C, respectively, for 4 h. The maximum density and Vickers Hardness (HV of sintered pellet samples were 2.85 g/cm3 (90.18% theoretical density (T.D. and 407, which appeared at 1200 °C and 900 °C, respectively.

Sintering of bi-layered porous structures: Stress development and shape evolution

DEFF Research Database (Denmark)

Ni, De Wei; Esposito, Vincenzo; Ramousse, Severine

viscosity of layers was determined as a function of temperature and density using a vertical sintering approach. The distortion in the bi-layer configurations was experimentally recorded and compared with the analytical calculations. The sintering mismatch stress was calculated from both the camber...... development and linear strain rate mismatch, which showed a good agreement....

In situ observation and neutron diffraction of NiTi powder sintering

International Nuclear Information System (INIS)

Chen, Gang; Liss, Klaus-Dieter; Cao, Peng

2014-01-01

This study investigated NiTi powder sintering behaviour from elemental powder mixtures of Ni/Ti and Ni/TiH 2 using in situ neutron diffraction and in situ scanning electron microscopy. The sintered porous alloys have open porosities ranging from 2.7% to 36.0%. In comparison to the Ni/Ti compact, dehydrogenation occurring in the Ni/TiH 2 compact leads to less densification yet higher chemical homogenization only after high-temperature sintering. For the first time, direct evidence of the eutectoid phase transformation of NiTi at 620 °C is reported by in situ neutron diffraction. A comparative study of cyclic stress–strain behaviours of the porous NiTi alloys made from Ni/Ti and Ni/TiH 2 compacts indicate that the samples sintered from the Ni/TiH 2 compact exhibited a much higher porosity, larger pore size, lower fracture strength, lower close-to-overall porosity ratio and lower Young’s modulus. Instead of enhanced densification by the use of TiH 2 as reported in the literature, this study shows an adverse effect of TiH 2 on powder densification in NiTi

Monitoring Sintering Burn-Through Point Using Infrared Thermography

Directory of Open Access Journals (Sweden)

Francisco G. Bulnes

2013-08-01

Full Text Available Sintering is a complex industrial process that applies heat to fine particles of iron ore and other materials to produce sinter, a solidified porous material used in blast furnaces. The sintering process needs to be carefully adjusted, so that the combustion zone reaches the bottom of the material just before the discharge end. This is known as the burnthrough point. Many different parameters need to be finely tuned, including the speed and the quantities of the materials mixed. However, in order to achieve good results, sintering control requires precise feedback to adjust these parameters. This work presents a sensor to monitor the sintering burn-through point based on infrared thermography. The proposed procedure is based on the acquisition of infrared images at the end of the sintering process. At this position, infrared images contain the cross-section temperatures of the mixture. The objective of this work is to process this information to extract relevant features about the sintering process. The proposed procedure is based on four steps: key frame detection, region of interest detection, segmentation and feature extraction. The results indicate that the proposed procedure is very robust and reliable, providing features that can be used effectively to control the sintering process.

Coating of the orthopaedic titanium alloys with sol-gel derived hydroxyapatite

International Nuclear Information System (INIS)

Milev, A.; Green, D.; Chai, C.S.; Ben-Nissan, B.

1999-01-01

Hydroxyapatite (HAp) is known to be both biocompatible and bioactive material, however, due to its poor mechanical properties and design limitations is not suitable for applying as a load bearing implant. This could be overcome by using appropriate metallic substrates covered with HAp, derived via different techniques. These coatings allow improved adhesion strength of the load bearing substrate to the bone, resulting in shorter healing periods as well as predictable behaviour of the implant for longer periods of time. There are different techniques of producing HAp appropriate for coating purposes. Due to the small particle size of the grains derived, sol-gel route is preferable where lower sintering temperatures are of primary importance. For better adhesion between substrate and hydroxyapatite coating, the surface of titanium substrate, in this study, was converted to titanium nitride and/or oxynitride. Sintering temperatures of 900 deg C have been used for producing crystalline HAp coatings. The control of sol-gel solutions and the analysis of the coatings were carried out using XRD, SEM and DTA techniques. Results obtained indicate high quality HAp coatings can be produced on titanium substrates especially with complex shapes that benefits over the other coating methods

Production of Poly(ε-Caprolactone)/Hydroxyapatite Composite Scaffolds with a Tailored Macro/Micro-Porous Structure, High Mechanical Properties, and Excellent Bioactivity.

Science.gov (United States)

Kim, Jong-Woo; Shin, Kwan-Ha; Koh, Young-Hag; Hah, Min Jin; Moon, Jiyoung; Kim, Hyoun-Ee

2017-09-22

We produced poro-us poly(ε-caprolactone) (PCL)/hydroxyapatite (HA) composite scaffolds for bone regeneration, which can have a tailored macro/micro-porous structure with high mechanical properties and excellent in vitro bioactivity using non-solvent-induced phase separation (NIPS)-based 3D plotting. This innovative 3D plotting technique can create highly microporous PCL/HA composite filaments by inducing unique phase separation in PCL/HA solutions through the non-solvent-solvent exchange phenomenon. The PCL/HA composite scaffolds produced with various HA contents (0 wt %, 10 wt %, 15 wt %, and 20 wt %) showed that PCL/HA composite struts with highly microporous structures were well constructed in a controlled periodic pattern. Similar levels of overall porosity (~78 vol %) and pore size (~248 µm) were observed for all the PCL/HA composite scaffolds, which would be highly beneficial to bone tissue regeneration. Mechanical properties, such as ultimate tensile strength and compressive yield strength, increased with an increase in HA content. In addition, incorporating bioactive HA particles into the PCL polymer led to remarkable enhancements in in vitro apatite-forming ability.

Fabrication of hydroxyapatite from fish bones waste using reflux method

Science.gov (United States)

Cahyanto, A.; Kosasih, E.; Aripin, D.; Hasratiningsih, Z.

2017-02-01

The aim of this present study was to investigate the fabrication of hydroxyapatites, which were synthesized from fish bone wastes using reflux method. The fish bone wastes collected from the restaurant were brushed and boiled at 100°C for 10 minutes to remove debris and fat. After drying, the fish bones were crushed, and ball milled into a fine powder. The fish bone wastes were then processed by refluxing using KOH and H3PO4 solutions. The samples were calcined at 900°C and characterized by X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectrometry (FT-IR). The XRD pattern of samples after treatment revealed that the peak of hydroxyapatite was observed and the bands of OH- and PO4 3- were observed by FT-IR. The scanning electron microscope evaluation of sample showed the entangled crystal and porous structure of hydroxyapatite. In conclusion, the hydroxyapatite was successfully synthesized from fish bone wastes using reflux method.

In vitro performance of Ag-incorporated hydroxyapatite and its adhesive porous coatings deposited by electrostatic spraying.

Science.gov (United States)

Gokcekaya, Ozkan; Webster, Thomas J; Ueda, Kyosuke; Narushima, Takayuki; Ergun, Celaletdin

2017-08-01

Bacterial infection of implanted materials is a significant complication that might require additional surgical operations for implant retrieval. As an antibacterial biomaterial, Ag-containing hydroxyapatite (HA) may be a solution to reduce the incidences of implant associated infections. In this study, pure, 0.2mol% and 0.3mol% Ag incorporated HA powders were synthesized via a precipitation method. Colloidal precursor dispersions prepared from these powders were used to deposit porous coatings onto titanium and stainless steel substrates via electrostatic spraying. The porous coating layers obtained with various deposition times and heat treatment conditions were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Scratch tests were conducted to assess the adhesion strength of the coating. Antibacterial activity of Ag-incorporated HA was tested towards Escherichia coli (E. coli) at various incubation times. Osteoblast adhesion on Ag-incorporated HA was evaluated to assess biocompatibility. Improvement in adhesion strength of the coating layer was observed after the heat treatment process due to mutual ionic diffusion at the interface. The Ag-incorporated HA killed all viable E. coli after 24h of incubation, whereas no antibacterial activity was detected with pure HA. In addition, in vitro cell culture tests demonstrated osteoblast adhesion similar to pure HA, which indicated good cytocompatibility. In summary, results of this study provided significant promise for the future study of Ag-incorporated HA for numerous medical applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Sodium-carbonate co-substituted hydroxyapatite ceramics

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Zoltan Z. Zyman

2013-12-01

Full Text Available Powders of sodium-carbonate co-substituted hydroxyapatite, having sodium content in the range of 0.25–1.5 wt.% with a 0.25 wt.% step, were prepared by a precipitation-solid state reaction route. Compacts of the powders were sintered in a CO2 flow (4 mL/min at 1100 °C for 2 h. The sintered ceramics contained sodium and carbonate ions in the ranges of 0–1.5 wt.% and 1.3–6 wt.%, respectively, which are typical impurity concentrations in biological apatite. A relationship between sodium and carbonate contents and the type of carbonate substitution was found. The total carbonate content progressively increased with the sodium content. The obtained ceramics showed an AB-type carbonate substitution. However, the substitution became more B-type as the sodium content increased. As a result, the carbonation was almost B-type (94 % for the highest sodium content (1.5 wt.%.

Microstructures and photocatalytic properties of porous ZnO films synthesized by chemical bath deposition method

International Nuclear Information System (INIS)

Wang Huihu; Dong, Shijie; Chang Ying; Zhou Xiaoping; Hu Xinbin

2012-01-01

Different porous ZnO film structures on the surface of alumina substrates were prepared through a simple chemical bath deposition method in the methanolic zinc acetate solution. The surface morphology and phase structure of porous ZnO film were determined by scanning electron microscopy (SEM) and X-ray diffraction (XRD), respectively. Both initial zinc acetate concentration and sintering temperature have great impact on the final film structures. With the increase of initial zinc acetate concentration, the porous structures can be finely tuned from circular nest like assemblies composed film into successive nest like film, and finally to globular aggregates composed film. By increasing the sintering temperature, the porous structure of successive nest like film can be further controlled. Furthermore, the crystallinity of photocatalysts also can be greatly improved. The photodegradation results of Methyl Orange revealed that porous ZnO film with successive nest like structure sintered at 500 °C exhibited the highest photocatalytic activity under UV illumination.

Porous biomorphic silicon carbide ceramics coated with hydroxyapatite as prospective materials for bone implants

Energy Technology Data Exchange (ETDEWEB)

Gryshkov, Oleksandr, E-mail: gryshkov@imp.uni-hannover.de [Institute for Multiphase Processes, Leibniz Universität Hannover, 30167 Hannover (Germany); Klyui, Nickolai I., E-mail: klyuini@ukr.net [College of Physics, Jilin University, 130012 Changchun (China); V. Lashkaryov Institute of Semiconductor Physics, National Academy of Science of Ukraine, 03028 Kyiv (Ukraine); Temchenko, Volodymyr P., E-mail: tvp@isp.kiev.ua [V. Lashkaryov Institute of Semiconductor Physics, National Academy of Science of Ukraine, 03028 Kyiv (Ukraine); Kyselov, Vitalii S., E-mail: kyselov@isp.kiev.ua [V. Lashkaryov Institute of Semiconductor Physics, National Academy of Science of Ukraine, 03028 Kyiv (Ukraine); Chatterjee, Anamika, E-mail: chatterjee@imp.uni-hannover.de [Institute for Multiphase Processes, Leibniz Universität Hannover, 30167 Hannover (Germany); Belyaev, Alexander E., E-mail: belyaev@isp.kiev.ua [V. Lashkaryov Institute of Semiconductor Physics, National Academy of Science of Ukraine, 03028 Kyiv (Ukraine); Lauterboeck, Lothar, E-mail: lauterboeck@imp.uni-hannover.de [Institute for Multiphase Processes, Leibniz Universität Hannover, 30167 Hannover (Germany); Iarmolenko, Dmytro, E-mail: iarmolenko.dmytro@isp.kiev.ua [V. Lashkaryov Institute of Semiconductor Physics, National Academy of Science of Ukraine, 03028 Kyiv (Ukraine); Glasmacher, Birgit, E-mail: glasmacher@imp.uni-hannover.de [Institute for Multiphase Processes, Leibniz Universität Hannover, 30167 Hannover (Germany)

2016-11-01

Porous and cytocompatible silicon carbide (SiC) ceramics derived from wood precursors and coated with bioactive hydroxyapatite (HA) and HA-zirconium dioxide (HA/ZrO{sub 2}) composite are materials with promising application in engineering of bone implants due to their excellent mechanical and structural properties. Biomorphic SiC ceramics have been synthesized from wood (Hornbeam, Sapele, Tilia and Pear) using a forced impregnation method. The SiC ceramics have been coated with bioactive HA and HA/ZrO{sub 2} using effective gas detonation deposition approach (GDD). The surface morphology and cytotoxicity of SiC ceramics as well as phase composition and crystallinity of deposited coatings were analyzed. It has been shown that the porosity and pore size of SiC ceramics depend on initial wood source. The XRD and FTIR studies revealed the preservation of crystal structure and phase composition of in the HA coating, while addition of ZrO{sub 2} to the initial HA powder resulted in significant decomposition of the final HA/ZrO{sub 2} coating and formation of other calcium phosphate phases. In turn, NIH 3T3 cells cultured in medium exposed to coated and uncoated SiC ceramics showed high re-cultivation efficiency as well as metabolic activity. The recultivation efficiency of cells was the highest for HA-coated ceramics, whereas HA/ZrO{sub 2} coating improved the recultivation efficiency of cells as compared to uncoated SiC ceramics. The GDD method allowed generating homogeneous HA coatings with no change in calcium to phosphorus ratio. In summary, porous and cytocompatible bio-SiC ceramics with bioactive coatings show a great promise in construction of light, robust, inexpensive and patient-specific bone implants for clinical application. - Highlights: • Synthesis and characterization of porous biomorphic SiC ceramics derived from wood • Successful deposition of bioactive calcium phosphate coatings using gas detonation deposition • Porosity and pore size of Si

Porous biomorphic silicon carbide ceramics coated with hydroxyapatite as prospective materials for bone implants

International Nuclear Information System (INIS)

Gryshkov, Oleksandr; Klyui, Nickolai I.; Temchenko, Volodymyr P.; Kyselov, Vitalii S.; Chatterjee, Anamika; Belyaev, Alexander E.; Lauterboeck, Lothar; Iarmolenko, Dmytro; Glasmacher, Birgit

2016-01-01

Porous and cytocompatible silicon carbide (SiC) ceramics derived from wood precursors and coated with bioactive hydroxyapatite (HA) and HA-zirconium dioxide (HA/ZrO 2 ) composite are materials with promising application in engineering of bone implants due to their excellent mechanical and structural properties. Biomorphic SiC ceramics have been synthesized from wood (Hornbeam, Sapele, Tilia and Pear) using a forced impregnation method. The SiC ceramics have been coated with bioactive HA and HA/ZrO 2 using effective gas detonation deposition approach (GDD). The surface morphology and cytotoxicity of SiC ceramics as well as phase composition and crystallinity of deposited coatings were analyzed. It has been shown that the porosity and pore size of SiC ceramics depend on initial wood source. The XRD and FTIR studies revealed the preservation of crystal structure and phase composition of in the HA coating, while addition of ZrO 2 to the initial HA powder resulted in significant decomposition of the final HA/ZrO 2 coating and formation of other calcium phosphate phases. In turn, NIH 3T3 cells cultured in medium exposed to coated and uncoated SiC ceramics showed high re-cultivation efficiency as well as metabolic activity. The recultivation efficiency of cells was the highest for HA-coated ceramics, whereas HA/ZrO 2 coating improved the recultivation efficiency of cells as compared to uncoated SiC ceramics. The GDD method allowed generating homogeneous HA coatings with no change in calcium to phosphorus ratio. In summary, porous and cytocompatible bio-SiC ceramics with bioactive coatings show a great promise in construction of light, robust, inexpensive and patient-specific bone implants for clinical application. - Highlights: • Synthesis and characterization of porous biomorphic SiC ceramics derived from wood • Successful deposition of bioactive calcium phosphate coatings using gas detonation deposition • Porosity and pore size of SiC ceramics depend on wood

Porous Nb-Ti based alloy produced from plasma spheroidized powder

Science.gov (United States)

Li, Qijun; Zhang, Lin; Wei, Dongbin; Ren, Shubin; Qu, Xuanhui

Spherical Nb-Ti based alloy powder was prepared by the combination of plasma spheroidization and mechanical alloying. Phase constituents, microstructure and surface state of the powder, and pore characteristics of the resulting porous alloy were investigated. The results show that the undissolved W and V in the mechanically alloyed powder is fully alloyed after spheroidization, and single β phase is achieved. Particle size of the spheroidized powder is in the range of 20-110 μm. With the decrease of particle size, a transformation from typical dendrite solidification structure to fine cell microstructure occurs. The surface of the spheroidized powder is coated by a layer of oxides consisting mainly of TiO2 and Nb2O5. Probabilities of sinter-neck formation and particle coalescence increases with increasing sintering temperature. Porous skeleton with relatively homogeneous pore distribution and open pore channel is formed after vacuum sintering at 1700 °C, and the porosity is 32%. The sintering kinetic analysis indicates that grain boundary diffusion is the primary mass transport mechanism during sintering process.

Decomposition of dual hydroxyapatite/fluoroapatite coatings on metal substrates

International Nuclear Information System (INIS)

Wei, M.; Evans, J.H.; Wentrup-Byrne, E.

2000-01-01

In order to prevent the formation of tricalcium phosphate (TCP), a relatively weak and rapidly biodegradable biomaterial, during sintering of hydroxyapatite (Hap) onto metal substrates, a novel two layer coating was applied. This was achieved by pre-coating the substrate with either Hap or fluorapatite (Fap) which preserved the purity of the Hap top coating. However, Fap is more stable thermally than Hap. The composition of Hap and Fap were determined by x-ray diffraction and infrared spectroscopy. A scanning electron microscope was also used to characterise the surface morphologiy of the coatings. By using Fap the formation of TCP was totally prevented through out the coatings at a sintering temperature of 1050 deg C at which a relatively dense Hap outer coating was produced. Copyright (2000) The Australian Ceramic Society

Preparation of steel slag porous sound-absorbing material using coal powder as pore former.

Science.gov (United States)

Sun, Peng; Guo, Zhancheng

2015-10-01

The aim of the study was to prepare a porous sound-absorbing material using steel slag and fly ash as the main raw material, with coal powder and sodium silicate used as a pore former and binder respectively. The influence of the experimental conditions such as the ratio of fly ash, sintering temperature, sintering time, and porosity regulation on the performance of the porous sound-absorbing material was investigated. The results showed that the specimens prepared by this method had high sound absorption performance and good mechanical properties, and the noise reduction coefficient and compressive strength could reach 0.50 and 6.5MPa, respectively. The compressive strength increased when the dosage of fly ash and sintering temperature were raised. The noise reduction coefficient decreased with increasing ratio of fly ash and reducing pore former, and first increased and then decreased with the increase of sintering temperature and time. The optimum preparation conditions for the porous sound-absorbing material were a proportion of fly ash of 50% (wt.%), percentage of coal powder of 30% (wt.%), sintering temperature of 1130°C, and sintering time of 6.0hr, which were determined by analyzing the properties of the sound-absorbing material. Copyright © 2015. Published by Elsevier B.V.

Porous biomorphic silicon carbide ceramics coated with hydroxyapatite as prospective materials for bone implants.

Science.gov (United States)

Gryshkov, Oleksandr; Klyui, Nickolai I; Temchenko, Volodymyr P; Kyselov, Vitalii S; Chatterjee, Anamika; Belyaev, Alexander E; Lauterboeck, Lothar; Iarmolenko, Dmytro; Glasmacher, Birgit

2016-11-01

Porous and cytocompatible silicon carbide (SiC) ceramics derived from wood precursors and coated with bioactive hydroxyapatite (HA) and HA-zirconium dioxide (HA/ZrO2) composite are materials with promising application in engineering of bone implants due to their excellent mechanical and structural properties. Biomorphic SiC ceramics have been synthesized from wood (Hornbeam, Sapele, Tilia and Pear) using a forced impregnation method. The SiC ceramics have been coated with bioactive HA and HA/ZrO2 using effective gas detonation deposition approach (GDD). The surface morphology and cytotoxicity of SiC ceramics as well as phase composition and crystallinity of deposited coatings were analyzed. It has been shown that the porosity and pore size of SiC ceramics depend on initial wood source. The XRD and FTIR studies revealed the preservation of crystal structure and phase composition of in the HA coating, while addition of ZrO2 to the initial HA powder resulted in significant decomposition of the final HA/ZrO2 coating and formation of other calcium phosphate phases. In turn, NIH 3T3 cells cultured in medium exposed to coated and uncoated SiC ceramics showed high re-cultivation efficiency as well as metabolic activity. The recultivation efficiency of cells was the highest for HA-coated ceramics, whereas HA/ZrO2 coating improved the recultivation efficiency of cells as compared to uncoated SiC ceramics. The GDD method allowed generating homogeneous HA coatings with no change in calcium to phosphorus ratio. In summary, porous and cytocompatible bio-SiC ceramics with bioactive coatings show a great promise in construction of light, robust, inexpensive and patient-specific bone implants for clinical application. Copyright © 2016 Elsevier B.V. All rights reserved.

Identification of Material Parameters for the Simulation of Acoustic Absorption of Fouled Sintered Fiber Felts

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Nicolas Lippitz

2016-08-01

Full Text Available As a reaction to the increasing noise pollution, caused by the expansion of airports close to residential areas, porous trailing edges are investigated to reduce the aeroacoustic noise produced by flow around the airframe. Besides mechanical and acoustical investigations of porous materials, the fouling behavior of promising materials is an important aspect to estimate the performance in long-term use. For this study, two sintered fiber felts were selected for a long-term fouling experiment where the development of the flow resistivity and accumulation of dirt was observed. Based on 3D structural characterizations obtained from X-ray tomography of the initial materials, acoustic models (Biot and Johnson–Champoux–Allard in the frame of the transfer matrix method were applied to the sintered fiber felts. Flow resistivity measurements and the measurements of the absorption coefficient in an impedance tube are the basis for a fouling model for sintered fiber felts. The contribution will conclude with recommendations concerning the modeling of pollution processes of porous materials.

Sol gel-derived hydroxyapatite films over porous calcium polyphosphate substrates for improved tissue engineering of osteochondral-like constructs.

Science.gov (United States)

Lee, Whitaik David; Gawri, Rahul; Pilliar, Robert M; Stanford, William L; Kandel, Rita A

2017-10-15

Integration of in vitro-formed cartilage on a suitable substrate to form tissue-engineered implants for osteochondral defect repair is a considerable challenge. In healthy cartilage, a zone of calcified cartilage (ZCC) acts as an intermediary for mechanical force transfer from soft to hard tissue, as well as an effective interlocking structure to better resist interfacial shear forces. We have developed biphasic constructs that consist of scaffold-free cartilage tissue grown in vitro on, and interdigitated with, porous calcium polyphosphate (CPP) substrates. However, as CPP degrades, it releases inorganic polyphosphates (polyP) that can inhibit local mineralization, thereby preventing the formation of a ZCC at the interface. Thus, we hypothesize that coating CPP substrate with a layer of hydroxyapatite (HA) might prevent or limit this polyP release. To investigate this we tested both inorganic or organic sol-gel processing methods, asa barrier coating on CPP substrate to inhibit polyP release. Both types of coating supported the formation of ZCC in direct contact with the substrate, however the ZCC appeared more continuous in the tissue formed on the organic HA sol gel coated CPP. Tissues formed on coated substrates accumulated comparable quantities of extracellular matrix and mineral, but tissues formed on organic sol-gel (OSG)-coated substrates accumulated less polyP than tissues formed on inorganic sol-gel (ISG)-coated substrates. Constructs formed with OSG-coated CPP substrates had greater interfacial shear strength than those formed with ISG-coated and non-coated substrates. These results suggest that the OSG coating method can modify the location and distribution of ZCC and can be used to improve the mechanical integrity of tissue-engineered constructs formed on porous CPP substrates. Articular cartilage interfaces with bone through a zone of calcified cartilage. This study describes a method to generate an "osteochondral-like" implant that mimics this

Physical-mechanical characterization of hydroxyapatite-titanium oxide composites made by the polymeric sponge method

International Nuclear Information System (INIS)

Galdino, A.G.S.; Zavaglia, C.A.C.

2011-01-01

Bioceramics have been used as bone reconstruction materials since last decades, where hydroxyapatite is one of the most used for this purpose. However, hydroxyapatite's mechanical strength is not so high when compared to other bioceramics. This work aimed on characterizing physically and mechanically composites of HA-TiO_2. Samples were made by the polymeric sponge method with 70% - 30% wt., 60% - 40% wt. and 50% - 50% wt. of HA - TiO_2, calcined at 550 deg C for sponge burning and sintered at 1250 deg C, 1300 deg C and 1350 deg C. Samples were submitted to mechanical essays of compression and Hardness Vickers and to physical essays of water absorption, apparent density, burning linear retraction and apparent density. Results showed relatively better than those of pure hydroxyapatite and they are in accordance with the literature. (author)

Characterization,Mechanical, and In Vitro Bioactivity Properties of Hydroxyapatite/Bioactive Glass Composite

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Israa Kahatan Sabree

2016-12-01

Full Text Available Bioactive ceramic materials can help bone reparation and regeneration by offering support to bone growth. Biological hydroxyapatite powder was prepared by burning animal bone followed by studying the mechanical properties of hydroxyapatite (HA/ (20wt.%, and 40wt.% of binary bioactive glass (70% SiO2- 30% CaO in order to evaluate the influence of composition on the compressive strength and hardness. HA-composite material exhibited increasing density, microhardness, and compressive strength with increasing amount of glass addition. X-ray diffraction after sintering at 1200°C showed no alter of HA to secondary phases while the hydroxyapatite/ bioactive glass composites contained a HA phase and different amounts of wollastonite phase, depending on the amount of bioglass added. In vitro tests, the samples were soaked in simulated body fluid (SBF for ten days in order to evaluate the change in compression strength, weight loss, and pH. The HA composite reinforced with 40 wt % bioglass showed highest compression strength, and lowest weight loss

Fabrication and evaluation of porous Ti–HA bio-nanomaterial by leaching process

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A.M. Omran

2015-05-01

Full Text Available A porous surface of Ti–HA composite was successfully fabricated by pulsed current activated sintering (PCAS, followed by leaching using diluted H3PO4. The Ti and HA powders were mixed at different contents of the HA, Ti-5, 10, 30 and 40 wt% HA powders. The mixed powders were pressed in a coated graphite die using pulsed current activated sintering (PCAS under pressure of 60 MPa at temperature of 1000 °C for 5 min. The sintered Ti–HA specimens were immersed in the eight kinds of leaching solutions at room temperature for 24 h. The leached specimen’s surfaces were characterized using XRD, SEM, EDX and Rockwell hardness. The XRD patterns after sintering show that many phases were detected at the sintered specimen surfaces such as; Ti2O, CaO, CaTiO3, TixPy in addition to the remaining Ti and HA. Furthermore, the high concentration H3PO4 leaching solution is more efficient than the low concentration. Also the produced porous surfaces of Ti–HA materials containing more than 30% HA have a low relative density and hardness than the commercial Ti–6Al–4V ELI alloy. In a word, the presence of porous surface coated by HA will promote the nucleation of the biological apatite created with the human tissue and increase the bonding between them. So, the produced porous materials are considered so easy for the muscle cells to permeate after transplanted with high coherence.

Ectopic osteogenesis and angiogenesis regulated by porous architecture of hydroxyapatite scaffolds with similar interconnecting structure in vivo

Science.gov (United States)

Li, Jinyu; Zhi, Wei; Xu, Taotao; Shi, Feng; Duan, Ke; Wang, Jianxin; Mu, Yandong; Weng, Jie

2016-01-01

The macro-pore sizes of porous scaffold play a key role for regulating ectopic osteogenesis and angiogenesis but many researches ignored the influence of interconnection between macro-pores with different sizes. In order to accurately reveal the relationship between ectopic osteogenesis and macro-pore sizes in dorsal muscle and abdominal cavities of dogs, hydroxyapatite (HA) scaffolds with three different macro-pore sizes of 500–650, 750–900 and 1100–1250 µm were prepared via sugar spheres-leaching process, which also had similar interconnecting structure determined by keeping the d/s ratio of interconnecting window diameter to macro-pore size constant. The permeability test showed that the seepage flow of fluid through the porous scaffolds increased with the increase of macro-pore sizes. The cell growth in three scaffolds was not affected by the macro-pore sizes. The in vivo ectopic implantation results indicated that the macro-pore sizes of HA scaffolds with the similar interconnecting structure have impact not only the speed of osteogenesis and angiogenesis but also the space distribution of newly formed bone. The scaffold with macro-pore sizes of 750–900 µm exhibited much faster angiogenesis and osteogenesis, and much more uniformly distribution of new bone than those with other macro-pore sizes. This work illustrates the importance of a suitable macro-pore sizes in HA scaffolds with the similar interconnecting structure which provides the environment for ectopic osteogenesis and angiogenesis. PMID:27699059

Deformation behavior of sintered nanocrystalline silver layers

International Nuclear Information System (INIS)

Zabihzadeh, S.; Van Petegem, S.; Duarte, L.I.; Mokso, R.; Cervellino, A.; Van Swygenhoven, H.

2015-01-01

The microstructure of porous silver layers produced under different low temperature pressure-assisted sintering conditions is characterized and linked with the mechanical behavior studied in situ during X-ray diffraction. Peak profile analysis reveals important strain recovery and hardening mechanism during cyclic deformation. The competition between both mechanisms is discussed in terms of porosity and grain size

Hidroxiapatita porosa produzida através do gelcasting de espumas visando aplicações biomédicas Porous hydroxyapatite prepared by gelcating of foams for biomedical applications

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P. Sepúlveda

1999-12-01

Full Text Available Hidroxiapatita porosa foi produzida por meio de uma nova técnica de processamento, visando aplicações na área de implantes ósseos. A produção do material poroso é feita através da produção de espumas pela agitação de suspensões cerâmicas aquosas contendo tensoativos adequados. A solidificação que segue é obtida pela adição de reagentes iniciadores da polimerização in situ de monômeros orgânicos, inicialmente incluídos nas composições, formando um gel. Este método permite a produção de corpos com formatos de alta complexidade e elevada resistência mecânica com níveis de porosidade próximos de 90%vol, que suportam corte e torneamento no estado a verde. Os aditivos orgânicos são eliminados a 300 °C e sinterização a 1350 °C é efetuada para consolidação da matriz. A otimização da resistência mecânica decorre da combinação entre uma matriz cerâmica de alta densidade a uma estrutura de poros esféricos com diâmetros que variam de 20-1000 mm possuindo inter-conecções de aproximadamente 10-100 mm, dependendo da densidade. O material sinterizado foi avaliado quanto a sua citoxicidade, utilizando-se o método quantitativo de formação de colônias que calcula o índice de citotoxicidade IC50(% após contato do extrato do material com células de mamíferos. Os resultados mostraram que o processo de fabricação e os reagentes utilizados não afetaram os baixos níveis de toxicidade do pó de hidroxiapatita que era originalmente de pureza biomédica.A novel technique has been applied to manufacture porous hydroxyapatite for implant applications. The process involved generation of foam from an aqueous suspension of the powder followed by in situ polymerisation of organic monomers, which had been previously added to the compositions. This method produces strong gelled and complex-shaped bodies with up to 90% porosity that can withstand machining in the green state. The organic additives are eliminated at

Strength behaviour of sintered steel from the view of design-relevant material data

International Nuclear Information System (INIS)

Sonsino, C.M.; Esper, F.J.; Leuze, G.

1982-01-01

A reliable design of sintered components and an aimed material's selection requires the knowledge of designrelevant material data as Cyclic stress-strain-curves, crack propagation and fracture toughness properties as well as statistically evaluated S-N-curves, because conventional material data as tensile strength, monotonic yield strength, elongation, area reduction and impact strength can lead to a false estimation of the material's fatigue behaviour. For this reason the powder metallurgical industry began to determine design-relevant material data on the example of the porous Fe-Cu-C- and Fe-Cu-Ni-alloys. The fatigue tests with notched specimen and different modes of loading show that porous sintered parts having mechanical notches are less sensitive to external notches than wrought steel, because crack-propagation is delayed by pores. The possibility to manufacture cyclic hardening alloys, their relative notch-insensitivity and with wrought steel comparable scatter of fatigue properties show the importance of sintered alloys as alternative materials. (orig.) [de

Sol-Gel Derived Hydroxyapatite Coating on Mg-3Zn Alloy for Orthopedic Application

Science.gov (United States)

Singh, Sanjay; Manoj Kumar, R.; Kuntal, Kishor Kumar; Gupta, Pallavi; Das, Snehashish; Jayaganthan, R.; Roy, Partha; Lahiri, Debrupa

2015-04-01

In recent years, magnesium and its alloys have gained a lot of interest as orthopedic implant constituents because their biodegradability and mechanical properties are closer to that of human bone. However, one major concern with Mg in orthopedics is its high corrosion rate that results in the reduction of mechanical integrity before healing the bone tissue. The current study evaluates the sol-gel-derived hydroxyapatite (HA) coating on a selected Mg alloy (Mg-3Zn) for decreasing the corrosion rate and increasing the bioactivity of the Mg surface. The mechanical integrity of the coating is established as a function of the surface roughness of the substrate and the sintering temperature of the coating. Coating on a substrate roughness of 15-20 nm and sintering at 400°C shows the mechanical properties in similar range of bone, thus making it suitable to avoid the stress-shielding effect. The hydroxyapatite coating on the Mg alloy surface also increases corrosion resistance very significantly by 40 times. Bone cells are also found proliferating better in the HA-coated surface. All these benefits together establish the candidature of sol-gel HA-coated Mg-3Zn alloy in orthopedic application.

Investigation on Mechanical Properties and Microstructure of Hydroxyapatite-SiCw Composite Bioceramics

Institute of Scientific and Technical Information of China (English)

无

2005-01-01

Hydroxyapatite-SiCw composite micropowder was synthesized using in-situ composite method,and hydroxyapatite-SiCw composite bioceramics with different content of SiCw were produced by hot pressing sintering method. The microstructures of the materials were analyzed by SEM, and the relative density, bending strength and fracture toughness of the materials were tested. The results show that the mechanical properties of composite material are best when the whisker content is 20-23.7% . The mechanical properties of the material are the best when the tensile stress acted on the composite material is parallel with the hot pressing plane, and they are the worst when the tensile stress acted on the composite material is normal to the hot pressing plane.

Influence of corn flour as pore forming agent on porous ceramic material based mullite: Morphology and mechanical properties

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Ayala-Landeros J.G.

2016-01-01

Full Text Available Porous material was processed by the mixing, molding and pressing the ceramic material, afterward burnout and sintering; through the forming porous, using corn flour at different concentration (10, 15 and 20 wt.% as a pore forming agent; in order to determinate the influence of porous on the mechanical, morphological and structural properties. The effect of the volume fraction of corn flour in the mullite matrix, at various sintering temperature from 1100, 1200, 1300 and 1500°C were tested by Diffraction X ray, showing changes in crystalline phases of mullite (3Al2O3-2SiO2, as result of sintered temperatures. Presence of talcum powder in formula, also cause the formation of the cordierite and cristobalite crystalline phases, giving stability and adhesion to the structure of ceramic material. When sintering at temperatures between 1300 to 1500°C, and it was used the concentration of corn flour 15-20 wt.% as forming agent porous, it was found the better mechanical properties. The scanning electron microscopy analysis shows the presence of open porosity and anisotropy.

One-stage explant-implant procedure of exposed porous orbital implants

DEFF Research Database (Denmark)

Toft, Peter B; Rasmussen, Marie L Roed; Prause, Jan Ulrik

2011-01-01

Purpose:  To investigate the risks of implant exposure after a combined explant-implant procedure in patients with an exposed porous orbital implant. Methods:  Twenty-four consecutive patients who had a combined explant-implant procedure of an exposed hydroxyapatite (21) or porous polyethylene (3...... at the same procedure in sockets without profound signs of infection. The procedure carries a possible risk of poor motility....

Glass-ceramic coating material for the CO2 laser based sintering of thin films as caries and erosion protection.

Science.gov (United States)

Bilandžić, Marin Dean; Wollgarten, Susanne; Stollenwerk, Jochen; Poprawe, Reinhart; Esteves-Oliveira, Marcella; Fischer, Horst

2017-09-01

The established method of fissure-sealing using polymeric coating materials exhibits limitations on the long-term. Here, we present a novel technique with the potential to protect susceptible teeth against caries and erosion. We hypothesized that a tailored glass-ceramic material could be sprayed onto enamel-like substrates to create superior adhesion properties after sintering by a CO 2 laser beam. A powdered dental glass-ceramic material from the system SiO 2 -Na 2 O-K 2 O-CaO-Al 2 O 3 -MgO was adjusted with individual properties suitable for a spray coating process. The material was characterized using X-ray fluorescence analysis (XRF), heating microscopy, dilatometry, scanning electron microscopy (SEM), grain size analysis, biaxial flexural strength measurements, fourier transform infrared spectroscopy (FTIR), and gas pycnometry. Three different groups of samples (each n=10) where prepared: Group A, powder pressed glass-ceramic coating material; Group B, sintered hydroxyapatite specimens; and Group C, enamel specimens (prepared from bovine teeth). Group B and C where spray coated with glass-ceramic powder. All specimens were heat treated using a CO 2 laser beam process. Cross-sections of the laser-sintered specimens were analyzed using laser scanning microscopy (LSM), energy dispersive X-ray analysis (EDX), and SEM. The developed glass-ceramic material (grain size d50=13.1mm, coefficient of thermal expansion (CTE)=13.310 -6 /K) could be spray coated on all tested substrates (mean thickness=160μm). FTIR analysis confirmed an absorption of the laser energy up to 95%. The powdered glass-ceramic material was successfully densely sintered in all sample groups. The coating interface investigation by SEM and EDX proved atomic diffusion and adhesion of the glass-ceramic material to hydroxyapatite and to dental enamel. A glass-ceramic material with suitable absorption properties was successfully sprayed and laser-sintered in thin films on hydroxyapatite as well as on

Corrosion behaviour of porous chromium carbide/oxide based ceramics in supercritical water

International Nuclear Information System (INIS)

Dong, Z.; Xin, T.; Chen, W.; Zheng, W.; Guzonas, D.

2011-01-01

Porous chromium carbide with a high density of open pores was fabricated by a reactive sintering method. Chromium oxide ceramics were obtained by re-oxidizing the porous chromium carbides formed. Some samples were added with yttria at 5 wt. %, prior to reactive sintering to form porous structures. Corrosion tests in SCW were performed at temperatures ranging from 375 o C to 625 o C with a fixed pressure at around 25∼30 MPa. The results show that chromium carbide is stable in SCW environments at temperatures up to 425 o C, above which disintegration of carbides through oxidation occurs. Porous chromium oxide samples show better corrosion resistance than porous chromium carbide, but disintegrate in SCW at around 625 o C. Among all the samples tested, chromium oxide ceramics with added yttria exhibited much better corrosion resistance compared with the pure chromium carbide/oxides. No evidence of weight change or disintegration of porous chromium oxides with 5 wt % added yttria was observed after exposure at 625 o C in SCW for 600 hours. (author)

Preparation and Luminescent Properties of the antibacterial materials of the La3+ Doped Sm3+-Hydroxyapatite

Science.gov (United States)

Lv, Yuguang; Shi, Qi; Jin, Yuling; Ren, Hengxin; Qin, Yushan; Wang, Bo; Song, Shanshan

2018-03-01

In this paper, the La3+-doped Sm3+ hydroxyapatite (La/Sm/HAP) complexes were prepared by a precipitation method. The sample was defined by IR spectra, fluorescence spectra and X ray diffraction analysis et al. The structure of complexes were discussed. The emission wavelength of heat treatment of Sm3+ do not change, but will affect the intensity of the peak Sm3+ luminescence properties and the occupy hydroxyapatite in the lattice Ca( II )and Ca( I ) loci with Sm3+ doped concentration and the proportion of the sintering temperature change and change: The nano hydroxyapatite complex of the La3+ doped samarium obtain the good fluorescence intensity, by La3+ doping content of Sm3+ were hydroxyapatite 6% (La3+, Sm3+ mole ratio) device. The complex of La3+ doped samarium HAP have Stable chemical property, fluorescence property and excellent biological activity. The ligand HAP absorbs energy or captures an electron-hole pair and then transfers it to the lanthanide ions. The catalytic activity influence of the La3+-doped Sm3+hydroxyapatite was discussed, the La/Sm/HAP had excellent antibacterial property, which used as potential biological antibacterial material.

Fabrication and characterization of porous hydroxyapatite ocular ...

Indian Academy of Sciences (India)

Unknown

risk of life or risk to the other eye of the patient. The lost eye can be ... fibrovascular growth are termed as integrated implants. Porous implants have the .... They were maintained under identical environment, management and standard diet with ...

Manufacturing of metallic porous structures to be used in capillary pumping systems

Directory of Open Access Journals (Sweden)

Eduardo Gonçalves Reimbrecht

2003-12-01

Full Text Available Sintered metallic porous structures have an application as capillary structures in two-phase heat transfer loops. In this work the manufacturing procedure of tubular porous structures for capillary pump application is discussed. The application of porous structures on capillary pumping systems requires porosity higher than 40% and pore size diameter lower than 20 µm. Carbonyl nickel powder with particle diameter between 3 and 7 µm and stainless steel AISI316L powder with particle diameter between 1 and 22 µm were used as raw material. Sintering under hydrogen atmosphere was performed both in a resistive furnace and in a plasma reactor. Temperature and time were the modified parameters to obtain suitable porosity and roundness on the samples. The porosity was measured using the Arquimedes Principle (MPIF-42, the roundness was evaluated using a simplified measurement technique of the sample diameter and the pore size distribution was determined by image analysis techniques. Images obtained by Scanning Electronic Microscopy were employed on the image analysis. The sintering parameters selected to manufacture nickel samples were 700 °C and 30 min resulting in a porosity of about 44%. The sintering parameters selected to manufacture stainless steel samples were 1000 °C and 30 min resulting in a porosity of about 40%.

Porosity Dependence of Piezoelectric Properties for Porous Potassium Niobate System Ceramics

Energy Technology Data Exchange (ETDEWEB)

Wada, S; Mase, Y; Shimizu, S; Maeda, K; Fujii, I; Nakashima, K; Pulpan, P; Miyajima, N, E-mail: swada@yamanashi.ac.jp [Interdisciplinary Graduate School of Medical and Engineering, University of Yamanashi, 4-4-37 Takeda, Kofu, Yamanashi 400-8510 (Japan)

2011-10-29

Porous potassium niobate (KNbO{sub 3}, KN) system ceramics were prepared by a conventional sintering method using carbon black (CB) nanoparticles. First, KN nanoparticles with a size of 100 nm was mixed with CB nanoparticles and binder using ball milling with ethanol. The mixture was dried, and pressed into pellets using uniaxial pressing. After binder burnout, these ceramics was sintered in air. Their piezoelectric properties were measured and discussed a relationship between porosity and piezoelectric properties. As the results, with increasing porosity, piezoelectric g33 constant increased significantly, which suggested that porous ceramics were effective for stress sensor application.

Porosity Dependence of Piezoelectric Properties for Porous Potassium Niobate System Ceramics

International Nuclear Information System (INIS)

Wada, S; Mase, Y; Shimizu, S; Maeda, K; Fujii, I; Nakashima, K; Pulpan, P; Miyajima, N

2011-01-01

Porous potassium niobate (KNbO 3 , KN) system ceramics were prepared by a conventional sintering method using carbon black (CB) nanoparticles. First, KN nanoparticles with a size of 100 nm was mixed with CB nanoparticles and binder using ball milling with ethanol. The mixture was dried, and pressed into pellets using uniaxial pressing. After binder burnout, these ceramics was sintered in air. Their piezoelectric properties were measured and discussed a relationship between porosity and piezoelectric properties. As the results, with increasing porosity, piezoelectric g33 constant increased significantly, which suggested that porous ceramics were effective for stress sensor application.

Two-step sintering of ultrafine-grained barium cerate proton conducting ceramics

International Nuclear Information System (INIS)

Wang, Siwei; Zhang, Lei; Zhang, Lingling; Brinkman, Kyle; Chen, Fanglin

2013-01-01

Ultra-fine grained dense BaZr 0.1 Ce 0.7 Y 0.1 Yb 0.1 O 3−δ (BZCYYb) ceramics have been successfully prepared via a two-step sintering method. Co-precipitation method has been adopted to prepare nano-sized BZCYYb precursors with an average particle size of 30 nm. By controlling the sintering profile, an average grain size of 184 nm was obtained for dense BZCYYb ceramics via the two-step sintering method, compared to 445 nm for the conventional sintered samples. The two-step sintered BZCYYb samples showed less impurity and an enhanced electrical conductivity compared with the conventional sintered ones. Further, the two-step sintering method was applied to fabricate anode supported solid oxide fuel cells (SOFCs) using BZCYYb as the electrolyte, resulting in dense ultrafine-grained electrolyte membranes and porous anode substrates with fine particles. Due to the reduced ohmic as well as polarization resistances, the maximum power output of the cells fabricated from the two-step sintering method reached 349 mW m −2 at 700 °C, significantly improved from 172 mW cm −2 for the conventional sintered cells, suggesting that two-step sintering method is very promising for optimizing the microstructure and thus enhancing the electrochemical performances for barium cerate based proton-conducting SOFCs.

Synthesis, characterization, biocompatibility of hydroxyapatite-natural polymers nanocomposites for dentistry applications.

Science.gov (United States)

Chung, Jin-Hwan; Kim, Young Kyung; Kim, Kyo-Han; Kwon, Tae-Yub; Vaezmomeni, Seyede Ziba; Samiei, Mohammad; Aghazadeh, Marzyeh; Davaran, Soodabeh; Mahkam, Mehrdad; Asadi, Ghale; Akbarzadeh, Abolfazl

2016-01-01

Hydroxyapatite (HA), the main mineral component of bones and teeth, was synthesized by using the reaction between calcium nitrate tetrahydrate Ca(NO3)2∙4H2O and diammonium hydrogen phosphate (NH4)2HPO4 (DAHP) with a chemical precipitation method. The objective of this study is to utilize novel inorganic-organic nanocomposites for biomedical applications. HA is an inorganic component (75% w) and chitosan, alginate and albumin (Egg white) are organic components of nanocomposites (25% w). Nanocomposites were prepared in deionized water solutions, at room temperature, using a mechanical and magnetic stirrer for 48 h. The microstructure and morphology of sintered n-HAP were tested at different preheating temperature and laser sintering speed with scanning electron microscopy (SEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR).

Suspension thermal spraying of hydroxyapatite: Microstructure and in vitro behaviour

Energy Technology Data Exchange (ETDEWEB)

Bolelli, Giovanni, E-mail: giovanni.bolelli@unimore.it [Department of Engineering “Enzo Ferrari”, Università di Modena e Reggio Emilia, Via Vignolese 905, 41125 Modena, MO (Italy); Bellucci, Devis; Cannillo, Valeria; Lusvarghi, Luca; Sola, Antonella [Department of Engineering “Enzo Ferrari”, Università di Modena e Reggio Emilia, Via Vignolese 905, 41125 Modena, MO (Italy); Stiegler, Nico; Müller, Philipp; Killinger, Andreas; Gadow, Rainer [Institute for Manufacturing Technologies of Ceramic Components and Composites (IMTCCC), Universität Stuttgart, Allmandring 7b, 70569 Stuttgart (Germany); Altomare, Lina; De Nardo, Luigi [Dipartimento di Chimica, Materiali e Ingegneria Chimica “G. Natta”, Politecnico di Milano, Via Mancinelli 7, I-20131 Milano (Italy)

2014-01-01

In cementless fixation of metallic prostheses, bony ingrowth onto the implant surface is often promoted by osteoconductive plasma-sprayed hydroxyapatite coatings. The present work explores the use of the innovative High Velocity Suspension Flame Spraying (HVSFS) process to coat Ti substrates with thin homogeneous hydroxyapatite coatings. The HVSFS hydroxyapatite coatings studied were dense, 27–37 μm thick, with some transverse microcracks. Lamellae were sintered together and nearly unidentifiable, unlike conventional plasma-sprayed hydroxyapatite. Crystallinities of 10%–70% were obtained, depending on the deposition parameters and the use of a TiO{sub 2} bond coat. The average hardness of layers with low (< 24%) and high (70%) crystallinity was ≈ 3.5 GPa and ≈ 4.5 GPa respectively. The distributions of hardness values, all characterised by Weibull modulus in the 5–7 range, were narrower than that of conventional plasma-sprayed hydroxyapatite, with a Weibull modulus of ≈ 3.3. During soaking in simulated body fluid, glassy coatings were progressively resorbed and replaced by a new, precipitated hydroxyapatite layer, whereas coatings with 70% crystallinity were stable up to 14 days of immersion. The interpretation of the precipitation behaviour was also assisted by surface charge assessments, performed through Z-potential measurements. During in vitro tests, HA coatings showed no cytotoxicity towards the SAOS-2 osteoblast cell line, and surface cell proliferation was comparable with proliferation on reference polystyrene culture plates. - Highlights: • Thin, dense HA layers were originated by HVSFS deposition of molten agglomerates of ≈ 1 μm. • Tensile adhesion strength of HVSFS HA onto Ti well above the threshold of ISO 13779-2 • Crystallinity (10–70%) is determined by system temperature during deposition. • Crystallinity controls the reactivity during immersion in simulated body fluid. • SAOS-2 osteoblast-like cells adhered well and

Hydroxyapatite/collagen bone-like nanocomposite.

Science.gov (United States)

Kikuchi, Masanori

2013-01-01

Our group has succeeded to synthesize material with bone-like nanostructure and bone-like inorganic and organic composition via self-organization mechanism between them using simultaneous titration method under controlled pH and temperature. The hydroxyapatite/collagen (HAp/Col) bone-like nanocomposite completely incorporated into bone remodeling process to be substituted by new bone. Cells cultured on the HAp/Col revealed very interesting reactions. Osteoblast-like MG63 cells showed upregulation of alkaline phosphatase >3 times greater than MG63 cells cultured on tissue culture polystyrene (TCPS). MG63 cells 3-dimensionally cultured in a "HAp/Col sponge," a porous HAp/Col having sponge-like viscoelasticity, accumulated calcium phosphate nodules on extracellular matrices they secreted. Bone marrow cells co-cultured with osteoblasts on HAp/Col differentiated to osteoclasts without differentiation supplements. This phenomenon is not found in cells cultured on hydroxyapatite ceramics and TCPS, and rarely in cells cultured on dentin. These results suggest that HAp/Col is a good candidate for tissue engineering of bone as well as bone filler. In a clinical test as a bone filler, the HAp/Col sponge was significantly better than porous β-tricalcium phosphate. The HAp/Col sponge has been approved by the Japanese government and will be used as greatly needed bone filler in patients. In addition to the above, HAp/Col coating on titanium revealed higher osteo-conductivity than HAp-coated titanium and bare titanium and improved direct bonding between titanium and newly formed bone. The HAp/Col coating may be used for metal devices requiring osseointegration.

Corrosion resistance characterization of porous alumina membrane supports

Energy Technology Data Exchange (ETDEWEB)

Dong Yingchao, E-mail: dongyc9@mail.ustc.edu.cn [Materials and Surface Science Institute (MSSI), University of Limerick, Limerick (Ireland); USTC Lab for Solid State Chemistry and Inorganic Membranes, Department of Materials Science and Engineering, University of Science and Technology of China (USTC) (China); Key Lab of Jiangxi Universities for Inorganic Membranes, National Engineering Research Center for Domestic and Building Ceramics, Jingdezhen Ceramic University (JCU) (China); Lin Bin [USTC Lab for Solid State Chemistry and Inorganic Membranes, Department of Materials Science and Engineering, University of Science and Technology of China (USTC) (China); Zhou Jianer [Key Lab of Jiangxi Universities for Inorganic Membranes, National Engineering Research Center for Domestic and Building Ceramics, Jingdezhen Ceramic University (JCU) (China); Zhang Xiaozhen [USTC Lab for Solid State Chemistry and Inorganic Membranes, Department of Materials Science and Engineering, University of Science and Technology of China (USTC) (China); Key Lab of Jiangxi Universities for Inorganic Membranes, National Engineering Research Center for Domestic and Building Ceramics, Jingdezhen Ceramic University (JCU) (China); Ling Yihan; Liu Xingqin; Meng Guangyao [USTC Lab for Solid State Chemistry and Inorganic Membranes, Department of Materials Science and Engineering, University of Science and Technology of China (USTC) (China); Hampshire, Stuart [Materials and Surface Science Institute (MSSI), University of Limerick, Limerick (Ireland)

2011-04-15

Tubular porous alumina ceramic membrane supports were fabricated by an extrusion-drying-sintering process and then characterized in detail in terms of corrosion resistance in both H{sub 2}SO{sub 4} and NaOH aqueous solutions. Variations in the properties of the alumina supports such as mass loss percent, mechanical strength, open porosity and pore size distribution were studied before and after corrosion under different conditions. In addition, the microstructures were analyzed using scanning electron microscopy, energy dispersive spectroscopy and X-ray diffraction before and after corrosion. The fabricated porous alumina supports offer possibilities for some potential applications as micro-filtration or ultra-filtration membrane supports, as well as in the pre-treatment of strongly acidic industrial waste-liquids. - Research highlights: {yields} Porous alumina membrane supports fabricated by extrusion-drying-sintering process. {yields} Corrosion resistance in 20 wt.% H{sub 2}SO{sub 4} and 1, 5, 10 wt.% NaOH aqueous solutions. {yields} Rapid mass loss and loss of flexural strength occurred in hot NaOH solution. {yields} Resistant to strong acid corrosion with low mass loss, low flexural strength loss. {yields} Porous alumina supports have potential for treatment of strong acid waste liquids.

Synthesis spherical porous hydroxyapatite/graphene oxide composites by ultrasonic-assisted method for biomedical applications.

Science.gov (United States)

Duan, Peizhen; Shen, Juan; Zou, Guohong; Xia, Xu; Jin, Bo; Yu, Jiaxin

2018-04-10

Spherical porous hydroxyapatite (SHA)/graphene oxide (GO) composites with different GO (w/w) content of 16%, 40%, and 71% have been fabricated through a facile and controllable ultrasonic-assisted method at room temperature. The products were characterized by x-ray diffraction, field emission scanning electron microscopy, thermogravimetric analysis, mechanical testing and biomimetic mineralization. Results showed SHA were covered by GO, and SHA/GO composites had an irregular surface with different degrees of wrinkles. The elastic modulus and hardness of SHA/GO-3 composites were up to 12.45 ± 0.33 GPa and 686.67 ± 26.95 MPa, which indicated that the contents of GO had an effect on SHA/GO composites. And the mechanical properties of SHA/GO-2 composites were similar to SHA particles. The biomimetic mineralization in SBF solution showed the bone-like apatite layer on composites surface, which demonstrated that the SHA/GO materials had osseointegration property. Moreover, in vitro cytocompatibility of SHA/GO-2 composites and pure GO were evaluated by cell adhesion and proliferation tests using MC3T3-E1 cells, which demonstrated that the SHA/GO composites can act as a good template for the cells growth and adhesion. These results suggested that the SHA/GO composites will be a promising material for biomedical application.

A Comparison of Fatigue Crack Growth in Human Enamel and Hydroxyapatite

OpenAIRE

Bajaj, Devendra; Nazari, Ahmad; Eidelman, Naomi; Arola, Dwayne

2008-01-01

Cracks and craze lines are often observed in the enamel of human teeth, but they rarely cause tooth fracture. The present study evaluates fatigue crack growth in human enamel, and compares that to the fatigue response of sintered hydroxyapatite (HAp) with similar crystallinity, chemistry and density. Miniature inset compact tension (CT) specimens were prepared that embodied a small piece of enamel (N=8) or HAp (N=6). The specimens were subjected to mode I cyclic loads and the steady state cra...

Micro- and Nano- Porous Adsorptive Materials for Removal of Contaminants from Water at Point-of-Use

Science.gov (United States)

Yakub, Ismaiel

Water is food, a basic human need and a fundamental human right, yet hundreds of millions of people around the world do not have access to clean drinking water. As a result, about 5000 people die each day from preventable water borne diseases. This dissertation presents the results of experimental and theoretical studies on three different types of porous materials that were developed for the removal of contaminants from water at point of use (household level). First, three compositionally distinct porous ceramic water filters (CWFs) were made from a mixture of redart clay and sieved woodchips and processed into frustum shape. The filters were tested for their flow characteristics and bacteria filtration efficiencies. Since, the CWFs are made from brittle materials, and may fail during processing, transportation and usage, the mechanical and physical properties of the porous clays were characterized, and used in modeling designed to provide new insights for the design of filter geometries. The mechanical/physical properties that were characterized include: compressive strength, flexural strength, facture toughness and resistance curve behavior, keeping in mind the anisotropic nature of the filter structure. The measured flow characteristics and mechanical/physical properties were then related to the underlying porosity and characteristic pore size. In an effort to quantify the adhesive interactions associated with filtration phenomena, atomic force microscopy (AFM) was used to measure the adhesion between bi-material pairs that are relevant to point-of-use ceramic water filters. The force microscopy measurements of pull-off force and adhesion energy were used to rank the adhesive interactions. Similarly, the adsorption of fluoride to hydroxyapatite-doped redart clay was studied using composites of redart clay and hydroxyapatite (C-HA). The removal of fluoride from water was explored by carrying out adsorption experiments on C-HA adsorbents with different ratios of

Direct laser metal sintering as a new approach to fabrication of an isoelastic functionally graded material for manufacture of porous titanium dental implants.

Science.gov (United States)

Traini, T; Mangano, C; Sammons, R L; Mangano, F; Macchi, A; Piattelli, A

2008-11-01

This work focuses on a titanium alloy implants incorporating a gradient of porosity, from the inner core to the outer surface, obtained by laser sintering of metal powder. Surface appearance, microstructure, composition, mechanical properties and fractography were evaluated. All the specimens were prepared by a selective laser sintering procedure using a Ti-6Al-4V alloy powder with a particle size of 1-10 microm. The morphological and chemical analyses were performed by SEM and energy dispersive X-ray spectroscopy. The flexure strength was determined by a three-point bend test using a universal testing machine. The surface roughness was investigated using a confocal scanning laser microscope. The surface roughness variation was statistically evaluated by use of a Chi square test. A p value of metal core consisted of columnar beta grains with alpha and beta laths within the grains. The alloy was composed of 90.08% Ti, 5.67% Al and 4.25% V. The Young's modulus of the inner core material was 104+/-7.7 GPa; while that of the outer porous material was 77+/-3.5 GPa. The fracture face showed a dimpled appearance typical of ductile fracture. In conclusion, laser metal sintering proved to be an efficient means of construction of dental implants with a functionally graded material which is better adapted to the elastic properties of the bone. Such implants should minimize stress shielding effects and improve long-term performance.

Manufacturing and characterization of porous SiC for flow channel inserts in dual-coolant blanket designs

International Nuclear Information System (INIS)

Bereciartu, Ainhoa; Ordas, Nerea; Garcia-Rosales, Carmen; Morono, Alejandro; Malo, Marta; Hodgson, Eric R.; Abella, Jordi; Sedano, Luis

2011-01-01

SiC is the primary candidate for the flow channel inserts in dual-coolant blanket concepts. Porous SiC ceramics are attractive candidates for this non-structural application, since they can satisfy the required properties through a low cost manufacturing route, compared to SiC f /SiC. This work shows first results of the manufacturing of porous SiC ceramics prepared with different amounts of Y 2 O 3 and Al 2 O 3 as sintering additives. C powders were used as pore-formers by their burnout during oxidation after sintering. Comparison of microstructure, porosity, flexural strength, thermal and electrical conductivity and corrosion under Pb-15.7Li of porous SiC without and with sintering additives is presented. The addition of 2.5 wt.% of Y 2 O 3 and Al 2 O 3 improves the mechanical properties, and reduces the thermal and electrical conductivity down to reasonable values. Preliminary corrosion tests under Pb-15.7 Li at 500 deg. C show that the absence of a dense coating on porous SiC leads to poor corrosion behavior.

Subtractive manufacturing of customized hydroxyapatite scaffolds for bone regeneration

Czech Academy of Sciences Publication Activity Database

Trunec, M.; Chlup, Zdeněk

2017-01-01

Roč. 43, č. 14 (2017), s. 11265-11273 ISSN 0272-8842 R&D Projects: GA MŠk(CZ) LQ1601 Institutional support: RVO:68081723 Keywords : tissue engineering applications * in-vivo * porous hydroxyapatite * phosphate bioceramics * suspensions * ceramics * laser * optimization * osteogenesis * deposition * Milling (A) * Porosity (B) * Apatite (D) * Biopmedical properties (E) * Scaffold Subject RIV: JH - Ceramics, Fire-Resistant Materials and Glass OBOR OECD: Ceramics Impact factor: 2.986, year: 2016

Ceramic and non-ceramic hydroxyapatite as a bone graft material: a brief review.

Science.gov (United States)

Dutta, S R; Passi, D; Singh, P; Bhuibhar, A

2015-03-01

Treatment of dental, craniofacial and orthopedic defects with bone graft substitutes has shown promising result achieving almost complete bone regeneration depending on product resorption similar to human bone's physicochemical and crystallographic characteristics. Among these, non-ceramic and ceramic hydroxyapatite being the main inorganic salt of bone is the most studied calcium phosphate material in clinical practices ever since 1970s and non-ceramic since 1985. Its "chemical similarity" with the mineralized phase of biologic bone makes it unique. Hydroxyapatite as an excellent carrier of osteoinductive growth factors and osteogenic cell populations is also useful as drug delivery vehicle regardless of its density. Porous ceramic and non-ceramic hydroxyapatite is osteoconductive, biocompatible and very inert. The need for bone graft material keeps on increasing with increased age of the population and the increased conditions of trauma. Recent advances in genetic engineering and doping techniques have made it possible to use non-ceramic hydroxyapatite in larger non-ceramic crystals and cluster forms as a successful bone graft substitute to treat various types of bone defects. In this paper we have mentioned some recently studied properties of hydroxyapatite and its various uses through a brief review of the literatures available to date.

Porous Core-Shell Nanostructures for Catalytic Applications

Science.gov (United States)

Ewers, Trevor David

Porous core-shell nanostructures have recently received much attention for their enhanced thermal stability. They show great potential in the field of catalysis, as reactant gases can diffuse in and out of the porous shell while the core particle is protected from sintering, a process in which particles coalesce to form larger particles. Sintering is a large problem in industry and is the primary cause of irreversible deactivation. Despite the obvious advantages of high thermal stability, porous core-shell nanoparticles can be developed to have additional interactive properties from the combination of the core and shell together, rather than just the core particle alone. This dissertation focuses on developing new porous core-shell systems in which both the core and shell take part in catalysis. Two types of systems are explored; (1) yolk-shell nanostructures with reducible oxide shells formed using the Kirkendall effect and (2) ceramic-based porous oxide shells formed using sol-gel chemistry. Of the Kirkendall-based systems, Au FexOy and Cu CoO were synthesized and studied for catalytic applications. Additionally, ZnO was explored as a potential shelling material. Sol-gel work focused on optimizing synthetic methods to allow for coating of small gold particles, which remains a challenge today. Mixed metal oxides were explored as a shelling material to make dual catalysts in which the product of a reaction on the core particle becomes a reactant within the shell.

Surface-selective laser sintering of thermolabile polymer particles using water as heating sensitizer

Energy Technology Data Exchange (ETDEWEB)

Antonov, E N; Krotova, L I; Minaev, N V; Minaeva, S A; Mironov, A V; Popov, V K [Institute on Laser and Information Technologies of the Russian Academy of Sciencies, Troitsk, Moscow (Russian Federation); Bagratashvili, V N [Department of Chemistry, M.V. Lomonosov Moscow State University, Moscow (Russian Federation)

2015-11-30

We report the implementation of a novel scheme for surface-selective laser sintering (SSLS) of polymer particles, based on using water as a sensitizer of laser heating and sintering of particles as well as laser radiation at a wavelength of 1.94 μm, corresponding to the strong absorption band of water. A method of sintering powders of poly(lactide-co-glycolide), a hydrophobic bioresorbable polymer, after modifying its surface with an aqueous solution of hyaluronic acid is developed. The sintering thresholds for wetted polymer are by 3 – 4 times lower than those for sintering in air. The presence of water restricts the temperature of the heated polymer, preventing its thermal destruction. Polymer matrices with a developed porous structure are obtained. The proposed SSLS method can be applied to produce bioresorbable polymer matrices for tissue engineering. (interaction of laser radiation with matter. laser plasma)

Development of strontium and magnesium substituted porous hydroxyapatite/poly(3,4-ethylenedioxythiophene) coating on surgical grade stainless steel and its bioactivity on osteoblast cells.

Science.gov (United States)

Gopi, D; Ramya, S; Rajeswari, D; Surendiran, M; Kavitha, L

2014-02-01

The present study deals with the successful development of bilayer coatings by electropolymerisation of poly(3,4-ethylenedioxythiophene) (PEDOT) on surgical grade stainless steel (316L SS) followed by the electrodeposition of strontium (Sr) and magnesium (Mg) substituted porous hydroxyapatite (Sr, Mg-HA). The bilayer coatings were characterised by Fourier transform infrared spectroscopy (FT-IR) and high resolution scanning electron microscopy (HRSEM). Corrosion resistance of the obtained coatings was investigated in Ringer's solution by electrochemical techniques and the results were in good agreement with those obtained from chemical analysis, namely inductively coupled plasma atomic emission spectrometry (ICP-AES). Also, the mechanical and biological properties of the bilayer coatings were analyzed. From the obtained results it was evident that the PEDOT/Sr, Mg-HA bilayer exhibited greater adhesion strength than the Sr, Mg-HA coated 316L SS. In vitro cell adhesion test of the Sr, Mg-HA coating on PEDOT coated specimen is found to be more bioactive compared to that of the single substituted hydroxyapatite (Sr or Mg-HA) on the PEDOT coated 316L SS. Thus, the PEDOT/Sr, Mg-HA bilayer coated 316L SS can serve as a prospective implant material for biomedical applications. Copyright © 2013 Elsevier B.V. All rights reserved.

Towards the synthesis of hydroxyapatite/protein scaffolds with controlled porosities: bulk and interfacial shear rheology of a hydroxyapatite suspension with protein additives.

Science.gov (United States)

Maas, Michael; Bodnar, Pedro Marcus; Hess, Ulrike; Treccani, Laura; Rezwan, Kurosch

2013-10-01

The synthesis of porous hydroxyapatite scaffolds is essential for biomedical applications such as bone tissue engineering and replacement. One way to induce macroporosity, which is needed to support bone in-growth, is to use protein additives as foaming agents. Another reason to use protein additives is the potential to introduce a specific biofunctionality to the synthesized scaffolds. In this work, we study the rheological properties of a hydroxyapatite suspension system with additions of the proteins bovine serum albumin (BSA), lysozyme (LSZ) and fibrinogen (FIB). Both the rheology of the bulk phase as well as the interfacial shear rheology are studied. The bulk rheological data provides important information on the setting behavior of the thixotropic suspension, which we find to be faster with the addition of FIB and LSZ and much slower with BSA. Foam bubble stabilization mechanisms can be rationalized via interfacial shear rheology and we show that it depends on the growth of interfacial films at the suspension/air interface. These interfacial films support the stabilization of bubbles within the ceramic matrix and thereby introduce macropores. Due to the weak interaction of the protein molecules with the hydroxyapatite particles of the suspension, we find that BSA forms the most stable interfacial films, followed by FIB. LSZ strongly interacts with the hydroxyapatite particles and thus only forms thin films with very low elastic moduli. In summary, our study provides fundamental rheological insights which are essential for tailoring hydroxyapatite/protein suspensions in order to synthesize scaffolds with controlled porosities. Copyright © 2013 Elsevier Inc. All rights reserved.

Vacuum-sintered body of a novel apatite for artificial bone

Science.gov (United States)

Tamura, Kenichi; Fujita, Tatsushi; Morisaki, Yuriko

2013-12-01

We produced regenerative artificial bone material and bone parts using vacuum-sintered bodies of a novel apatite called "Titanium medical apatite (TMA®)" for biomedical applications. TMA was formed by chemically connecting a Ti oxide molecule with the reactive [Ca10(PO4)6] group of Hydroxyapatite (HAp). The TMA powders were kneaded with distilled water, and solid cylinders of compacted TMA were made by compression molding at 10 MPa using a stainless-steel vessel. The TMA compacts were dried and then sintered in vacuum (about 10-3 Pa) or in air using a resistance heating furnace in the temperature range 1073-1773 K. TMA compacts were sintered at temperatures greater than 1073 K, thus resulting in recrystallization. The TMA compact bodies sintered in the range 1273-1773 K were converted into mixtures composed of three crystalline materials: α-TCP (tricalcium phosphate), β-TCP, and Perovskite-CaTiO3. The Perovskite crystals were stable and hard. In vacuum-sintering, the Perovskite crystals were transformed into fibers (approximately 1 µm in diameter × 8 µm in length), and the fiber distribution was uniform in various directions. We refer to the TMA vacuum-sintered bodies as a "reinforced composite material with Perovskite crystal fibers." However, in atmospheric sintering, the Perovskite crystals were of various sizes and were irregularly distributed as a result of the effect of oxygen. After sintering temperature at 1573 K, the following results were obtained: the obtained TMA vacuum-sintered bodies (1) were white, (2) had a density of approximately 2300 kg/m3 (corresponding to that of a compact bone or a tooth), and had a thermal conductivity of approximately 31.3 W/(m·K) (corresponding to those of metal or ceramic implants). Further, it was possible to cut the TMA bodies into various forms with a cutting machine. An implant made of TMA and inserted into a rabbit jaw bone was covered by new bone tissues after just one month because of the high

Effect of ball-milling time on the structural characteristics of biomedical porous Ti-Sn-Nb alloy

Energy Technology Data Exchange (ETDEWEB)

Nouri, Alireza, E-mail: alireza_nouri@yahoo.com [CQM-Centro de Quimica da Madeira, MMRG, Universidade da Madeira, Campus Universitario da Penteada, 9000-390 Funchal (Portugal); Institute for Technology Research and Innovation, Deakin University, Geelong, Victoria 3217 (Australia); Hodgson, Peter D. [Institute for Technology Research and Innovation, Deakin University, Geelong, Victoria 3217 (Australia); Wen Cuie [IRIS, Faculty of Engineering and Industrial Sciences, Swinburne University of Technology, 543-454 Burwood Road, Hawthorn, Victoria 3122 Australia (Australia)

2011-07-20

The structural characteristics of biomedical porous materials are crucial for bone tissue to grow into a porous structure and can also influence the fixation and remodeling between the implant and the human tissues. The current study has been investigating the effect of the ball-milling variable of time on the structural characteristics and pore morphology of a biomedical porous Ti-16Sn-4Nb (wt.%) alloy. The alloy was synthesized using high-energy ball milling for different periods of time, and the porous Ti-16Sn-4Nb alloy was fabricated by using a space holder sintering process. The resultant powder particles, bulk, and porous samples were characterized using a scanning electron microscope (SEM), laser particle-size analyzer, chemical analysis, X-ray diffraction analysis (XRD), and the Vickers hardness test. The results indicated that the inner pore surface, pore wall architecture, degree of porosity, pore size and the inter-pore connectivity of the sintered porous alloy are all considerably affected by ball-milling time.

The Influence of Surface Treatment by Hydrogenation on the Biocompatibility of Different Hydroxyapatite Materials

International Nuclear Information System (INIS)

Palcevskis, E; Dindune, A; Dekhtyar, Y; Polyaka, N; Veljovic, D; Sammons, R L

2011-01-01

The influence of hydrogenation on the biocompatibility of different hydroxyapatite (HAP) materials was tested. Materials consisted of pure HAP, HAP substituted with manganese (Mn +2 ) and with magnesium (Mg +2 ) - all axially pressed and conventionally sintered for 2 h at 1200 deg. C; pure HAP isostatic pressed and sintered by a microwave technique for 15 min at temperature of 1200 deg. C. Biocompatibility was compared by enumeration of the number of osteoblast-like cells to the materials before and after hydrogenation. Obtained results show that the osteoblastic cells demonstrated a higher ability to attach to HAP if its surface was negatively charged. Hydrogenation altered the surface potential; HAP substituted with manganese - HAP(Mn) and with magnesium - HAP(Mg) demonstrated the highest ability to engineer the charge.

Nano-Hydroxyapatite/Fluoridated and Unfluoridated Bioactive Glass Composites: Structural Analysis and Bioactivity Evaluation

International Nuclear Information System (INIS)

Batra, Uma; Kapoor, Seema; Sharma, J. D.

2011-01-01

Biphasic bioceramic composites containing nano-hydroxyapatite (HAP) and nanosized bioactive glasses have been prepared in the form of pellets and have been examined for the effects of bioglass concentrations and sintering temperature on the structural transformations and bioactivity behavior. Pure stoichiometric nano-HAP was synthesized using sol-gel technique. Two bioglasses synthesized in this work--fluoridated bioglass (Cao-P 2 O 5 -Na 2 O 3 -CaF 2 ) and unfluoridated bioglass (Cao-P 2 O 5 -Na 2 O 3 ) designated as FBG and UFBG respectively, were added to nano-HAP with concentrations of 5, 10, 12 and 15%. The average particle sizes of synthesized HAP and bioglasses were 23 nm and 35 nm, respectively. The pellets were sintered at four different temperatures i.e. 1000 deg. C, 1150 deg. C, 1250 deg. C and 1350 deg. C. The investigations involved study of structural and bioactivity behavior of green and sintered pellets and their deviations from original materials i.e. HAP, FBG and UFBG, using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The phase composition of the sintered pellets was found to be non-stoichiometric HAP with α-TCP (tricalcium phosphate) and β-TCP. It was revealed from SEM images that bonding mechanism was mainly solid state sintering for all pellets sintered at 1000 deg. C and 1150 deg. C and also for pellets with lower concentrations of bioglass i.e. 5% and 10% sintered at 1250 deg. C. Partly liquid phase sintering was observed for pellets with higher bioglass concentrations of 12% and 15% sintered at 1250 deg. C and same behaviour was noted for pellets at all concentrations of bioglasses at 1350 deg. C. The sintered density, hardness and compression strength of pellets have been influenced both by the concentration of the bioglasses and sintering temperature. It was observed that the biological HAP layer formation was faster on the green pellets surface than on pure HAP and sintered pellets, showing higher bioactivity in the

Effect of yttria addition on the stability of porous chromium oxide ceramics in supercritical water

International Nuclear Information System (INIS)

Dong Ziqiang; Chen Weixing; Zheng Wenyue; Guzonas, Dave

2013-01-01

Porous chromium oxide (Cr 2 O 3 ) ceramics were prepared by oxidizing highly porous chromium carbides that were obtained by a reactive sintering method, and were evaluated at temperatures ranging from 375 °C to 625 °C in supercritical water (SCW) environments with a fixed pressure of 25–30 MPa. Reactive element yttrium was introduced to the porous oxide ceramic by adding various amounts of yttria of 5, 10 and 20 wt.%, respectively, prior to reactive sintering. The exposure in SCW shows that the porous chromium oxide is quite stable in SCW at 375 °C. However, the stability decreased with increasing temperature. It is well known that chromium oxide can be oxidized to soluble chromium (VI) species in SCW when oxygen is present. Adding yttria increases the stability of chromium oxide in SCW environments. However, adding yttria higher than 5 wt.% increased the weight loss of porous chromium oxide samples because of the direct dissociation of Y 2 O 3 in SCW.

Microstructure characterization of porous microalloyed aluminium-silicate ceramics

Directory of Open Access Journals (Sweden)

Purenović Jelena

2011-01-01

Full Text Available Kaolinite and bentonite clay powders mixed with active additives, based on Mg(NO32 and Al(NO32, sintered at high temperatures produce very porous ceramics with microcrystalline and amorphous regions and highly developed metalized surfaces (mainly with magnesium surplus. Microstructure investigations have revealed non-uniform and highly porous structure with broad distribution of grain size, specifically shaped grains and high degree of agglomeration. The ceramics samples were characterized by scanning electron microscopy (SEM, energy dispersive spectrometer (EDS, X-ray diffraction analysis (XRD and IR spectroscopy analysis, prior and after treatment in “synthetic water”, i.e. in aqueous solution of arsenic-salt. Grain size distribution for untreated and treated samples was done with software SemAfore 4. It has shown great variety in size distribution of grains from clay powders to sintered samples.

A Bone Graft Substitutes Hydroxyapatite Coated Gentamycin (Bonigent) As Drug Delivery System

International Nuclear Information System (INIS)

Rusnah Mustaffa; Fauziah Othman; Asmah Rahmat; Mohd Reusmaazran Yusof; Shaaban Kasim; Narimah Abu Baka; Nasani Nasrul

2014-01-01

Porous hydroxyapatite coated with antibiotic gentamycin for drug delivery system is namely Bonigent. In this product, antibiotic (gentamycin) is coated into the scaffolds HA porous and Would then be released slowly into the bone tissue upon implantation, this way would increase drug penetration, thus avoiding systemic infection, preventing the formation of biofilm and improved healing. When a foreign material (implants or scaffolds of bone graft substitutes) is introduced into the body, there would be normally formation of biofilm that can lead to systemic infection and cause device failure. Surgeon will use antibiotic such as gentamycin to avoid these effects. The purpose of this project is to investigate the feasibility of fabricating a drug delivery system (DDS) that serves dual functions, to combating biofilms and to enhance bone in growths. We also successfully producing a scaffold HA bone graft substitutes incorporated with antibiotic gentamycin to combating bio-film and prevent the failure medical device implant for healthy and human nation. Bone graft substitutes into porous scaffolds suitable for drug delivery; loading the scaffolds with gentamycin; and study release rate in vivo were studied. Porous bone grafts substitutes are coated with antibiotic gentamycin by immerse technique. In order to limit biofilm formation, biomaterials loaded with suitable antibiotics can be used as a preventative measure. The biomaterials hydroxyapatite (HA) is an osteoconductive space filler and is produced locally by Malaysian Nuclear Agency. Porous HA and HA/ TCP has the potential to be used as synthetic bone graft materials because it is bioactive and biocompatible with bone tissues. Development of a product as bone graft substitute (BGS) with special ability of delivering drug (gentamycin) to bone tissue for better and more effective healing process. Characterization of the physical analysis, porosity, surface morphology by Scanning Electron Microscopy Analysis (SEM) and

Cartilage regeneration using a porous scaffold, a collagen sponge incorporating a hydroxyapatite/chondroitinsulfate composite

International Nuclear Information System (INIS)

Ohyabu, Yohimi; Adegawa, Takuro; Yoshioka, Tomohiko; Ikoma, Toshiyuki; Uemura, Toshimasa; Tanaka, Junzo

2010-01-01

Because cartilage has limited potential for self-repair, tissue engineering is expected to replace the present therapies for damaged cartilage, such as total knee arthroplasty. However, scaffolds suitable for cartilage tissue engineering have not been established. We synthesized a novel porous scaffold, a collagen sponge incorporating a hydroxyapatite/chondroitinsulfate composite (pCol-HAp/ChS), containing materials which resemble extracellular matrices in bone and cartilage tissues, which needs high compressive strength for clinical use. HAp/ChS had smaller crystals and a larger total surface area than HAp. SEM images showed pCol-HAp/ChS to have the roughest surface compared with pCol and pCol-HAp. The mechanical properties suggest that pCol-HAp/ChS and pCol/HAp are similar, and superior to pCol. Seeding experiments showed a uniform distribution of mesenchymal stem cells (MSCs) in pCol-HAp/ChS and pCol/HAp. Safranin O, Toluidine blue and Alcian blue staining after 2 weeks of culture revealed pCol-HAp/ChS to be the most chondrogenic in each case. In addition, MSCs in pCol-HAp/ChS produced more glycosaminoglycans, a cartilage matrix, than those in pCol-HAp. Further, pCol-HAp/ChS regenerated 15 times more cartilaginous tissue than pCol. From these results, pCol-HAp/ChS is expected to be a candidate for a scaffold for cartilage tissue engineering in place of collagen sponge.

Cartilage regeneration using a porous scaffold, a collagen sponge incorporating a hydroxyapatite/chondroitinsulfate composite

Energy Technology Data Exchange (ETDEWEB)

Ohyabu, Yohimi, E-mail: ooyabu.yoshimi@aist.go.jp [Department of Metallurgy and Ceramics Science, Tokyo Institute of Technology, 2-12-1, S7-5 Ookayama, Meguro, Tokyo 152-8550 (Japan); Nanotechnology Research Institute (NRI), National Institute of Advanced Industrial Science and Technology (AIST), Central-4, 1-1-1 Higashi, Tsukuba, Ibaraki, 305-8566 (Japan); Adegawa, Takuro; Yoshioka, Tomohiko [Department of Metallurgy and Ceramics Science, Tokyo Institute of Technology, 2-12-1, S7-5 Ookayama, Meguro, Tokyo 152-8550 (Japan); Ikoma, Toshiyuki [Biomaterials Center, National Institute for Materials Science, 1-1 Sengen, Tsukuba, Ibaraki, 305-0047 (Japan); Uemura, Toshimasa [Nanotechnology Research Institute (NRI), National Institute of Advanced Industrial Science and Technology (AIST), Central-4, 1-1-1 Higashi, Tsukuba, Ibaraki, 305-8566 (Japan); Tanaka, Junzo [Department of Metallurgy and Ceramics Science, Tokyo Institute of Technology, 2-12-1, S7-5 Ookayama, Meguro, Tokyo 152-8550 (Japan)

2010-10-15

Because cartilage has limited potential for self-repair, tissue engineering is expected to replace the present therapies for damaged cartilage, such as total knee arthroplasty. However, scaffolds suitable for cartilage tissue engineering have not been established. We synthesized a novel porous scaffold, a collagen sponge incorporating a hydroxyapatite/chondroitinsulfate composite (pCol-HAp/ChS), containing materials which resemble extracellular matrices in bone and cartilage tissues, which needs high compressive strength for clinical use. HAp/ChS had smaller crystals and a larger total surface area than HAp. SEM images showed pCol-HAp/ChS to have the roughest surface compared with pCol and pCol-HAp. The mechanical properties suggest that pCol-HAp/ChS and pCol/HAp are similar, and superior to pCol. Seeding experiments showed a uniform distribution of mesenchymal stem cells (MSCs) in pCol-HAp/ChS and pCol/HAp. Safranin O, Toluidine blue and Alcian blue staining after 2 weeks of culture revealed pCol-HAp/ChS to be the most chondrogenic in each case. In addition, MSCs in pCol-HAp/ChS produced more glycosaminoglycans, a cartilage matrix, than those in pCol-HAp. Further, pCol-HAp/ChS regenerated 15 times more cartilaginous tissue than pCol. From these results, pCol-HAp/ChS is expected to be a candidate for a scaffold for cartilage tissue engineering in place of collagen sponge.

Improvement of the compressive strength of a cuttlefish bone-derived porous hydroxyapatite scaffold via polycaprolactone coating.

Science.gov (United States)

Kim, Beom-Su; Kang, Hyo Jin; Lee, Jun

2013-10-01

Cuttlefish bones (CBs) have emerged as attractive biomaterials because of their porous structure and components that can be converted into hydroxyapatite (HAp) via a hydrothermal reaction. However, their brittleness and low strength restrict their application in bone tissue engineering. Therefore, to improve the compressive strength of the scaffold following hydrothermal conversion to a HAp form of CB (CB-HAp), the scaffold was coated using a polycaprolactone (PCL) polymer at various concentrations. In this study, raw CB was successfully converted into HAp via a hydrothermal reaction. We then evaluated their surface properties and composition by scanning electron microscopy and X-ray diffraction analysis. The CB-HAp coated with PCL showed improved compressive performance and retained a microporous structure. The compressive strength was significantly increased upon coating with 5 and 10% PCL, by 2.09- and 3.30-fold, respectively, as compared with uncoated CB-HAp. However, coating with 10% PCL resulted in a reduction in porosity. Furthermore, an in vitro biological evaluation demonstrated that MG-63 cells adhered well, proliferated and were able to be differentiated on the PCL-coated CB-HAp scaffold, which was noncytotoxic. These results suggest that a simple coating method is useful to improve the compressive strength of CB-HAp for bone tissue engineering applications. Copyright © 2013 Wiley Periodicals, Inc.

A novel one-pot process for near-net-shape fabrication of open-porous resorbable hydroxyapatite/protein composites and in vivo assessment

International Nuclear Information System (INIS)

Mueller, Berit; Koch, Dietmar; Lutz, Rainer; Schlegel, Karl A.; Treccani, Laura; Rezwan, Kurosch

2014-01-01

We present a mild one-pot freeze gelation process for fabricating near-net, complex-shaped hydroxyapatite scaffolds and to directly incorporate active proteins during scaffold processing. In particular, the direct protein incorporation enables a simultaneous adjustment and control of scaffold microstructure, porosity, resorbability and enhancement of initial mechanical and handling stability. Two proteins, serum albumin and lysozyme, are selected and their effect on scaffold stability and microstructure investigated by biaxial strength tests, electron microscopy, and mercury intrusion porosimetry. The resulting hydroxyapatite/protein composites feature adjustable porosities from 50% to 70% and a mechanical strength ranging from 2 to 6 MPa comparable to that of human spongiosa without any sintering step. Scaffold degradation behaviour and protein release are assessed by in vitro studies. A preliminary in vivo assessment of scaffold biocompatibility and resorption behaviour in adult domestic pigs is discussed. After implantation, composites were resorbed up to 50% after only 4 weeks and up to 65% after 8 weeks. In addition, 14% new bone formation after 4 weeks and 37% after 8 weeks were detected. All these investigations demonstrate the outstanding suitability of the one-pot-process to create, in a customisable and reliable way, biocompatible scaffolds with sufficient mechanical strength for handling and surgical insertion, and for potential use as biodegradable bone substitutes and versatile platform for local drug delivery. - Highlights: • We present a one-pot process for directly incorporating protein into HAp scaffolds. • The effect of two model proteins, BSA and LSZ, on scaffold properties is analysed. • HAp/protein scaffolds feature a mechanical strength comparable to human spongiosa. • BSA incorporation in scaffolds leads to strength increase despite porosity increment. • New bone formation in-vivo exceeds established xenograft bone substitutes

Damage Behavior of Sintered Fiber Felts

Directory of Open Access Journals (Sweden)

Nicolas Lippitz

2015-04-01

Full Text Available The reduction of aircraft noise is important due to a rising number of flights and the growth of urban centers close to airports. During landing, a significant part of the noise is generated by flow around the airframe. To reduce that noise porous trailing edges are investigated. Ideally, the porous materials should to be structural materials as well. Therefore, the mechanical properties and damage behavior are of major interest. The aim of this study is to show the change of structure and the damage behavior of sintered fiber felts, which are promising materials for porous trailing edges, under tensile loading using a combination of tensile tests and three dimensional computed tomography scans. By stopping the tensile test after a defined stress or strain and scanning the sample, it is possible to correlate structural changes and the development of damage to certain features in the stress-strain curve and follow the damage process with a high spatial resolution. Finally, the correlation between material structure and mechanical behavior is demonstrated.

Porous material neutron detector

Science.gov (United States)

Diawara, Yacouba [Oak Ridge, TN; Kocsis, Menyhert [Venon, FR

2012-04-10

A neutron detector employs a porous material layer including pores between nanoparticles. The composition of the nanoparticles is selected to cause emission of electrons upon detection of a neutron. The nanoparticles have a maximum dimension that is in the range from 0.1 micron to 1 millimeter, and can be sintered with pores thereamongst. A passing radiation generates electrons at one or more nanoparticles, some of which are scattered into a pore and directed toward a direction opposite to the applied electrical field. These electrons travel through the pore and collide with additional nanoparticles, which generate more electrons. The electrons are amplified in a cascade reaction that occurs along the pores behind the initial detection point. An electron amplification device may be placed behind the porous material layer to further amplify the electrons exiting the porous material layer.

An Investigation of Sintering Parameters on Titanium Powder for Electron Beam Melting Processing Optimization.

Science.gov (United States)

Drescher, Philipp; Sarhan, Mohamed; Seitz, Hermann

2016-12-01

Selective electron beam melting (SEBM) is a relatively new additive manufacturing technology for metallic materials. Specific to this technology is the sintering of the metal powder prior to the melting process. The sintering process has disadvantages for post-processing. The post-processing of parts produced by SEBM typically involves the removal of semi-sintered powder through the use of a powder blasting system. Furthermore, the sintering of large areas before melting decreases productivity. Current investigations are aimed at improving the sintering process in order to achieve better productivity, geometric accuracy, and resolution. In this study, the focus lies on the modification of the sintering process. In order to investigate and improve the sintering process, highly porous titanium test specimens with various scan speeds were built. The aim of this study was to decrease build time with comparable mechanical properties of the components and to remove the residual powder more easily after a build. By only sintering the area in which the melt pool for the components is created, an average productivity improvement of approx. 20% was achieved. Tensile tests were carried out, and the measured mechanical properties show comparatively or slightly improved values compared with the reference.

Preparation and characterization of composites based on the blends of collagen, chitosan and hyaluronic acid with nano-hydroxyapatite.

Science.gov (United States)

Sionkowska, Alina; Kaczmarek, Beata

2017-09-01

3D porous composites based on the blend of chitosan, collagen and hyaluronic acid with the addition of nano-hydroxyapatite were prepared. SEM images for the composites were made and the structure was assessed. Mechanical properties were studied using a Zwick&Roell Testing Mashine. In addition, the porosity and density of composites were measured. The concentration of calcium ions released from the material was detected by the complexometric titration method. The results showed that in 3D porous sponge based on the blend of chitosan, collagen and hyaluronic acid, inorganic particles of nanohydroxyapatite can be incorporated, as well as that the properties of 3D composites depend on the material composition. Mechanical parameters and thermal stability of ternary biopolymeric blends were improved by the addition of hydroxyapatite. Moreover, the porosity of ternary materials was higher than in materials based on pure chitosan or collagen. All composites were characterized by a porous structure with interconnected pores. Calcium ions can be released from the composite during its degradation in water. Copyright © 2017 Elsevier B.V. All rights reserved.

Manufacturing and characterization of porous SiC for flow channel inserts in dual-coolant blanket designs

Energy Technology Data Exchange (ETDEWEB)

Bereciartu, Ainhoa [CEIT and Tecnun (University of Navarra), Manuel de Lardizabal 15, 20018 San Sebastian (Spain); Ordas, Nerea, E-mail: nordas@ceit.es [CEIT and Tecnun (University of Navarra), Manuel de Lardizabal 15, 20018 San Sebastian (Spain); Garcia-Rosales, Carmen [CEIT and Tecnun (University of Navarra), Manuel de Lardizabal 15, 20018 San Sebastian (Spain); Morono, Alejandro; Malo, Marta; Hodgson, Eric R. [CIEMAT, Avenida Complutense 22, 28040 Madrid (Spain); Abella, Jordi [Institut Quimic de Sarria, University Ramon Llull, Via Augusta 390, 08017 Barcelona (Spain); Sedano, Luis [CIEMAT, Avenida Complutense 22, 28040 Madrid (Spain)

2011-10-15

SiC is the primary candidate for the flow channel inserts in dual-coolant blanket concepts. Porous SiC ceramics are attractive candidates for this non-structural application, since they can satisfy the required properties through a low cost manufacturing route, compared to SiC{sub f}/SiC. This work shows first results of the manufacturing of porous SiC ceramics prepared with different amounts of Y{sub 2}O{sub 3} and Al{sub 2}O{sub 3} as sintering additives. C powders were used as pore-formers by their burnout during oxidation after sintering. Comparison of microstructure, porosity, flexural strength, thermal and electrical conductivity and corrosion under Pb-15.7Li of porous SiC without and with sintering additives is presented. The addition of 2.5 wt.% of Y{sub 2}O{sub 3} and Al{sub 2}O{sub 3} improves the mechanical properties, and reduces the thermal and electrical conductivity down to reasonable values. Preliminary corrosion tests under Pb-15.7 Li at 500 deg. C show that the absence of a dense coating on porous SiC leads to poor corrosion behavior.

Quantitative analysis of vascular colonisation and angio-conduction in porous silicon-substituted hydroxyapatite with various pore shapes in a chick chorioallantoic membrane (CAM) model.

Science.gov (United States)

Magnaudeix, Amandine; Usseglio, Julie; Lasgorceix, Marie; Lalloue, Fabrice; Damia, Chantal; Brie, Joël; Pascaud-Mathieu, Patricia; Champion, Eric

2016-07-01

The development of scaffolds for bone filling of large defects requires an understanding of angiogenesis and vascular guidance, which are crucial processes for bone formation and healing. There are few investigations on the ability of a scaffold to support blood vessel guidance and it this is of great importance because it relates to the quality and dispersion of the blood vessel network. This work reports an analysis of vascularisation of porous silicon-substituted hydroxyapatite (SiHA) bioceramics and the effects of pore shape on vascular guidance using an expedient ex ovo model, the chick embryo chorioallantoic membrane (CAM) assay. Image analysis of vascularised implants assessed the vascular density, fractal dimension and diameter of blood vessels at two different scales (the whole ceramic and pores alone) and was performed on model SiHA ceramics harbouring pores of various cross-sectional geometries (circles, square, rhombus, triangles and stars). SiHA is a biocompatible material which allows the conduction of blood vessels on its surface. The presence of pores did not influence angiogenesis related-parameters (arborisation, fractal dimension) but pore geometry affected the blood vessel guidance and angio-conductive potential (diameter and number of the blood vessels converging toward the pores). The measured angles of pore cross-section modulated the number and diameter of blood vessels converging to pores, with triangular pores appearing of particular interest. This result will be used for shaping ceramic scaffolds with specific porous architecture to promote vascular colonisation and osteointegration. An expedient and efficient method, using chick embryo chorioallantoic membrane (CAM) assays, has been set up to characterise quantitatively the angiogenesis and the vascular conduction in scaffolds. This approach complements the usual cell culture assays and could replace to a certain extent in vivo experiments. It was applied to silicon

Study the properties of dense hydroxyapatite-extract from cow bone

International Nuclear Information System (INIS)

Sri Asliza, M.A.; Zaheruddin, K.; Shahrizal, H.

2009-01-01

In this study, natural hydroxyapatite (HA) was extracted from clean cow bone by treatment with NaOH and heating at high temperature before ground into fine powder. The HA powder were than mixed together with binder for several hours. Dense HA were formed in die steel mould by using uniaxially pressing method. Sample was sintered at different temperature 1150, 1200, 1250 and 1300 degree Celsius for several hours. The phases of specimen were identified using X-ray diffraction (XRD). The mechanical properties were analyzed using three-point bending testing and the microstructure was observed by scanning electron microscopy. From XRD results, natural HA shows phase of pure HA up to 1250 degree Celsius and fracture strength results indicated that the mechanical properties of specimen increase as temperature increase. From microstructure observation using SEM, HA specimen shows initial stages of sintering process at temperature 1150 degree Celsius and show changes in microstructure evolution as temperature increase up to 1300 degree Celsius. (author)

Optimising the bioreceptivity of porous glass tiles based on colonization by the alga Chlorella vulgaris

Energy Technology Data Exchange (ETDEWEB)

Ferrándiz-Mas, V., E-mail: v.ferrandiz@imperial.ac.uk [Department of Civil and Environmental Engineering, Imperial College London, London SW7 2BU (United Kingdom); Bond, T., E-mail: t.bond@imperial.ac.uk [Department of Civil and Environmental Engineering, Imperial College London, London SW7 2BU (United Kingdom); Zhang, Z., E-mail: zhen.zhang14@imperial.ac.uk [Department of Civil and Environmental Engineering, Imperial College London, London SW7 2BU (United Kingdom); Melchiorri, J., E-mail: jpmelchiorri@gmail.com [ARBOREA Research, Bessemer Building, Prince Consort Road, London SW7 2AZ (United Kingdom); Cheeseman, C.R., E-mail: c.cheeseman@imperial.ac.uk [Department of Civil and Environmental Engineering, Imperial College London, London SW7 2BU (United Kingdom)

2016-09-01

Green façades on buildings can mitigate greenhouse gas emissions. An option to obtain green facades is through the natural colonisation of construction materials. This can be achieved by engineering bioreceptive materials. Bioreceptivity is the susceptibility of a material to be colonised by living organisms. The aim of this research was to develop tiles made by sintering granular waste glass that were optimised for bioreceptivity of organisms capable of photosynthesis. Tiles were produced by pressing recycled soda-lime glass with a controlled particle size distribution and sintering compacted samples at temperatures between 680 and 740 °C. The primary bioreceptivity of the tiles was evaluated by quantifying colonisation by the algae Chlorella vulgaris (C. vulgaris), which was selected as a model photosynthetic micro-organism. Concentrations of C. vulgaris were measured using chlorophyll-a extraction. Relationships between bioreceptivity and the properties of the porous glass tile, including porosity, sorptivity, translucency and pH are reported. Capillary porosity and water sorptivity were the key factors influencing the bioreceptivity of porous glass. Maximum C. vulgaris growth and colonisation was obtained for tiles sintered at 700 °C, with chlorophyll-a concentrations reaching up to 11.1 ± 0.4 μg/cm{sup 2} of tile. Bioreceptivity was positively correlated with sorptivity and porosity and negatively correlated with light transmittance. The research demonstrates that the microstructure of porous glass, determined by the processing conditions, significantly influences bioreceptivity. Porous glass tiles with high bioreceptivity that are colonised by photosynthetic algae have the potential to form carbon-negative façades for buildings and green infrastructure. - Highlights: • Porous tiles made by sintering waste glass at variable temperatures • Bioreceptivity assessed by measuring colonisation by the algae C. vulgaris • Tiles sintered at 700 °C gave

Optimising the bioreceptivity of porous glass tiles based on colonization by the alga Chlorella vulgaris

International Nuclear Information System (INIS)

Ferrándiz-Mas, V.; Bond, T.; Zhang, Z.; Melchiorri, J.; Cheeseman, C.R.

2016-01-01

Green façades on buildings can mitigate greenhouse gas emissions. An option to obtain green facades is through the natural colonisation of construction materials. This can be achieved by engineering bioreceptive materials. Bioreceptivity is the susceptibility of a material to be colonised by living organisms. The aim of this research was to develop tiles made by sintering granular waste glass that were optimised for bioreceptivity of organisms capable of photosynthesis. Tiles were produced by pressing recycled soda-lime glass with a controlled particle size distribution and sintering compacted samples at temperatures between 680 and 740 °C. The primary bioreceptivity of the tiles was evaluated by quantifying colonisation by the algae Chlorella vulgaris (C. vulgaris), which was selected as a model photosynthetic micro-organism. Concentrations of C. vulgaris were measured using chlorophyll-a extraction. Relationships between bioreceptivity and the properties of the porous glass tile, including porosity, sorptivity, translucency and pH are reported. Capillary porosity and water sorptivity were the key factors influencing the bioreceptivity of porous glass. Maximum C. vulgaris growth and colonisation was obtained for tiles sintered at 700 °C, with chlorophyll-a concentrations reaching up to 11.1 ± 0.4 μg/cm"2 of tile. Bioreceptivity was positively correlated with sorptivity and porosity and negatively correlated with light transmittance. The research demonstrates that the microstructure of porous glass, determined by the processing conditions, significantly influences bioreceptivity. Porous glass tiles with high bioreceptivity that are colonised by photosynthetic algae have the potential to form carbon-negative façades for buildings and green infrastructure. - Highlights: • Porous tiles made by sintering waste glass at variable temperatures • Bioreceptivity assessed by measuring colonisation by the algae C. vulgaris • Tiles sintered at 700 °C gave maximum

Nanocrystalline hydroxyapatite doped with magnesium and zinc: Synthesis and characterization

Energy Technology Data Exchange (ETDEWEB)

Kalita, Samar J. [Department of Mechanical, Materials and Aerospace Engineering, University of Central Florida, Orlando, FL 32816-2450 (United States)]. E-mail: samar@mail.ucf.edu; Bhatt, Himesh A. [Department of Mechanical, Materials and Aerospace Engineering, University of Central Florida, Orlando, FL 32816-2450 (United States)

2007-05-16

During recent years, there have been efforts in developing nanocrystalline bioceramics, to enhance their mechanical and biological properties for use in tissue engineering applications. In this research, we made an attempt to synthesize nanocrystalline bioactive hydroxyapatite (Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}, HAp) ceramic powder in the lower-end of nano-range (2-10 nm), using a simple low-temperature sol-gel technique and studied its densification behavior. We further studied the effects of metal ion dopants during synthesis on powder morphology, and the properties of the sintered structures. Calcium nitrate and triethyl phosphite were used as precursors for calcium and phosphorous, respectively, for sol-gel synthesis. Calculated quantities of magnesium oxide and zinc oxide were incorporated as dopants into amorphous dried powder, prior to calcination at 250-550 {sup o}C. The synthesized powders were analyzed for their phases using X-ray diffraction technique and characterized for powder morphology and particle size using transmission electron microscopy (TEM). TEM analysis showed that the average particle size of the synthesized powders were in the range of 2-10 nm. The synthesized nano-powders were uniaxially compacted and then sintered at 1250 {sup o}C and 1300 {sup o}C for 6 h, separately, in air. A maximum average sintered density of 3.29 g/cm{sup 3} was achieved in structures sintered at 1300 {sup o}C, developed from nano-powder doped with magnesium. Vickers hardness testing was performed to determine the hardness of the sintered structures. Uniaxial compression tests were performed to evaluate the mechanical properties. Bioactivity and biodegradation behavior of the sintered structures were assessed in simulated body fluid (SBF) and maintained in a dynamic state.

Influence of pentavalent dopant addition to polarization and bioactivity of hydroxyapatite

International Nuclear Information System (INIS)

Dhal, Jharana; Bose, Susmita; Bandyopadhyay, Amit

2013-01-01

Influence of pentavalent tantalum doping in bulk hydroxyapatite (HAp) ceramics has been investigated for polarizability and bioactivity. Phase analysis from X-ray diffraction measurement indicates that increasing dopant concentration decreased the amount of HAp phase and increased β-TCP and/or α-TCP phases during sintering at 1250 °C in a muffle furnace. Results from thermally stimulated depolarization current (TSDC) measurements showed that doping hindered charge storage ability in HAp ceramics, and doped samples stored fewer charge compared to pure HAp. However, doping enhanced wettability of HAp samples, which was improved further due to polarization. In vitro human osteoblast cell–material interaction study revealed an increase in bioactivity due to dopant addition and polarization compared to pure HAp. This increase in bioactivity was attributed to the increase in wettability due to surface charge and dopant addition. - Highlights: • Tantalum doping makes HAp unstable during sintering at 1250 °C and forms TCP. • Tantalum doping reduces charge storage ability of HAp ceramics. • Even with lower charge storage ability tantalum doping improves wettability. • Tantalum doping enhances bioactivity of calcium phosphate based sintered compacts

Fabrication of low thermal expansion SiC/ZrW{sub 2}O{sub 8} porous ceramics

Energy Technology Data Exchange (ETDEWEB)

Poowancum, A; Matsumaru, K; Juarez-Ramirez, I; Ishizaki, K [Department of Mechanical Engineering, Nagaoka University of Technology, 1603-1 Kamitomioka, Nagaoka, Niigata 940-2188 (Japan); Torres-Martinez, L M [Universidad Autonoma de Nuevo Leon, Av. Universidad s/n, San Nicolas de los Garza, NL, C.P. 66451 (Mexico); Fu, Z Y [State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan, Hubei, 430070 (China); Lee, S W, E-mail: anurat@ishizaki.nagaokaut.ac.jp [Department of Environment Engineering, Sun Moon University, 100, Kalsan-ri, Tangjeong-myeon, Asan, Chungnam 336-708 (Korea, Republic of)

2011-03-15

Low or zero thermal expansion porous ceramics are required for several applications. In this work near zero thermal expansion porous ceramics were fabricated by using SiC and ZrW{sub 2}O{sub 8} as positive and negative thermal expansion materials, respectively, bonded by soda lime glass. The mixture of SiC, ZrW{sub 2}O{sub 8} and soda lime glass was sintered by Pulsed Electric Current Sintering (PECS, or sometimes called Spark Plasma Sintering, SPS) at 700 deg. C. Sintered samples with ZrW{sub 2}O{sub 8} particle size smaller than 25 {mu}m have high thermal expansion coefficient, because ZrW{sub 2}O{sub 8} has the reaction with soda lime glass to form Na{sub 2}ZrW{sub 3}O{sub 12} during sintering process. The reaction between soda lime glass and ZrW{sub 2}O{sub 8} is reduced by increasing particle size of ZrW{sub 2}O{sub 8}. Sintered sample with ZrW{sub 2}O{sub 8} particle size 45-90 {mu}m shows near zero thermal expansion.

The drug release study of ceftriaxone from porous hydroxyapatite scaffolds.

Science.gov (United States)

Al-Sokanee, Zeki N; Toabi, Abedl Amer H; Al-Assadi, Mohammed J; Alassadi, Erfan A S

2009-01-01

Hydroxyapatite (HAP) is an important biomedical material that is used for grafting osseous defects. It has an excellent bioactivity and biocompatibility properties. To isolate hydroxyapatite, pieces of cleaned cattle's bone were heated at different temperature range from 400 degrees C up to 1,200 degrees C. A reasonable yield of 60.32% w/w HAP was obtained at temperature range from 1,000 degrees C to 1,200 degrees C. Fourier transform infrared spectra and the thermogravimetric measurement showed a clear removal of organic at 600 degrees C as well as an excellent isolation of HAP from the bones which was achieved at 1,000-1,200 degrees C. This was also confirmed from X-ray diffraction of bone sample heated at 1,200 degrees C. The concentration ions were found to be sodium, potassium, lithium, zinc, copper, iron, calcium, magnesium, and phosphate present in bones within the acceptable limits for its role in the bioactivity property of HAP. Glucose powder was used as a porosifier. Glucose was novel and excellent as porogen where it was completely removed by heating, giving an efficient porosity in the used scaffolds. The results exhibited that the ceftriaxone drug release was increased with increasing the porosity. It was found that a faster, higher, and more regular drug release was obtained from the scaffold with a porosity of 10%.

Vancomycin–chitosan composite deposited on post porous hydroxyapatite coated Ti6Al4V implant for drug controlled release

Energy Technology Data Exchange (ETDEWEB)

Yang, Chi-Chuan [Department of Materials Science and Engineering, National Chung Hsing, University 250, Kuo-Kuang Road, Taichung 40227, Taiwan (China); Lin, Chien-Chung [Department of Materials Science and Engineering, National Chung Hsing, University 250, Kuo-Kuang Road, Taichung 40227, Taiwan (China); Department of Orthopaedic Surgery, Taichung Armed Force General Hospital, 348, Sec. 2, Jhongshan Road, Taiping City, Taichung 411, Taiwan (China); Liao, Jiunn-Wang [Graduate Institute of Veterinary Pathobiology, National Chung Hsing, University 250, Kuo-Kuang Road, Taichung 40227, Taiwan (China); Yen, Shiow-Kang, E-mail: skyen@dragon.nchu.edu.tw [Department of Materials Science and Engineering, National Chung Hsing, University 250, Kuo-Kuang Road, Taichung 40227, Taiwan (China)

2013-05-01

Through the hydrogen bonds and the deprotonation, the vancomycin–chitosan composite has been originally deposited on Ti4Al4V by electrochemical technology. However, the rapid destruction of the hydrogen bonding between them by polar water molecules during immersion tests revealed 80% drug burst in a few hours. In this study, the post porous hydroxyapatite (HA) coated Ti4Al4V is prepared for the subsequent electrolytic deposition of vancomycin–chitosan composite to control the drug release. As expected, the initial burst is reduced to 55%, followed by a steady release about 20% from day 1 to day 5 and a slower release of the retained 25% after day 6, resulting in bacterial inhibition zone diameter of 30 mm which can last for more than a month in antibacterial tests, compared with the coated specimen without HA gradually loosing inhibition zone after 21 days. Besides, the cell culture indicates that the vancomycin–chitosan/HA composite coated has enhanced the proliferation, the differentiation and the mineralization of the osteoblast-like cell. In general, it is helpful for the osteointegration on permanent implants. Consistently, it effectively provides the prophylaxis and therapy of osteomyelitis according to the results of the rabbit infection animal model. - Highlights: ► The releasing curve of the vancomycin–chitosan/HA composite revealed three periods. ► The drug release sustained one month due to the effect of post porous HA coating. ► The composite coating could treat the osteomyelitis in the rabbit infection model.

Superplastically foaming method to make closed pores inclusive porous ceramics

International Nuclear Information System (INIS)

Kishimoto, Akira; Hayashi, Hidetaka

2011-01-01

Porous ceramics incorporates pores to improve several properties including thermal insulation maintaining inherenet ceramic properties such as corrosion resistance and large mechanical strength. Conventional porous ceramics is usually fabricated through an insufficient sintering. Since the sintering accompanies the exclusion of pores, it must be terminated at the early stage to maintain the high porosity, leading to degraded strength and durability. Contrary to this, we have innovated superplastically foaming method to make ceramic foams only in the solid state. In this method, the previously inserted foam agent evaporates after the full densification of matrix at around the sintering temperature. Closed pores expand utilizing the superplastic deformation driven by the evolved gas pressure. The typical features of this superplastically foaming method are listed as follows, 1. The pores are introduced after sintering the solid polycrystal. 2. Only closed pores are introduced, improving the insulation of gas and sound in addition to heat. 3. The pore walls are fully densified expecting a large mechanical strength. 4. Compared with the melt foaming method, this method is practical because the fabrication temperature is far below the melting point and it does not need molds. 5. The size and the location pores can be controlled by the amount and position of the foam agent.

Hexagonal OsB2: Sintering, microstructure and mechanical properties

International Nuclear Information System (INIS)

Xie, Zhilin; Lugovy, Mykola; Orlovskaya, Nina; Graule, Thomas; Kuebler, Jakob; Mueller, Martin; Gao, Huili; Radovic, Miladin; Cullen, David A.

2015-01-01

Highlights: • ReB 2 -type hexagonal OsB 2 powder has been densified by spark plasma sintering. • The sintered OsB 2 contains ∼80 wt.% hexagonal and ∼20 wt.% orthorhombic phases. • The average grain size of the sintered OsB 2 sample was 0.56 ± 0.26 μm. • H = 31 ± 9 GPa and E = 574 ± 112 GPa measured by nanoindentation. - Abstract: The metastable high pressure ReB 2 -type hexagonal OsB 2 bulk ceramics was produced by spark plasma sintering. The phase composition, microstructure, and mechanical behavior of the sintered OsB 2 were studied by X-ray diffraction, optical microscopy, TEM, SEM, EDS, and nanoindentation. The produced ceramics was rather porous and contained a mixture of hexagonal (∼80 wt.%) and orthorhombic (∼20 wt.%) phases as identified by X-ray diffraction and EBSD analysis. Two boron-rich phases, which do not contain Os, were also identified by TEM and SEM/EDS analysis. Nanoindentation measurements yielded a hardness of 31 ± 9 GPa and Young’s modulus of 574 ± 112 GPa, indicating that the material is rather hard and very stiff; however, it is very prone to crack formation and propagation, which is indicative of a very brittle nature of this material. Improvements in the sintering regime are required in order to produce dense, homogeneous and single phase hexagonal OsB 2 bulk ceramics

A microstructural study of the degradation and calcium release from hydroxyapatite-calcium oxide ceramics made by infiltration.

Science.gov (United States)

Zhang, Qinghao; Schmelzer, Eva; Gerlach, Jörg C; Nettleship, Ian

2017-04-01

Hydroxyapatite pellets, partially densified in a low-temperature heat treatment, were infiltrated with calcium nitrate solution followed by in-situ precipitation of Ca(OH) 2 and CaCO 3 . The infiltrated bodies were then densified to high relative density and the calcium carbonate transformed to calcium oxide during sintering and resulted in biphasic hydroxyapatite-CaO ceramics. This work investigated the influence of the infiltration on surface morphology, weight change, and microstructural-level degradation caused by exposure to saline at pH=7.4 and a temperature of 20°C. The CaO rendered the materials more susceptible to degradation, and released calcium into the saline faster than single phase, calcium deficient hydroxyapatite (HA) that were used as a control. In consequence, these ceramics could be used to release calcium into the culture microenvironments of bone tissue or bone marrow cells next to a scaffold surface. Copyright © 2016 Elsevier B.V. All rights reserved.

Understanding the Biocompatibility of Sintered Calcium Phosphate with Ratio of [Ca]/[P] = 1.50

Directory of Open Access Journals (Sweden)

Feng-Lin Yen

2012-01-01

Full Text Available Biocompatibility of sintered calcium phosphate pellets with [Ca]/[P] = 1.50 was determined in this study. Calcium pyrophosphate (CPP phase formed on the sintered pellets immersed in a normal saline solution for 14 d at 37∘C. The intensities of hydroxyapatite (HA reflections in the X-ray diffraction (XRD patterns of the pellets were retrieved to as-sintered state. The pellet surface morphology shows that CPP crystallites were clearly present and make an amorphous calcium phosphate (ACP to discriminate against become to the area of slice join together. In addition, the intensities of the CPP reflections in the XRD patterns were the highest when the pellets were immersed for 28 d. When the CPP powders were extracted from the pellets after immersion in the solution for 14 d, the viability of 3T3 cells remained above 90% for culture times from 1 to 4 d. The pellet surface morphology observed using optical microscopy showed that the cells did not adhere to the bottom of the sintered pellets when cultured for 4 d; however, some CPP phase precipitates were formed, as confirmed by XRD. In consequence, the results suggest that the sintered HA powders are good materials for use in biomedical applications because of their good biocompatibility.

Low temperature sintering of hyperstoichiometric uranium dioxide

International Nuclear Information System (INIS)

Chevrel, H.

1991-12-01

In the lattice of uranium dioxide with hyperstoichiometric oxygen content (UO 2+x ), each additional oxygen atoms is introduced by shifting two anions from normal sites to interstitial ones, thereby creating two oxygen vacancies. The point defects then combine to form complex defects comprising several interstitials and vacancies. The group of anions (3x) in the interstitial position participate in equilibria promoting the creation of uranium vacancies thereby considerably increasing uranium self-diffusion. However, uranium grain boundaries diffusion governs densification during the first two stages of sintering of uranium dioxide with hyperstoichiometric oxygen content, i.e., up to 93% of the theoretical density. Surface diffusion and evaporation-condensation, which are considerably accentuated by the hyperstoichiometric deviation, play an active role during sintering by promoting crystalline growth during the second and third stages of sintering. U 8 O 8 can be added to adjust the stoichiometry and to form a finely porous structure and thus increase the pore area subjected to surface phenomena. The composition with an O/U ratio equal to 2.25 is found to densify the best, despite a linear growth in sintering activation energy with hyperstoichiometric oxygen content, increasing from 300 kj.mol -1 for UO 2.10 to 440 kJ.mol -1 for UO 2.25 . Seeds can be introduced to obtain original microstructures, for example the presence of large grains in small-grain matrix

Testing of porous SiC with dense coating under relevant conditions for Flow Channel Insert application

Energy Technology Data Exchange (ETDEWEB)

Ordás, N., E-mail: nordas@ceit.es [CEIT and Tecnun (University of Navarra), Manuel de Lardizábal 15, 20018 San Sebastián (Spain); Bereciartu, A.; García-Rosales, C. [CEIT and Tecnun (University of Navarra), Manuel de Lardizábal 15, 20018 San Sebastián (Spain); Moroño, A.; Malo, M.; Hodgson, E.R. [CIEMAT, Avenida Complutense 22, 28040 Madrid (Spain); Abellà, J.; Colominas, S. [Institut Químic de Sarrià, University Ramon Llull, Via Augusta 390, 08017 Barcelona (Spain); Sedano, L. [CIEMAT, Avenida Complutense 22, 28040 Madrid (Spain)

2014-10-15

Highlights: • Porous SiC coated by CVD with a dense coating was developed for Flow Channel Inserts (FCI) in dual-coolant blanket concept. • Porous SiC was obtained following the sacrificial template technique, using Al{sub 2}O{sub 3} and Y{sub 2}O{sub 3} as sintering additives. • Flexural strength, thermal and electrical conductivity, and microstructure of uncoated and coated porous SiC are presented. • Adhesion of coating to porous SiC and its corrosion behavior under Pb-17.5Li at 700 °C are shown. - Abstract: Thermally and electrically insulating porous SiC ceramics are attractive candidates for Flow Channel Inserts (FCI) in dual-coolant blanket concepts thanks to its relatively inexpensive manufacturing route. To prevent tritium permeation and corrosion by Pb-15.7 a dense coating has to be applied on the porous SiC. Despite not having structural function, FCI must exhibit sufficient mechanical strength to withstand strong thermal gradients and thermo-electrical stresses during operation. This work summarizes the results on the development of coated porous SiC for FCI. Porous SiC was obtained following the sacrificial template technique, using Al{sub 2}O{sub 3} and Y{sub 2}O{sub 3} as sintering additives and a carbonaceous phase as pore former. Sintering was performed in inert gas at 1850–1950 °C during 15 min to 3 h, followed by oxidation at 650 °C to eliminate the carbonaceous phase. The most promising bulk materials were coated with a ∼30 μm thick dense SiC by CVD. Results on porosity, bending tests, thermal and electrical conductivity are presented. The microstructure of the coating, its adhesion to the porous SiC and its corrosion behavior under Pb-17.5Li are also shown.

Hydroxyapatite coatings produced on commercially pure titanium by micro-arc oxidation

Energy Technology Data Exchange (ETDEWEB)

Huang Yong [College of Materials Science and Engineering, South China University of Technology, Guangzhou 510641 (China); Wang Yingjun [College of Materials Science and Engineering, South China University of Technology, Guangzhou 510641 (China); Ning Chengyun [College of Materials Science and Engineering, South China University of Technology, Guangzhou 510641 (China); Nan Kaihui [College of Materials Science and Engineering, South China University of Technology, Guangzhou 510641 (China); Han Yong [State Key Laboratory for Mechanical Behavior of Materials, Xi' an Jiaotong University, Xi' an 710049 (China)

2007-09-15

A porous hydroxyapatite (HA) coating on commercially pure titanium was prepared by micro-arc oxidation (MAO) in electrolytic solution containing calcium acetate and {beta}-glycerol phosphate disodium salt pentahydrate ({beta}-GP). The thickness, phase, composition morphology and biocompatibility of the oxide coating were characterized by x-ray diffraction (XRD), electron probe microanalysis (EPMA), scanning electron microscopy (SEM) with an energy dispersive x-ray spectrometer (EDS) and cell culture. The thickness of the MAO film was about 20 {mu}m, and the coating was porous and uneven without any apparent interface to the titanium substrates. The result of XRD showed that the porous coating was made up of HA film. The favorable osteoblast cell affinity gives HA film good biocompatibility. HA coatings are expected to have significant uses for medical applications such as dental implants and artificial bone joints.

Hydroxyapatite coatings produced on commercially pure titanium by micro-arc oxidation.

Science.gov (United States)

Huang, Yong; Wang, Yingjun; Ning, Chengyun; Nan, Kaihui; Han, Yong

2007-09-01

A porous hydroxyapatite (HA) coating on commercially pure titanium was prepared by micro-arc oxidation (MAO) in electrolytic solution containing calcium acetate and beta-glycerol phosphate disodium salt pentahydrate (beta-GP). The thickness, phase, composition morphology and biocompatibility of the oxide coating were characterized by x-ray diffraction (XRD), electron probe microanalysis (EPMA), scanning electron microscopy (SEM) with an energy dispersive x-ray spectrometer (EDS) and cell culture. The thickness of the MAO film was about 20 microm, and the coating was porous and uneven without any apparent interface to the titanium substrates. The result of XRD showed that the porous coating was made up of HA film. The favorable osteoblast cell affinity gives HA film good biocompatibility. HA coatings are expected to have significant uses for medical applications such as dental implants and artificial bone joints.

Hydroxyapatite coatings produced on commercially pure titanium by micro-arc oxidation

International Nuclear Information System (INIS)

Huang Yong; Wang Yingjun; Ning Chengyun; Nan Kaihui; Han Yong

2007-01-01

A porous hydroxyapatite (HA) coating on commercially pure titanium was prepared by micro-arc oxidation (MAO) in electrolytic solution containing calcium acetate and β-glycerol phosphate disodium salt pentahydrate (β-GP). The thickness, phase, composition morphology and biocompatibility of the oxide coating were characterized by x-ray diffraction (XRD), electron probe microanalysis (EPMA), scanning electron microscopy (SEM) with an energy dispersive x-ray spectrometer (EDS) and cell culture. The thickness of the MAO film was about 20 μm, and the coating was porous and uneven without any apparent interface to the titanium substrates. The result of XRD showed that the porous coating was made up of HA film. The favorable osteoblast cell affinity gives HA film good biocompatibility. HA coatings are expected to have significant uses for medical applications such as dental implants and artificial bone joints

Independent Factors Affecting Postoperative Complication Rates After Custom-Made Porous Hydroxyapatite Cranioplasty: A Single-Center Review of 109 Cases.

Science.gov (United States)

Still, Megan; Kane, Abdoulaye; Roux, Alexandre; Zanello, Marc; Dezamis, Edouard; Parraga, Eduardo; Sauvageon, Xavier; Meder, Jean-François; Pallud, Johan

2018-06-01

Cranioplasties are an important neurosurgical procedure not only for improved cosmesis but also for improved functional recovery after craniectomy with a large cranial defect. The aim of this study was to identify predictive factors of postcranioplasty complications using custom-made porous hydroxyapatite cranioplasty. Retrospective review was performed of all patients who underwent a reconstructive cranioplasty using custom-made hydroxyapatite at our institution between February 2008 and September 2017. Postoperative complications considered included bacterial infection, seizures, hydrocephalus requiring ventricular shunt placement, and cranioplasty-to-bone shift. Variables associated at P < 0.1 level in unadjusted analysis were entered into backward stepwise logistic regression models. Of 109 patients included, 15 (13.8%) experienced postoperative infection, with craniectomy performed at an outside institution (adjusted odds ratio [OR] 10.37 [95% confidence interval [CI], 2.03-75.27], P = 0.012) and a previous infection at the surgical site (adjusted OR 6.15 [95%CI, 1.90-19.92], P = 0.003) identified as independent predictors. Six patients (5.5%) experienced postoperative seizures, with stroke (ischemic and hemorrhagic) as a reason for craniectomy (adjusted OR 11.68 [95% CI, 2.56-24.13], P < 0.001) and the presence of seizures in the month before cranioplasty (adjusted OR 9.39 [95% CI, 2.04-127.67], P = 0.002) identified as independent predictors. Four patients (3.7%) experienced postcranioplasty hydrocephalus necessitating shunt placement, and 5 patients (4.6%) experienced cranioplasty-to-bone shift ≥5 mm, but no significant predictive factors were identified for either complication. This study identified possible predictive factors for postcranioplasty complications to help identify at-risk patients, guide prophylactic care, and improve morbidity of this important surgical procedure. Copyright © 2018 Elsevier Inc. All rights reserved.

Coupling of HDPE/hydroxyapatite composites by silane-based methodologies.

Science.gov (United States)

Sousa, R A; Reis, R L; Cunha, A M; Bevis, M J

2003-06-01

Several coupling treatments based on silane chemicals were investigated for the development of high density (HDPE)/hydroxyapatite (HA) composites. Two HA powders, sintered HA (HAs) and non sintered HA (HAns), were studied in combination with five silanes, namely y-methacryloxy propyltrimethoxy silane (MEMO), 3-(2-aminoethyl)aminopropyltrimethoxy silane (DAMO), vinyltrimethoxy silane (VTMO), 3-aminopropyltriethoxy silane (AMEO) and trimethoxypropyl silane (PTMO). The HA particles were treated by a dipping in method or by spraying with silane solutions. After drying, the treated powders were compounded with HDPE or HDPE with acrylic acid and/or organic peroxide and subsequently compression molded. The tensile test specimens obtained from the molded plates were tensile tested and their fracture surfaces were observed by scanning electron microscopy (SEM). For the sintered HA (HAs) composites, the most effective coupling treatments concerning stiffness are those based on MEMO and AMEO. The low influence of these coupling procedures on strength is believed to be associated to the low volume fraction and the relatively smooth surface of the used HA particles. For the non-sintered HA (HAns) composites, it was possible to improve significantly both the stiffness and the strength. Amino silanes demonstrated to be highly efficient concerning strength enhancement. The higher effectiveness of the coupling treatments for HAns filled composites is attributed to their higher particle surface area, smaller particle size distribution and expected higher chemical reactivity. For both cases, the improvement in mechanical performance after the coupling treatment is consistent with the enhancement in interfacial adhesion observed by SEM.

Processing of porous zirconia ceramics by direct consolidation with starch

International Nuclear Information System (INIS)

Garrido, Liliana B; Albano, Maria P

2008-01-01

Porous ceramics are used especially for those environments with high temperatures, heavy wear and in a corrosive medium. Zirconium-based materials are useful for such applications as sensors, filters, support for catalytic reactions, porous components for sofc and in biomedical applications. A conventional method for producing porous ceramics consists of the addition and later decomposition by calcination (pyrolisis) of different organic materials that act as pore formers. Several wet processing possibilities have been developed. Among these is a technique of direct consolidation with starch. This process begins with the preparation of an aqueous suspension of the ceramic with the dispersants needed to stabilize it, to which the starch is added. After casting in a waterproof mold, the suspension thermally hardens into the desired shape. The dry compacts undergo the sintering cycle to obtain pieces almost in their final form. This study aims to optimize the processing of porous zirconium ceramics using starch as a pore and binder forming agent. Zirconium with 3% yttrium molar stabilized in tetragonal phase was used. The aqueous suspensions (52-55% vol) of the zirconium-starch mixtures with different compositions were stabilized with a commercial solution of ammonium polyacrylate as a dispersant and were hardened in plastic molds at 90 o C for 30 min. The influence of added volume of starch on the physical characteristics of the pieces in green state was established while maintaining the temperature, the gelling time and the conditions of constant drying. The sintering was carried out at 1000-1500 o C-2h. The characteristics of the sintered product were evaluated by measuring density, volumetric contraction, intrusion of Hg and the evolution of the crystalline phases by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The microstructural properties of ceramic (pore volume, the relation between open and closed porosity, size distribution, morphology of

The influence of sintering temperature on microstructure and mechanical properties of Ni-Al intermetallics fabricated by SPS

Energy Technology Data Exchange (ETDEWEB)

Thömmes, A., E-mail: thoemmes.alexander@gmail.com; Shevtsova, L. I., E-mail: edeliya2010@mail.ru; Laptev, I. S., E-mail: ilya-laptev-nstu@mail.ru; Mul, D. O., E-mail: ddariol@yandex.ru [Novosibirsk State Technical University, Novosibirsk, 630073 (Russian Federation); Mali, V. I., E-mail: vmali@mail.ru; Anisimov, A. G., E-mail: anis@hydro.nsc.ru [Lavrentyev Institute of Hydrodynamics SB RAS, Novosibirsk, 630090 (Russian Federation)

2015-10-27

In the present study PN85Yu15 was used as elemental powder to produce a sintered compound with Ni3Al as main phase. The Spark Plasma Sintering (SPS) technique is used to compact the powders. The powder was sintered in a temperature range between 1000°C and 1150°C to observe the influence of the sintering temperature on the microstructure and the mechanical properties. The microstructure was observed with optical microscope (OM), the phase composition was characterized by X-ray diffraction (XRD) technique. Density and microhardness were observed and compared the values with the results of other researchers. The compressive-, density- and microhardness tests show as clear result that with increasing the sintering temperature nearly all properties become better and also the microstructure studies show that porous places become less.

A Simple Method to Functionalize the Surface of Plasma Electrolytic Oxidation Produced TiO2 Coatings for Growing Hydroxyapatite

International Nuclear Information System (INIS)

Teng, Huan-Ping; Yang, Chia-Jung; Lin, Jia-Fu; Huang, Yu-Hsin; Lu, Fu-Hsing

2016-01-01

Highlights: • TiO 2 coatings with porous surfaces were produced by plasma electrolytic oxidation. • Simple pre-immersion in K 2 HPO 4 could functionalize the surfaces of the TiO 2 . • Such pre-immersion enhanced substantially the growth of hydroxyapatite in SBF. • Growth mechanisms of hydroxyapatite via the pre-immersion have been proposed. • MTT assay shows great osteoblast-like cell activity on the obtained hydroxyapatite. - Abstract: Conventionally, hydrothermal treatment was often used to modify the TiO 2 surface prior to the growth of hydroxyapatite (HA) that is one of the most important implant biomaterials. In this work, a simple pre-immersion of the obtained TiO 2 in a weak base, instead of the conventionally high pressure-temperature hydrothermal pre-treatment, was conducted prior to the growth of HA. Firstly, anatase TiO 2 coatings with porous surfaces were produced by plasma electrolytic oxidation with optimized processing parameters. X-ray diffraction patterns and field-emission microscopy reveal that the anatase TiO 2 films with porous surfaces were produced by plasma electrolytic oxidation. Subsequently, the films were pre-immersed in 0.1–2 M K 2 HPO 4 solutions for only 10 min. Fourier transform infrared spectroscopy shows that the −OH functional groups were generated after such pre-immersion, which could enhance significantly the growth of a single phase of HA in simulated body fluid (SBF). Growth mechanisms of HA via the pre-immersion treatment and soaking in SBF have been proposed. Moreover, the proliferation rate and attachment of the MG-63 osteoblast cells were greatly enhanced on the obtained HA compared to that without the immersion pre-treatment from the MTT assay and morphology analyses. This simple immersion pre-treatment evidently provides an easy route for the growth of HA and has great potential for biomedical applications.

Effect of process control agent on the porous structure and mechanical properties of a biomedical Ti-Sn-Nb alloy produced by powder metallurgy.

Science.gov (United States)

Nouri, A; Hodgson, P D; Wen, C E

2010-04-01

The influence of different amounts and types of process control agent (PCA), i.e., stearic acid and ethylene bis-stearamide, on the porous structure and mechanical properties of a biomedical Ti-16Sn-4Nb (wt.%) alloy was investigated. Alloy synthesis was performed on elemental metal powders using high-energy ball milling for 5h. Results indicated that varying the PCA content during ball milling led to a drastic change in morphology and particle-size distribution of the ball-milled powders. Porous titanium alloy samples sintered from the powders ball milled with the addition of various amounts of PCA also revealed different pore morphology and porosity. The Vickers hardness of the sintered titanium alloy samples exhibited a considerable increase with increasing PCA content. Moreover, the addition of larger amounts of PCA in the powder mixture resulted in a significant increase in the elastic modulus and peak stress for the sintered porous titanium alloy samples under compression. It should also be mentioned that the addition of PCA introduced contamination (mainly carbon and oxygen) into the sintered porous product. Crown Copyright 2009. Published by Elsevier Ltd. All rights reserved.

Sintering of Fine Particles in Suspension Plasma Sprayed Coatings

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Leszek Latka

2010-07-01

Full Text Available Suspension plasma spraying is a process that enables the production of finely grained nanometric or submicrometric coatings. The suspensions are formulated with the use of fine powder particles in water or alcohol with some additives. Subsequently, the suspension is injected into plasma jet and the liquid additives evaporate. The remaining fine solids are molten and subsequently agglomerate or remain solid, depending on their trajectory in the plasma jet. The coating’s microstructure results from these two groups of particles arriving on a substrate or previously deposited coating. Previous experimental studies carried out for plasma sprayed titanium oxide and hydroxyapatite coatings enabled us to observe either a finely grained microstructure or, when a different suspension injection mode was used, to distinguish two zones in the microstructure. These two zones correspond to the dense zone formed from well molten particles, and the agglomerated zone formed from fine solid particles that arrive on the substrate in a solid state. The present paper focuses on the experimental and theoretical analysis of the formation process of the agglomerated zone. The experimental section establishes the heat flux supplied to the coating during deposition. In order to achieve this, calorimetric measurements were made by applying experimental conditions simulating the real coatings’ growth. The heat flux was measured to be in the range from 0.08 to 0.5 MW/m2,depending on the experimental conditions. The theoretical section analyzes the sintering during the coating’s growth, which concerns the fine particles arriving on the substrate in the solid state. The models of volume, grain boundary and surface diffusion were analyzed and adapted to the size and chemistry of the grains, temperature and time scales corresponding to the suspension plasma spraying conditions. The model of surface diffusion was found to best describe the sintering during suspension

Biomimetic apatite-coated porous PVA scaffolds promote the growth of breast cancer cells

International Nuclear Information System (INIS)

Ye, Mao; Mohanty, Pravansu; Ghosh, Gargi

2014-01-01

Recapitulating the native environment of bone tissue is essential to develop in vitro models of breast cancer bone metastasis. The bone is a composite material consisting of organic matrix and inorganic mineral phase, primarily hydroxyapatite. In this study, we report the mineralization of porous poly vinyl alcohol (PVA) scaffolds upon incubation in modified Hanks' Balanced Salt Solution (HBSS) for 14 days. Scanning electron microscopy, energy dispersive X-ray analysis, and X-ray diffraction analysis revealed that the deposited minerals have composition similar to hydroxyapatite. The study demonstrated that the rate of nucleation and growth of minerals was faster on surfaces of less porous scaffolds. However, upon prolonged incubation, formation of mineral layer was observed on the surface of all the scaffolds. In addition, the study also demonstrated that 3D mineralization only occurred for scaffolds with highly interconnected porous networks. The mineralization of the scaffolds promoted the adsorption of serum proteins and consequently, the adhesion and proliferation of breast cancer cells. - Highlights: • Porous PVA scaffolds fabricated via mechanical agitation followed by freeze-drying. • Mineralization of the scaffold was carried out by utilizing biomimetic approach. • Mineralization resulted in increased protein adsorption on the scaffold. • Increased breast cancer cell growth was observed on mineralized scaffolds

Biomimetic apatite-coated porous PVA scaffolds promote the growth of breast cancer cells

Energy Technology Data Exchange (ETDEWEB)

Ye, Mao; Mohanty, Pravansu; Ghosh, Gargi, E-mail: gargi@umich.edu

2014-11-01

Recapitulating the native environment of bone tissue is essential to develop in vitro models of breast cancer bone metastasis. The bone is a composite material consisting of organic matrix and inorganic mineral phase, primarily hydroxyapatite. In this study, we report the mineralization of porous poly vinyl alcohol (PVA) scaffolds upon incubation in modified Hanks' Balanced Salt Solution (HBSS) for 14 days. Scanning electron microscopy, energy dispersive X-ray analysis, and X-ray diffraction analysis revealed that the deposited minerals have composition similar to hydroxyapatite. The study demonstrated that the rate of nucleation and growth of minerals was faster on surfaces of less porous scaffolds. However, upon prolonged incubation, formation of mineral layer was observed on the surface of all the scaffolds. In addition, the study also demonstrated that 3D mineralization only occurred for scaffolds with highly interconnected porous networks. The mineralization of the scaffolds promoted the adsorption of serum proteins and consequently, the adhesion and proliferation of breast cancer cells. - Highlights: • Porous PVA scaffolds fabricated via mechanical agitation followed by freeze-drying. • Mineralization of the scaffold was carried out by utilizing biomimetic approach. • Mineralization resulted in increased protein adsorption on the scaffold. • Increased breast cancer cell growth was observed on mineralized scaffolds.

A comparative evaluation of porous hydroxyapatite bone graft with and without platelet-rich plasma in the treatment of periodontal intrabony osseous defects: A clinico-Radiographic study

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Gouri Bhatia

2018-01-01

Full Text Available Background: Today, regenerative attempts for treatment of periodontal disease focus on the introduction of a filler material into the defect in hope of inducing bone regeneration. The purpose of this study was to clinically and radiographically evaluate the use of porous hydroxyapatite bone graft with and without platelet-rich plasma (PRP in the treatment of intrabony defects. Materials and Methods: The study was carried out in ten patients between 18 and 60 years. Patients with pocket depth ≥5 mm and radiographic evidence of vertical bone loss in the affected site were randomly assigned to treatment with a combination of PRP + Hydroxyapatite (HA (test sites or HA alone (control sites. The parameters were compared at baseline and 6 months postoperatively. Results: There was a statistically significant reduction in probing depth and gain in clinical attachment in both the groups individually (more in experimental group; however, on comparing the two groups, the net reduction was not significant. Radiographic assessment showed a decrease in the defect size in both the groups. Conclusion: PRP in addition to a bone graft in the treatment of intrabony defects is safe and shows improved defect fill as compared to the use of bone graft alone.

Application of interconnected porous hydroxyapatite ceramic block for onlay block bone grafting in implant treatment: A case report.

Science.gov (United States)

Ohta, Kouji; Tada, Misato; Ninomiya, Yoshiaki; Kato, Hiroki; Ishida, Fumi; Abekura, Hitoshi; Tsuga, Kazuhiro; Takechi, Masaaki

2017-12-01

Autogenous block bone grafting as treatment for alveolar ridge atrophy has various disadvantages, including a limited availability of sufficiently sized and shaped grafts, donor site morbidity and resorption of the grafted bone. As a result, interconnected porous hydroxyapatite ceramic (IP-CHA) materials with high porosity have been developed and used successfully in orthopedic cases. To the best of the author's knowledge, this is the first report of clinical application of an IP-CHA block for onlay grafting for implant treatment in a patient with horizontal alveolar atrophy. The present study performed onlay block grafting using an IP-CHA block to restore bone volume for implant placement in the alveolar ridge area without collecting autogenous bone. Dental X-ray findings revealed that the border of the IP-CHA block became increasingly vague over the 3-year period, whereas CT scanning revealed that the gap between the block and bone had a smooth transition, indicating that IP-CHA improved the process of integration with host bone. In follow-up examinations over a period of 5 years, the implants and superstructures had no problems. An IP-CHA block may be useful as a substitute for onlay block bone grafting in implant treatment.

Preparation of bioactive porous HA/PCL composite scaffolds

Energy Technology Data Exchange (ETDEWEB)

Zhao, J.; Guo, L.Y.; Yang, X.B. [Key Laboratory of Advanced Technologies of Materials (Ministry of Education), School of Materials Science and Engineering, Southwest Jiaotong University, Chengdu 610031 (China); Weng, J. [Key Laboratory of Advanced Technologies of Materials (Ministry of Education), School of Materials Science and Engineering, Southwest Jiaotong University, Chengdu 610031 (China)], E-mail: jweng@swjtu.cn

2008-12-30

Porous hydroxyapatite (HA) bioceramic scaffold has been widely attracted the attention to act as a three-dimensional (3D) template for cell adhesion, proliferation, differentiation and thus promoting bone and cartilage regeneration because of its osteoinduction. However, the porous bioceramic scaffold is fragile so that it is not suitable to be applied in clinic for bone repair or replacement. Therefore, it is significant to improve the mechanical property of porous HA bioceramics while the interconnected structure is maintained for tissue ingrowth in vivo. In the present research, a porous composite scaffold composed of HA scaffold and polycaprolactone (PCL) lining was fabricated by the method of polymer impregnating to produce HA scaffold coated with PCL lining. Subsequently, the composite scaffolds were deposited with biomimetic coating for improving the bioactivity. The HA/PCL composite scaffolds with improved mechanical property and bioactivity is expected to be a promising bone substitute in tissue engineering applications.

Preparation of bioactive porous HA/PCL composite scaffolds

International Nuclear Information System (INIS)

Zhao, J.; Guo, L.Y.; Yang, X.B.; Weng, J.

2008-01-01

Porous hydroxyapatite (HA) bioceramic scaffold has been widely attracted the attention to act as a three-dimensional (3D) template for cell adhesion, proliferation, differentiation and thus promoting bone and cartilage regeneration because of its osteoinduction. However, the porous bioceramic scaffold is fragile so that it is not suitable to be applied in clinic for bone repair or replacement. Therefore, it is significant to improve the mechanical property of porous HA bioceramics while the interconnected structure is maintained for tissue ingrowth in vivo. In the present research, a porous composite scaffold composed of HA scaffold and polycaprolactone (PCL) lining was fabricated by the method of polymer impregnating to produce HA scaffold coated with PCL lining. Subsequently, the composite scaffolds were deposited with biomimetic coating for improving the bioactivity. The HA/PCL composite scaffolds with improved mechanical property and bioactivity is expected to be a promising bone substitute in tissue engineering applications

Frittage micro-ondes en cavité monomode de biocéramiques Microwaves sintering of bioceramics in a single mode cavity

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Savary Etienne

2013-11-01

Full Text Available Le but premier de cette étude est de montrer la faisabilité du frittage direct en cavité micro-ondes monomode de deux biomatériaux céramiques : l'hydroxyapatite et le phosphate tri-calcique. Ainsi, cette étude montre que ce procédé a permis d'obtenir, en des temps très courts, inférieurs à 20 minutes, des échantillons denses présentant des microstructures fines. Les caractérisations mécaniques sur les échantillons frittés par micro-ondes ont révélé des valeurs de module d'élasticité et de dureté supérieures à celles généralement obtenues sur des échantillons frittés de manière conventionnelle. Ces résultats sont discutés en fonction de la microstructure obtenue et des différents paramètres expérimentaux : granulométrie des poudres, température de frittage, temps d'irradiation micro-ondes. The main purpose of this study consists in investigating the direct microwaves sintering in a single mode cavity of two bioceramics: hydroxyapatite and tri-calcium phosphate. Thus, dense samples presenting fine microstructures are successfully obtained in less than 20 minutes of irradiation. The resulting mechanical characterizations on microwaves sintered samples evidence higher Young's modulus and hardness values than those usually reported on conventionally sintered samples. Those results are discussed according to the microstructures observed and the experimental parameters such as powders granulometries, sintering temperatures, microwaves irradiation times.

Formation of hydroxyapatite on Ti-coated Ti-Zr-Cu-Pd bulk metallic glass

International Nuclear Information System (INIS)

Qin, F.X.; Wang, X.M.; Wada, T.; Xie, G.Q.; Asami, K.; Inoue, A.

2009-01-01

In this research, Ti coating was conducted on Ti 40 Zr 10 Cu 36 Pd 14 bulk metallic glass (BMG) in order to increase the formation rate of hydroxyapatite layer. The formation behavior of bone-like hydroxyapatite on Ti-coated and uncoated Ti 40 Zr 10 Cu 36 Pd 14 bulk metallic glasses (BMGs) was studied. The surface morphology of Ti-coated and uncoated Ti 40 Zr 10 Cu 36 Pd 14 BMG was investigated by scanning electron microscopy and energy dispersive X-ray spectroscopy. The results revealed that the alkali pretreatment in 5 M NaOH solution at 60degC for 24 h had a beneficial effect on the formation of porous sodium titanate on Ti-coated Ti 40 Zr 10 Cu 36 Pd 14 BMG. A bone-like hydroxyapatite layer was able to form on the alkali-treated Ti-coated Ti 40 Zr 10 Cu 36 Pd 14 BMG after a short-time immersion in simulated body fluid (SBF). On the contrary, hydroxyapatite formation was not observed on the uncoated Ti 40 Zr 10 Cu 36 Pd 14 BMG after the same chemical treatments. (author)

Investigation of porosity and fractal properties of the sintered metal and semiconductor layers in the MDS capacitor structure

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Skatkov Leonid

2012-01-01

Full Text Available MDS capacitor (metal - dielectric - semiconductor is a structure in which metal plate is represented by compact bulk-porous pellets of niobium sintered powder, and semiconductor plate - by pyrolytic layer of MnO2. In the present paper we report the results of investigation of microporosity of sintered Nb and pyrolytic MnO2 and also the fractal properties of semiconductor layer.

Effects of talc and clay addition on pressureless sintering of porous ...

Indian Academy of Sciences (India)

Administrator

costs as well as decreasing the sintering temperature are required ... In the glass ceramics, the talc and clay was widely used as a flux to decrease ... nitrogen–gas pressure of 0⋅3 MPa. .... rate-controlling for high diffusion velocity and diffusion.

An Investigation of Sintering Parameters on Titanium Powder for Electron Beam Melting Processing Optimization

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Philipp Drescher

2016-12-01

Full Text Available Selective electron beam melting (SEBM is a relatively new additive manufacturing technology for metallic materials. Specific to this technology is the sintering of the metal powder prior to the melting process. The sintering process has disadvantages for post-processing. The post-processing of parts produced by SEBM typically involves the removal of semi-sintered powder through the use of a powder blasting system. Furthermore, the sintering of large areas before melting decreases productivity. Current investigations are aimed at improving the sintering process in order to achieve better productivity, geometric accuracy, and resolution. In this study, the focus lies on the modification of the sintering process. In order to investigate and improve the sintering process, highly porous titanium test specimens with various scan speeds were built. The aim of this study was to decrease build time with comparable mechanical properties of the components and to remove the residual powder more easily after a build. By only sintering the area in which the melt pool for the components is created, an average productivity improvement of approx. 20% was achieved. Tensile tests were carried out, and the measured mechanical properties show comparatively or slightly improved values compared with the reference.

Experimental studies on a new highly porous hydroxyapatite matrix for obliterating open mastoid cavities.

Science.gov (United States)

Punke, Christoph; Zehlicke, Thorsten; Boltze, Carsten; Pau, Hans Wilhelm

2008-09-01

In an initial preliminary study, the applicability of a new high-porosity hydroxyapatite (HA) ceramic for obliterating large open mastoid cavities was proven and tested in an animal model (bulla of guinea pig). Experimental study. NanoBone, a highly porous matrix consisting of 76% hydroxyl apatite and 24% silicone dioxide fabricated in a sol-gel technique, was administered unilaterally into the opened bullae of 30 guinea pigs. In each animal, the opposite bulla was filled with Bio-Oss, a bone substitute consisting of a portion of mineral bovine bone. Histologic evaluations were performed 1, 2, 3, 4, 5, and 12 weeks after the implantation. After an initial phase in which the ceramic granules were surrounded by inflammatory cells (1-2 wk), there were increasing signs of vascularization. Osteoneogenesis and-at the same time-resorption of the HA ceramic were observed after the third week. No major difference in comparison to the bovine bone material could be found. Our results confirm the favorable qualities of the new ceramic reported in association with current maxillofacial literature. Conventional HA granules used for mastoid obliteration to date often showed problems with prolonged inflammatory reactions and, finally, extrusions. In contrast to those ceramics, the new material seems to induce more osteoneogenesis and undergoes early resorption probably due to its high porosity. Overall, it is similar to the bovine bone substance tested on the opposite ear in each animal. Further clinical studies may reveal whether NanoBone can be an adequate material for obliterating open mastoid cavities in patients.

Microwave sintering of cordierite ceramic precursors obtained by starch direct consolidation

International Nuclear Information System (INIS)

Sandoval, M.L.; Talou, M.H.; Camerucci, M.A.; Universidad Nacional de Mar Del Plata; Souto, P.M. de; Kiminami, R.H.G.A.

2009-01-01

Microwave sintering of cordierite disk precursors (mixture of kaolin, talc and alumina) with potato starch was studied. Green disks were obtained by thermal consolidation of stable aqueous suspensions of the ceramic powders (29.6 % vol.) with potato starch (11.5 % vol.) at 75 and 85 deg C, 4h; drying (50 deg C,12h) and calcination (650 deg C, 2h). The reaction-sintering by microwave heating (power: 2.45 GHz; heating rate: 50 deg C/min) at different temperatures (1250-1330 deg C) and dwell times (10-20 min) was carried out. For comparative purposes, the reaction-sintering by conventional heating was analyzed (1330 deg C, 4h a 3 deg C/min). The evolution of the phases as a function of temperature and time was studied by XRD analysis. The developed microstructures (dense or porous) were characterized by density and porosity measurements, and SEM. The obtained results were analyzed in relation to the characteristics of starch behavior in aqueous suspension at temperature and the employed consolidation and sintering conditions. (author)

Effect of polymer and additive on the structure and property of porous stainless steel hollow fiber

Energy Technology Data Exchange (ETDEWEB)

Ma, Xiao-Hua; Bai, Yu; Cao, Yue; Xu, Zhen-Liang [East China University of Science and Technology, Shanghai (China)

2014-08-15

Porous stainless steel hollow fiber has been widely used due to its high mechanical strength, excellent thermal conductivity and good sealing properties compared with other porous supports. We successfully prepared porous stainless steel hollow fibers using polyacrylonitrile (PAN) as polymer via dry-wet spinning followed by sintering through temperature programming method. The PAN concentration had an obvious impact on the structure and property of porous stainless steel hollow fiber even if it would be burned off during sintering. The results showed that the morphology could be tuned by adjusting the concentration of PAN. With increasing PAN concentration in casting solution for spinning, the viscosity was increased dramatically, resulting in much compact structures with high pure water flux (higher than 3x10{sup 5} L·m{sup -2}·h{sup -1}·Pa{sup -1}). A more dense structure could be obtained by adding additive polyvinylpyrrolidone (PVP) as viscosity enhancer.

Preparation of porous ceramics from nanocrystalline zirconia and its microstructure

International Nuclear Information System (INIS)

Nikitin, D.S.; Zhukov, V.A.; Kul'kov, S.N.; Perkov, V.V.; Buyakova, S.P.

2004-01-01

The behaviour of ZrO 2 (Y) nanocrystalline powder under pressing, the effect of forming pressure, the temperature and the time of sintering on the structure of the sintered porous ceramics are under study. It is shown that on pressing the fracturing of powder particles and their agglomerates takes place even at low pressures (≅50 MPa). The change of densification mechanisms is revealed - from quasi-liquid displacement of powder particles at the beginning of mechanical action to fracture of coarse structural elements. It is established that a strong skeleton responsible for needed porosity is formed even at the initial stage of sintering [ru

Synthesis, bioactivity and zeta potential investigations of chlorine and fluorine substituted hydroxyapatite.

Science.gov (United States)

Fahami, Abbas; Beall, Gary W; Betancourt, Tania

2016-02-01

Chlorine and fluorine substituted hydroxyapatites (HA-Cl-F) with different degrees of ion replacement were successfully prepared by the one step mechanochemical activation method. X-ray diffraction (XRD) and FT-IR spectra indicated that substitution of these anions in milled powders resulted in the formation of pure hydroxyapatite phase except for the small observed change in the lattice parameters and unit cell volumes of the resultant hydroxyapatite. Microscopic observations showed that the milled product had a cluster-like structure made up of polygonal and spherical particles with an average particle size of approximately ranged from 20±5 to 70±5nm. The zeta potential of milled samples was performed at three different pH (5, 7.4, and 9). The obtained zeta potential values were negative for all three pH values. Negative zeta potential was described to favor osseointegration, apatite nucleation, and bone regeneration. The bioactivity of samples was investigated on sintered pellets soaked in simulated body fluid (SBF) solution and apatite crystals formed on the surface of the pellets after being incubated for 14days. Zeta potential analysis and bioactivity experiment suggested that HA-Cl-F will lead to the formation of new apatite particles and therefore be a potential implant material. Copyright © 2015 Elsevier B.V. All rights reserved.

Mag-seeding of rat bone marrow stromal cells into porous hydroxyapatite scaffolds for bone tissue engineering.

Science.gov (United States)

Shimizu, Kazunori; Ito, Akira; Honda, Hiroyuki

2007-09-01

Bone tissue engineering has been investigated as an alternative strategy for autograft transplantation. In the process of tissue engineering, cell seeding into three-dimensional (3-D) scaffolds is the first step for constructing 3-D tissues. We have proposed a methodology of cell seeding into 3-D porous scaffolds using magnetic force and magnetite nanoparticles, which we term Mag-seeding. In this study, we applied this Mag-seeding technique to bone tissue engineering using bone marrow stromal cells (BMSCs) and 3-D hydroxyapatite (HA) scaffolds. BMSCs were magnetically labeled with our original magnetite cationic liposomes (MCLs) having a positive surface charge to improve adsorption to cell surface. Magnetically labeled BMSCs were seeded onto a scaffold, and a 1-T magnet was placed under the scaffold. By using Mag-seeding, the cells were successfully seeded into the internal space of scaffolds with a high cell density. The cell seeding efficiency into HA scaffolds by Mag-seeding was approximately threefold larger than that by static-seeding (conventional method, without a magnet). After a 14-d cultivation period using the osteogenic induction medium by Mag-seeding, the level of two representative osteogenic markers (alkaline phosphatase and osteocalcin) were significantly higher than those by static-seeding. These results indicated that Mag-seeding of BMSCs into HA scaffolds is an effective approach to bone tissue engineering.

Hexagonal OsB{sub 2}: Sintering, microstructure and mechanical properties

Energy Technology Data Exchange (ETDEWEB)

Xie, Zhilin [Department of Mechanical and Aerospace Engineering, University of Central Florida, Orlando, FL 32816 (United States); Lugovy, Mykola [Department of Mechanical and Aerospace Engineering, University of Central Florida, Orlando, FL 32816 (United States); Institute for Problems of Materials Science, 3 Krzhizhanivskii Str., Kyiv 03142 (Ukraine); Orlovskaya, Nina, E-mail: Nina.Orlovskaya@ucf.edu [Department of Mechanical and Aerospace Engineering, University of Central Florida, Orlando, FL 32816 (United States); Graule, Thomas; Kuebler, Jakob [Empa, Swiss Federal Laboratories for Materials Science and Technology, Laboratory for High Performance Ceramics, CH-8600 Dubendorf (Switzerland); Mueller, Martin [Laboratory of Mechanical Metallurgy, EPFL, CH-1015 Lausanne (Switzerland); Gao, Huili [Department of Mechanical Engineering, Texas A& M University, College Station, TX 77843 (United States); Radovic, Miladin [Department of Materials Science and Engineering, Texas A& M University, College Station, TX 77843 (United States); Cullen, David A. [Materials Science & Technology Division, Oak Ridge National Laboratory, Oak Ridge, TN 37831 (United States)

2015-06-15

Highlights: • ReB{sub 2}-type hexagonal OsB{sub 2} powder has been densified by spark plasma sintering. • The sintered OsB{sub 2} contains ∼80 wt.% hexagonal and ∼20 wt.% orthorhombic phases. • The average grain size of the sintered OsB{sub 2} sample was 0.56 ± 0.26 μm. • H = 31 ± 9 GPa and E = 574 ± 112 GPa measured by nanoindentation. - Abstract: The metastable high pressure ReB{sub 2}-type hexagonal OsB{sub 2} bulk ceramics was produced by spark plasma sintering. The phase composition, microstructure, and mechanical behavior of the sintered OsB{sub 2} were studied by X-ray diffraction, optical microscopy, TEM, SEM, EDS, and nanoindentation. The produced ceramics was rather porous and contained a mixture of hexagonal (∼80 wt.%) and orthorhombic (∼20 wt.%) phases as identified by X-ray diffraction and EBSD analysis. Two boron-rich phases, which do not contain Os, were also identified by TEM and SEM/EDS analysis. Nanoindentation measurements yielded a hardness of 31 ± 9 GPa and Young’s modulus of 574 ± 112 GPa, indicating that the material is rather hard and very stiff; however, it is very prone to crack formation and propagation, which is indicative of a very brittle nature of this material. Improvements in the sintering regime are required in order to produce dense, homogeneous and single phase hexagonal OsB{sub 2} bulk ceramics.

Antibacterial activity and biocompatibility of three-dimensional nanostructured porous granules of hydroxyapatite and zinc oxide nanoparticles—an in vitro and in vivo study

International Nuclear Information System (INIS)

Grenho, L; Salgado, C L; Monteiro, F J; Fernandes, M H; Ferraz, M P

2015-01-01

Ceramic scaffolds are widely studied in the bone tissue engineering field due to their potential in regenerative medicine. However, adhesion of microorganisms on biomaterials with subsequent formation of antibiotic-resistant biofilms is a critical factor in implant-related infections. Therefore, new strategies are needed to address this problem. In the present study, three-dimensional and interconnected porous granules of nanostructured hydroxyapatite (nanoHA) incorporated with different amounts of zinc oxide (ZnO) nanoparticles were produced using a simple polymer sponge replication method. As in vitro experiments, granules were exposed to Staphylococcus aureus and Staphylococcus epidermidis and, after 24 h, the planktonic and sessile populations were assessed. Cytocompatibility towards osteoblast-like cells (MG63 cell line) was also evaluated for a period of 1 and 3 days, through resazurin assay and imaging flow cytometry analysis. As in vivo experiments, nanoHA porous granules with and without ZnO nanoparticles were implanted into the subcutaneous tissue in rats and their inflammatory response after 3, 7 and 30 days was examined, as well as their antibacterial activity after 1 and 3 days of S. aureus inoculation. The developed composites proved to be especially effective at reducing bacterial activity in vitro and in vivo for a weight percentage of 2% ZnO, with a low cell growth inhibition in vitro and no differences in the connective tissue growth and inflammatory response in vivo. Altogether, these results suggest that nanoHA–ZnO porous granules have a great potential to be used in orthopaedic and dental applications as a template for bone regeneration and, simultaneously, to restrain biomaterial-associated infections. (paper)

Antibacterial activity and biocompatibility of three-dimensional nanostructured porous granules of hydroxyapatite and zinc oxide nanoparticles—an in vitro and in vivo study

Science.gov (United States)

Grenho, L.; Salgado, C. L.; Fernandes, M. H.; Monteiro, F. J.; Ferraz, M. P.

2015-08-01

Ceramic scaffolds are widely studied in the bone tissue engineering field due to their potential in regenerative medicine. However, adhesion of microorganisms on biomaterials with subsequent formation of antibiotic-resistant biofilms is a critical factor in implant-related infections. Therefore, new strategies are needed to address this problem. In the present study, three-dimensional and interconnected porous granules of nanostructured hydroxyapatite (nanoHA) incorporated with different amounts of zinc oxide (ZnO) nanoparticles were produced using a simple polymer sponge replication method. As in vitro experiments, granules were exposed to Staphylococcus aureus and Staphylococcus epidermidis and, after 24 h, the planktonic and sessile populations were assessed. Cytocompatibility towards osteoblast-like cells (MG63 cell line) was also evaluated for a period of 1 and 3 days, through resazurin assay and imaging flow cytometry analysis. As in vivo experiments, nanoHA porous granules with and without ZnO nanoparticles were implanted into the subcutaneous tissue in rats and their inflammatory response after 3, 7 and 30 days was examined, as well as their antibacterial activity after 1 and 3 days of S. aureus inoculation. The developed composites proved to be especially effective at reducing bacterial activity in vitro and in vivo for a weight percentage of 2% ZnO, with a low cell growth inhibition in vitro and no differences in the connective tissue growth and inflammatory response in vivo. Altogether, these results suggest that nanoHA-ZnO porous granules have a great potential to be used in orthopaedic and dental applications as a template for bone regeneration and, simultaneously, to restrain biomaterial-associated infections.

Densification, phase stability and in vitro biocompatibility property of hydroxyapatite-10 wt% silver composites.

Science.gov (United States)

Nath, Shekhar; Kalmodia, Sushma; Basu, Bikramjit

2010-04-01

In this paper, we demonstrate how a simple fabrication route, i.e., pressureless sintering of mechanically mixed powders can be employed to develop hydroxyapatite (HAp, Ca(10)(PO(4))(6)(OH)(2))-silver (Ag) bioceramic composites with superior combination of physical (hardness, toughness), non-cytotoxicity, cytocompatiblity and anti-microbial property. The densification results show that such composites can be sintered at 1200 degrees C for 2 h near to theoretical density (>98% rho(th).) An important observation is that the dissociation of HAp phase can be prevented during sintering up to 1300 degrees C for 2 h in HAp-10 wt% Ag composites. The stability of HAp in presence of silver is discussed in reference to the results obtained using XRD, FTIR and Raman spectroscopy. The hardness values of the composites are comparable (approximately 6.5 GPa) to that of pure HAp, despite of the presence of softer Ag particles. The sintered composites exhibit modest crack growth resistance property and their toughness varies in the range of 0.9-1.2 MPa m(0.5), depending on sintering temperature. For selected samples, the in vitro characterization was performed using mouse fibroblast (L929) and human osteosarcoma (MG63) cell lines. The combination of biochemical assays (MTT, ALP and osteocalcin) confirm that HAp-10 wt% Ag biocomposites have comparable or even better cellular viability, osteogenic differentiation and bone mineralization as well as osteoinduction property. Antibacterial experiments involving gram-negative bacteria, Escherichia coli confirm excellent bactericidal property of HAp-10 wt% Ag composites, sintered using mechanically mixed powders.

New method of synthesis and in vitro studies of a porous biomaterial

International Nuclear Information System (INIS)

Wers, E.; Lefeuvre, B.; Pellen-Mussi, P.; Novella, A.; Oudadesse, H.

2016-01-01

Biomaterials for bone reconstruction represent a widely studied area. In this paper, a new method of synthesis of a porous glass–ceramic obtained by thermal treatment is presented. The prepared biomaterial was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and induced couple plasma-optical emission spectroscopy (ICP-OES), mercury porosimetry and by the Archimedes method. In vitro evaluations in a simulated body fluid (SBF) and in contact with SaOS_2 human osteoblasts were also carried out. The porous glass–ceramic is composed of a total porous network of 60% suitable for body fluid and cell infiltration, with pore sizes varying from 60 nm to 143 μm. The presence of two crystalline phases decreases the kinetic of bioactivity compared to an amorphous biomaterial (bioactive glass). A hydroxyapatite layer appears from 15 days of immersion on the surface and inside the pores, showing a biodegradation and a bioactivity in four steps. Cytotoxicity assessments present an increase of the cellular viability after 72 h proving the non-cytotoxic effect of the glass–ceramic. Thus, the results of these different studies indicate that the porous biomaterial may have a potential application for the bone regeneration. This paper also presents the novelty of this method. It is a rapid synthesis which combines simplicity and low cost. This represents an advantage for an eventual industrialization. - Highlights: • The new method of synthesis of a porous glass–ceramic is reproducible. • The porous glass–ceramic possesses a total porosity of 60%. • The biomaterial shows a bioactivity in four steps with hydroxyapatite formation. • 82% of cellular viability is observed on the surface of the biomaterial.

New method of synthesis and in vitro studies of a porous biomaterial

Energy Technology Data Exchange (ETDEWEB)

Wers, E., E-mail: wers.eric@hotmail.com [Equipe Chimie du Solide et Matériaux, UMR CNRS 6226, Sciences Chimiques de Rennes, Université de Rennes 1, Université Européenne de Bretagne, 263 avenue du Général Leclerc, 35042 Rennes Cedex (France); Lefeuvre, B. [Equipe Chimie du Solide et Matériaux, UMR CNRS 6226, Sciences Chimiques de Rennes, Université de Rennes 1, Université Européenne de Bretagne, 263 avenue du Général Leclerc, 35042 Rennes Cedex (France); Pellen-Mussi, P.; Novella, A. [Equipe Chimie du Solide et Matériaux, UMR CNRS 6226, Sciences Chimiques de Rennes, Université de Rennes 1, Université Européenne de Bretagne, 2 avenue du Professeur Léon Bernard, 35042 Rennes Cedex (France); Oudadesse, H. [Equipe Chimie du Solide et Matériaux, UMR CNRS 6226, Sciences Chimiques de Rennes, Université de Rennes 1, Université Européenne de Bretagne, 263 avenue du Général Leclerc, 35042 Rennes Cedex (France)

2016-04-01

Biomaterials for bone reconstruction represent a widely studied area. In this paper, a new method of synthesis of a porous glass–ceramic obtained by thermal treatment is presented. The prepared biomaterial was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and induced couple plasma-optical emission spectroscopy (ICP-OES), mercury porosimetry and by the Archimedes method. In vitro evaluations in a simulated body fluid (SBF) and in contact with SaOS{sub 2} human osteoblasts were also carried out. The porous glass–ceramic is composed of a total porous network of 60% suitable for body fluid and cell infiltration, with pore sizes varying from 60 nm to 143 μm. The presence of two crystalline phases decreases the kinetic of bioactivity compared to an amorphous biomaterial (bioactive glass). A hydroxyapatite layer appears from 15 days of immersion on the surface and inside the pores, showing a biodegradation and a bioactivity in four steps. Cytotoxicity assessments present an increase of the cellular viability after 72 h proving the non-cytotoxic effect of the glass–ceramic. Thus, the results of these different studies indicate that the porous biomaterial may have a potential application for the bone regeneration. This paper also presents the novelty of this method. It is a rapid synthesis which combines simplicity and low cost. This represents an advantage for an eventual industrialization. - Highlights: • The new method of synthesis of a porous glass–ceramic is reproducible. • The porous glass–ceramic possesses a total porosity of 60%. • The biomaterial shows a bioactivity in four steps with hydroxyapatite formation. • 82% of cellular viability is observed on the surface of the biomaterial.

Microstructure and properties of gravity sintered 316l stainless steel powder with nickel boride addition

Directory of Open Access Journals (Sweden)

Božić Dušan

2016-01-01

Full Text Available The present work demonstrates a procedure for synthesis of stainless steel powder by gravity sintering method. As an additive to the basic powder, NiB powder was added in the amount of 0.2 - 1.0 wt.%. Gravity sintering was done in vacuum, at the temperatures of 1100°C-1250°C, in the course of 3 - 60 min, using ceramic mould. Structural characterization was conducted by XRD, and microstructural analysis by optical and scanning electron microscope (SEM. Mechanical properties were investigated by tensile tests with steel rings. Density and permeability were determined by standard techniques for porous samples. Gravity sintered stainless steel with NiB addition had more superior mechanical and physico-chemical properties compared to stainless steel obtained by standard powder metallurgy procedures - pressing and sintering. [Projekat Ministarstva nauke Republike Srbije, br. 172005

Designing porous metallic glass compact enclosed with surface iron oxides

Energy Technology Data Exchange (ETDEWEB)

Cho, Jae Young; Park, Hae Jin; Hong, Sung Hwan; Kim, Jeong Tae; Kim, Young Seok; Park, Jun-Young; Lee, Naesung [Hybrid Materials Center (HMC), Faculty of Nanotechnology and Advanced Materials Engineering, Sejong University, 209 Neungdong-ro, Gwangjin-gu, Seoul 143-747 (Korea, Republic of); Seo, Yongho [Graphene Research Institute (GRI) & HMC, Faculty of Nanotechnology and Advanced Materials Engineering, Sejong University, 209 Neungdong-ro, Gwangjin-gu, Seoul 143-747 (Korea, Republic of); Park, Jin Man, E-mail: jinman_park@hotmail.com [Global Technology Center, Samsung Electronics Co., Ltd, 129 Samsung-ro, Yeongtong-gu, Suwon-si, Gyeonggi-do 443-742 (Korea, Republic of); Kim, Ki Buem, E-mail: kbkim@sejong.ac.kr [Hybrid Materials Center (HMC), Faculty of Nanotechnology and Advanced Materials Engineering, Sejong University, 209 Neungdong-ro, Gwangjin-gu, Seoul 143-747 (Korea, Republic of)

2015-06-25

Highlights: • Porous metallic glass compact was developed using electro-discharge sintering process. • Uniform PMGC can only be achieved when low electrical input energy was applied. • Functional iron-oxides were formed on the surface of PMGCs by hydrothermal technique. - Abstract: Porous metallic glass compact (PMGC) using electro-discharge sintering (EDS) process of gas atomized Zr{sub 41.2}Ti{sub 13.8}Cu{sub 12.5}Ni{sub 10}Be{sub 22.5} metallic glass powder was developed. The formation of uniform PMGC can only be achieved when low electrical input energy was applied. Functional iron-oxides were formed on the surface of PMGCs by hydrothermal technique. This finding suggests that PMGC can be applied in the new area such as catalyst via hydrothermal technique and offer a promising guideline for using the metallic glasses as a potential functional application.

The effects of processing parameters on the properties of micro-scale porous surface for a micro-channel reactor

International Nuclear Information System (INIS)

Feng, Yanbing; Mei, Deqing; Qian, Miao; Yi, Zoudongyi; Chen, Zichen

2017-01-01

To improve the performance of hydrogen production via a microchannel reactor with a porous surface, the process of layered powder sintering and dissolution method is optimized, and the effects of processing parameters on the morphological and mechanical properties of the porous surface structure are studied. Based on the preliminary experiments, three key parameters in the process are the size of the NaCl particle, the compaction pressure, and the sintering temperature. Besides, the porous surface structures are evaluated by the specific surface area and compression strength to optimize the influencing variables. Results show that the specific surface area of porous surface structure is determined mainly by the size of NaCl particle, while the pressure and temperature have little influence unexpectedly within the range of experimental condition. With the increase of temperature and pressure, the compression strength will be enhanced, but the increase of the size of NaCl particles will cause the decrease of compression strength. The optimum compaction pressure, sintering temperature, and size of the NaCl particle are obtained respectively. Finally, the optimum parameters have been used to manufacture the micro-channel catalyst support with a porous surface, and its hydrogen production can be maximumly enhanced by 90% compared with the surface fabricated with NaCl particles of 125–150 µ m. (paper)

Scaffolds for bone regeneration made of hydroxyapatite microspheres in a collagen matrix

Energy Technology Data Exchange (ETDEWEB)

Cholas, Rahmatullah, E-mail: rahmat.cholas@gmail.com; Kunjalukkal Padmanabhan, Sanosh, E-mail: sanosh2001@gmail.com; Gervaso, Francesca; Udayan, Gayatri; Monaco, Graziana; Sannino, Alessandro; Licciulli, Antonio

2016-06-01

Biomimetic scaffolds with a structural and chemical composition similar to native bone tissue may be promising for bone tissue regeneration. In the present work hydroxyapatite mesoporous microspheres (mHA) were incorporated into collagen scaffolds containing an ordered interconnected macroporosity. The mHA were obtained by spray drying of a nano hydroxyapatite slurry prepared by the precipitation technique. X-ray diffraction (XRD) analysis revealed that the microspheres were composed only of hydroxyapatite (HA) phase, and energy-dispersive x-ray spectroscopy (EDS) analysis revealed the Ca/P ratio to be 1.69 which is near the value for pure HA. The obtained microspheres had an average diameter of 6 μm, a specific surface area of 40 m{sup 2}/g as measured by Brunauer-Emmett-Teller (BET) analysis, and Barrett-Joyner-Halenda (BJH) analysis showed a mesoporous structure with an average pore diameter of 16 nm. Collagen/HA-microsphere (Col/mHA) composite scaffolds were prepared by freeze-drying followed by dehydrothermal crosslinking. SEM observations of Col/mHA scaffolds revealed HA microspheres embedded within a porous collagen matrix with a pore size ranging from a few microns up to 200 μm, which was also confirmed by histological staining of sections of paraffin embedded scaffolds. The compressive modulus of the composite scaffold at low and high strain values was 1.7 and 2.8 times, respectively, that of pure collagen scaffolds. Cell proliferation measured by the MTT assay showed more than a 3-fold increase in cell number within the scaffolds after 15 days of culture for both pure collagen scaffolds and Col/mHA composite scaffolds. Attractive properties of this composite scaffold include the potential to load the microspheres for drug delivery and the controllability of the pore structure at various length scales. - Highlights: • Mesoporous hydroxyapatite microsphere(mHA) synthesized by spray drying method • Porous collagen/mHA composite scaffold made by freeze

Stationary and Dynamic Permeability and Coupling Coefficient Measurements in Sintered Glass Bead Systems

Science.gov (United States)

Gueven, I.; Steeb, H.; Luding, S.

2014-12-01

Electrokinetic waves describe the coupling between seismic and electromagnetic waves that exist in porous media. The coupling between them arise from an electrochemical boundary layer between grain and fluid interface of saturated porous media. Acoustical waves cause a disturbance of the electrical fluid charge within the double layer, which therefore creates an electric streaming current (seismoelectric effect). Inversely, electromagnetic waves can generate mechanical signals (electroseismic effect). Electrokinetic conversion potentially combines high seismic resolution with good electromagnetic hydrocarbon sensitivity. The (stationary and frequency-dependent) streaming potential coefficient is a key property, which gives rise to the coupling between electromagnetic and acoustical waves. It depends strongly on the fluid conductivity, porosity, tortuosity, permeability, pore throat and zeta potential of porous media. We examine experimentally both, the stationary and dynamic permeabilities and coupling coefficients of sintered glass bead systems. For this purpose a multi-purpose measuring cell was developed which allows us to carry out - besides common ultrasound experiments - also to perform stationary and frequency-dependent permeability and coupling coefficient measurements. For the experiments sintered mono- and slightly polydisperse glass bead samples with different glass bead diameters between 0.4 and 8mm and porosities ranging between 21 and 39% were used. The stationary and dynamic permeability and streaming potential measurements are supported by μCT scans which enable us a deeper insight into the porous medium. Based on the μCT scans of the produced sintered glass bead samples essential influence parameters, like tortuosity, porosity, effective particle diameters and pore throats in different regions of the entire scanned region have been analyzed in detail to understand the laboratory experiments, cf. Illustration 1. In addition lattice Boltzmann

A bioactive metallurgical grade porous silicon-polytetrafluoroethylene sheet for guided bone regeneration applications.

Science.gov (United States)

Chadwick, E G; Clarkin, O M; Raghavendra, R; Tanner, D A

2014-01-01

The properties of porous silicon make it a promising material for a host of applications including drug delivery, molecular and cell-based biosensing, and tissue engineering. Porous silicon has previously shown its potential for the controlled release of pharmacological agents and in assisting bone healing. Hydroxyapatite, the principle constituent of bone, allows osteointegration in vivo, due to its chemical and physical similarities to bone. Synthetic hydroxyapatite is currently applied as a surface coating to medical devices and prosthetics, encouraging bone in-growth at their surface and improving osseointegration. This paper examines the potential for the use of an economically produced porous silicon particulate-polytetrafluoroethylene sheet for use as a guided bone regeneration device in periodontal and orthopaedic applications. The particulate sheet is comprised of a series of microparticles in a polytetrafluoroethylene matrix and is shown to produce a stable hydroxyapatite on its surface under simulated physiological conditions. The microstructure of the material is examined both before and after simulated body fluid experiments for a period of 1, 7, 14 and 30 days using Scanning Electron Microscopy. The composition is examined using a combination of Energy Dispersive X-ray Spectroscopy, Thin film X-ray diffraction, Attenuated Total Reflectance-Fourier Transform Infrared Spectroscopy and the uptake/release of constituents at the fluid-solid interface is explored using Inductively Coupled Plasma-Optical Emission Spectroscopy. Microstructural and compositional analysis reveals progressive growth of crystalline, 'bone-like' apatite on the surface of the material, indicating the likelihood of close bony apposition in vivo.

Electrophoretic Deposition of Hydroxyapatite Film Containing Re-Doped MoS₂ Nanoparticles.

Science.gov (United States)

Shalom, Hila; Feldman, Yishay; Rosentsveig, Rita; Pinkas, Iddo; Kaplan-Ashiri, Ifat; Moshkovich, Alexey; Perfilyev, Vladislav; Rapoport, Lev; Tenne, Reshef

2018-02-26

Films combining hydroxyapatite (HA) with minute amounts (ca. 1 weight %) of (rhenium doped) fullerene-like MoS₂ (IF) nanoparticles were deposited onto porous titanium substrate through electrophoretic process (EPD). The films were analyzed by scanning electron microscopy (SEM), X-ray diffraction and Raman spectroscopy. The SEM analysis showed relatively uniform coatings of the HA + IF on the titanium substrate. Chemical composition analysis using energy dispersive X-ray spectroscopy (EDS) of the coatings revealed the presence of calcium phosphate minerals like hydroxyapatite, as a majority phase. Tribological tests were undertaken showing that the IF nanoparticles endow the HA film very low friction and wear characteristics. Such films could be of interest for various medical technologies. Means for improving the adhesion of the film to the underlying substrate and its fracture toughness, without compromising its biocompatibility are discussed at the end.

Solvent/Non-Solvent Sintering To Make Microsphere Scaffolds

Science.gov (United States)

Laurencin, Cato T.; Brown, Justin L.; Nair, Lakshmi

2011-01-01

A solvent/non-solvent sintering technique has been devised for joining polymeric microspheres to make porous matrices for use as drug-delivery devices or scaffolds that could be seeded with cells for growing tissues. Unlike traditional sintering at elevated temperature and pressure, this technique is practiced at room temperature and pressure and, therefore, does not cause thermal degradation of any drug, protein, or other biochemical with which the microspheres might be loaded to impart properties desired in a specific application. Also, properties of scaffolds made by this technique are more reproducible than are properties of comparable scaffolds made by traditional sintering. The technique involves the use of two miscible organic liquids: one that is and one that is not a solvent for the affected polymer. The polymeric microspheres are placed in a mold having the size and shape of the desired scaffold, then the solvent/non-solvent mixture is poured into the mold to fill the void volume between the microspheres, then the liquid mixture is allowed to evaporate. Some of the properties of the resulting scaffold can be tailored through choice of the proportions of the liquids and the diameter of the microspheres.

Synthesis, bioactivity and zeta potential investigations of chlorine and fluorine substituted hydroxyapatite

International Nuclear Information System (INIS)

Fahami, Abbas; Beall, Gary W.; Betancourt, Tania

2016-01-01

Chlorine and fluorine substituted hydroxyapatites (HA-Cl–F) with different degrees of ion replacement were successfully prepared by the one step mechanochemical activation method. X-ray diffraction (XRD) and FT-IR spectra indicated that substitution of these anions in milled powders resulted in the formation of pure hydroxyapatite phase except for the small observed change in the lattice parameters and unit cell volumes of the resultant hydroxyapatite. Microscopic observations showed that the milled product had a cluster-like structure made up of polygonal and spherical particles with an average particle size of approximately ranged from 20 ± 5 to 70 ± 5 nm. The zeta potential of milled samples was performed at three different pH (5, 7.4, and 9). The obtained zeta potential values were negative for all three pH values. Negative zeta potential was described to favor osseointegration, apatite nucleation, and bone regeneration. The bioactivity of samples was investigated on sintered pellets soaked in simulated body fluid (SBF) solution and apatite crystals formed on the surface of the pellets after being incubated for 14 days. Zeta potential analysis and bioactivity experiment suggested that HA-Cl–F will lead to the formation of new apatite particles and therefore be a potential implant material. - Highlights: • Cl"− and F"− substituted hydroxyapatite was synthesized by mechanochemical process. • Structural features were influenced strongly by incorporation of different ions. • Microscopic observations showed a mean particle size of around 20 ± 5 to 70 ± 5 nm. • The bioactivity properties indicated that apatite was successfully formed.

Synthesis, bioactivity and zeta potential investigations of chlorine and fluorine substituted hydroxyapatite

Energy Technology Data Exchange (ETDEWEB)

Fahami, Abbas, E-mail: fahami@txstate.edu [Materials Science, Engineering and Commercialization Program, Texas State University, San Marcos, TX 78666 (United States); Beall, Gary W. [Department of Chemistry and Biochemistry, Texas State University, 601 University Drive, San Marcos, TX 78666 (United States); Physics Department, Faculty of Science, King Abdulaziz University, Jeddah 21589 (Saudi Arabia); Betancourt, Tania [Materials Science, Engineering and Commercialization Program, Texas State University, San Marcos, TX 78666 (United States); Department of Chemistry and Biochemistry, Texas State University, 601 University Drive, San Marcos, TX 78666 (United States)

2016-02-01

Chlorine and fluorine substituted hydroxyapatites (HA-Cl–F) with different degrees of ion replacement were successfully prepared by the one step mechanochemical activation method. X-ray diffraction (XRD) and FT-IR spectra indicated that substitution of these anions in milled powders resulted in the formation of pure hydroxyapatite phase except for the small observed change in the lattice parameters and unit cell volumes of the resultant hydroxyapatite. Microscopic observations showed that the milled product had a cluster-like structure made up of polygonal and spherical particles with an average particle size of approximately ranged from 20 ± 5 to 70 ± 5 nm. The zeta potential of milled samples was performed at three different pH (5, 7.4, and 9). The obtained zeta potential values were negative for all three pH values. Negative zeta potential was described to favor osseointegration, apatite nucleation, and bone regeneration. The bioactivity of samples was investigated on sintered pellets soaked in simulated body fluid (SBF) solution and apatite crystals formed on the surface of the pellets after being incubated for 14 days. Zeta potential analysis and bioactivity experiment suggested that HA-Cl–F will lead to the formation of new apatite particles and therefore be a potential implant material. - Highlights: • Cl{sup −} and F{sup −} substituted hydroxyapatite was synthesized by mechanochemical process. • Structural features were influenced strongly by incorporation of different ions. • Microscopic observations showed a mean particle size of around 20 ± 5 to 70 ± 5 nm. • The bioactivity properties indicated that apatite was successfully formed.

Formation of a sodium bicarbonate cluster in the structure of sodium-substituted hydroxyapatite

Science.gov (United States)

Tkachenko, M. V.; Kamzin, A. S.

2015-02-01

Ceramic sodium-substituted carbonated hydroxyapatite has been synthesized using the method of the solid-phase reaction in the temperature range of 640-820°C in water vapor. It has been established that substitutions of Ca2+ ions in the cation and anion subsystems with Na+ ions and the PO{4/3-} and OH- groups with CO{3/2-} ions lead to a considerable acceleration of the shrinkage and synthesis of dense ceramics at substantially lower temperatures than in the case of unsubstituted hydroxyapatite. Sintering in water vapor leads to densification of carbonate groups in channel positions, which induces the appearance of orderings of A2 and B2 types (bands with wave numbers 867 and 865 cm-1 in IR spectra, respectively) as well as the protonation of carbonate groups both in A and B sites and the formation of sodium bicarbonate clusters (856 and 859 cm-1) in addition to carbonate ordering of A1 and B1 types (879 and 872 cm-1).

Improved mechanical properties of hydroxyapatite whisker-reinforced poly(L-lactic acid) scaffold by surface modification of hydroxyapatite.

Science.gov (United States)

Fang, Zhou; Feng, Qingling

2014-02-01

To improve the mechanical properties of porous hydroxyapatite/poly(L-lactic acid) (HA/PLLA) composites, HA whiskers with high crystallinity and high aspect ratio were synthesized. HA whiskers were modified with γ-aminopropyltriethoxysilane (APTES) to improve the interface between HA whiskers and PLLA. The composite scaffold consists of a porous PLLA matrix with HA whiskers distributed homogeneously. The morphology and the distributions of pore sizes of PLLA scaffold was not influenced by introducing HA whiskers, while the mechanical properties were improved. Both the compressive strength and compressive modulus were increased with the weight ratio of APTES-modified HA whiskers up to 30 wt.%, but only up to 15 wt.% for non-modified HA whiskers. With more than 15 wt.% HA whiskers, the mechanical properties of HA/PLLA scaffold were better improved with APTES-modified HA whiskers than non-modified. The HA whisker/PLLA scaffold with high porosity and improved mechanical properties is attractive in the application of tissue engineering. Copyright © 2013 Elsevier B.V. All rights reserved.

Manufacturing And High Temperature Oxidation Properties Of Electro-Sprayed Fe-24.5% Cr-5%Al Powder Porous Metal

Directory of Open Access Journals (Sweden)

Lee Kee-Ahn

2015-06-01

Full Text Available Fe-Cr-Al based Powder porous metals were manufactured using a new electro-spray process, and the microstructures and high-temperature oxidation properties were examined. The porous materials were obtained at different sintering temperatures (1350°C, 1400°C, 1450°C, and 1500°C and with different pore sizes (500 μm, 450 μm, and 200 μm. High-temperature oxidation experiments (TGA, Thermal Gravimetry Analysis were conducted for 24 hours at 1000°C in a 79% N2+ 21% O2, 100 mL/min. atmosphere. The Fe-Cr-Al powder porous metals manufactured through the electro-spray process showed more-excellent oxidation resistance as sintering temperature and pore size increased. In addition, the fact that the densities and surface areas of the abovementioned powder porous metals had the largest effects on the metal’s oxidation properties could be identified.

Ceramic modifications of porous titanium: effects on macrophage activation.

Science.gov (United States)

Scislowska-Czarnecka, A; Menaszek, E; Szaraniec, B; Kolaczkowska, E

2012-12-01

Porous titanium is one of the most widely used implant materials because of its mechanical properties, however, it is also characterised by low bioactivity. To improve the above parameter we prepared three modifications of the porous (30 wt%) titanium (Ti) surface by covering it with bioactive hydroxyapatite (HA), bioglass (BG) and calcium silicate (CS). Subsequently we tested the impact of the modifications on macrophages directing the inflammatory response that might compromise the implant bioactivity. In the study we investigated the in vitro effects of the materials on murine cell line RAW 264.7 macrophage adherence, morphology and activation (production/release of metalloproteinase MMP-9 and pro- and anti-inflammatory cytokines). CS Ti decreased the macrophage adherence and up-regulated the release of several pro-inflammatory mediators, including TNF-α, IL-6, IL-12. Also HA Ti reduced the cell adherence but other parameters were generally not increased, except of TNF-α. In contrast, BG Ti improved macrophage adherence and either decreased production of multiple mediators (MMP-9, TNF-α, IFN-γ, MCP-1) or did not change it in comparison to the porous titanium. We can conclude that analyzing the effects on the inflammatory response initiated by macrophages in vitro, calcium silicate did not improve the biological properties of the porous titanium. The improved bioactivity of titanium was, however, achieved by the application of the hydroxyapatite and bioglass layers. The present in vitro results suggest that these materials, HA Ti and especially BG Ti, may be suitable for in vivo application and thus justify their further investigation. Copyright © 2012 Elsevier Ltd. All rights reserved.

[Investigation of a new highly porous hydroxyapatite matrix for obliterating open mastoid cavities - application in guinea pigs bulla].

Science.gov (United States)

Punke, C; Zehlicke, T; Boltze, C; Pau, H W

2009-04-01

Many different techniques for obliterating open mastoid cavity have been described. The results after the application of alloplastic materials like Hydroxyapatite and Tricalciumphosphate were poor due to long-lasting resorption. Extrusion of those materials has been described. We investigated the applicability of a new high-porosity ceramic for obliterating large open mastoid cavities and tested it in an animal model (bulla of guinea pig). A highly porous matrix (NanoBone) bone-inductor fabricated in a sol-gel-technique was administered unilaterally into the opened bullae of 30 guinea pigs. In each animal the opposite bulla was filled with Bio-Oss, a bone substitute consisting of a portion of mineral bovine bone. Histological evaluations were performed 1, 2, 3, 4, 5 and 12 weeks after the implantation. After the initial phase with an inflammatory reaction creating a loose granulation tissue, we observed the formation of trabeculare bone within the fourth week in both groups. From the fifth week on we found osteoclasts on the surface of NanoBone and Bio-Oss with consecutive degradation of both materials. In our animal model study we found beneficial properties of the used bone-inductors NanoBone and Bio-Oss for obliterating open mastoid cavities.

Photoacoustic spectroscopy investigation of sintered zinc-tin-oxide ceramics

Directory of Open Access Journals (Sweden)

Ivetić Tamara B.

2007-01-01

Full Text Available In this paper the changes that occurred in differently activated ZnO-SnO2 and sintered samples were investigated using photoacoustic spectroscopy. ZnO and SnO2 powders, mixed in the molar ratio 2:1, were mechanically activated in a planetary ball mill for 10-160 min. The mixtures were pres­sed and isothermally sintered at 1300°C for two hours. X-ray diffraction analysis of the obtained sintered samples was performed in order to investigate changes of the phase composition and confirmed only the presence of a pure zinc stannate (Zn2SnO4 phase in all the sintered samples as a result of the solid state reaction and reaction sintering between the starting ZnO and SnO2 powders. The microstructure of the sintered sam­ples was examined by scanning electron microscopy and showed that mechanical activation leads to the formation of a structure with reduced particle size which accelerates spinel formation. Grain growth of the spinel phase slows down the densification process and together with the agglomerates formed during mechanical activation causes the appearance of a porous microstructure. The photoacoustic (PA phase and amplitude spectra of the sintered samples were recorded as a function of the chopped frequency of the laser beam used (red laser with a power of 25 mW, λ=632 nm in a thermal-transmission detection configuration. PA experimental data were analyzed using the Rosenzweig-Gersho thermal-piston model, which enabled determination of the thermal diffusivity, ZT (m2s-1, diffusion coefficient of the minority free carriers D (m2s-1 and the optical absorption coefficient (m-1. The detected differences of the measured thermal-electrical properties of the obtained Zn2SnO4 ceramics indicate changes in the material induced by the different preparation procedure of the starting powders before the sintering process.

Production of zirconia - hydroxyapatite (Z Ha) by using the co-precipitation method and studies of densification

International Nuclear Information System (INIS)

Silva, Viviane V.; Domingues, Rosana Z.

1997-01-01

Hydroxyapatite (Ha) is one of the materials most bio compatible with human bones and teeth, but its mechanical properties, especially toughness, are insufficient for hard tissue. Recent studies demonstrated that ceramics can be toughened by zirconium particles disperse in them, due to transformation, microcracking, and/or crack diffraction toughening mechanisms. The objective of this study is to characterize zirconia-toughened hydroxy apatite powders prepared by precipitation method by XRD, IR spectroscopy, TEM, TAG, DTA and BET analysis. The density of their ceramics was determined by mercury picnometry method. It was discussed the influence of addition of zirconium in different compositions and phases (Zr O 2 or Zr(OH) 4 ), compacting pressure and sintering temperature on zirconia - hydroxyapatite composites (ZHA). The results show that there is not any kind of reaction or chemical interaction between both phases of the composite materials. (author)

Introducing the fluorine doped natural hydroxyapatite-titania nanobiocomposite ceramic

Energy Technology Data Exchange (ETDEWEB)

Karamian, Ebrahim [Advanced Materials Research Center, Faculty of Materials Engineering, Najafabad Branch, Islamic Azad University, Najafabad (Iran, Islamic Republic of); Abdellahi, Majid, E-mail: M.Abdellahi@Pa.iut.ac.ir [Advanced Materials Research Center, Faculty of Materials Engineering, Najafabad Branch, Islamic Azad University, Najafabad (Iran, Islamic Republic of); Khandan, Amirsalar [Young Researchers and Elite Club, Khomeinishahr Branch, Islamic Azad University, Isfahan (Iran, Islamic Republic of); Abdellah, Sana [Advanced Materials Research Center, Faculty of Materials Engineering, Najafabad Branch, Islamic Azad University, Najafabad (Iran, Islamic Republic of)

2016-09-15

In the present research, natural hydroxyapatite (NHA) was synthesized from bovine bones and then fluorine was doped into the NHA matrix to produce fluorine doped NHA (FNHA; natural fluor-hydroxyapatite) in optimum conditions. At the end an FNHA-TiO{sub 2} nanobiocomposite ceramic with excellent biocompatibility and good chemical stability was synthesized through a mechanochemical route and a subsequent two step sintering (TSS) process. Thermal gravimetric analysis (TGA), Differential scanning calorimetry (DSC), X-ray fluorescence (XRF), X-ray diffraction (XRD), scanning electron microscopy (SEM), inductive coupled plasma (ICP), and energy-dispersive X-ray spectroscopy (EDX) were used as the means for gathering and analysis of the results. According to the obtained results, TiO{sub 2} can prevent early decomposition of FNHA by the formation of the CaTiO{sub 3} phases and hence strengthen the interactions between the apatite particles which results in the increase of the mechanical properties. Besides, TiO{sub 2} provides more Si−OH nucleation sites for the formation of the apatite layers and hence more bioactivity. - Highlights: • This work begins with preparing natural hydroxyapatite from bovine bones via a simple method. • With increasing the TiO{sub 2} content reinforced in FNHA matrix, the compaction increases. • TiO{sub 2} can prevent early decomposition of FNHA by the formation of CaTiO{sub 3} phase. • TiO{sub 2} can strengthen the interactions between the apatite particles and increase of compaction. • With increasing TiO{sub 2} content, the Si−OH nucleation sites increases lead to more bioactivity.

Sintering and densification; new techniques: sinter forging

International Nuclear Information System (INIS)

Winnubst, A.J.A.

1998-01-01

In this chapter pressure assisted sintering methods will be described. Attention will mainly be paid to sinter forging as a die-wall free uniaxial pressure sintering technique, where large creep strains are possible. Sinter forging is an effective tool to reduce sintering temperature and time and to obtain a nearly theoretically dense ceramic. In this way grain size in tetragonal zirconia ceramics can be reduced down to 100 nm. Another important phenomenon is the reduction of the number density and size of cracks and flaws resulting in higher strength and improved reliability, which is of utmost importance for engineering ceramics. The creep deformation during sinter forging causes a rearrangement of the grains resulting in a reduction of interatomic spaces between grains, while grain boundary (glassy) phases can be removed. The toughness and in some cases the wear resistance is enhanced after sinter forging as a result of the grain-boundary-morphology improvement. (orig.)

Influence of Porous Spherical-Shaped Hydroxyapatite on Mechanical Strength and Bioactive Function of Conventional Glass Ionomer Cement

Directory of Open Access Journals (Sweden)

Szu-Yu Chiu

2017-01-01

Full Text Available Glass-ionomer-cement (GIC is helpful in Minimal Intervention Dentistry because it releases fluoride ions and is highly biocompatible. The aim of this study is to investigate the mechanisms by which hydroxyapatite (HAp improves the mechanical strength and bioactive functioning of GIC when these materials are combined to make apatite ionomer cement (AIC. A conventional GIC powder was mixed with porous, spherical-HAp particles (HApS, crystalline HAp (HAp200 or one of two types of cellulose. The micro-compressive strengths of the additive particles were measured, and various specimens were evaluated with regard to their compressive strengths (CS, fluoride release concentrations (fluoride electrode and multi-element release concentrations. The AIC was found to release higher concentrations of fluoride (1.2 times and strontium ions (1.5 times compared to the control GIC. It was detected the more release of calcium originated from HApS than HAp200 in AIC. The CS of the AIC incorporating an optimum level of HAp was also significantly higher than that of the GIC. These results suggest that adding HAp can increase the release concentration of ions required for remineralization while maintaining the CS of the GIC. This effect does not result from a physical phenomenon, but rather from chemical reactions between the HAp and polyacrylic acid of GIC.

Synthesis and antibacterial evaluation of calcinated Ag-doped nano-hydroxyapatite with dispersibility.

Science.gov (United States)

Furuzono, Tsutomu; Motaharul, Mazumder; Kogai, Yasumichi; Azuma, Yoshinao; Sawa, Yoshiki

2015-05-01

Dispersible hydroxyapatite (HAp) nanoparticles are very useful for applying a monolayer to implantable medical devices using the nano-coating technique. To improve tolerance to infection on implanted medical devices, silver-doped HAp (Ag-HAp) nanoparticles with dispersiblity and crystallinity were synthesized, avoiding calcination-induced sintering, and evaluated for antibacterial activity. The Ca10-xAgx(PO4)6(OH)2 with x = 0 and 0.2 were prepared by wet chemical processing at 100°C. Before calcination at 700°C for 2 h, two kinds of anti-sintering agents, namely a Ca(NO3)2 (Ca salt) and a polyacrylic acid/Ca salt mixture (PAA-Ca), were used. Escherichia coli was used to evaluate the antibacterial activity of the nanopowder. When PAA-Ca was used as an anti-sintering agent in calcination to prepare the dispersible nanoparticles, strong metallic Ag peaks were observed at 38.1° and 44.3° (2θ) in the X-ray diffraction (XRD) profile. However, the Ag peak was barely observed when Ca salt was used alone as the anti-sintering agent. Thus, using Ca salt alone was more effective for preparation of dispersible Ag-HAp than PAA-Ca. The particle average size of Ag-HAp with 0.5 mol% of Ag content was found to be 325 ± 70 nm when the formation of large particleaggregations was prevented, as determined by dynamic light scattering instrument. The antibacterial activity of the Ag-HAp nanoparticles possessing 0.5 mol% against E. coli was greater than 90.0%. Dispersible and crystalline nano Ag-HAp can be obtained by using Ca salt alone as an anti-sintering agent. The nanoparticles showed antibacterial activity.

Influencing Factors for the Microstructure and Mechanical Properties of Micro Porous Titanium Manufactured by Metal Injection Molding

Directory of Open Access Journals (Sweden)

Zhen Lu

2016-04-01

Full Text Available Porous titanium is a new structural and functional material. It is widely used in many fields since it integrates the properties of biomaterials with those of metallic foam. A new technology that combines both the preparation and forming of porous materials has been proposed in this paper. Moreover, a new solder was developed that could be employed in the joining of porous materials. Influencing factors for microstructure and mechanical properties of the parent material and joint interface are identified. Metal injection molding (MIM technology was used for fabricating porous materials. The feedstock for injection molding of porous titanium powders was prepared from titanium powders and a polymer-based binder system. In addition, the proportion of powder loading and binders was optimized. Through MIM technology, a porous titanium filter cartridge was prepared. For the purpose of investigating the thermal debinding technology of the filter cartridge, effects of the sintering temperature on the porosity, morphology of micropores and mechanical properties were analyzed. It could be found that when the sintering temperature increased, the relative density, bending and compression strength of the components also increased. Moreover, the porosity reached 32.28% when the sintering temperature was 1000 °C. The microstructure morphology indicated that micropores connected with each other. Meanwhile, the strength of the components was relatively high, i.e., the bending and compression strength was 65 and 60 MPa, respectively. By investigating the joining technology of porous filter cartridges, the ideal components of the solder and pressure were determined. Further research revealed that the micropore structure of the joint interface is the same as that of the parent material, and that the bending strength of the joint interface is 40 MPa.

Characterization and formation of hydroxyapatite on Ti6Al4V coated by plasma electrolytic oxidation

International Nuclear Information System (INIS)

Durdu, Salih; Deniz, Ömer Faruk; Kutbay, Işıl; Usta, Metin

2013-01-01

Highlights: ► Ti6Al4V alloys were coated by PEO in calcium acetate and β-calcium glycerophosphate. ► Hydroxyapatite and calcium apatite based phases were directly formed on Ti6Al4V. ► Hydroxyapatite coatings were characterized systematically for different times. ► After 5 min, hydroxyapatite and calcium based phases begin to form on the coating. ► HAp on the coating is amorphous due to the rapid solidification during PEO. - Abstract: In this study, Ti6Al4V alloy was coated in the solution consisting of calcium acetate (CA) and β-calcium glycerophosphate (β-Ca-GP) by plasma electrolytic oxidation (PEO) to produce hydroxyapatite and calcium apatite-based composite used as of bioactive and biocompatible materials in biomedical applications. The phase structures, surface morphologies, functional groups of molecules, chemical compositions of the surfaces and the binding energies of atoms in the coating were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR) and X-ray photoelectron spectroscopy (XPS), respectively. Anatase, rutile, calcium oxide, titanium phosphide, whitlockite, tri-calcium phosphate (TCP), perovskite calcium titanate and hydroxyapatite phases on the coating were detected by XRD analysis. The surface of coatings produced by PEO method has a porous structure. The amount of amorphous hydroxyapatite is the highest value for the coating produced at 5 min in XPS and ATR-FTIR results, whereas the amount of crystalline hydroxyapatite has the highest value for coating produced at 120 min in XRD results.

Environment-oriented low-cost porous mullite ceramic membrane supports fabricated from coal gangue and bauxite

Energy Technology Data Exchange (ETDEWEB)

Lü, Qikai [Institute of Urban Environment, Chinese Academy of Sciences, Xiamen (China); Ningbo Urban Environment Observation and Research Station-NUEORS, Chinese Academy of Sciences, Ningbo (China); School of Chemistry and Chemical Engineering, South China University of Technology, Guangzhou (China); Dong, Xinfa [School of Chemistry and Chemical Engineering, South China University of Technology, Guangzhou (China); Zhu, Zhiwen [Institute of Urban Environment, Chinese Academy of Sciences, Xiamen (China); Ningbo Urban Environment Observation and Research Station-NUEORS, Chinese Academy of Sciences, Ningbo (China); Dong, Yingchao, E-mail: ycdong@iue.ac.cn [Institute of Urban Environment, Chinese Academy of Sciences, Xiamen (China); Ningbo Urban Environment Observation and Research Station-NUEORS, Chinese Academy of Sciences, Ningbo (China)

2014-05-01

Highlights: • Coal gangue was recycled to fabricate low-cost porous mullite membrane supports. • A unique volume-expansion occurred due to a mullitization-crystal-growth process. • A porous structure consists of glassy particles and embedded mullite crystals. - Abstract: Porous mullite ceramic supports for filtration membrane were successfully fabricated via recycling of coal gangue and bauxite at sintering temperatures from 1100 to 1500 °C with corn starch as pore-forming agent. The dynamic sintering behaviors, phase evolution, shrinkage, porosity and pore size, gas permeation flux, microstructure and mechanical property were systematically studied. A unique volume-expansion stage was observed at increased temperatures from 1276 to 1481 °C caused by a mullitization-crystal-growth process. During this stage, open porosity increases and pore size distributions broaden, which result in a maximum of nitrogen gas flux at 1400 °C. The X-ray diffraction results reveal that secondary mullitization took place from 1100 °C and the major phase is mullite with a content of ∼84.7 wt.% at 1400 °C. SEM images show that the as-fabricated mullite supports have a porous microstructure composed of sintered glassy particles embedded with inter-locked mullite crystals, which grew gradually with increasing temperature from rod-like into blocky-like morphologies. To obtain mullite membrane supports with sufficient porosity and acceptable mechanical strength, the relationship between porosity and mechanical strength was investigated, which was fitted using a parabolic equation.

Production and analysis of hydroxyapatite from Australian corals via hydrothermal process

International Nuclear Information System (INIS)

Hu, J.; Russell, J.; Ben-Nissan, B.

1999-01-01

Since the 1970s it is well known that if a biocompatible ceramic prosthesis with appropriate interconnected pores is used, growth of hard and soft tissue into the surface pores will be observed. A very strong attachment and hence the resultant mechanical and chemical bond to the existing surrounding tissue will be produced. Current artificial eyes although widely used encounter various problems due to the their motility and fail to deliver natural movement. They also cause sagging of the lids due to unsupported weight of the prosthesis. It is expected that application of a porous bioceramic such as the hydroxyapatite can generate good bonding to the tissue and hence a life-like eye movement. Hydroxyapatite (HAp) and related calcium phosphates have been studied for many years as implant materials, due to their similarity with the mineral phase of bone. From the point of view of biocompatibility, HAp seems to be the most suitable ceramic material for tissue replacement implants. Hydroxyapatite ceramics do not exhibit any cytoxic effects. It shows excellent biocompatibility with hard and soft tissues. Moreover, HAp can directly bond to the bone. Various preparation methods for HAp including the hydrothermal method have been used. The hydrothermal method was first used for hydroxyapatite formation directly from corals in 1974 by Roy and Linnehan. Complete replacement of aragonite by phosphatic material was achieved under 270degC and 103MPa using the hydrothermal process. This process has the disadvantage that the hydrothermal treatment must be carried out at a relatively high temperature under very high pressure. In 1996, HAp derived from Indian coral using hydrothermal process was developed by Sivakumar et al. However, the resultant material was in the form of a powder. Australia has rich variety of corals. Their application for implants have been studied very little. In this study, Australian corals selected were used for hydroxyapatite conversion. A new hydrothermal

Alumina-zirconium ceramics synthesis by selective laser sintering/melting

International Nuclear Information System (INIS)

Shishkovsky, I.; Yadroitsev, I.; Bertrand, Ph.; Smurov, I.

2007-01-01

In the present paper, porous refractory ceramics synthesized by selective laser sintering/melting from a mixture of zirconium dioxide, aluminum and/or alumina powders are subjected to optical metallography and X-ray analysis to study their microstructure and phase composition depending on the laser processing parameters. It is shown that high-speed laser sintering in air yields ceramics with dense structure and a uniform distribution of the stabilizing phases. The obtained ceramic-matrix composites may be used as thermal and electrical insulators and wear resistant coating in solid oxide fuel cells, crucibles, heating elements, medical tools. The possibility to reinforce refractory ceramics by laser synthesis is shown on the example of tetragonal dioxide of zirconium with hardened micro-inclusion of Al 2 O 3 . By applying finely dispersed Y 2 O 3 powder inclusions, the type of the ceramic structure is significantly changed

Thermal and structural characterization of synthetic and natural nanocrystalline hydroxyapatite.

Science.gov (United States)

Sofronia, Ancuta M; Baies, Radu; Anghel, Elena M; Marinescu, Cornelia A; Tanasescu, Speranta

2014-10-01

The aim of this work was to study the thermal stability on heating and to obtain the processing parameters of synthetic and bone-derived hydroxyapatite over temperatures between room temperature and 1400°C by thermal analysis (thermogravimetry (TG)/differential scanning calorimetry (DSC) and thermo-mechanical analysis-TMA). Structural and surface modifications related to samples origin and calcination temperature were investigated by Fourier transformed infrared (FTIR) and Raman spectroscopy, X-ray diffraction (XRD) and BET method. FTIR spectra indicated that the organic constituents and carbonate are no longer present in the natural sample calcined at 800°C. Raman spectra highlighted the decomposition products of the hydroxyapatite. The calcination treatment modifies the processes kinetics of the synthetic samples, being able to isolate lattice water desorption processes of decarbonization and the dehydroxylation processes. Shrinkage of calcined synthetic sample increases by 10% compared to uncalcined synthetic powder. From the TMA correlated with TG analysis and heat capacity data it can be concluded that sintering temperature of the synthetic samples should be chosen in the temperature range of the onset of dehydroxylation and the temperature at which oxyapatite decomposition begins. Copyright © 2014 Elsevier B.V. All rights reserved.

Concentrated solar energy used for sintering magnesium titanates for electronic applications

Science.gov (United States)

Apostol, Irina; Rodríguez, Jose; Cañadas, Inmaculada; Galindo, Jose; Mendez, Senen Lanceros; de Abreu Martins, Pedro Libȃnio; Cunha, Luis; Saravanan, Kandasamy Venkata

2018-04-01

Solar energy is an important renewable source of energy with many advantages: it is unlimited, clean and free. The main objective of this work was to sinter magnesium titanate ceramics in a solar furnace using concentrated solar energy, which is a novel and original process. The direct conversion of solar power into high temperature makes this process simple, feasible and ecologically viable/environmentally sustainable. We performed the solar sintering experiments at Plataforma Solar de Almeria-CIEMAT, Spain. This process takes place in a vertical axis solar furnace (SF5-5 kW) hosting a mobile flat mirror heliostat, a fixed parabolic mirror concentrator, an attenuator and a test table the concentrator focus. We sintered (MgO)0.63(TiO2)0.37, (MgO)0.49(TiO2)0.51, (MgO)0.50(TiO2)0.50 ceramics samples in air at about 1100 °C for a duration of 16 min, 1 h, 2 h and 3 h in the solar furnace. The MgO/TiO2 ratio and the dwell time was varied in order to obtain phase pure MgTiO3 ceramic. We obtained a pure MgTiO3 geikielite phase by solar sintering of (MgO)0.63(TiO2)0.37 samples at 1100 °C (16 min-3 h). Samples of (MgO)0.63(TiO2)0.37, solar sintered at 1100 °C for 3 h, resulted in well-sintered, non-porous samples with good density (3.46 g/cm3). The sintered samples were analyzed by XRD for phase determination. The grain and surface morphology was observed using SEM. Electrical measurements were carried out on solar sintered samples. The effect of processing parameters on microstructure and dielectric properties were investigated and is presented.

Electrophoretic Deposition of Hydroxyapatite Film Containing Re-Doped MoS2 Nanoparticles

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Hila Shalom

2018-02-01

Full Text Available Films combining hydroxyapatite (HA with minute amounts (ca. 1 weight % of (rhenium doped fullerene-like MoS2 (IF nanoparticles were deposited onto porous titanium substrate through electrophoretic process (EPD. The films were analyzed by scanning electron microscopy (SEM, X-ray diffraction and Raman spectroscopy. The SEM analysis showed relatively uniform coatings of the HA + IF on the titanium substrate. Chemical composition analysis using energy dispersive X-ray spectroscopy (EDS of the coatings revealed the presence of calcium phosphate minerals like hydroxyapatite, as a majority phase. Tribological tests were undertaken showing that the IF nanoparticles endow the HA film very low friction and wear characteristics. Such films could be of interest for various medical technologies. Means for improving the adhesion of the film to the underlying substrate and its fracture toughness, without compromising its biocompatibility are discussed at the end.

Heating of Porous Icy Dust Aggregates

Energy Technology Data Exchange (ETDEWEB)

Sirono, Sin-iti [Earth and Environmental Sciences, Nagoya University, Tikusa-ku, Furo-cho, Nagoya 464-8601 (Japan)

2017-06-10

At the beginning of planetary formation, highly porous dust aggregates are formed through coagulation of dust grains. Outside the snowline, the main component of an aggregate is H{sub 2}O ice. Because H{sub 2}O ice is formed in amorphous form, its thermal conductivity is extremely small. Therefore, the thermal conductivity of an icy dust aggregate is low. There is a possibility of heating inside an aggregate owing to the decay of radionuclides. It is shown that the temperature increases substantially inside an aggregate, leading to crystallization of amorphous ice. During the crystallization, the temperature further increases sufficiently to continue sintering. The mechanical properties of icy dust aggregates change, and the collisional evolution of dust aggregates is affected by the sintering.

Carbonate hydroxyapatite and silicon-substituted carbonate hydroxyapatite

DEFF Research Database (Denmark)

Bang, L T; Long, B D; Othman, R

2014-01-01

The present study investigates the chemical composition, solubility, and physical and mechanical properties of carbonate hydroxyapatite (CO3Ap) and silicon-substituted carbonate hydroxyapatite (Si-CO3Ap) which have been prepared by a simple precipitation method. X-ray diffraction (XRD), Fourier......(3-)) site and also entered simultaneously into the hydroxyapatite structure. The Si-substituted CO3Ap reduced the powder crystallinity and promoted ion release which resulted in a better solubility compared to that of Si-free CO3Ap. The mean particle size of Si-CO3Ap was much finer than that of CO3Ap...

The manufacture of synthetic non-sintered and degradable bone grafting substitutes.

Science.gov (United States)

Gerike, W; Bienengräber, V; Henkel, K-O; Bayerlein, T; Proff, P; Gedrange, T; Gerber, Th

2006-02-01

A new synthetic bone grafting substitute (NanoBone, ARTOSS GmbH, Germany) is presented. This is produced by a new technique, the sol-gel-method. This bone grafting substitute consists of nanocrystalline hydroxyapatite (HA) and nanostructured silica (SiO2). By achieving a highly porous structure good osteoconductivity can be seen. In addition, the material will be completely biodegraded and new own bone is formed. It has been demonstrated that NanoBone is biodegraded by osteoclasts in a manner comparable to the natural bone remodelling process.

Hydraulical and acoustical properties of porous sintered glass bead systems: experiments, theory, & simulations

NARCIS (Netherlands)

Güven, Ibrahim

2016-01-01

Wave and transport phenomena through porous media are of great importance in science and industrial applications, because they involve the interaction of various physical mechanisms and can provide useful informations of the structure of the porous medium. Despite the extensive application in modern

Preparation and evaluation of cerium oxide-bovine hydroxyapatite composites for biomedical engineering applications.

Science.gov (United States)

Gunduz, O; Gode, C; Ahmad, Z; Gökçe, H; Yetmez, M; Kalkandelen, C; Sahin, Y M; Oktar, F N

2014-07-01

The fabrication and characterization of bovine hydroxyapatite (BHA) and cerium oxide (CeO2) composites are presented. CeO2 (at varying concentrations 1, 5 and 10wt%) were added to calcinated BHA powder. The resulting mixtures were shaped into green cylindrical samples by powder pressing (350MPa) followed by sintering in air (1000-1300°C for 4h). Density, Vickers microhardness (HV), compression strength, scanning electron microscopy (SEM) and X-ray diffraction (XRD) studies were performed on the products. The sintering behavior, microstructural characteristics and mechanical properties were evaluated. Differences in the sintering temperature (for 1wt% CeO2 composites) between 1200 and 1300°C, show a 3.3% increase in the microhardness (564 and 582.75HV, respectively). Composites prepared at 1300°C demonstrate the greatest compression strength with comparable results for 5 and 10wt% CeO2 content (106 and 107MPa) which are significantly better than those for 1wt% and those that do not include any CeO2 (90 and below 60MPa, respectively). The results obtained suggest optimal parameters to be used in preparation of BHA and CeO2 composites, while also highlighting the potential of such materials in several biomedical engineering applications. Copyright © 2014 Elsevier Ltd. All rights reserved.

Microarc oxidized TiO2 based ceramic coatings combined with cefazolin sodium/chitosan composited drug film on porous titanium for biomedical applications.

Science.gov (United States)

Wei, Daqing; Zhou, Rui; cheng, Su; Feng, Wei; Li, Baoqiang; Wang, Yaming; Jia, Dechang; Zhou, Yu; Guo, Haifeng

2013-10-01

Porous titanium was prepared by pressureless sintering of titanium beads with diameters of 100, 200, 400 and 600 μm. The results indicated that the mechanical properties of porous titanium changed significantly with different bead diameters. Plastic deformations such as necking phenomenon and dimple structure were observed on the fracture surface of porous titanium sintered by beads with diameter of 100 μm. However, it was difficult to find this phenomenon on the porous titanium with a titanium bead diameter of 600 μm. The microarc oxidized coatings were deposited on its surface to improve the bioactivity of porous titanium. Furthermore, the cefazolin sodium/chitosan composited films were fabricated on the microarc oxidized coatings for overcoming the inflammation due to implantation, showing good slow-release ability by addition of chitosan. And the release kinetic process of cefazolin sodium in composited films could be possibly fitted by a polynomial model. Copyright © 2013 Elsevier B.V. All rights reserved.

A New Highly Bioactive Composite for Scaffold Applications: A Feasibility Study

Directory of Open Access Journals (Sweden)

Antonella Sola

2011-01-01

Full Text Available Hydroxyapatite (HA has been widely investigated as scaffolding material for bone tissue engineering, mainly for its excellent biocompatibility. Presently, there is an increasing interest in the composites of hydroxyapatite with bioactive glasses, with the aim to obtain systems with improved bioactivity or mechanical properties. Moreover, modifying the ratio between bioactive glass and hydroxyapatite results in the possibility of controlling the reaction rate of the composite scaffold in the human body. However, high temperature treatments are usually required in order to sinter HA-based composites, causing the bioactive glass to crystallize into a glass-ceramic, with possible negative effects on its bioactivity. In the present research work, a glass composition belonging to the Na2O-CaO-P2O5-SiO2 system, with a reduced tendency to crystallize, is applied to realize HA-based composites. The novel samples can be sintered at a relative low temperature (750 °C compared to the widely studied HA/45S5 Bioglass® composites. This fact greatly helps to preserve the amorphous nature of the glass, with excellent effects in terms of bioactivity, according to in vitro tests. As a first application, the obtained composites are also tested to realize highly porous scaffolds by means of the standard burning out method.

Porous stainless steel hollow fiber membranes via dry-wet spinning

NARCIS (Netherlands)

Luiten-Olieman, Maria W.J.; Winnubst, Aloysius J.A.; Nijmeijer, Arian; Wessling, Matthias; Benes, Nieck Edwin

2011-01-01

Porous stainless steel hollow fibers have been prepared via the dry–wet spinning process, based on phase inversion of a particle loaded polymer solution, followed by sintering. The morphology of the green fibers combines sponge like structures and macro voids, and is related to the dynamics of the

Phase composition, microstructure, and mechanical properties of porous Ti-Nb-Zr alloys prepared by a two-step foaming powder metallurgy method.

Science.gov (United States)

Rao, X; Chu, C L; Zheng, Y Y

2014-06-01

Porous Ti-Nb-Zr alloys with different porosities from 6.06 to 62.8% are prepared by a two-step foaming powder metallurgy method using TiH2, Nb, and Zr powders together with 0 to 50wt% of NH4HCO3. The effects of the amounts of Nb and Zr as well as the sintering temperature (1473 to 1673K) on their phase composition, porosity, morphology, and mechanical characteristics are investigated. By controlling the porosity, Nb and Zr concentrations as well as the sintering temperature, porous Ti-Nb-Zr alloys with different mechanical properties can be obtained, for example, the hardness between 290 and 63HV, the compressive strength between 1530.5 and 73.4MPa, and the elastic modulus between 10.8 and 1.2GPa. The mechanical properties of the sintered porous Ti-Nb-Zr alloys can be tailored to match different requirements for the human bones and are thus potentially useful in the hard tissue implants. Copyright © 2014 Elsevier Ltd. All rights reserved.

EXAFS study on dynamic structural property of porous morph-genetic SiC

International Nuclear Information System (INIS)

Ding, J.; Sun, B.H.; Fan, T.X.; Zhang, D.; Kamada, M.; Ogawa, H.; Guo, Q.X.

2005-01-01

Novel porous morph-genetic silicon carbide has been fabricated through sintering treatment, after infiltrating the methyl organic silicone resin to the bio-template. Its dynamic transition of structure during sintering process is investigated by extended X-ray absorption fine structure (EXAFS) for the first time. By analyzing Si K-edge EXAFS, it is found that the coordination number of the nearest C shell remains almost unchanged while that of the nearest Si shell dramatically changes when the structure is transformed from amorphous into crystalline state

Design of polymer-biopolymer-hydroxyapatite biomaterials for bone tissue engineering: Through molecular control of interfaces

Science.gov (United States)

Verma, Devendra

-containing scaffolds. Hydroxyapatite-containing chitosan/PgA scaffolds maintained their structural integrity under wet conditions. These scaffolds showed extremely porous (97.4%) and interconnected architecture. These scaffolds also promoted cell adhesion, proliferation and differentiation, Osteoblast cells formed nodular structure on thin films and scaffold. Mineralization of these nodules was confirmed by alizarin red S staining. Even after 20 days of seeding, all the cells were found alive. Our results indicated that chitosan-PgA-hydroxyapatite composite scaffolds have high potential for bone tissue engineering. This dissertation represents a comprehensive study on design of novel bone biomaterials through tailoring of interfaces in nanocomposites of polymers, biopolymer and hydroxyapatite.

Effects of sintering temperature on the corrosion behavior of AZ31 alloy with Ca–P sol–gel coating

Energy Technology Data Exchange (ETDEWEB)

Niu, Bo [School of Materials Science and Engineering, Liaoning University of Technology, Jinzhou, Liaoning Province, 121001 (China); Shi, Ping, E-mail: p_shi@sohu.com [School of Materials Science and Engineering, Liaoning University of Technology, Jinzhou, Liaoning Province, 121001 (China); Wei, Donghua [School of Materials Science and Engineering, Liaoning University of Technology, Jinzhou, Liaoning Province, 121001 (China); E, Shanshan [School of Mathematics and Physics, Bohai University, Jinzhou, Liaoning Province, 121013 (China); Li, Qiang; Chen, Yang [School of Materials Science and Engineering, Liaoning University of Technology, Jinzhou, Liaoning Province, 121001 (China)

2016-04-25

To slow down the initial biodegradation rate of magnesium alloy, calcium phosphate (Ca–P) coatings were prepared on AZ31 magnesium alloy by a sol–gel technique. To study the effects of sintering temperature on microstructure, bonding strength and corrosion behavior of the coatings, scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD) and an adhesive strength test were used to characterize the coatings. The corrosion resistance of the coatings was investigated by immersion test and electrochemical corrosion techniques in simulated body fluid (SBF) solution. It shows that the sol–gel coatings consist of Ca{sub 2}P{sub 2}O{sub 7}, mixture of Ca{sub 2}P{sub 2}O{sub 7}, Ca{sub 3}(PO{sub 4}){sub 2} and hydroxyapatite, and hydroxyapatite, by sintering respectively at 300 °C, 400 °C and 500 °C. There are major cracks on the coatings. The crack area portion on the coating and the bonding strength at the interface between the calcium phosphate coating and the bare AZ31 increases, and the corrosion resistance of the coated AZ31 in SBF decreases with increasing sintering temperatures from 300 °C to 500 °C. Based on our investigations, the corrosion resistance of the coated AZ31 in SBF depends mainly on the crack area portion on the coatings, rather than on the coating phase stability. - Highlights: • Ca–P coating was prepared on AZ31 alloy by a sol–gel technique. • Crack area portion in the coating increases with temperatures. • Bonding strength between Ca–P coating and substrate increases with temperatures. • Corrosion resistance of the coated AZ31 in SBF decreases with temperatures. • Corrosion resistance of the coated AZ31 depends mainly on the crack area portion.

Porous SiO2/HAp Coatings on Cp-Titanium Grade 1 Surfaces Produced by Electrophoretic Deposition

Directory of Open Access Journals (Sweden)

Moskalewicz T.

2016-12-01

Full Text Available Porous hydroxyapatite doped SiO2 coatings were electrophoretically deposited (EPD on commercially pure titanium. The influence of EPD parameters on coatings quality was investigated. Microstructural observation was done using transmission and scanning electron microscopy as well as X-ray diffractometry.

Morphological analysis and modelling of sintering and of sintered materials

International Nuclear Information System (INIS)

Jernot, Jean-Paul

1982-01-01

This research thesis addresses the study of solid phase sintering of metallic powders, and aims at describing as precisely as possible the different involved matter transport mechanisms, first by using a thermodynamic approach to sintering. Sintering diagrams are also used to determine prevailing mechanisms. The microstructure of sintered materials has been studied by using image quantitative analysis, thus by using a morphological approach to sintering. Morphological parameters allow, on the one hand, the evolution of powders during sintering to be followed, and, on the other hand, sintered products to be correctly characterised. Moreover, the author reports the study of the evolution of some physical properties of sintered materials with respect to their microstructure parameters. This leads to the development of a modelling of the behaviour of these materials [fr

Study on acoustical properties of sintered bronze porous material for transient exhaust noise of pneumatic system

Science.gov (United States)

Li, Jingxiang; Zhao, Shengdun; Ishihara, Kunihiko

2013-05-01

A novel approach is presented to study the acoustical properties of sintered bronze material, especially used to suppress the transient noise generated by the pneumatic exhaust of pneumatic friction clutch and brake (PFC/B) systems. The transient exhaust noise is impulsive and harmful due to the large sound pressure level (SPL) that has high-frequency. In this paper, the exhaust noise is related to the transient impulsive exhaust, which is described by a one-dimensional aerodynamic model combining with a pressure drop expression of the Ergun equation. A relation of flow parameters and sound source is set up. Additionally, the piston acoustic source approximation of sintered bronze silencer with cylindrical geometry is presented to predict SPL spectrum at a far-field observation point. A semi-phenomenological model is introduced to analyze the sound propagation and reduction in the sintered bronze materials assumed as an equivalent fluid with rigid frame. Experiment results under different initial cylinder pressures are shown to corroborate the validity of the proposed aerodynamic model. In addition, the calculated sound pressures according to the equivalent sound source are compared with the measured noise signals both in time-domain and frequency-domain. Influences of porosity of the sintered bronze material are also discussed.

Development of implant/interconnected porous hydroxyapatite complex as new concept graft material.

Directory of Open Access Journals (Sweden)

Kazuya Doi

Full Text Available BACKGROUND: Dental implant has been successfully used to replace missing teeth. However, in some clinical situations, implant placement may be difficult because of a large bone defect. We designed novel complex biomaterial to simultaneously restore bone and place implant. This complex was incorporated implant into interconnected porous calcium hydroxyapatite (IP-CHA. We then tested this Implant/IP-CHA complex and evaluated its effect on subsequent bone regeneration and implant stability in vivo. METHODOLOGY/PRINCIPAL FINDINGS: A cylinder-type IP-CHA was used in this study. After forming inside of the cylinder, an implant was placed inside to fabricate the Implant/IP-CHA complex. This complex was then placed into the prepared bone socket in the femur of four beagle-Labrador hybrid dogs. As a control, implants were placed directly into the femur without any bone substrate. Bone sockets were allowed to heal for 2, 3 and 6 months and implant stability quotients (ISQ were measured. Finally, tissue blocks containing the Implant/IP-CHA complexes were harvested. Specimens were processed for histology and stained with toluidine blue and bone implant contact (BIC was measured. The ISQs of complex groups was 77.8±2.9 in the 6-month, 72.0±5.7 in the 3-month and 47.4±11.0 in the 2-month. There was no significant difference between the 3- or 6-month complex groups and implant control groups. In the 2-month group, connective tissue, including capillary angiogenesis, was predominant around the implants, although newly formed bone could also be observed. While, in the 3 and 6-month groups, newly formed bone could be seen in contact to most of the implant surface. The BICs of complex groups was 2.18±3.77 in the 2-month, 44.03±29.58 in the 3-month, and 51.23±8.25 in the 6-month. Significant difference was detected between the 2 and 6-month. CONCLUSIONS/SIGNIFICANCE: Within the results of this study, the IP-CHA/implant complex might be able to achieve both

Artificial Bone and Teeth through Controlled Ice Growth in Colloidal Suspensions

International Nuclear Information System (INIS)

Tomsia, Antoni P.; Saiz, Eduardo; Deville, Sylvain

2007-01-01

The formation of regular patterns is a common feature of many solidification processes involving cast materials. We describe here how regular patterns can be obtained in porous alumina and hydroxyapatite (HAP) by controlling the freezing of ceramic slurries followed by subsequent ice sublimation and sintering, leading to multilayered porous ceramic structures with homogeneous and well-defined architecture. These porous materials can be infiltrated with a second phase of choice to yield biomimetic nacre-like composites with improved mechanical properties, which could be used for artificial bone and teeth applications. Proper control of the solidification patterns provides powerful means of control over the final functional properties. We discuss the relationships between the experimental results, ice growth fundamentals, the physics of ice and the interaction between inert particles and the solidification front during directional freezing

Alumina Coating To Realize Desired Pore Characteristics Of Sintered Diatomite Membrane

Directory of Open Access Journals (Sweden)

Ha J.-H.

2015-06-01

Full Text Available Porous ceramic membranes prepared from natural materials such as diatomite, have lately attracted great interest in industrial applications due to their cost-effectiveness. In this study, we attempted to prepare an alumina coating to be deposited over a sintered diatomite-kaolin composite support layer in order to reduce the largest pore size to below 0.4 μm; such a coating could be potentially used in water treatment applications for bacterial removal.

Fabrication of naturel pumice/hydroxyapatite composite for biomedical engineering.

Science.gov (United States)

Komur, Baran; Lohse, Tim; Can, Hatice Merve; Khalilova, Gulnar; Geçimli, Zeynep Nur; Aydoğdu, Mehmet Onur; Kalkandelen, Cevriye; Stan, George E; Sahin, Yesim Muge; Sengil, Ahmed Zeki; Suleymanoglu, Mediha; Kuruca, Serap Erdem; Oktar, Faik Nuzhet; Salman, Serdar; Ekren, Nazmi; Ficai, Anton; Gunduz, Oguzhan

2016-07-07

We evaluated the Bovine hydroxyapatite (BHA) structure. BHA powder was admixed with 5 and 10 wt% natural pumice (NP). Compression strength, Vickers micro hardness, Fourier transform infrared spectroscopy, scanning electron microscopy (SEM) and X-ray diffraction studies were performed on the final NP-BHA composite products. The cells proliferation was investigated by MTT assay and SEM. Furthermore, the antimicrobial activity of NP-BHA samples was interrogated. Variances in the sintering temperature (for 5 wt% NP composites) between 1000 and 1300 °C, reveal about 700 % increase in the microhardness (~100 and 775 HV, respectively). Composites prepared at 1300 °C demonstrate the greatest compression strength with comparable result for 5 wt% NP content (87 MPa), which are significantly better than those for 10 wt% and those that do not include any NP (below 60 MPa, respectively). The results suggested the optimal parameters for the preparation of NP-BHA composites with increased mechanical properties and biocompatibility. Changes in micro-hardness and compression strength can be tailored by the tuning the NP concentration and sintering temperature. NP-BHA composites have demonstrated a remarkable potential for biomedical engineering applications such as bone graft and implant.

Nanostructured Si-substituted hydroxyapatite coatings for biomedical applications

Energy Technology Data Exchange (ETDEWEB)

Rau, Julietta V., E-mail: giulietta.rau@ism.cnr.it [Istituto di Struttura della Materia, Consiglio Nazionale delle Ricerche, Via del Fosso del Cavaliere, 100-00133 Rome (Italy); Fosca, Marco [Istituto di Struttura della Materia, Consiglio Nazionale delle Ricerche, Via del Fosso del Cavaliere, 100-00133 Rome (Italy); Cacciotti, Ilaria [Università di Roma “Tor Vergata”, Dipartimento di Ingegneria Industriale,UR INSTM “Roma Tor Vergata”, Via del Politecnico, 1-00133 Rome (Italy); Laureti, Sara [Istituto di Struttura della Materia, Consiglio Nazionale delle Ricerche, Via Salaria km 29.300-00016 Monterotondo Scalo (RM) (Italy); Bianco, Alessandra [Università di Roma “Tor Vergata”, Dipartimento di Ingegneria Industriale,UR INSTM “Roma Tor Vergata”, Via del Politecnico, 1-00133 Rome (Italy); Teghil, Roberto [Università della Basilicata, Dipartimento di Scienze, Via dell' Ateneo Lucano 10-85100, Potenza (Italy)

2013-09-30

In the present work, the Si-HAp coatings were deposited on titanium substrates by Pulsed Laser Deposition technique. For deposition, the Si-HAp targets (1.4 wt.% of Si), produced starting from wet synthesized powders, were used. The properties of coatings were investigated by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, atomic force microscopy and Vickers microhardness. The obtained Si-HAp coatings presented a nanosized structure, proper thickness and hardness for applications in orthopedical and dental surgery, aimed at improving the stability and the osteointegration of bone implants. - Highlights: ► Pulsed Laser Deposition method was applied to coat heated Titanium supports. ► Films were deposited using a target of Silicon-Hydroxyapatite sintered ceramics. ► Nanostructured crystalline hard film was grown replicating target composition. ► Prepared coating could be used for orthopedic and dental implants applications.

Nanostructured Si-substituted hydroxyapatite coatings for biomedical applications

International Nuclear Information System (INIS)

Rau, Julietta V.; Fosca, Marco; Cacciotti, Ilaria; Laureti, Sara; Bianco, Alessandra; Teghil, Roberto

2013-01-01

In the present work, the Si-HAp coatings were deposited on titanium substrates by Pulsed Laser Deposition technique. For deposition, the Si-HAp targets (1.4 wt.% of Si), produced starting from wet synthesized powders, were used. The properties of coatings were investigated by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, atomic force microscopy and Vickers microhardness. The obtained Si-HAp coatings presented a nanosized structure, proper thickness and hardness for applications in orthopedical and dental surgery, aimed at improving the stability and the osteointegration of bone implants. - Highlights: ► Pulsed Laser Deposition method was applied to coat heated Titanium supports. ► Films were deposited using a target of Silicon-Hydroxyapatite sintered ceramics. ► Nanostructured crystalline hard film was grown replicating target composition. ► Prepared coating could be used for orthopedic and dental implants applications

Integration approach for developing a high-performance biointerface: Sequential formation of hydroxyapatite and calcium carbonate by an improved alternate soaking process

International Nuclear Information System (INIS)

Watanabe, Junji; Akashi, Mitsuru

2008-01-01

Biointerfaces are crucial for regulating biofunctions. An effective method of producing new biomaterials is surface modification, in particular, the hybrid organic-inorganic approach. In this paper, we propose a method for the sequential formation of hydroxyapatite and calcium carbonate on porous polyester membranes by using an improved alternate soaking process. The resulting hybrid membranes were characterized in terms of their calcium and phosphorus ion contents; further, their structure was analyzed by scanning electron microscopy (SEM), X-ray diffraction (XRD), and infrared spectroscopy (IR). As a typical biofunction, protein adsorption by these hybrid membranes was investigated. Sequential hydroxyapatite and calcium carbonate formation on the membranes was successfully achieved, and the total amounts of hydroxyapatite and calcium carbonate formed were precisely regulated by the preparative conditions. The SEM and XRD characterizations were verified by comparing with the IR results. The amount of adsorbed protein correlated well with not only the amount of hydroxyapatite formed but also the combined amounts of hydroxyapatite and calcium carbonate formed. The results indicate that the hybrid membranes can function as high-performance biointerfaces that are capable of loading biomolecules such as proteins

Characteristic evaluation of cooling technique using liquid nitrogen and metal porous media

International Nuclear Information System (INIS)

Tanno, Yusuke; Ito, Satoshi; Hashizume, Hidetoshi

2014-01-01

A remountable high-temperature superconducting magnet, whose segments can be mounted and demounted repeatedly, has been proposed for construction and maintenance of superconducting magnet and inner reactor components of a fusion reactor. One of the issues in this design is that the performance of the magnet deteriorates by a local temperature rise due to Joule heating in jointing regions. In order to prevent local temperature rise, a cooling system using a cryogenic coolant and metal porous media was proposed and experimental studies have been carried out using liquid nitrogen. In this study, flow and heat transfer characteristics of cooling system using subcooled liquid nitrogen and bronze particle sintered porous media are evaluated through experiments in which the inlet degree of subcooling and flow rate of the liquid nitrogen. The flow characteristics without heat input were coincided with Ergun’s equation expressing single-phase flow in porous materials. The obtained boiling curve was categorized into three conditions; convection region, nucleate boiling region and mixed region with nucleate and film boiling. Wall superheat did not increase drastically with porous media after departure from nucleate boiling point, which is different from a situation of usual boiling curve in a smooth tube. The fact is important characteristic to cooling superconducting magnet to avoid its quench. Heat transfer coefficient with bronze particle sintered porous media was at least twice larger than that without the porous media. It was also indicated qualitatively that departure from nucleate boiling point and heat transfer coefficient depends on degree of subcooling and mass flow rate. The quantitative evaluation of them and further discussion for the cooling system will be performed as future tasks

Ultrafine-grained porous titanium and porous titanium/magnesium composites fabricated by space holder-enabled severe plastic deformation

Energy Technology Data Exchange (ETDEWEB)

Qi, Yuanshen, E-mail: yuanshen.qi@monash.edu [Centre for Advanced Hybrid Materials, Department of Materials Engineering, Monash University, Clayton, Victoria 3800 (Australia); Contreras, Karla G. [Monash Institute of Medical Engineering, Faculty of Engineering, Monash University, Clayton, Victoria 3800 (Australia); Jung, Hyun-Do [Liquid Processing & Casting Technology R& D Group, Korea Institute of Industrial Technology, Incheon 406-840 (Korea, Republic of); Department of Materials Science and Engineering, Seoul National University, Seoul 151-742 (Korea, Republic of); Kim, Hyoun-Ee [Department of Materials Science and Engineering, Seoul National University, Seoul 151-742 (Korea, Republic of); Advanced Institutes of Convergence Technology, Seoul National University, Gwanggyo, Yeongtong-gu, Suwon-si, Gyeonggi-do 443-270 (Korea, Republic of); Lapovok, Rimma [Centre for Advanced Hybrid Materials, Department of Materials Engineering, Monash University, Clayton, Victoria 3800 (Australia); Estrin, Yuri, E-mail: yuri.estrin@monash.edu [Centre for Advanced Hybrid Materials, Department of Materials Engineering, Monash University, Clayton, Victoria 3800 (Australia); Laboratory of Hybrid Nanostructured Materials, NUST MISiS, Moscow 119490 (Russian Federation)

2016-02-01

Compaction of powders by equal channel angular pressing (ECAP) using a novel space holder method was employed to fabricate metallic scaffolds with tuneable porosity. Porous Ti and Ti/Mg composites with 60% and 50% percolating porosity were fabricated using powder blends with two kinds of sacrificial space holders. The high compressive strength and good ductility of porous Ti and porous Ti/Mg obtained in this way are believed to be associated with the ultrafine grain structure of the pore walls. To understand this, a detailed electron microscopy investigation was employed to analyse the interface between Ti/Ti and Ti/Mg particles, the grain structures in Ti particles and the topography of pore surfaces. It was found that using the proposed compaction method, high quality bonding between particles was obtained. Comparing with other powder metallurgy methods to fabricate Ti with an open porous structure, where thermal energy supplied by a laser beam or high temperature sintering is essential, the ECAP process conducted at a relatively low temperature of 400 °C was shown to produce unique properties. - Highlights: • Porous Ti and porous Ti/Mg composite scaffolds were fabricated successfully. • Space holder-enabled severe plastic deformation was first used in this application. • Silicon particles as sacrificial space holders were used for the first time. • Ultrafine-grained microstructure and good bonding between particles were obtained. • Good preosteoblast cell response to as-manufactured porous Ti was achieved.

Development and characterization of a novel porous small intestine submucosa-hydroxyapatite scaffold for bone regeneration

Energy Technology Data Exchange (ETDEWEB)

Castilla Bolaños, Maria Alejandra, E-mail: ma.castilla964@uniandes.edu.co; Buttigieg, Josef; Briceño Triana, Juan Carlos

2017-03-01

The fabricated small intestine submucosa (SIS) – hydroxyapatite (HAp) sponges can act as biomimetic scaffolds to be utilized in tissue engineering and regeneration. Here we developed SIS-HAp sponges and investigated their mechanical, physical and chemical characteristics using scanning electron microscopy, Fourier transformed infrared spectroscopy, uniaxial compression, porosity, and swelling testing techniques. The results demonstrated mechanical properties superior to comparable bone substitutes fabricated with similar methods. SIS-HAp scaffolds possess an interconnected macroporosity, similar to that of trabecular bone, hence presenting a novel biomaterial that may serve as a superior bone substitute and tissue scaffold. - Highlights: • Small intestine submucosa (SIS) – hydroxyapatite (HAp) scaffolds were developed. • SIS-HAp scaffolds possess a trabecular bone-like structure. • FTIR indicated a molecular interaction between the organic groups of SIS and HAp. • SIS-HAp sponges presented a superior Young modulus to comparable bone substitutes.

Development and characterization of a novel porous small intestine submucosa-hydroxyapatite scaffold for bone regeneration

International Nuclear Information System (INIS)

Castilla Bolaños, Maria Alejandra; Buttigieg, Josef; Briceño Triana, Juan Carlos

2017-01-01

The fabricated small intestine submucosa (SIS) – hydroxyapatite (HAp) sponges can act as biomimetic scaffolds to be utilized in tissue engineering and regeneration. Here we developed SIS-HAp sponges and investigated their mechanical, physical and chemical characteristics using scanning electron microscopy, Fourier transformed infrared spectroscopy, uniaxial compression, porosity, and swelling testing techniques. The results demonstrated mechanical properties superior to comparable bone substitutes fabricated with similar methods. SIS-HAp scaffolds possess an interconnected macroporosity, similar to that of trabecular bone, hence presenting a novel biomaterial that may serve as a superior bone substitute and tissue scaffold. - Highlights: • Small intestine submucosa (SIS) – hydroxyapatite (HAp) scaffolds were developed. • SIS-HAp scaffolds possess a trabecular bone-like structure. • FTIR indicated a molecular interaction between the organic groups of SIS and HAp. • SIS-HAp sponges presented a superior Young modulus to comparable bone substitutes.

PCL-coated hydroxyapatite scaffold derived from cuttlefish bone: In vitro cell culture studies

International Nuclear Information System (INIS)

Milovac, Dajana; Gamboa-Martínez, Tatiana C.; Ivankovic, Marica; Gallego Ferrer, Gloria; Ivankovic, Hrvoje

2014-01-01

In the present study, we examined the potential of using highly porous poly(ε-caprolactone) (PCL)-coated hydroxyapatite (HAp) scaffold derived from cuttlefish bone for bone tissue engineering applications. The cell culture studies were performed in vitro with preosteoblastic MC3T3-E1 cells in static culture conditions. Comparisons were made with uncoated HAp scaffold. The attachment and spreading of preosteoblasts on scaffolds were observed by Live/Dead staining Kit. The cells grown on the HAp/PCL composite scaffold exhibited greater spreading than cells grown on the HAp scaffold. DNA quantification and scanning electron microscopy (SEM) confirmed a good proliferation of cells on the scaffolds. DNA content on the HAp/PCL scaffold was significantly higher compared to porous HAp scaffolds. The amount of collagen synthesis was determined using a hydroxyproline assay. The osteoblastic differentiation of the cells was evaluated by determining alkaline phosphatase (ALP) activity and collagen type I secretion. Furthermore, cell spreading and cell proliferation within scaffolds were observed using a fluorescence microscope. - Highlights: • Hydroxyapatite/poly(ε-caprolactone) scaffold with interconnected pores was prepared • Cytotoxicity test showed that the scaffold was not cytotoxic towards MC3T3-E1 cells • The scaffold supported the attachment, proliferation and differentiation of cells • A 3D cell colonization was confirmed using the fluorescence microscopy • The scaffold might be a promising candidate for bone tissue engineering

Characterization of hydroxyapatite coatings deposited by hydrothermal electrochemical method on NaOH immersed Ti6Al4V

International Nuclear Information System (INIS)

He, Daihua; Liu, Ping; Liu, Xinkuan; Ma, Fengcang; Chen, Xiaohong; Li, Wei; Du, Jiandi; Wang, Pu; Zhao, Jun

2016-01-01

The hydrothermal electrochemical method was used to deposit hydroxyapatite coating on Ti6Al4V. In order to improve the bonding strength between the coating and substrate, the substrates were modified by 8 M NaOH solution before the deposition. The effects of immersing time on the substrate, on the hydroxyapatite coating, and on the bonding strength were studied. X-Ray Diffraction, Scanning Electron Microscope, Fourier Transform Infrared Spectroscopy and Drop Shape Analysis Method were applied. And the crystallinity of hydroxyapatite coating was calculated. The results show that immersing treatment effects the phase compositions, the microstructure and the wettability of the substrate surface. A porous, three-dimensional network structure is formed on the Ti6Al4V surface through the NaOH immersion. The pore size and depth increase with the increase of immersing time from 12 to 48 h. The surface microstructure of Ti6Al4V with 60 h′ immersion time was different from the others. The modification treatment can improve the bonding strength between hydroxyapatite coating and the substrate obviously. The value of the bonding strength with the substrate immersed for 48 h is larger than those of the others. A bone-like apatite layer forms on the coating after 3 days of soaking in SBF, implying with good bioactivity of the hydroxyapatite coatings deposited by the method. The surface characteristics of the sample immersed with 48 h are more conductive to the deposition of hydroxyapatite and to the improvement of the bonding strength. The formation mechanism of hydroxyapatite coating deposited by hydrothermal electrochemical method was discussed. - Highlights: • Immerse Ti6Al4V alloy with NaOH solution for different immersing time. • We deposit hydroxyapatite coating by hydrothermal electrochemical method. • We examine changes of composition, microstructure, bonding strength and bioactivity of the hydroxyapatite coating. • 48 h is the optimal immersing time. • We

Stem cell engineered bone with calcium-phosphate coated porous titanium scaffold or silicon hydroxyapatite granules for revision total joint arthroplasty.

Science.gov (United States)

García-Gareta, Elena; Hua, Jia; Rayan, Faizal; Blunn, Gordon W

2014-06-01

Aseptic loosening in total joint replacements (TJRs) is mainly caused by osteolysis which leads to a reduction of the bone stock necessary for implant fixation in revision TJRs. Our aim was to develop bone tissue-engineered constructs based on scaffolds of clinical relevance in revision TJRs to reconstitute the bone stock at revision operations by using a perfusion bioreactor system (PBRS). The hypothesis was that a PBRS will enhance mesenchymal stem cells (MSCs) proliferation and osteogenic differentiation and will provide an even distribution of MSCs throughout the scaffolds when compared to static cultures. A PBRS was designed and implemented. Scaffolds, silicon substituted hydroxyapatite granules and calcium-phosphate coated porous TiAl6V4 cylinders, were seeded with MSCs and cultured either in static conditions or in the PBRS at 0.75 mL/min. Statistically significant increased cell proliferation and alkaline phosphatase activity was found in samples cultured in the PBRS. Histology revealed a more even cell distribution in the perfused constructs. SEM showed that cells arranged in sheets. Long cytoplasmic processes attached the cells to the scaffolds. We conclude that a novel tissue engineering approach to address the issue of poor bone stock at revision operations is feasible by using a PBRS.

Physical-mechanical characterization of hydroxyapatite-titanium oxide composites made by the polymeric sponge method; Caracterizacao fisico-mecanica de compositos porosos de hidroxiapatita-titania confeccionados pelo metodo da esponja polimerica

Energy Technology Data Exchange (ETDEWEB)

Galdino, A.G.S.; Zavaglia, C.A.C. [Universidade Estadual de Campinas (FEM/UNICAMP), SP (Brazil)

2011-07-01

Bioceramics have been used as bone reconstruction materials since last decades, where hydroxyapatite is one of the most used for this purpose. However, hydroxyapatite's mechanical strength is not so high when compared to other bioceramics. This work aimed on characterizing physically and mechanically composites of HA-TiO{sub 2}. Samples were made by the polymeric sponge method with 70% - 30% wt., 60% - 40% wt. and 50% - 50% wt. of HA - TiO{sub 2}, calcined at 550 deg C for sponge burning and sintered at 1250 deg C, 1300 deg C and 1350 deg C. Samples were submitted to mechanical essays of compression and Hardness Vickers and to physical essays of water absorption, apparent density, burning linear retraction and apparent density. Results showed relatively better than those of pure hydroxyapatite and they are in accordance with the literature. (author)

Asymmetric designed sintered metal filter elements in the HTF process of LILW vitrification plant

International Nuclear Information System (INIS)

Roehlig, Rainer

2005-01-01

Sintered metal filter elements have been used for years and have been successfully in operation in different application. The technical and economical advantages of only recently developed asymmetric Metallic Membranes elements, which operate as a surface filter, will be shown in comparison with standard sintered metal filter cartridges. The permeability, particle retention and back flushing performance have been improved. In order to achieve this, an asymmetric structure was designed in which an active filtration layer is applied onto a coarse porous metal support material made out of the same alloy. The economical benefits for customers are low maintenance and reduced investment cost as well as defined particle retention as is required by the users

In vivo immuno-reactivity analysis of the porous three-dimensional chitosan/SiO2 and chitosan/SiO2 /hydroxyapatite hybrids.

Science.gov (United States)

Guo, Mengxia; Dong, Yifan; Xiao, Jiangwei; Gu, Ruicai; Ding, Maochao; Huang, Tao; Li, Junhua; Zhao, Naru; Liao, Hua

2018-05-01

Inorganic/organic hybrid silica-chitosan (CS) scaffolds have promising potential for bone defect repair, due to the controllable mechanical properties, degradation behavior, and scaffold morphology. However, the precise in vivo immuno-reactivity of silica-CS hybrids with various compositions is still poorly defined. In this study, we fabricated the three-dimensional (3D) interconnected porous chitosan-silica (CS/SiO 2 ) and chitosan-silica-hydroxyapatite (CS/SiO 2 /HA) hybrids, through sol-gel process and 3D plotting skill, followed by the naturally or freeze drying separately. Scanning electron microscopy demonstrated the hybrids possessed the uniform geometric structure, while, transmission electron microscopy displayed nanoscale silica, or HA nanoparticles dispersed homogeneously in the CS matrix, or CS/silica hybrids. After intramuscular implantation, CS/SiO 2 and CS/SiO 2 /HA hybrids triggered a local and limited monocyte/macrophage infiltration and myofiber degeneration. Naturally dried CS/SiO 2 hybrid provoked a more severe inflammation than the freeze-dried ones. Dendritic cells were attracted to invade into the implants embedded-muscle, but not be activated to prime the adaptive immunity, because the absence of cytotoxic T cells and B cells in muscle received the implants. Fluorescence-activated cell sorting (FACS) analysis indicated the implanted hybrids were incapable to initiate splenocytes activation. Plasma complement C3 enzyme linked immunosorbent assay (ELISA) assay showed the hybrids induced C3 levels increase in early implanting phase, and the subsequent striking decrease. Thus, the present results suggest that, in vivo, 3D plotted porous CS/SiO 2 and CS/SiO 2 /HA hybrids are relatively biocompatible in vivo, which initiate a localized inflammatory procedure, instead of a systematic immune response. © 2018 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 106A: 1223-1235, 2018. © 2018 Wiley Periodicals, Inc.

Preparation and characterization of new dental porcelains, using K-feldspar and quartz raw materials. Effect of B2O3 additions on sintering and mechanical properties.

Science.gov (United States)

Harabi, Abdelhamid; Guerfa, Fatiha; Harabi, Esma; Benhassine, Mohamed-Tayeb; Foughali, Lazhar; Zaiou, Soumia

2016-08-01

The aim of this work was to determine the effect of temperature and boric oxide (B2O3) addition on sintering and mechanical properties of a newly developed dental porcelain (DP) prepared from local Algerian raw materials. Based on a preliminary work, the new selected composition was 75wt.% feldspar, 20wt.% quartz and 5wt.% kaolin. It was prepared by sintering the mixture at different temperatures (1100-1250°C). The optimum sintering conditions gave a relatively higher density (2.47g/cm(3)) and excellent mechanical properties. The three point flexural strength (3PFS) and Martens micro-hardness of dental porcelains were 149MPa and 2600MPa, respectively. This obtained 3PFS value is more than four times greater than that of hydroxyapatite (HA) value (about 37MPa) sintered under the same conditions. However, the sintering temperature was lowered by about 25 and 50°C for 3 and 5wt.% B2O3 additions, respectively. But, it did not improve furthermore the samples density and their mechanical properties. It has also been found that B2O3 additions provoke a glass matrix composition variation which delays the leucite formation during sintering. Copyright © 2016 Elsevier B.V. All rights reserved.

Electrospinning synthesis of 3D porous NiO nanorods as anode material for lithium-ion batteries

Directory of Open Access Journals (Sweden)

Wei Kong Xiang

2016-06-01

Full Text Available Three-dimensional NiO nanorods were synthesized as anode material by electrospinning method. X-ray diffraction results revealed that the product sintered at 400 °C had impure metallic nickel phase which, however, became pure NiO phase as the sintering temperature rose. Nevertheless, the nanorods sintered at 400, 500 and 600 °C had similar diameters (∼200 nm.The NiO nanorod material sintered at 500 °C was chip-shaped with a diameter of 200 nm and it exhibited a porous 3D structure. The nanorod sintered at 500 °C had the optimal electrochemical performance. Its discharge specific capacity was 1127 mAh·g−1 initially and remained as high as 400 mAh·g−1 at a current density of 55 mA·g−1 after 50 cycles.

Influence of sintering atmospheres on the aluminium sintering characteristics

International Nuclear Information System (INIS)

Mintzer, S.; Bermudez Belkys, S.

1993-01-01

This paper describes the aluminium powder (Al) cool compacted (at 95% from theoretical density) which was sintered at 903 K during 4 hours at different atmospheres; oxidizing (air), inert Argon (Ar), Nitrogen (N) and high vacuum. The results obtained show: a) porosity measurements; greater porosity when sintering in Ar and air. b) Metallographic and Scanning observations: many fine pores (< 1 μm) and pore lines distributed at random, at air sintering and greater pores distributed preferentially near the surface, in Ar and N atmospheres. c) Dimensional changes: tendency to contraction of the samples at N and vacuum sintering and expansion in Ar or air. d) Mechanical properties: greater strength and fluence stresses at air and N sintering. The analysis of the results is performed considering sintering modes in presence of an oxide layer and dropped inert gases. (Author)

Hydroxyapatite synthesis on solid surfaces using a biological approach

International Nuclear Information System (INIS)

Wang, A; Mei, J; Tse, Y Y; Jones, I P; Sammons, R L

2012-01-01

Many naturally occurring mineralisation processes yield hydroxyapatite (HA) or related salts, but biological routes to calcification have not generally been exploited for production of hydroxyapatite for clinical and industrial applications. Serratia sp. NCIMB 40259 is a non-pathogenic Gram-negative bacterium which is capable of growing as a biofilm on many surfaces and can be used to form HA coatings on a variety of polymeric and metallic materials, including titanium. Here we review previous work and report the results of more recent studies on the influence of titanium compositional and surface properties on Serratia adherence and proliferation and biomineralisation on commercially pure titanium (cp Ti) discs and a Ti mesh. Bacterial adherence was equivalent on cpTi and Ti6Al4V, and biofilms formed on both rough and mirror-polished cpTi surfaces. Embedded alumina particles and alkali treatment did not noticeably alter the precipitation of Serratia HA, nor the structure of the coating in comparison with non-treated substrates. Coatings were retained after sintering at 800°C in argon, although the original curved plate-like crystals changed to nano-scale β-tricalcium phosphate particles. A phosphorous-rich diffusion zone formed at the coating-titanium interface. Bacterial mineralisation may have applications as a method for producing coatings on implants in non load-bearing sites, and non-clinical applications where a high surface area is the major concern.

Hydroxyapatite synthesis on solid surfaces using a biological approach

Science.gov (United States)

Wang, A.; Mei, J.; Tse, Y. Y.; Jones, I. P.; Sammons, R. L.

2012-12-01

Many naturally occurring mineralisation processes yield hydroxyapatite (HA) or related salts, but biological routes to calcification have not generally been exploited for production of hydroxyapatite for clinical and industrial applications. Serratia sp. NCIMB 40259 is a non-pathogenic Gram-negative bacterium which is capable of growing as a biofilm on many surfaces and can be used to form HA coatings on a variety of polymeric and metallic materials, including titanium. Here we review previous work and report the results of more recent studies on the influence of titanium compositional and surface properties on Serratia adherence and proliferation and biomineralisation on commercially pure titanium (cp Ti) discs and a Ti mesh. Bacterial adherence was equivalent on cpTi and Ti6Al4V, and biofilms formed on both rough and mirror-polished cpTi surfaces. Embedded alumina particles and alkali treatment did not noticeably alter the precipitation of Serratia HA, nor the structure of the coating in comparison with non-treated substrates. Coatings were retained after sintering at 800°C in argon, although the original curved plate-like crystals changed to nano-scale β-tricalcium phosphate particles. A phosphorous-rich diffusion zone formed at the coating-titanium interface. Bacterial mineralisation may have applications as a method for producing coatings on implants in non load-bearing sites, and non-clinical applications where a high surface area is the major concern.

A new hydroxyapatite-based biocomposite for bone replacement

Energy Technology Data Exchange (ETDEWEB)

Bellucci, Devis, E-mail: devis.bellucci@unimore.it [Department of Engineering “Enzo Ferrari”, University of Modena and Reggio Emilia, Via Vignolese 905, 41125 Modena (Italy); Sola, Antonella [Department of Engineering “Enzo Ferrari”, University of Modena and Reggio Emilia, Via Vignolese 905, 41125 Modena (Italy); Gazzarri, Matteo; Chiellini, Federica [Laboratory of Bioactive Polymeric Materials for Biomedical and Environmental Applications (BIOlab) and UdR INSTM, Department of Chemistry and Industrial Chemistry, University of Pisa, Via Vecchia Livornese 1291, 56122S. Piero a Grado, Pisa (Italy); Cannillo, Valeria [Department of Engineering “Enzo Ferrari”, University of Modena and Reggio Emilia, Via Vignolese 905, 41125 Modena (Italy)

2013-04-01

Since the 1970s, various types of ceramic, glass and glass–ceramic materials have been proposed and used to replace damaged bone in many clinical applications. Among them, hydroxyapatite (HA) has been successfully employed thanks to its excellent biocompatibility. On the other hand, the bioactivity of HA and its reactivity with bone can be improved through the addition of proper amounts of bioactive glasses, thus obtaining HA-based composites. Unfortunately, high temperature treatments (1200 °C ÷ 1300 °C) are usually required in order to sinter these systems, causing the bioactive glass to crystallize into a glass–ceramic and hence inhibiting the bioactivity of the resulting composite. In the present study novel HA-based composites are realized and discussed. The samples can be sintered at a relatively low temperature (800 °C), thanks to the employment of a new glass (BG{sub C}a) with a reduced tendency to crystallize compared to the widely used 45S5 Bioglass®. The rich glassy phase, which can be preserved during the thermal treatment, has excellent effects in terms of in vitro bioactivity; moreover, compared to composites based on 45S5 Bioglass® having the same HA/glass proportions, the samples based on BG{sub C}a displayed an earlier response in terms of cell proliferation. - Highlights: ► New apatite/bioglass composites are proposed and sintered at low temperature. ► The samples' glassy phase is preserved and the apatite decomposition is avoided. ► The rich glassy phase in the samples results in an excellent bioactivity. ► The samples are able to support cell adhesion and proliferation. ► The samples support faster cell proliferation compared to 45S5Bioglass-composites.

A new hydroxyapatite-based biocomposite for bone replacement

International Nuclear Information System (INIS)

Bellucci, Devis; Sola, Antonella; Gazzarri, Matteo; Chiellini, Federica; Cannillo, Valeria

2013-01-01

Since the 1970s, various types of ceramic, glass and glass–ceramic materials have been proposed and used to replace damaged bone in many clinical applications. Among them, hydroxyapatite (HA) has been successfully employed thanks to its excellent biocompatibility. On the other hand, the bioactivity of HA and its reactivity with bone can be improved through the addition of proper amounts of bioactive glasses, thus obtaining HA-based composites. Unfortunately, high temperature treatments (1200 °C ÷ 1300 °C) are usually required in order to sinter these systems, causing the bioactive glass to crystallize into a glass–ceramic and hence inhibiting the bioactivity of the resulting composite. In the present study novel HA-based composites are realized and discussed. The samples can be sintered at a relatively low temperature (800 °C), thanks to the employment of a new glass (BG C a) with a reduced tendency to crystallize compared to the widely used 45S5 Bioglass®. The rich glassy phase, which can be preserved during the thermal treatment, has excellent effects in terms of in vitro bioactivity; moreover, compared to composites based on 45S5 Bioglass® having the same HA/glass proportions, the samples based on BG C a displayed an earlier response in terms of cell proliferation. - Highlights: ► New apatite/bioglass composites are proposed and sintered at low temperature. ► The samples' glassy phase is preserved and the apatite decomposition is avoided. ► The rich glassy phase in the samples results in an excellent bioactivity. ► The samples are able to support cell adhesion and proliferation. ► The samples support faster cell proliferation compared to 45S5Bioglass-composites

Analysis of the compressive behaviour of the three-dimensional printed porous titanium for dental implants using a modified cellular solid model.

Science.gov (United States)

Gagg, Graham; Ghassemieh, Elaheh; Wiria, Florencia E

2013-09-01

A set of cylindrical porous titanium test samples were produced using the three-dimensional printing and sintering method with samples sintered at 900 °C, 1000 °C, 1100 °C, 1200 °C or 1300 °C. Following compression testing, it was apparent that the stress-strain curves were similar in shape to the curves that represent cellular solids. This is despite a relative density twice as high as what is considered the threshold for defining a cellular solid. As final sintering temperature increased, the compressive behaviour developed from being elastic-brittle to elastic-plastic and while Young's modulus remained fairly constant in the region of 1.5 GPa, there was a corresponding increase in 0.2% proof stress of approximately 40-80 MPa. The cellular solid model consists of two equations that predict Young's modulus and yield or proof stress. By fitting to experimental data and consideration of porous morphology, appropriate changes to the geometry constants allow modification of the current models to predict with better accuracy the behaviour of porous materials with higher relative densities (lower porosity).

Elaboration and characterization of an iodate-substituted hydroxyapatite cement

International Nuclear Information System (INIS)

Coulon, A.; Campayo, L.; Laurencin, D.; Grandjean, A.; Cau Dit Coumes, C.; Rossignol, S.

2015-01-01

In the last decades, robust host matrices have been developed to guarantee a durable confinement of some of the most mobile radionuclides. In this work, we describe a novel method for iodine incorporation into an iodate-substituted hydroxyapatite by means of a cementation route. Such a material is obtained from a stoichiometric mixture of tetra-calcium-phosphate (TTCP)/tricalcium-phosphate (αTCP)/sodium iodate with a molar ratio 1/2/0.5. This material corresponds to an iodine incorporation content ∼6.5 wt.%. The evolution of this system during the early age (followed by calorimetric and conductimetric measurements) was compared to the same cementitious system without iodate. Results show that sodium iodate acts as a retarder that can be appropriate to control setting for an industrial application. The delay is due to the precipitation of non-cohesive intermediate phases like calcium iodate that are then totally consumed when the crystallization of hydroxyapatite occurs. At later age, a porous bulk material consisting of traces of TTCP and αTCP particles covered by needles is obtained. The composition of these needles is in agreement with that of the desired iodate-containing apatite. (authors)

Performance of laser sintered Ti-6Al-4V implants with bone-inspired porosity and micro/nanoscale surface roughness in the rabbit femur.

Science.gov (United States)

Cohen, David J; Cheng, Alice; Sahingur, Kaan; Clohessy, Ryan M; Hopkins, Louis B; Boyan, Barbara D; Schwartz, Zvi

2017-04-28

Long term success of bone-interfacing implants remains a challenge in compromised patients and in areas of low bone quality. While surface roughness at the micro/nanoscale can promote osteogenesis, macro-scale porosity is important for promoting mechanical stability of the implant over time. Currently, machining techniques permit pores to be placed throughout the implant, but the pores are generally uniform in dimension. The advent of laser sintering provides a way to design and manufacture implants with specific porosity and variable dimensions at high resolution. This approach enables production of metal implants that mimic complex geometries found in biology. In this study, we used a rabbit femur model to compare osseointegration of laser sintered solid and porous implants. Ti-6Al-4V implants were laser sintered in a clinically relevant size and shape. One set of implants had a novel porosity based on human trabecular bone; both sets had grit-blasted/acid-etched surfaces. After characterization, implants were inserted transaxially into rabbit femora; mechanical testing, micro-computed tomography (microCT) and histomorphometry were conducted 10 weeks post-operatively. There were no differences in pull-out strength or bone-to-implant contact. However, both microCT and histomorphometry showed significantly higher new bone volume for porous compared to solid implants. Bone growth was observed into porous implant pores, especially near apical portions of the implant interfacing with cortical bone. These results show that laser sintered Ti-6Al-4V implants with micro/nanoscale surface roughness and trabecular bone-inspired porosity promote bone growth and may be used as a superior alternative to solid implants for bone-interfacing implants.

Behavior of porous beryllium under thermomechanical loading. Part 6. Effect of pressure on the microstructure of plasma-sprayed beryllium

International Nuclear Information System (INIS)

Hanafee, J.E.; Snell, E.O.

1975-01-01

The effects of pressure and specimen preparation on the microstructure of two grades of porous plasma-sprayed beryllium were determined. One grade, P-1, was sintered after spraying while the other grade, P-10, was tested in the as-sprayed condition. the principal microstructural characteristics studied were grain size: grain morphology, and void distribution and size. It was found that machining can readily cause a significant dense surface layer on the porous beryllium specimens, and that the dense surface layer can be removed by etching. There was substantial difference in microstructure between the P-1 sintered and P-10 unsintered specimens both before and after being subjected to shock waves and static compression. (U.S.)

Development of carbon nanotube-reinforced hydroxyapatite bioceramics

International Nuclear Information System (INIS)

Kealley, Catherine; Elcombe, Margaret; Riessen, Arie van; Ben-Nissan, Besim

2006-01-01

This paper reports development of a production method to create a composite material that is biocompatible, which will have high mechanical strength and resilience, and be able to withstand exposure to the physiological environment. The chemical precipitation conditions necessary for the production of single-phase synthetic hydroxyapatite (HAp) and a HAp and carbon nanotube (CNT) composite material have been optimised. Neutron diffraction patterns collected before and after sintering show that the nanotubes have remained intact within the structure, while most of the remaining soot has burnt off. Small-angle neutron scattering, in conjunction with scanning electron microscopy (SEM), also shows preservation of the CNTs. Hot isostatically pressed samples showed excellent densification. Neutron diffraction data has enabled the positions of the hydroxide bonds to be determined, and shown that the addition of the CNTs has had no effect on the structural parameters of the HAp phase, with the exception of a slight reduction in the unit cell parameter a

Development of carbon nanotube-reinforced hydroxyapatite bioceramics

Energy Technology Data Exchange (ETDEWEB)

Kealley, Catherine [Department of Chemistry, Materials and Forensic Science, University of Technology, Sydney, P.O. Box 123, Broadway, NSW (Australia); Elcombe, Margaret [Bragg Institute, Australian Nuclear Science and Technology Organisation, PMB 1, Menai, NSW (Australia); Riessen, Arie van [Materials Research Group, Curtin University of Technology, GPO Box U1987, Perth, WA (Australia); Ben-Nissan, Besim [Department of Chemistry, Materials and Forensic Science, University of Technology, Sydney, P.O. Box 123, Broadway, NSW (Australia)]. E-mail: Besim.Ben-Nissan@uts.edu.au

2006-11-15

This paper reports development of a production method to create a composite material that is biocompatible, which will have high mechanical strength and resilience, and be able to withstand exposure to the physiological environment. The chemical precipitation conditions necessary for the production of single-phase synthetic hydroxyapatite (HAp) and a HAp and carbon nanotube (CNT) composite material have been optimised. Neutron diffraction patterns collected before and after sintering show that the nanotubes have remained intact within the structure, while most of the remaining soot has burnt off. Small-angle neutron scattering, in conjunction with scanning electron microscopy (SEM), also shows preservation of the CNTs. Hot isostatically pressed samples showed excellent densification. Neutron diffraction data has enabled the positions of the hydroxide bonds to be determined, and shown that the addition of the CNTs has had no effect on the structural parameters of the HAp phase, with the exception of a slight reduction in the unit cell parameter a.

Histological and biomechanical analysis of porous additive manufactured implants made by direct metal laser sintering: a pilot study in sheep.

Science.gov (United States)

Stübinger, Stefan; Mosch, Isabel; Robotti, Pierfrancesco; Sidler, Michéle; Klein, Karina; Ferguson, Stephen J; von Rechenberg, Brigitte

2013-10-01

It was the aim of this study to analyze osseointegrative properties of porous additive manufactured titanium implants made by direct metal laser sintering in a sheep model after an implantation period of 2 and 8 weeks. Three different types of implants were placed in the pelvis of six sheep. In each sheep were placed three standard machined (M), three sandblasted and etched (SE), and three porous additive manufactured (AM) implants. Of these three implants (one per type) were examined histologically and six implants were tested biomechanically. Additionally a semiquantitative histomorphometrical and qualitative fluorescent microscopic analysis were performed. After 2 and 8 weeks bone-to-implant-contact (BIC) values of the AM surface (2w: 20.49% ± 5.18%; 8w: 43.91% ± 9.69%) revealed no statistical significant differences in comparison to the M (2w: 20.33% ± 11.50%; 8w: 25.33% ± 4.61%) and SE (2w: 43.67 ± 12.22%; 8w: 53.33 ± 8.96%) surfaces. AM surface showed the highest increase of the BIC between the two observation time points. Considering the same implantation period histomorphometry and fluorescent labelling disclosed no significant differences in the bone surrounding the three implants groups. In contrast Removal-torque-test showed a significant improve in fixation strength (P ≤ 0.001) for the AM (1891.82 ± 308, 44 Nmm) surface after eight weeks in comparison to the M (198.93±88,04 Nmm) and SE (730.08 ± 151,89 Nmm) surfaces. All three surfaces (M, SE, and AM) showed sound osseointegration. AM implants may offer a possible treatment option in clinics for patients with compromised bone situations. Copyright © 2013 Wiley Periodicals, Inc., a Wiley Company.

Analysis of key factors influencing the evaporation performances of an oriented linear cutting copper fiber sintered felt

Science.gov (United States)

Pan, Minqiang; Zhong, Yujian

2018-01-01

Porous structure can effectively enhance the heat transfer efficiency. A kind of micro vaporizer using the oriented linear cutting copper fiber sintered felt is proposed in this work. Multiple long cutting copper fibers are firstly fabricated with a multi-tooth tool and then sintered together in parallel to form uniform thickness metal fiber sintered felts that provided a characteristic of oriented microchannels. The temperature rise response and thermal conversion efficiency are experimentally investigated to evaluate the influences of porosity, surface structure, feed flow rate and input power on the evaporation characteristics. It is indicated that the temperature rise response of water is mainly affected by input power and feed flow rate. High input power and low feed flow rate present better temperature rise response of water. Porosity rather than surface structure plays an important role in the temperature rise response of water at a relatively high input power. The thermal conversion efficiency is dominated by the input power and surface structure. The oriented linear cutting copper fiber sintered felts for three kinds of porosities show better thermal conversion efficiency than that of the oriented linear copper wire sintered felt when the input power is less than 115 W. All the sintered felts have almost the same performance of thermal conversion at a high input power.

Influences of the steam sterilization on the properties of calcium phosphate porous bioceramics.

Science.gov (United States)

Li, Xiangfeng; Guo, Bo; Xiao, Yumei; Yuan, Tun; Fan, Yujiang; Zhang, Xingdong

2016-01-01

The influences of steam sterilization on the physicochemical properties of calcium phosphate (Ca-P) porous bioceramics, including β-tricalcium phosphate (β-TCP), biphasic calcium phosphate (BCP) and hydroxyapatite (HA) are investigated. After being steam sterilized in an autoclave (121 °C for 40 min), the porous bioceramics are dried and characterized. The steam sterilization has no obvious effects on the phase composition, thermal stability, pH value and dissolubility of β-TCP porous bioceramic, but changes its morphology and mechanical strength. Meanwhile, the steam sterilization leads to the significant changes of the morphology, phase composition, pH value and dissolubility of BCP porous bioceramic. The increase of dissolubility and mechanical strength, the decrease of pH value of the immersed solution and partial oriented growth of crystals are also observed in HA porous bioceramic after steam sterilization. These results indicate that the steam sterilization can result in different influences on the physicochemical properties of β-TCP, BCP and HA porous bioceramics, thus the application of the steam sterilization on the three kinds of Ca-P porous bioceramics should be considered carefully based on the above changed properties.

Human bone ingrowth into a porous tantalum acetabular cup

Directory of Open Access Journals (Sweden)

Gregory N. Haidemenopoulos

2017-11-01

Full Text Available Porous Tantalum is increasingly used as a structural scaffold in orthopaedic applications. Information on the mechanisms of human bone ingrowth into trabecular metal implants is rather limited. In this work we have studied, qualitatively, human bone ingrowth into a retrieved porous tantalum monoblock acetabular cup using optical microscopy, scanning electron microscopy and energy dispersive X-ray analysis. According to the results and taking into account the short operational life (4 years of the implant, bone ingrowth on the acetabular cup took place in the first two-rows of porous tantalum cells to an estimated depth of 1.5 to 2 mm. The bone material, grown inside the first raw of cells, had almost identical composition with the attached bone on the cup surface, as verified by the same Ca:P ratio. Bone ingrowth has been a gradual process starting with Ca deposition on the tantalum struts, followed by bone formation into the tantalum cells, with gradual densification of the bone tissue into hydroxyapatite. A critical step in this process has been the attachment of bone material to the tantalum struts following the topology of the porous tantalum scaffold. These results provide insight to the human bone ingrowth process into porous tantalum implants.

Hydroxyapatite-diamondlike carbon nanocomposite films

International Nuclear Information System (INIS)

Narayan, Roger J.

2005-01-01

Hydroxyapatite is a bioactive ceramic that mimics the mineral composition of natural bone. Conventional plasma-sprayed hydroxyapatite coatings demonstrate poor adhesion and poor mechanical integrity. We have developed hydroxyapatite-diamondlike carbon bilayer film. The diamondlike carbon interlayer serves to prevent metal ion release and improve adhesion of the hydroxyapatite film. These films were characterized using X-ray photoelectron spectroscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Raman spectroscopy, nanoindentation, and microscratch adhesion testing. Based on the results of this study, hydroxyapatite-diamondlike carbon bilayers demonstrate promise for use in several orthopedic implants

Hydroxyapatite-diamondlike carbon nanocomposite films

Energy Technology Data Exchange (ETDEWEB)

Narayan, Roger J. [School of Materials Science and Engineering, Georgia Institute of Technology, Atlanta, GA 30332-0245 (United States)]. E-mail: roger.narayan@mse.gatech.edu

2005-05-15

Hydroxyapatite is a bioactive ceramic that mimics the mineral composition of natural bone. Conventional plasma-sprayed hydroxyapatite coatings demonstrate poor adhesion and poor mechanical integrity. We have developed hydroxyapatite-diamondlike carbon bilayer film. The diamondlike carbon interlayer serves to prevent metal ion release and improve adhesion of the hydroxyapatite film. These films were characterized using X-ray photoelectron spectroscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Raman spectroscopy, nanoindentation, and microscratch adhesion testing. Based on the results of this study, hydroxyapatite-diamondlike carbon bilayers demonstrate promise for use in several orthopedic implants.

Effect of nano-hydroxyapatite reinforcement in mechanically alloyed NiTi composites for biomedical implant

International Nuclear Information System (INIS)

Akmal, Muhammad; Raza, Ahmad; Khan, Muhammad Mudasser; Khan, M. Imran; Hussain, Muhammad Asif

2016-01-01

Equi-atomic NiTi alloy composites reinforced with 0, 2, 4 and 6 vol.% nano-hydroxyapatite (HA) were successfully synthesized using pressureless sintering. Pure Ni and Ti elements were ball milled for 10 h in order to produce a mechanically alloyed equi-atomic NiTi alloy (MA-NiTi). Mechanically alloyed NiTi and HA powders were blended, compacted and then sintered for 3 h at 1325 K. The sintered density varied inversely with volume percent of HA reinforcement. The X-Ray diffraction spectra and SEM images showed the formation of multiple phases like NiTi, NiTi 2 , Ni 3 Ti, and Ni 4 Ti 3 . The back scattered-SEM image analysis confirmed the presence of Ni-rich and Ti-rich phases with increasing HA content. The 6 vol.% HA reinforced composite showed Ni 3 Ti as the major phase having the highest hardness value which can be attributed to the presence of relatively harder phases along with higher HA content as a reinforcement. The composite of MA-NiTi with 2 vol.% HA manifested the most desirable results in the form of better sintering density mainly due to the minute decomposition of NiTi into other phases. Therefore, the 2 vol.% reinforced MA-NiTi composite can be exploited as a novel material for manufacturing biomedical implants. - Highlights: • NiTi-HA composites were synthesized using powder metallurgy route. • New phases such as NiTi 2 , Ni 3 Ti and Ni 4 Ti 3 were observed for sintered composites. • Mechanical properties enhanced with the increasing content of HA and new phases. • No martensitic transformation was observed for all composites by DSC analysis. • 2 vol.% HA composite is a novel candidate for biomedical implants.

Effect of nano-hydroxyapatite reinforcement in mechanically alloyed NiTi composites for biomedical implant

Energy Technology Data Exchange (ETDEWEB)

Akmal, Muhammad, E-mail: muhammad.akmal@giki.edu.pk [Faculty of Materials and Chemical Engineering, GIK Institute of Engineering Sciences and Technology, Topi 23640 (Pakistan); Raza, Ahmad, E-mail: ahmadrazac@yahoo.com [Faculty of Materials and Chemical Engineering, GIK Institute of Engineering Sciences and Technology, Topi 23640 (Pakistan); Khan, Muhammad Mudasser; Khan, M. Imran [Faculty of Materials and Chemical Engineering, GIK Institute of Engineering Sciences and Technology, Topi 23640 (Pakistan); Hussain, Muhammad Asif [Department of Chemical Engineering, Kangwon National University, Samcheok, 25913 (Korea, Republic of)

2016-11-01

Equi-atomic NiTi alloy composites reinforced with 0, 2, 4 and 6 vol.% nano-hydroxyapatite (HA) were successfully synthesized using pressureless sintering. Pure Ni and Ti elements were ball milled for 10 h in order to produce a mechanically alloyed equi-atomic NiTi alloy (MA-NiTi). Mechanically alloyed NiTi and HA powders were blended, compacted and then sintered for 3 h at 1325 K. The sintered density varied inversely with volume percent of HA reinforcement. The X-Ray diffraction spectra and SEM images showed the formation of multiple phases like NiTi, NiTi{sub 2}, Ni{sub 3}Ti, and Ni{sub 4}Ti{sub 3}. The back scattered-SEM image analysis confirmed the presence of Ni-rich and Ti-rich phases with increasing HA content. The 6 vol.% HA reinforced composite showed Ni{sub 3}Ti as the major phase having the highest hardness value which can be attributed to the presence of relatively harder phases along with higher HA content as a reinforcement. The composite of MA-NiTi with 2 vol.% HA manifested the most desirable results in the form of better sintering density mainly due to the minute decomposition of NiTi into other phases. Therefore, the 2 vol.% reinforced MA-NiTi composite can be exploited as a novel material for manufacturing biomedical implants. - Highlights: • NiTi-HA composites were synthesized using powder metallurgy route. • New phases such as NiTi{sub 2}, Ni{sub 3}Ti and Ni{sub 4}Ti{sub 3} were observed for sintered composites. • Mechanical properties enhanced with the increasing content of HA and new phases. • No martensitic transformation was observed for all composites by DSC analysis. • 2 vol.% HA composite is a novel candidate for biomedical implants.

Formation of nano-hydroxyapatite crystal in situ in chitosan-pectin polyelectrolyte complex network

International Nuclear Information System (INIS)

Li Junjie; Zhu Dunwan; Yin Jianwei; Liu Yuxi; Yao Fanglian; Yao Kangde

2010-01-01

Hydroxyapatite (HA)/polysaccharide composites have been widely used in bone tissue engineering due to their chemical similarity to natural bone. Polymer matrix-mediated synthesis of nano-hydroxyapatite is one of the simplest models for biomimetic. In this article, the nano-hydroxyapatite/chitosan-pectin (nHCP) composites were prepared through in situ mineralization of hydroxyapatite in chitosan-pectin polyelectrolyte complex (PEC) network. The formation processes of nHCP were investigated by X-ray diffraction (XRD) analysis. The interactions between nHA crystal and chitosan-pectin PEC networks were studied using Fourier Transform Infrared Spectroscopy (FTIR) and Differential Scanning Calorimetry (DSC). The morphology and structure of nHA crystal were characterized by XRD and Transmission Electron Microscope (TEM). Results suggested that the interfacial interactions between nano-hydroxyapatite crystal and chitosan-pectin PEC network assist the site specific nucleation and growth of nHA nanoparticles. The nHA crystals grow along the c-axis. In this process, pH value is the main factor to control the nucleation and growth of nHA crystal in chitosan-pectin PEC networks, because both the interactions' strength between nHA crystal and chitosan-pectin and diffusion rate of inorganic ions depend on the pH value of the reaction system. Apart from the pH value, the chitosan/pectin ratio and [Ca 2+ ] also take important effects on the formation of nHA crystal. An effective way to control the size of nHA crystal is to adjust the content of pectin and [Ca 2+ ]. It is interesting that the Zeta potential of nHCP composites is about - 30 mV when the chitosan/pectin ratio ≤ 1:1, and the dispersion solution of nHCP composites has higher stability, which provides the possibility to prepare 3D porous scaffolds with nHCP for bone tissue engineering.

Formation of nano-hydroxyapatite crystal in situ in chitosan-pectin polyelectrolyte complex network

Energy Technology Data Exchange (ETDEWEB)

Li Junjie [Department of Polymer Science and Key Laboratory of Systems Bioengineering of Ministry of Education, School of Chemical Engineering and Technology, Tianjin University, Tianjin, 300072 (China); Research Institute of Polymeric Materials, Tianjin University, Tianjin, 300072 (China); Zhu Dunwan [Institute of Biomedical Engineering, Chinese Academy of Medical Sciences and Peking Union Medical College, Tianjin, 300072 (China); Yin Jianwei; Liu Yuxi [Department of Polymer Science and Key Laboratory of Systems Bioengineering of Ministry of Education, School of Chemical Engineering and Technology, Tianjin University, Tianjin, 300072 (China); Yao Fanglian, E-mail: yaofanglian@tju.edu.cn [Department of Polymer Science and Key Laboratory of Systems Bioengineering of Ministry of Education, School of Chemical Engineering and Technology, Tianjin University, Tianjin, 300072 (China); Yao Kangde [Research Institute of Polymeric Materials, Tianjin University, Tianjin, 300072 (China)

2010-07-20

Hydroxyapatite (HA)/polysaccharide composites have been widely used in bone tissue engineering due to their chemical similarity to natural bone. Polymer matrix-mediated synthesis of nano-hydroxyapatite is one of the simplest models for biomimetic. In this article, the nano-hydroxyapatite/chitosan-pectin (nHCP) composites were prepared through in situ mineralization of hydroxyapatite in chitosan-pectin polyelectrolyte complex (PEC) network. The formation processes of nHCP were investigated by X-ray diffraction (XRD) analysis. The interactions between nHA crystal and chitosan-pectin PEC networks were studied using Fourier Transform Infrared Spectroscopy (FTIR) and Differential Scanning Calorimetry (DSC). The morphology and structure of nHA crystal were characterized by XRD and Transmission Electron Microscope (TEM). Results suggested that the interfacial interactions between nano-hydroxyapatite crystal and chitosan-pectin PEC network assist the site specific nucleation and growth of nHA nanoparticles. The nHA crystals grow along the c-axis. In this process, pH value is the main factor to control the nucleation and growth of nHA crystal in chitosan-pectin PEC networks, because both the interactions' strength between nHA crystal and chitosan-pectin and diffusion rate of inorganic ions depend on the pH value of the reaction system. Apart from the pH value, the chitosan/pectin ratio and [Ca{sup 2+}] also take important effects on the formation of nHA crystal. An effective way to control the size of nHA crystal is to adjust the content of pectin and [Ca{sup 2+}]. It is interesting that the Zeta potential of nHCP composites is about - 30 mV when the chitosan/pectin ratio {<=} 1:1, and the dispersion solution of nHCP composites has higher stability, which provides the possibility to prepare 3D porous scaffolds with nHCP for bone tissue engineering.

Fabrication of a Ti porous microneedle array by metal injection molding for transdermal drug delivery.

Science.gov (United States)

Li, Jiyu; Liu, Bin; Zhou, Yingying; Chen, Zhipeng; Jiang, Lelun; Yuan, Wei; Liang, Liang

2017-01-01

Microneedle arrays (MA) have been extensively investigated in recent decades for transdermal drug delivery due to their pain-free delivery, minimal skin trauma, and reduced risk of infection. However, porous MA received relatively less attention due to their complex fabrication process and ease of fracturing. Here, we present a titanium porous microneedle array (TPMA) fabricated by modified metal injection molding (MIM) technology. The sintering process is simple and suitable for mass production. TPMA was sintered at a sintering temperature of 1250°C for 2 h. The porosity of TPMA was approximately 30.1% and its average pore diameter was about 1.3 μm. The elements distributed on the surface of TPMA were only Ti and O, which may guarantee the biocompatibility of TPMA. TPMA could easily penetrate the skin of a human forearm without fracture. TPMA could diffuse dry Rhodamine B stored in micropores into rabbit skin. The cumulative permeated flux of calcein across TPMA with punctured skin was 27 times greater than that across intact skin. Thus, TPMA can continually and efficiently deliver a liquid drug through open micropores in skin.

Fabrication of a Ti porous microneedle array by metal injection molding for transdermal drug delivery.

Directory of Open Access Journals (Sweden)

Jiyu Li

Full Text Available Microneedle arrays (MA have been extensively investigated in recent decades for transdermal drug delivery due to their pain-free delivery, minimal skin trauma, and reduced risk of infection. However, porous MA received relatively less attention due to their complex fabrication process and ease of fracturing. Here, we present a titanium porous microneedle array (TPMA fabricated by modified metal injection molding (MIM technology. The sintering process is simple and suitable for mass production. TPMA was sintered at a sintering temperature of 1250°C for 2 h. The porosity of TPMA was approximately 30.1% and its average pore diameter was about 1.3 μm. The elements distributed on the surface of TPMA were only Ti and O, which may guarantee the biocompatibility of TPMA. TPMA could easily penetrate the skin of a human forearm without fracture. TPMA could diffuse dry Rhodamine B stored in micropores into rabbit skin. The cumulative permeated flux of calcein across TPMA with punctured skin was 27 times greater than that across intact skin. Thus, TPMA can continually and efficiently deliver a liquid drug through open micropores in skin.

Design and Fabrication of Porous Yttria-Stabilized Zirconia Ceramics for Hot Gas Filtration Applications

Science.gov (United States)

Shahini, Shayan

Hot gas filtration has received growing attention in a variety of applications over the past few years. Yttria-stabilized zirconia (YSZ) is a promising candidate for such an application. In this study, we fabricated disk-type porous YSZ filters using the pore forming procedure, in which poly methyl methacrylate (PMMA) was used as the pore-forming agent. After fabricating the pellets, we characterized them to determine their potential for application as gas filters. We investigated the effect of sintering temperature, polymer particle size, and polymer-to-ceramic ratio on the porosity, pore size, gas permeability, and Vickers hardness of the sintered pellets. Furthermore, we designed two sets of experiments to investigate the robustness of the fabricated pellets--i.e., cyclic heating/cooling and high temperature exposure. This study ushers in a robust technique to fabricate such porous ceramics, which have the potential to be utilized in hot gas filtration.

Porous stainless steel for biomedical applications

Directory of Open Access Journals (Sweden)

Sabrina de Fátima Ferreira Mariotto

2011-01-01

Full Text Available Porous 316L austenitic stainless steel was synthesized by powder metallurgy with relative density of 0.50 and 0.30 using 15 and 30 wt. (% respectively of ammonium carbonate and ammonium bicarbonate as foaming agents. The powders were mixed in a planetary ball mill at 60 rpm for 10 minutes. The samples were uniaxially pressed at 287 MPa and subsequently vacuum heat treated in two stages, the first one at 200 ºC for 5 hours to decompose the carbonate and the second one at 1150 ºC for 2 hours to sinter the steel. The sintered samples had a close porous structure and a multimodal pore size distribution that varied with the foaming agent and its concentration. The samples obtained by addition of 30 wt. (% of foaming agents had a more homogeneous porous structure than that obtained with 15 wt. (%. The MTT cytotoxicity test (3-[4,5-dimethylthiazol]-2,5-diphenyltetrazolium bromide was used to evaluate the mitochondrial activity of L929 cells with samples for periods of 24, 48, and 72 hours. The cytotoxicity test showed that the steel foams were not toxic to fibroblast culture. The sample with the best cellular growth, therefore the most suitable for biomedical applications among those studied in this work, was produced with 30 wt. (% ammonium carbonate. In this sample, cell development was observed after 48 hours of incubation, and there was adhesion and spreading on the material after 72 hours. Electrochemical experiments using a chloride-containing medium were performed on steel foams and compared to massive steel. The massive steel had a better corrosion performance than the foams as the porosity contributes to increase the surface area exposed to the corrosive medium.

Preparation and Characteristics of Porous Ceramics by a foaming Technology at Low Temperature

Science.gov (United States)

Zhang, H. Q.; Wang, S. P.; Wen, J.; Wu, N.; Xu, S. H.

2017-12-01

Recycling and converting coal gangue and red mud into porous ceramics with good performance is a feasible disposal route. In this present work, porous foam ceramics was prepared using coal gangue and red mud as main raw materials at low sintering temperature, The amount of coal gangue and red mud were up to 70 wt%. To regulate the forming and sintering performance of the product, quartz sands and clay material were added to the formula. The green body was formed by a foaming technology using aluminum powders as foaming agents at room temperature. After foamed, the specimens were dried at 60-80 °C, and then calcined at 1060°C. Effects of concentration of NaOH and amount of aluminum powders on the phase, mechanical properties and microstructure were investigated here. Such study is expected to provide a new utilization route of the coal gangue and red mud, and brings both intensive environmental and economic benefits.

Behavior of porous tungsten under shock compression at room temperature

International Nuclear Information System (INIS)

Dandekar, D.P.; Lamothe, R.M.

1977-01-01

This work reports the results of room-temperature shock-compression experiments on porous tungsten. The porous tungsten was fabricated by sintering 1-μm tungsten particles. The initial density of the material was 15290 kg/m 3 . Around 97% of the pores in the material were interconnected. The main features of the results are as follows: (1) porous tungsten behaves as a linear elastic material to 1.43 GPa; (2) the shock wave following the elastic precursor is unstable in the material in the stress range 1.43--2.7 GPa; (3) a stable two-wave structure is established at and above 6.4 GPa; (4) the response of porous tungsten is accurately described by the Mie-Grueneisen equation of state at stresses above 4.9 GPa, the stress at which the voids suffer a complete extinction in the material; (5) the deformations induced in the material due to shock compression are irreversible; (6) the recentered Hugoniot of porous tungsten becomes stiffer with the increasing magnitude of initial compressive stress