Effect of ZnO on phase emergence, microstructure and surface modifications of calcium phosphosilicate glass/glass-ceramics having iron oxide

International Nuclear Information System (INIS)

Sharma, K.; Dixit, A.; Bhattacharya, S.; Jagannath; Deo, M.N.; Kothiyal, G.P.

2010-01-01

The effect of ZnO on phase emergence and microstructure properties of glass and glass-ceramics with composition 25SiO 2 -50CaO-15P 2 O 5 -(10 - x)Fe 2 O 3 -xZnO (where x = 0, 2, 5, 7 mol%) has been studied. They have been characterized using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM). Surface modifications of these glass-ceramics in simulated body fluid have been studied using Fourier transform infrared reflection spectroscopy (FTIR), XPS and SEM. Results have shown a decrease in the fraction of non-bridging oxygen with increase in zinc oxide content. Emergence of crystalline phases in glass-ceramics at different heat treatment temperatures was studied using XRD. When glass is heat treated at 800 deg. C calcium phosphate, hematite and magnetite are developed as major phases in the glass-ceramics samples with ZnO up to 5 mol%. In addition to these, calcium silicate (Ca 3 Si 2 O 7 ) phase is also observed when glass is heat treated at 1000 deg. C. The microstructure of the glass-ceramics heat treated at 800 deg. C exhibits the formation of nano-size (40-50 nm) grains. On heat treatment at 1000 deg. C crystallites grow to above 50 nm size and more than one phase are observed in the microstructure. The formation of thin flake-like structure with coarse particles is observed at high zinc oxide concentration (x = 7 mol%). In vitro studies have shown the surface modifications and formation of Ca-P-rich layer on the glass-ceramics when immersed in simulated body fluids (SBF) for different durations. The bioactive response was found to depend on ZnO content.

Investigating the effect of SiO2-TiO 2-CaO-Na 2O-ZnO bioactive glass doped hydroxyapatite: characterisation and structural evaluation.

Science.gov (United States)

Yatongchai, Chokchai; Wren, Anthony W; Curran, Declan J; Hampshire, Stuart; Towler, Mark R

2014-07-01

The effects of increasing bioactive glass additions, SiO2-TiO2-CaO-Na2O-ZnO up to 25 wt% in increments of 5 wt%, on the physical and mechanical properties of hydroxyapatite (HA) sintered at 900, 1000, 1100 and 1200 °C for 2 h was investigated. Increasing both the glass content and the temperature resulted in increased HA decomposition. This resulted in the formation of a number of bioactive phases. However the presence of the liquidus glass phase did not result in increased densification levels. At 1000 and 1100 °C the additions of 5 wt% glass resulted in a decrease in density which never recovered with increasing glass content. At 1200 °C a cyclic pattern resulted from increasing glass content. There was no direct relationship between strength and density with all samples experiencing no change or a decrease in strength with increasing glass content. Weibull statistics displayed no pattern with increasing glass content.

CoO-doped MgO-Al2O3-SiO2-colored transparent glass-ceramics with high crystallinity

Science.gov (United States)

Tang, Wufu; Zhang, Qian; Luo, Zhiwei; Yu, Jingbo; Gao, Xianglong; Li, Yunxing; Lu, Anxian

2018-02-01

To obtain CoO-doped MgO-Al2O3-SiO2 (MAS)-colored transparent glass-ceramics with high crystallinity, the glass with the composition 21MgO-21Al2O3-54SiO2-4B2O3-0.2CoO (in mol %) was prepared by conventional melt quenching technique and subsequently thermal treated at several temperatures. The crystallization behavior of the glass, the precipitated crystalline phases and crystallinity were analyzed by X-ray diffraction (XRD). The microstructure of the glass-ceramics was characterized by field emission scanning electron microscopy (FSEM). The transmittance of glass-ceramic was measured by UV spectrophotometer. The results show that a large amount of α-cordierite (indianite) with nano-size was precipitated from the glass matrix after treatment at 1020 °C for 3 h. The crystallinity of the transparent glass-ceramic reached up to 97%. Meanwhile, the transmittance of the glass-ceramic was 74% at 400 nm with a complex absorption band from 450 nm to 700 nm. In addition, this colored transparent glass-ceramic possessed lower density (2.469 g/cm3), lower thermal expansion coefficient (1.822 × 10-6 /℃), higher Vickers hardness (9.1 GPa) and higher bending strength (198 MPa) than parent glass.

Bending strength of glass-ceramics based on 3CaO.P{sub 2}O{sub 5}-SiO{sub 2}-MgO glass system; Resistencia a fratura de vitroceramicos do sistema 3CaO.P{sub 2}O{sub 5}-SiO{sub 2}-MgO

Energy Technology Data Exchange (ETDEWEB)

Daguano, J.K.M.F.; Suzuki, P.A.; Santos, C. [Universidade de Sao Paulo (EEL/USP), Lorena, SP (Brazil). Escola de Engenharia de Lorena. Dept. de Engenharia de Materiais; Fernandes, M.H.V. [Universidade de Aveiro (UAveiro/CECICO), Aveiro (Portugal). Centro de Investigacao em Materiais Ceramicos e Compositos. Dept. de Engenharia Ceramica e do Vidro; Elias, C.N. [Instituto Militar de Engenharia (IME), Rio de Janeiro, RJ (Brazil). Lab. de Biomateriais

2009-07-01

In this work, the Modulus of Rupture of bioactive glass-ceramic based on 3CaO.P{sub 2}O{sub 5}-SiO{sub 2}-MgO system was investigated, aiming its use in bone-restorations. The mechanical property was correlated with microstructural and crystallographic features of this material. High-purity starting-powders, CaCO{sub 3}, SiO{sub 2}, MgO, Ca (H{sub 2}PO{sub 4}).H{sub 2}O, were used in this study. The powders were mixed in a stoichiometric ratio, using planetary ball-mill. The suspensions were dried, sieved and melted at 1600 deg C, for 4h. The casting ones were cooled quickly until annealing temperature 700 deg C, in which remained for 2h, with controlled cooling-rate until ambient temperature. Bulks of glass were heat-treated with temperatures varying between 700 deg C and 1100 deg C, for 4h, being after that, cooled at 3 deg C/min. Bioactive glass and glass-ceramic were characterized by HRXRD (high resolution X-ray diffraction), where whitlockite was main phase. The microstructure was analyzed by scanning electronic microscopy. Modulus of Rupture was determined by four-point bending testing using specimens of 1.5 x 2 x 25 mm and glasses presented strength near to 70MPa, while glass ceramics treated at 975 deg C-4h, presented bending strength of 120MPa. (author)

The effect on phase separation of the oxidation state of molybdenum in a Na2O-B2O3-SiO2 glass

International Nuclear Information System (INIS)

Kawamoto, Y.; Clemens, K.; Tomozawa, M.; Warden, J.T.

1981-01-01

The effect of oxidation state on phase separation was studied for 13Na 2 O, 49B 2 O 3 , 38SiO 2 (mol%) glasses containing 1 mol% Mo oxide. The glasses were melted under various conditions to vary the oxidation states of Mo ions. The oxidation states of Mo ions were determined by chemical analysis and ESR. The crystallisation tendency, the immiscibility temperature, and the phase separation morphology of the glasses were examined by DTA, x-ray diffraction, opalescence method, and replica electron microscopy. Glasses containing Mo 4+ ions have a great tendency to precipitate MoO 2 crystals. The immiscibility temperature of glass goes through a minimum when the oxidation states of Mo ions are changed. It was suggested that there is an optimum oxidation state to prevent crystallisation and to suppress the phase separation tendency of this system. (author)

Microstructure and mechanical properties of low-activation glass-ceramic joining and coating for SiC/SiC composites

International Nuclear Information System (INIS)

Katoh, Yutai; Kotani, M.; Kohyama, A.; Montorsi, M.; Salvo, M.; Ferraris, M.

2000-01-01

Calcia-alumina (CA) glass-ceramic was studied as a candidate low-activation joining and sealing material for SiC/SiC components for fusion blanket and diverter structures, in terms of microstructural stability and mechanical properties. The CA glass-ceramic joining and seal coating were applied to the Hi-Nicalon TM SiC fiber-reinforced SiC matrix composites in which the matrix had been formed through chemical vapor infiltration and polymer impregnation and pyrolysis methods. Microstructural characterization was carried out for the joined and coated materials by optical and scanning electron microscopy (SEM). The mechanical property of the joint was evaluated through a shear test on sandwich joints. The average shear strength of the joined structures was 28 MPa at room temperature. Fractography revealed that the fracture occurred in the glass phase and the shear strength may be improved by reduction of the glass fraction

Preparation and spectral analysis of a new Tb3+-doped CaO-MgO-SiO2 glass ceramics

International Nuclear Information System (INIS)

Cheng Jinshu; Tian Peijing; Zheng Weihong; Xie Jun; Chen Zhenxia

2009-01-01

Tb 3+ -doped CaO-MgO-SiO 2 glass ceramics have been prepared and characterized. The structure and optical properties of the glass ceramics were studied by XRD, SEM, Raman, and fluorescence spectra. The precipitated crystalline phase in the glass ceramics was columnar CaMgSi 2 O 6 . Raman spectra showed the introduction of rare earth nearly had no influence on the sample structure. Fluorescence measurements showed that Tb 3+ ions entered into the diopside crystalline phase and induced a much stronger emission in the glass ceramics than that in the corresponding glass. With increase of Tb 3+ content and the introduction of Gd 3+ , the fluorescence intensity of the luminescent glass ceramic increased

Percolative ionic conduction in the LiAlSiO4 glass-ceramic system

International Nuclear Information System (INIS)

Biefeld, R.M.; Pike, G.E.; Johnson, R.T. Jr.

1977-01-01

The effect f crystallinity on the lithium ion conductivity in LiAlSiO 4 glass and glass-ceramic solid electrolytes has been determined. The ionic conductivity is thermally activated with an activation energy and pre-exponential factor that change in a marked and nonsimple manner as the volume fraction of crystallinity changes. These results are explained by using a continuum percolation model (effective-medium approximation) which assumes that ionic conduction in the glass-ceramic is almost entirely within the glass phase until the crystalline volume fraction rises above approx. 55%. The LiAlSiO 4 system would seem to be nearly ideal for application of percolation theory since the crystalline phase, β eucryptite, has nearly the same composition as the glass phase. Hence, as the crystallite volume fraction increases in the glass ceramic, the residual glass composition and conductivity remain the same. This is the first application of percolation theory to ionic transport in glass-ceramics and excellent agreement is obtained between theory and experiment for the LiAlSiO 4 system

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.)

A Novel SOFC/SOEC Sealing Glass with a Low SiO2 Content and a High Thermal Expansion Coefficient  

DEFF Research Database (Denmark)

Kiebach, Wolff-Ragnar; Agersted, Karsten; Zielke, Philipp

2017-01-01

phase boundaries. To reduce the amount of Si emission, a low Si containing sealing glass (chemical composition: 48 mol% CaO, 19 mol% ZnO, 21 mol% B2O3 and 12 mol% SiO2) was developed at DTU. In this presentation, the results from thermal characterization, like thermal expansion coefficient, glass......Solid oxide cells require seals that can function in harsh, elevated temperature environments. In the case of solid oxide electrolysis (SOEC), also a low Si content is desired, since Si impurities from the glass sealing can be transported to the active fuel electrode and poison the Ni-YSZ triple...... transition temperature, crystallization temperature, etc., of the glass will be presented. Additionally, the crystallization behavior of the glass was analyzed by in-situ X-ray diffraction, recording temperature resolved XRD spectra from 30 °C up to 900 °C. Furthermore, the long-term stability...

Determination of ionic conductivity in the Bi-Si-O and Pb-Si-O glasses

Directory of Open Access Journals (Sweden)

Karczewski J.

2018-03-01

Full Text Available Impedance spectroscopy measurements in various gas atmospheres were carried out in order to explain the doubts about the type of carriers and the mechanism of electrical conductivity in Bi-Si-O and Pb-Si-O glasses. In bismuth silicate glass, a typical ionic conductivity with oxygen ions as charge carriers was observed. The level of electrical conductivity of the glass at 400 °C was 5 × 10-8 S·cm-1, with the activation energy of 1.3 eV and was independent of measuring atmosphere. In the case of lead silicate glasses, the conductivity changed with measuring atmosphere. Two types of charge carriers: oxygen ions and proton ions were postulated. Proton conductivity measured in wet argon at temperature 400 °C was estimated at the level of 4 × 10-8 S·cm-1 while the oxygen ions conductivity in such conditions was 78 × 10-8 S·cm-1. We suggest that both types of charge carriers are transported along the same conduction paths using oxygen defects in the glass structure.

TiO2 effect on crystallization mechanism and physical properties of nano glass-ceramics of MgO-Al2O3-SiO2 glass system.

Science.gov (United States)

Jo, Sinae; Kang, Seunggu

2013-05-01

The effect of TiO2 on the degree of crystallization, thermal properties and microstructure for MgO-Al2O3-SiO2 glass-ceramics system containing 0-13 wt% TiO2 and 0-1.5 wt% B2O3 in which the cordierite is the main phase was studied. Using Kissinger and Augis-Bennett equations, the activation energy, 510 kJ/mol and Avrami constant, 1.8 were calculated showing the surface-oriented crystallization would be preferred. The alpha-cordierite phase was generated in the glass-ceramics of containing TiO2 of 0-5.6 wt%. However, for the glass-ceramics of TiO2 content above 7 wt%, an alpha-cordierite disappeared and micro-cordierite phase was formed. The glass-ceramics of no TiO2 added had spherical crystals of few tens nanometer size spread in the matrix. As TiO2 content increased up to 5.6 wt%, a lump of dendrite was formed. In the glass-ceramics containing TiO2 7-13 wt%, in which the main phase is micro-cordierite, the dendrite crystal disappeared and a few hundred nanometer sized crystal particles hold tightly each other were generated. The thermal conductivity of glass-ceramics of both a-cordierite and micro-cordierite base decreased with TiO2 contend added. The thermal conductivity of glass-ceramics of 1.5 wt% TiO2 added was 3.4 W/mK which is 36% higher than that of glass-ceramics of no TiO2 added. The sintering temperature for 1.5 wt% TiO2 glass-ceramics was 965 degrees C which could be concluded as to apply to LTCC process for LED packaging.

EFFECT OF CaO/SiO₂ AND HEAT TREATMENT ON THE MICROSTRUCTURE OF GLASS-CERAMICS FROM BLAST FURNACE SLAG

Directory of Open Access Journals (Sweden)

Chunshai Xie

2016-05-01

Full Text Available Glass-ceramics, with molten blast furnace (BF slag as the major raw material, were prepared successfully by the melting method. The effect of the CaO/SiO₂ ratio in the molten BF slag and heat treatment on the viscosity and microstructure of glass-ceramics produced from BF slag were traced using the melt property tester, DSC, XRD and SEM. The results showed that increasing the CaO/SiO₂ ratio of BF slag caused a decrease not only in the viscosity of the BF slag at high temperature but also in the nucleation and crystallization temperature for the preparation of glass-ceramics. The content of akermanite-gehlenite increased as the CaO/SiO₂ ratio increased from 0.30 to 0.63. With increasing nucleation and crystallization temperature, the crystalline phases remain unchanged, but the crystal shape changes from granular to flaky. The optimum CaO/SiO₂ ratio was found to be 0.44, resulting in diopside as the main crystalline phase, augite as the secondary crystalline phase and a small mount of akermanite-gehlenite after appropriate heat treatment i.e. nucleation at 775°C and crystallization at 920°C.

Crack-resistant Al2O3-SiO2 glasses.

Science.gov (United States)

Rosales-Sosa, Gustavo A; Masuno, Atsunobu; Higo, Yuji; Inoue, Hiroyuki

2016-04-07

Obtaining "hard" and "crack-resistant" glasses have always been of great important in glass science and glass technology. However, in most commercial glasses both properties are not compatible. In this work, colorless and transparent xAl2O3-(100-x)SiO2 glasses (30 ≤ x ≤ 60) were fabricated by the aerodynamic levitation technique. The elastic moduli and Vickers hardness monotonically increased with an increase in the atomic packing density as the Al2O3 content increased. Although a higher atomic packing density generally enhances crack formation in conventional oxide glasses, the indentation cracking resistance increased by approximately seven times with an increase in atomic packing density in binary Al2O3-SiO2 glasses. In particular, the composition of 60Al2O3 • 40SiO2 glass, which is identical to that of mullite, has extraordinary high cracking resistance with high elastic moduli and Vickers hardness. The results indicate that there exist aluminosilicate compositions that can produce hard and damage-tolerant glasses.

Sol-Gel synthesis of MgO-SiO2 glass compositions having stable liquid-liquid immiscibility

Science.gov (United States)

Bansal, Narottam P.

1987-01-01

MgO-SiO2 glasses containing up to 15 mol % MgO, which could not have been prepared by the conventional glass melting method due to the presence of stable liquid-liquid immiscibility, were synthesized by the sol-gel technique. Clear and transparent gels were obtained from the hydrolysis and polycondensation of silicon tetraethoxide (TEOS) and magnesium nitrate hexahydrate when the water/TEOS mole ratio was four or more. The gelling time decreased with increase in magnesium content, water/TEOS ratio, and reaction temperature. Magnesium nitrate hexahydrate crystallized out of the gels containing 15 and 20 mol % MgO on slow drying. This problem was partially alleviated by drying the gels quickly at higher temperatures. Monolithic gel samples were prepared using glycerol as the drying control additive. The gels were subjected to various thermal treatments and characterized by several methods. No organic groups could be detected in the glasses after heat treatments to approx. 800 C, but trace amounts of hydroxyl groups were still present. No crystalline phase was found from X-ray diffraction in the gel samples to approx. 890 C. At higher temperatures, alpha quartz precipitated out as the crystalline phase in gels containing up to 10 mol % MgO. The overall activation energy for gel formation in 10MgO-90SiO2 (mol %) system for water/TEOS mole ratio of 7.5 was calculated to be 58.7 kJ/mol.

Crystallization behavior and properties of BaO-Al2O3-2SiO2 glass matrices

Science.gov (United States)

Drummond, Charles H., III; Bansal, Narottam P.

1990-01-01

Glass of stoichiometric celsian composition, BaO-Al2O3-SiO2, has a density of 3.39 g/cu cm, a thermal expansion coefficient of 6.6 x 10 to the -6th/C, a glass-transition temperature of 910 C, and a dilatometric softening point of 925 C. On heat treatment, only hexacelsian crystallized out on the surface, but both celsian and hexacelsian were present in the bulk. Effects of cold isostatic pressing (CIP), sintering, and hot-pressing, in the presence and absence of an additive, on the formation of the celsian phase in the glass have been studied. CIP'd samples, after appropriate heat treatments, always crystallized out as celsian, whereas presence of 5-10 wt pct of an additive was necessary for formation of celsian in sintered as well as hot-pressed specimens. Green density increased with CIP'ing pressure but had no effect on sintered density. Hot-pressing resulted in fully dense samples.

Dependence of glass-forming ability on starting compositions in Y2O3–Al2O3–SiO2 system

OpenAIRE

Yixiang Chen; Zengchao Yang; Bin He; Guanghua Liu; Jiangtao Li; Liang Wu

2011-01-01

The dependence of glass-forming ability on starting compositions in Y2O3–Al2O3–SiO2 (YAS) system has been investigated by melting experiment. Transparent YAS glasses have been prepared under the condition of furnace cooling instead of quenching. It is found that, in the YAS ternary phase diagram, the compositions on the Y3Al5O12–SiO2 line and with 52-68 mol% SiO2 have a higher glass-forming ability to produce pure glass. For the compositions with too much or less SiO2 or with Y/Al = 5/3, 1/1,...

Dependence of glass-forming ability on starting compositions in Y2O3–Al2O3–SiO2 system

Directory of Open Access Journals (Sweden)

Yixiang Chen

2011-09-01

Full Text Available The dependence of glass-forming ability on starting compositions in Y2O3–Al2O3–SiO2 (YAS system has been investigated by melting experiment. Transparent YAS glasses have been prepared under the condition of furnace cooling instead of quenching. It is found that, in the YAS ternary phase diagram, the compositions on the Y3Al5O12–SiO2 line and with 52-68 mol% SiO2 have a higher glass-forming ability to produce pure glass. For the compositions with too much or less SiO2 or with Y/Al = 5/3, 1/1, or 1/3, crystallization occurs with the formation of Y3Al5O12, Y2Si2O7, Al6Si2O13, or SiO2. The densities of the YAS glasses increase with decreasing SiO2 contents and increasing Y/Al ratios, and for the samples with Y/Al = 3/5 there is a good linear relationship between the density and SiO2 content.

Bioactivity of gel-glass powders in the CaO-SiO2 system: a comparison with ternary (CaO-P2O5-SiO2) and quaternary glasses (SiO2-CaO-P2O5-Na2O).

Science.gov (United States)

Saravanapavan, Priya; Jones, Julian R; Pryce, Russell S; Hench, Larry L

2003-07-01

Bioactive glasses react chemically with body fluids in a manner that is compatible with the repair processes of the tissues. This results in the formation of an interfacial bond between the glasses and living tissue. Bioactive glasses also stimulate bone-cell proliferation. This behavior is dependent on the chemical composition as well as the surface texture of the glasses. It has been recently reported that gel-derived monolith specimens in the binary SiO2 - CaO are bioactive over a similar molar range of SiO2 content as the previously studied ternary CaO-P2O5-SiO2 system. In this report, the preparation and bioactivity of the binary gel-glass powder with 70 mol % SiO2 is discussed and its bioactivity is compared with the melt-derived 45S5 (quaternary) Bioglass and sol-gel-derived 58S (ternary) bioactive gel-glass compositions. Dissolution kinetic parameters K(1) and K(2) were also computed based on the silicon release for all glass powders. It was shown that the simple two-component SiO2-CaO gel-glass powder is bioactive with comparable dissolution rates as the clinically used melt-derived 45S5 Bioglass powder and extensively studied sol-gel-derived 58S gel-glass powder. Copyright 2003 Wiley Periodicals, Inc.

UV-VUV laser induced phenomena in SiO2 glass

International Nuclear Information System (INIS)

Kajihara, Koichi; Ikuta, Yoshiaki; Oto, Masanori; Hirano, Masahiro; Skuja, Linards; Hosono, Hideo

2004-01-01

Creation and annihilation of point defects were studied for SiO 2 glass exposed to ultraviolet (UV) and vacuum UV (VUV) lights to improve transparency and radiation toughness of SiO 2 glass to UV-VUV laser light. Topologically disordered structure of SiO 2 glass featured by the distribution of Si-O-Si angle is a critical factor degrading transmittance near the fundamental absorption edge. Doping with terminal functional groups enhances the structural relaxation and reduces the number of strained Si-O-Si bonds by breaking up the glass network without creating the color centers. Transmittance and laser toughness of SiO 2 glass for F 2 laser is greatly improved in fluorine-doped SiO 2 glass, often referred as 'modified silica glass'. Interstitial hydrogenous species are mobile and reactive at ambient temperature, and play an important role in photochemical reactions induced by exposure to UV-VUV laser light. They terminate the dangling-bond type color centers, while enhancing the formation of the oxygen vacancies. These findings are utilized to develop a deep-UV optical fiber transmitting ArF laser photons with low radiation damage

The effect of CaO/SiO2 molar ratio of CaO-Al2O3-SiO2 glasses on their structure and reactivity in alkali activated system.

Science.gov (United States)

Kucharczyk, Sylwia; Sitarz, Maciej; Zajac, Maciej; Deja, Jan

2018-04-05

The influence of CaO/SiO 2 molar ratio of calcium aluminosilicate glasses on resulting structure and reactivity was investigated. Chemical compositions of glasses were chosen to mimic the composition of the fly ash and slag amorphous phase. Understanding the reactivity of these materials is of high importance allowing further development of the composite cements to limit the environmental footprint of cement industry. Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy were employed to examine the structure of glasses. Reactivity of the glasses was analyzed on paste samples after 1, 2, 7, 28 and 90days of curing by means of thermogravimetry (TGA), X-ray diffraction (XRD) and FTIR. Spectroscopic results emphasize dependence of the structure on the chemical composition of the glasses. The higher CaO/SiO 2 the more depolymerized the glass network is, though there is no direct correlation with the reactivity. Significant differences in reactivity is observed primarily between the glasses of peraluminous (CaO/Al 2 O 3 1). Amongst the pastes made of glasses of percalcic region a higher degree of reaction at later ages is observed for the paste containing glass of lower CaO/SiO 2 molar ratio. This is due to both degree of depolimerization and the nature of these glasses (pozzolanic and hydraulic materials). No difference of degree of reaction has been observed within the glasses of CaO/SiO 2 lower than 1. Copyright © 2018 Elsevier B.V. All rights reserved.

The effect of CaO/SiO2 molar ratio of CaO-Al2O3-SiO2 glasses on their structure and reactivity in alkali activated system

Science.gov (United States)

Kucharczyk, Sylwia; Sitarz, Maciej; Zajac, Maciej; Deja, Jan

2018-04-01

The influence of CaO/SiO2 molar ratio of calcium aluminosilicate glasses on resulting structure and reactivity was investigated. Chemical compositions of glasses were chosen to mimic the composition of the fly ash and slag amorphous phase. Understanding the reactivity of these materials is of high importance allowing further development of the composite cements to limit the environmental footprint of cement industry. Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy were employed to examine the structure of glasses. Reactivity of the glasses was analyzed on paste samples after 1, 2, 7, 28 and 90 days of curing by means of thermogravimetry (TGA), X-ray diffraction (XRD) and FTIR. Spectroscopic results emphasize dependence of the structure on the chemical composition of the glasses. The higher CaO/SiO2 the more depolymerized the glass network is, though there is no direct correlation with the reactivity. Significant differences in reactivity is observed primarily between the glasses of peraluminous (CaO/Al2O3 1). Amongst the pastes made of glasses of percalcic region a higher degree of reaction at later ages is observed for the paste containing glass of lower CaO/SiO2 molar ratio. This is due to both degree of depolimerization and the nature of these glasses (pozzolanic and hydraulic materials). No difference of degree of reaction has been observed within the glasses of CaO/SiO2 lower than 1.

Crack-resistant Al2O3–SiO2 glasses

Science.gov (United States)

Rosales-Sosa, Gustavo A.; Masuno, Atsunobu; Higo, Yuji; Inoue, Hiroyuki

2016-01-01

Obtaining “hard” and “crack-resistant” glasses have always been of great important in glass science and glass technology. However, in most commercial glasses both properties are not compatible. In this work, colorless and transparent xAl2O3–(100–x)SiO2 glasses (30 ≤ x ≤ 60) were fabricated by the aerodynamic levitation technique. The elastic moduli and Vickers hardness monotonically increased with an increase in the atomic packing density as the Al2O3 content increased. Although a higher atomic packing density generally enhances crack formation in conventional oxide glasses, the indentation cracking resistance increased by approximately seven times with an increase in atomic packing density in binary Al2O3–SiO2 glasses. In particular, the composition of 60Al2O3•40SiO2 glass, which is identical to that of mullite, has extraordinary high cracking resistance with high elastic moduli and Vickers hardness. The results indicate that there exist aluminosilicate compositions that can produce hard and damage-tolerant glasses. PMID:27053006

The crystallization behaviour and bioactivity of wollastonite glass-ceramic based on Na2O–K2O–CaO–SiO2–F glass system

Directory of Open Access Journals (Sweden)

S.M. Salman

2015-09-01

Full Text Available The study concerns about the crystallization behaviour and in vitro bioactivity of a glass-ceramic prepared from a series of glasses in the Na2O–K2O–CaO–SiO2–F system. A minor amount of cerium oxide was also added instead of calcium oxide in some selective glass batches. The main crystalline phases, formed after the appropriate heat treatments, were wollastonite solid solution and pseudo-wollastonite-like phases. There is a preferential tendency for wollastonite (CaSiO3 to accommodate K, Na, F, and Ce ions in its structure forming wollastonite solid solution with variable formulas. The bioactivity of the resulting crystalline materials was examined in vitro by immersion in simulated body fluid at 37 °C. An increase of the surface bioactivity of glass-ceramic with the Na2O/K2O replacement was observed which is attributed to the augmentation solubility of the crystalline sample. On the other hand, the bioactivity of the crystalline sample with CeO2/CaO replacement was improved by the crystallization of pseudo-wollastonite phase together with wollastonite solid solution phase.

Crystallization of cristobalite from glass phase in mullite ceramics with excess SiO{sub 2} compositions; Sirika kajo muraito seramikkusu chu no garasuso no kesshoka kyodo

Energy Technology Data Exchange (ETDEWEB)

Sato, Takashi; Sugai, Mikio; Nakagawa, Zenbee [Akita University, Akita (Japan). Faculty of Engineering and Resource Science; Sawabe, Yoshinari [Sumitomo Chemical Corp., Ibaraki (Japan). Tsukuba Research Laboratory; Oya, Yutaka [Gifu University, Gifu (Japan). Faculty of Engineering

1999-09-01

Crystallization of glass phase to cristobalite was investigated in mullite-glass ceramics with excess SiO{sub 2} compositions (5.3-16.4 mass %), namely, higher than stoichiometric mullite. Starting powders were prepared by alkoxide hydrolysis method. Compact specimens were sintered at 1600 degree C above the eutectic temperature (1587 degree C) for 2 h. Crystallization treatment was carried out at 1500 degree C, below the eutectic temperature, for times from 4 h to 96 h. Crystallization of glass phase proceeded from the surface of the specimen toward its inner part, in linear dependence on the annealing time. At the polished surface of the specimen, crystallization started in large glass pockets and the crystallized area extended spherically toward the inner part. This phenomenon suggests that nucleation occurs at the minimum parts in the elastic energy generated by the volume change involved in the crystallization of glass phase to cristobalite. (author)

Crystallization behavior of Li2O-SiO2, Na2O-SiO2 and Na2O-CaO-SiO2 glasses; Li2O-SiO2, Na2O-SiO2, Na2O-CaO-SiO2 kei glass no kessho sekishutsu kyodo

Energy Technology Data Exchange (ETDEWEB)

Tsutsumi, K.; Otake, J.; Nagasaka, T.; Hino, M. [Tohoku University, Sendai (Japan)

1998-06-01

It has been known that crystallization of mold powder is effective on the disturbance of heat transfer between mold and solidified shell in production of middle carbon steel slabs in continuous casting process. But it has not yet been made clear which composition of mold powder is the most suitable for crystallization. The crystallization behavior of Li2O-SiO2, Na2O-SiO2 and Na2O-CaO-SiO2 glasses was observed by differential thermal analysis (DTA) and hot-thermocouple methods with DTA in the present work. As a result, addition of alkaline metal and alkaline earth metal oxides to SiO2 increased the critical cooling rate for glass formation in binary system of Li2O-SiO2 and Na2O-SiO2 and Li2O-SiO2 system crystallized easier than Na2O-SiO2 system. In ternary system of Na2O-CaO-SiO2, addition of Na2O hurried the critical cooling rate at CaO/SiO2=0.93 mass ratio, but the rate was almost constant in the composition range of more than 15 mass% Na2O. The slag of CaO/SiO2=0.93 made the rate faster than the slag of CaO/SiO2=0.47 at constant content of 10mass% Na2O. 17 refs., 10 figs., 3 tabs.

LOW-TEMPERATURE SINTERED (ZnMg2SiO4 MICROWAVE CERAMICS WITH TiO2 ADDITION AND CALCIUM BOROSILICATE GLASS

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BO LI

2011-03-01

Full Text Available The low-temperature sintered (ZnMg2SiO–TiO2 microwave ceramic using CaO–B2O3–SiO2 (CBS as a sintering aid has been developed. Microwave properties of (Zn1-xMgx2SiO4 base materials via sol-gel method were highly dependent on the Mg-substituted content. Further, effects of CBS and TiO2 additives on the crystal phases, microstructures and microwave characteristics of (ZnMg2SiO4 (ZMS ceramics were investigated. The results indicated that CBS glass could lower the firing temperature of ZMS dielectrics effectively from 1170 to 950°C due to the liquid-phase effect, and significantly improve the sintering behavior and microwave properties of ZMS ceramics. Moreover, ZMS–TiO2 ceramics showed the biphasic structure and the abnormal grain growth was suppressed by the pinning effect of second phase TiO2. Proper amount of TiO2 could tune the large negative temperature coefficient of resonant frequency (tf of ZMS system to a near zero value. (Zn0.8Mg0.22SiO4 codoped with 10 wt.% TiO2 and 3 wt.% CBS sintered at 950°C exhibits the dense microstructure and excellent microwave properties: εr = 9.5, Q·f = 16 600 GHz and tf = −9.6 ppm/°C.

The phase transformation and crystallization kinetics of (1 - x)Li2O-xNa2O-Al2O3-4SiO2 glasses

International Nuclear Information System (INIS)

Wang, Moo-Chin; Li, Wang-Long; Cheng, Chih-Wei; Chang, Kuo-Ming; Chen, Yong-Feng; Hsi, Chi-Shiung

2010-01-01

The phase transformation and crystallization kinetics of (1 - x)Li 2 O-xNa 2 O-Al 2 O 3 -4SiO 2 glasses have been studied by using differential thermal analysis (DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron diffraction (ED) analysis. The crystallization temperature at the exothermic peak increases from 1171 to 1212 K when the Na 2 O content increases from 0 to 0.6 mol. The crystalline phase is composed of spodumene crystallization when the Na 2 O content increases from 0 to 0.6 mol. The activation energy of spodumene crystallization decreases from 444.0 ± 22.2 to 284.0 ± 10.8 kJ mol -1 when the Na 2 O content increases from 0 to 0.4 mol. Moreover, the activation energy increases from 284.0 ± 10.8 to 446.0 ± 23.2 kJ mol -1 when the Na 2 O content increases from 0.4 to 0.6 mol. The crystallization parameters m and n approach 2, indicating that the surface nucleation and two-dimensional growth are dominant in (1 - x)Li 2 O-xNa 2 O-Al 2 O 3 -4SiO 2 glasses.

TaxHf1−xB2–SiC multiphase oxidation protective coating for SiC-coated carbon/carbon composites

International Nuclear Information System (INIS)

Ren, Xuanru; Li, Hejun; Fu, Qiangang; Li, Kezhi

2014-01-01

Highlights: • Ta x Hf 1−x B 2 –SiC coating was prepared on SiC coated C/C by in-situ reaction method. • TaB 2 and HfB 2 were introduced in the form of solid solution Ta x Hf 1−x B 2 . • The coating could protect C/C for 1480 h with only 0.57% mass loss at 1773 K in air. • Oxidation layer consists of out Ta–Si–O compound layer and inner SiO 2 glass layer. • Ta–Si–O compound silicate layer presents a better stability than SiO 2 glass layer. - Abstract: A Ta x Hf 1−x B 2 –SiC coating was prepared by in-situ reaction method on SiC coated C/C composites. Ta x Hf 1−x B 2 phase is the form of solid solution between TaB 2 and HfB 2 . Isothermal oxidation behavior at 1773 K and ablation behavior of the coated C/C were tested. Ta x Hf 1−x B 2 –SiC/SiC coating could protect the C/C from oxidation at 1773 K for 1480 h and ablation above 2200 K for 40 s. During oxidation, oxides of Ta and Hf atoms exist as “pinning phases” in the compound glass layer consisted of outer Ta–Si–O compound silicate layer and inner SiO 2 glass layer, which was responsible for the excellent oxidation resistance

Effect of calcium fluoride on sintering behaviour of SiO2-CaO-Na2O-MgO glass-ceramic system

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Bahman Mirhadi

2012-09-01

Full Text Available The crystallization characteristics of glasses based on the SiO2-CaO-Na2O-MgO (SCNM system containing calcium fluoride (CaF2 have been investigated by differential thermal analysis (DTA, X-ray diffraction (XRD and scanning electron microscopy (SEM. The partial replacement of CaO by CaF2 in the studied glass-ceramics led to the development of different crystalline phase assemblages, including wollastonite and diopside using various heat-treatment processes. With the increase of CaF2 content, the crystallization temperature of the glass and the strength of the crystallization peak temperature decreases. Addition of CaF2 up to 6.0 mol%, as expected, improved the sinterability. This sample reached to maximum density by sintering at 950 °C.

Preparation and encapsulation performance of Al_2O_3-SiO_2-B_2O_3 glass-ceramic for high temperature thermal storage

International Nuclear Information System (INIS)

Li, Ruguang; Zhu, Jiaoqun; Zhou, Weibing; Cheng, Xiaomin; Liu, Fengli

2017-01-01

Highlights: • Al_2O_3-B_2O_3-SiO_2 has good chemical durability, corrosion resistance and dense structure. • The material rarely used in high temperature thermal storage. • The material was prepared and characterized in the paper. - Abstract: In this paper, Al_2O_3-SiO_2-B_2O_3 glass-ceramic was prepared and characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM), further, the porosity was detected by Archimedes principle, thermo physical properties were investigated by differential scanning calorimeter (DSC), respectively. The phase composition was detected by XRD, and the morphology was observed by SEM. The results indicated that the thermal conductivities of the Al_2O_3-SiO_2-B_2O_3 glass-ceramic were between 1.3 and 1.5 W·(m·K)"−"1, and the material had good thermal stability in the range of 300–900 °C. The porosity and apparent density were increased with the temperature. The porosity of Al_2O_3-SiO_2-B_2O_3 glass-ceramic in ranging from 1.2 to 9.6%, the apparent density were between 2.12 and 2.67 g·cm"−"3, and heat capacities were between 0.64 and 0.79 kJ/(kg·K). All the results indicated that the Al_2O_3-SiO_2-B_2O_3 glass-ceramic can be applied as encapsulation material in high temperature latent thermal energy storage.

SiO2 Glass Density to Lower-Mantle Pressures

DEFF Research Database (Denmark)

Petitgirard, Sylvain; Malfait, Wim J.; Journaux, Baptiste

2017-01-01

and present Earth. SiO2 is the main constituent of Earth's mantle and is the reference model system for the behavior of silicate melts at high pressure. Here, we apply our recently developed x-ray absorption technique to the density of SiO2 glass up to 110 GPa, doubling the pressure range...... for such measurements. Our density data validate recent molecular dynamics simulations and are in good agreement with previous experimental studies conducted at lower pressure. Silica glass rapidly densifies up to 40 GPa, but the density trend then flattens to become asymptotic to the density of SiO2 minerals above 60...... GPa. The density data present two discontinuities at similar to 17 and similar to 60 GPa that can be related to a silicon coordination increase from 4 to a mixed 5/6 coordination and from 5/6 to sixfold, respectively. SiO2 glass becomes denser than MgSiO3 glass at similar to 40 GPa, and its density...

Effect of MoO3 addition on phase separation in borosilicate glasses

International Nuclear Information System (INIS)

Wakabayashi, Hajimu; Yamanaka, Hiroshi; Terai, Ryohei; Fukumoto, Shinji.

1987-01-01

The effect of MoO 3 addition on the phase separation of sodium borosilicate glasses has been studied by electron microscopic observation and electrical conductivity measurement. With increasing MoO 3 addition, the immiscibility temperatures rose, the growth rate of phase separation increased, and the immiscibility region in the Na 2 O-B 2 O 3 -SiO 2 system extended. When MoO 3 more than 5 mol% was added to the glasses, two stages of phase separation appeared ; one is metastable immiscibility, which takes place below the liquidus temperature, and the other is stable immiscibility, occurring above the liquidus temperature. The present experiment confirmed that the conductivity measurement of molten glasses is usefull to detect phase separation in the glasses, giving some suggestions for preventing the separation of molybdates in nuclear waste glasses and also for controlling the micro-pore sizes of porous glasses. (author)

The influence of phosphorus precursors on the synthesis and bioactivity of SiO2-CaO-P 2O 5 sol-gel glasses and glass-ceramics.

Science.gov (United States)

Siqueira, Renato Luiz; Zanotto, Edgar Dutra

2013-02-01

Bioactive glasses and glass-ceramics of the SiO(2)-CaO-P(2)O(5) system were synthesised by means of a sol-gel method using different phosphorus precursors according to their respective rates of hydrolysis-triethylphosphate (OP(OC(2)H(5))(3)), phosphoric acid (H(3)PO(4)) and a solution prepared by dissolving phosphorus oxide (P(2)O(5)) in ethanol. The resulting materials were characterised by differential scanning calorimetry and thermogravimetry, X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy coupled with energy dispersive X-ray spectroscopy and by in vitro bioactivity tests in acellular simulated body fluid. The different precursors significantly affected the main steps of the synthesis, beginning with the time required for gel formation. The most striking influence of these precursors was observed during the thermal treatments at 700-1,200 °C that were used to convert the gels into glasses and glass-ceramics. The samples exhibited very different mineralisation behaviours; especially those prepared using the phosphoric acid, which had a reduced onset temperature of crystallisation and an increased resistance to devitrification. However, all resulting materials were bioactive. The in vitro bioactivity of these materials was strongly affected by the heat treatment temperature. In general, their bioactivity decreased with increasing treatment temperature. For crystallised samples obtained above 900 °C, the bioactivity was favoured by the presence of two crystalline phases: wollastonite (CaSiO(3)) and tricalcium phosphate (α-Ca(3)(PO(4))(2)).

Structure and crystallization of SiO2 and B2O3 doped lithium disilicate glasses from theory and experiment.

Science.gov (United States)

Erlebach, Andreas; Thieme, Katrin; Sierka, Marek; Rüssel, Christian

2017-09-27

Solid solutions of SiO 2 and B 2 O 3 in Li 2 O·2SiO 2 are synthesized and characterized for the first time. Their structure and crystallization mechanisms are investigated employing a combination of simulations at the density functional theory level and experiments on the crystallization of SiO 2 and B 2 O 3 doped lithium disilicate glasses. The remarkable agreement of calculated and experimentally determined cell parameters reveals the preferential, kinetically controlled incorporation of [SiO 4 ] and [BO 4 ] at the Li + lattice sites of the Li 2 O·2SiO 2 crystal structure. While the addition of SiO 2 increases the glass viscosity resulting in lower crystal growth velocities, glasses containing B 2 O 3 show a reduction of both viscosities and crystal growth velocities. These observations could be rationalized by a change of the chemical composition of the glass matrix surrounding the precipitated crystal phase during the course of crystallization, which leads to a deceleration of the attachment of building units required for further crystal growth at the liquid-crystal interface.

Crystallization and thermo-mechanical properties of Li2O-ZnO-CaOSiO2 glass-ceramics with In2O3 and Fe2O3 additives

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Saad M. Salman

2015-12-01

Full Text Available Li2O-ZnO-CaO-SiO2 based glasses were prepared by the conventional melting technique and subsequently converted to glass-ceramics by controlled crystallization. The nucleation and crystallization temperatures were determined by differential thermal analysis (DTA. The effects of adding In2O3 and Fe2O3 addition on the crystallization behaviour and thermo-mechanical properties of the prepared glass-ceramics were investigated. A study on the microstructure, close to the internal phases of the resulting glass-ceramics, was followed by using scanning electron microscope (SEM. The dilatometric thermal expansion and Vickers’ microhardness of the crystalline products were also evaluated. The crystalline phases that can be found in the resulting glass-ceramics, identified by X-ray diffraction (XRD analysis, are α-quartz-[SiO2], lithium zinc silicate-[Li2ZnSiO4], lithium disilicate-[Li2Si2O5], wollastonite-[CaSiO3], wollastonite containing iron, ferrobustamite-[(Ca0.79Fe0.21SiO3], and lithium indium silicate of pyroxene type-[LiInSi2O6]. Average thermal expansion coefficient (in the temperature range 25–700 °C decreased from 191×10-7 1/°C to 115×10-7 1/°C and the Vickers’ microhardness increased from 3.56 to 5.44 GPa with the increase of In2O3 and Fe2O3 contents in the glass-ceramics. The changes in the obtained expansion coefficient and microhardness were due to the formation of different phases which in turn influenced the rigidity/bonding and microstructure in the resultant glass-ceramics.

Characterizing the residual glass in a MgO/Al2O3/SiO2/ZrO2/Y2O3 glass-ceramic

Science.gov (United States)

Seidel, Sabrina; Patzig, Christian; Wisniewski, Wolfgang; Gawronski, Antje; Hu, Yongfeng; Höche, Thomas; Rüssel, Christian

2016-01-01

The non-isochemical crystallization of glasses leads to glass-ceramics in which the chemical composition of the amorphous matrix differs from that of the parent glass. It is challenging to solely analyse the properties of these residual glassy phases because they frequently contain finely dispersed crystals. In this study, the composition of the residual glass matrix after the crystallization of a glass with the mol% composition 50.6 SiO2 · 20.7 MgO · 20.7 Al2O3 · 5.6 ZrO2 · 2.4 Y2O3 is analysed by scanning transmission electron microscopy (STEM) including energy dispersive X-ray analysis (EDXS). A batch of the residual glass with the determined composition is subsequently melted and selected properties are analysed. Furthermore, the crystallization behaviour of this residual glass is studied by X-ray diffraction, scanning electron microscopy including electron backscatter diffraction and STEM-EDXS analyses. The residual glass shows sole surface crystallization of indialite and multiple yttrium silicates while bulk nucleation does not occur. This is in contrast to the crystallization behaviour of the parent glass, in which a predominant bulk nucleation of spinel and ZrO2 is observed. The crystallization of the residual glass probably leads to different crystalline phases when it is in contact to air, rather than when it is enclosed within the microstructure of the parent glass-ceramics. PMID:27734918

Phytic acid derived bioactive CaO-P2O5-SiO2 gel-glasses.

Science.gov (United States)

Li, Ailing; Qiu, Dong

2011-12-01

The possibility of using phytic acid as a precursor to synthesize CaO-P(2)O(5)-SiO(2) glasses by sol-gel method has been explored and the pseudo ternary phase diagram has been established. It was shown that gel-glasses over a broader range of compositions could be prepared compared to other phosphorus precursors or melt-quenching method. Furthermore, phytic acid was found to assist calcium being incorporated into glass networks. In vitro tests in simulated body fluid (SBF) were performed on the above gel-glasses and it was found that they were bioactive over a much broader compositional range especially at high phosphate content, thus enabling one to design bioactive materials with various degradation rates by adjusting the phosphate content.

Beyond sixfold coordinated Si in SiO2 glass at ultrahigh pressures.

Science.gov (United States)

Prescher, Clemens; Prakapenka, Vitali B; Stefanski, Johannes; Jahn, Sandro; Skinner, Lawrie B; Wang, Yanbin

2017-09-19

We investigated the structure of SiO 2 glass up to 172 GPa using high-energy X-ray diffraction. The combination of a multichannel collimator with diamond anvil cells enabled the measurement of structural changes in silica glass with total X-ray diffraction to previously unachievable pressures. We show that SiO 2 first undergoes a change in Si-O coordination number from fourfold to sixfold between 15 and 50 GPa, in agreement with previous investigations. Above 50 GPa, the estimated coordination number continuously increases from 6 to 6.8 at 172 GPa. Si-O bond length shows first an increase due to the fourfold to sixfold coordination change and then a smaller linear decrease up to 172 GPa. We reconcile the changes in relation to the oxygen-packing fraction, showing that oxygen packing decreases at ultrahigh pressures to accommodate the higher than sixfold Si-O coordination. These results give experimental insight into the structural changes of silicate glasses as analogue materials for silicate melts at ultrahigh pressures.

Microstructure, Thermal, Mechanical, and Dielectric Properties of BaO-CaO-Al2O3-B2O3-SiO2 Glass-Ceramics

Science.gov (United States)

Li, Bo; Bian, Haibo; Fang, Yi

2017-12-01

BaO-CaO-Al2O3-B2O3-SiO2 (BCABS) glass-ceramics were prepared via the method of controlled crystallization. The effect of CaO modification on the microstructure, phase evolution, as well as thermal, mechanical, and dielectric properties was investigated. XRD identified that quartz is the major crystal phase; cristobalite and bazirite are the minor crystal phases. Moreover, the increase of CaO could inhibit the phase transformation from quartz to cristobalite, but excessive CaO would increase the porosity of the ceramics. Additionally, with increasing the amount of CaO, the thermal expansion curve tends to be linear, and subsequently the CTE value decreases gradually, which is attributed to the decrease of cristobalite with high CTE and the formation of CaSiO3 with low CTE. The results indicated that a moderate amount of CaO helps attaining excellent mechanical, thermal, and dielectric properties, that is, the specimen with 9 wt% CaO sintered at 950 °C has a high CTE value (11.5 × 10-6/°C), a high flexural strength (165.7 MPa), and good dielectric properties (ɛr = 6.2, tanδ = 1.8 × 10-4, ρ = 4.6 × 1011 Ω•cm).

Evaluation of liquid-phase sintering SiC using as additive the system Al2O3/DyO3

International Nuclear Information System (INIS)

Oliveira, M.R.; Atilio, I.; Garcia, G.C.R.; Ribeiro, S.

2012-01-01

The objective of this work was to study the liquid-phase sintering SiC with additives that has not been studied yet, Al 2 O 3 /Dy 2 O 3 , with 10% in volume. The powders were mixed, dried, and pressed in uniaxial and isostatic pressing. It was studied the melting temperature of the additives and bars were sintered at temperatures of 1900, 1950 e 2000 deg C, with averaged linear shrinkage of 17%, phase transformations of β-SiC into α-SiC and formation of Dy 3 Al 5 O 12 at all temperatures. The results showed that for further densification, the temperature of 1950 deg C is enough for a higher densification, with a low wetting angle, transformations of SiC and formation of Dy 3 Al 5 O 12 . (author)

Crystallization behavior of (1 - x)Li2O.xNa2O.Al2O3.4SiO2 glasses

International Nuclear Information System (INIS)

Wang, Moo-Chin; Cheng, Chih-Wei; Chang, Kuo-Ming; Hsi, Chi-Shiung

2010-01-01

The crystallization behavior of the (1 - x)Li 2 O.xNa 2 O.Al 2 O 3 .4SiO 2 glasses has been investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), electron diffraction (ED) and energy dispersive spectroscopy (EDS). The crystalline phase was composed of β-spodumene. The isothermal crystallization kinetics of β-spodumene from the (1 - x)Li 2 O.xNa 2 O.Al 2 O 3 .4SiO 2 glasses has also been studied by a quantitative X-ray diffraction method. The activation energy of β-spodumene formation decreases from 359.2 to 317.8 kJ/mol when the Na 2 O content increases from 0 to 0.4 mol and it increases from 317.8 to 376.9 kJ/mol when the Na 2 O content increases from 0.4 to 0.6 mol. The surface nucleation and plate-like growth were dominant in the crystallization of the (1 - x)Li 2 O.xNa 2 O.Al 2 O 3 .4SiO 2 glasses.

Effect of V2O5 on SrO-ZnO-B2O3-SiO2 glass-ceramics for high temperature sealant application

Science.gov (United States)

Tiwari, Babita; Bhatacharya, S.; Dixit, A.; Gadkari, S. C.; Kothiyal, G. P.

2012-06-01

Glasses in the SrO-ZnO-B2O3-SiO2 (SZBS) system with and without V2O5 were prepared by melt-quench method and transformed into glass-ceramics by controlled crystallization. Investigated glasses and glass-ceramics have thermal expansion coefficients (TEC) in the range of 95-120 × 10-7/°C (30-600 °C), which match closely with TEC of other components of solid oxide fuel cell (SOFC). Study of thermo-physical properties of SZBS glasses revealed the network modifying effect of V2O5. Addition of V2O5 increases the TEC and decreases the viscosity of the glass which is beneficial for making seal with Crofer-22-APU. Microstructural investigations have shown good bonding of SZBS glasses with Crofer-22-APU. Elemental line scans indicate that inter-diffusion of Fe, Cr and Si across interface, which is thought to be responsible for good bonding with Crofer-22-APU.

A molecular dynamics study of the atomic structure of (CaO)x(SiO2)1-x glasses.

Science.gov (United States)

Mead, Robert N; Mountjoy, Gavin

2006-07-27

The local atomic environment of Ca in (CaO)x(SiO2)1-x glasses is of interest because of the role of Ca in soda-lime glass, the application of calcium silicate glasses as biomaterials, and the previous experimental measurement of the Ca-Ca correlation in CaSiO(3) glass. Molecular dynamics has been used to obtain models of (CaO)x(SiO2)1-x glasses with x = 0, 0.1, 0.2, 0.3, 0.4, and 0.5, and with approximately 1000 atoms and size approximately 25 A. As expected, the models contain a tetrahedral silica network, the connectivity of which decreases as x increases. In the glass-forming region, i.e., x = 0.4 and 0.5, Ca has a mixture of 6- and 7-fold coordination. Bridging oxygen makes an important contribution to the coordination of Ca, with most bridging oxygens coordinated to 2 Si plus 1 Ca. The x = 0.5 model is in reasonable agreement with previous experimental studies, and does not substantiate the previous theory of cation ordering, which predicted Ca arranged in sheets. In the phase-separated region, i.e., x = 0.1 and 0.2, there is marked clustering of Ca.

The structure of ZrO2 phases and deviltrification processes in a Ca-Zr-Si-O-based glass ceramic: a combined a-XRD and XAS study

International Nuclear Information System (INIS)

Meneghini, C.; Mobilio, S.

2004-01-01

The structure of Zr atomic environment in a CaO-ZrO 2 -Si 2 glass ceramic as a function of thermal treatments has been studied, combining X-ray absorption spectroscopy (XAS), X-ray diffraction (XRD) and anomalous XRD (a-XRD) techniques. The analysis of XRD patterns demonstrates that the devitrification process proceeds through the partial segregation of Zr-depleted phases (wollastonite-like) and Zr-rich phases (Zr oxides). The XAS and a-XRD measurements at the Zr K-edge have been exploited in order to obtain a closer insight into the atomic structure around the Zr atoms. In the as-quenched glass the Zr atom is sixfold coordinated to O atoms in an amorphous environment rich in Ca and Si. Thermal treatment firstly (T=1273-1323 K) causes partial segragation of Zr in the form of an oxide with a tetragonal zirconia (t-ZrO 2 ) crystalline structure. Raising the temperature (T=1373 K) causes the formation of ZrO 2 crystallites in the monoclinic crystallographic phase (baddeleyite, m-ZrO 2 ). Analysis of the XAS data shows that a considerable amount of Zr remains in an amorphous calcium silicate phase. (orig.)

Lead recovery and high silica glass powder synthesis from waste CRT funnel glasses through carbon thermal reduction enhanced glass phase separation process

Energy Technology Data Exchange (ETDEWEB)

Xing, Mingfei [Henan Key Laboratory Cultivation Base of Mine Environmental Protection and Ecological Remediation, Henan Polytechnic University, Jiaozuo 454000 Henan China (China); Institute of Resource and Environment, Henan Polytechnic University, Jiaozuo 454000 Henan China (China); Fu, Zegang [Institute of Resource and Environment, Henan Polytechnic University, Jiaozuo 454000 Henan China (China); Wang, Yaping, E-mail: wangyp326@163.com [School of Surveying and Land Information Engineering, Henan Polytechnic University, Jiaozuo 454000, Henan China (China); Wang, Jingyu [Institute of Resource and Environment, Henan Polytechnic University, Jiaozuo 454000 Henan China (China); Zhang, Zhiyuan [Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085 (China)

2017-01-15

Highlights: • CRT funnel glass was remelted with B{sub 2}O{sub 3} in reducing atmosphere. • A part of PbO was reduced into Pb and detached from the glass phase. • The rest of PbO and other metal oxides were mainly concentrated in the B{sub 2}O{sub 3} phase. • PbO enriched in the interconnected B{sub 2}O{sub 3} phase can be completely leached out by HNO{sub 3}. • High silica glass powder(SiO{sub 2} purity >95%) was obtained after the leaching process. - Abstract: In this study, a novel process for the removal of toxic lead from the CRT funnel glass and synchronous preparation of high silica glass powder was developed by a carbon-thermal reduction enhanced glass phase separation process. CRT funnel glass was remelted with B{sub 2}O{sub 3} in reducing atmosphere. In the thermal process, a part of PbO contained in the funnel glass was reduced into metallic Pb and detached from the glass phase. The rest of PbO and other metal oxides (including Na{sub 2}O, K{sub 2}O, Al{sub 2}O{sub 3,} BaO and CaO) were mainly concentrated in the boric oxide phase. The metallic Pb phase and boric oxide phase were completely leached out by 5 mol/L HNO{sub 3}. The lead removal rate was 99.80% and high silica glass powder (SiO{sub 2} purity >95 wt%) was obtained by setting the temperature, B{sub 2}O{sub 3} added amount and holding time at 1000 °C, 20% and 30 mins, respectively. The prepared high silicate glass powders can be used as catalyst carrier, semipermeable membranes, adsorbents or be remelted into high silicate glass as an ideal substitute for quartz glass. Thus this study proposed an eco-friendly and economical process for recycling Pb-rich electronic glass waste.

In vitro evaluation of bioactivity of SiO2-CaO-P2O5-Na2O-CaF2-ZnO glass-ceramics

Science.gov (United States)

Riaz, Madeeha; Zia, Rehana; Saleemi, Farhat; Bashir, Farooq; Hossain, Tousif; Kayani, Zohra

2014-09-01

Zinc is an essential trace element that stimulates bone formation but it is also known as an inhibitor of apatite crystal growth. In this work addition of ZnO to SiO2-CaO-P2O5-Na2O-CaF2 glass-ceramic system was made by conventional melt-quenching technique. DSC curves showed that the addition of ZnO moved the endothermic and exothermic peaks to lower temperatures. X-ray diffraction analysis did not reveal any additional phase caused by ZnO addition and showed the presence of wollastonite and hydroxyapatite crystalline phases only in all the glass-ceramic samples. As bio-implant apatite forming ability is an essential condition, the surface reactivity of the prepared glass-ceramic specimens was studied in vitro in Kokubo's simulated body fluid (SBF) [1] with ion concentration nearly equal to human blood plasma for 30 days at 37 °C under static condition. Atomic absorption spectroscopy (AAS) was used to study the changes in element concentrations in soaking solutions and XRD, FT-IR and SEM were used to elucidate surface properties of prepared glass-ceramics, which confirmed the formation of HCAp on the surface of all glass-ceramics. It was found that the addition of ZnO had a positive effect on bioactivity of glass-ceramics and made it a potential candidate for restoration of damaged bones.

Y-Si-Al-O-N Glass Fibers.

Science.gov (United States)

The excellent mechanical properties and outstanding water corrosion resistance of Y -Si-Al-O- N glasses indicate that they are attractive candidate...materials for forming into high performance glass fibers. Fibers of glasses containing, respectively,3.2 and 6.6 wt% N were drawn freehand in air, and

Structural aspects of B2O3-substituted (PbO)0.5(SiO2)0.5 glasses

International Nuclear Information System (INIS)

Sudarsan, V.; Kulshreshtha, S.K.; Shrikhande, V.K.; Kothiyal, G.P.

2002-01-01

Lead borosilicate glasses having general formulae (PbO) 0.5-x (SiO 2 ) 0.5 (B 2 O 3 ) x with 0.0≤x≤0.4 and (PbO) 0.5 (SiO 2 ) 0.5-y (B 2 O 3 ) y with 0.0≤y≤0.5 have been prepared by a conventional melt-quench method and characterized by 29 Si, 11 B magic angle spinning (MAS) NMR techniques and infrared spectroscopy, as regards their structural features. From 29 Si NMR results, it has been inferred that with increasing concentration of boron oxide, (PbO) 0.5-x (SiO 2 ) 0.5 (B 2 O 3 )x glasses exhibit a systematic increase in the number of Q 4 structural units of Si at the expense of Q 2 structural units, along with the formation of Si-O-B linkages. On the other hand, for (PbO) 0.5 (SiO 2 ) 0.5-y (B 2 O 3 ) y glasses, there is no direct interaction between SiO 2 and B 2 O 3 in the glass network, as revealed by the 29 Si MAS NMR studies. Boron exists in both trigonal and tetrahedral configurations for these two series of glasses and for the (PbO) 0.5 (SiO 2 ) 0.5-y (B 2 O 3 ) y series of glasses; the relative concentration of these two structural units remains almost constant with increasing B 2 O 3 concentration. In contrast, for (PbO) 0.5-x (SiO 2 ) 0.5 (B 2 O 3 ) x glasses, there is a slight increase in the number of BO 3 structural units above x = 0.2, as there is a competition between SiO 2 and B 2 O 3 for interaction with Pb 2+ , thereby leading to the formation of BO 3 structural units. For both series of glasses, the thermal expansion coefficient is found to decrease with increasing B 2 O 3 concentration, the effect being more pronounced for the (PbO) 0.5-x (SiO 2 ) 0.5 (B 2 O 3 ) x series of glasses due to the increased concentration of Q 4 structural units of silicon and better cross-linking as a result of the formation of Si-O-B-type linkages. (author)

Crystallisation of Ba1-xSrxZn2Si2O7 from BaO/SrO/ZnO/SiO2 glass with different ZrO2 and TiO2 concentrations

Science.gov (United States)

Vladislavova, Liliya; Kracker, Michael; Zscheckel, Tilman; Thieme, Christian; Rüssel, Christian

2018-04-01

The effect of different nucleation agents such as ZrO2 and TiO2 was investigated for a first time with respect to their crystallisation behaviour in the glass system BaO-SrO-ZnO-SiO2. In all studied glasses, a Ba1-xSrxZn2Si2O7 (0.1 ≤ x ≤ 0.9) solid solution crystallized. This phase was first described in 2015 to possess a similar structure as the high temperature phase of BaZn2Si2O7 and a thermal expansion close to zero or even negative. It may find applications e.g. as cook panels, telescope mirrors, and furnace windows. Kinetic parameters of the crystallisation process were determined by supplying different heating rates in a differential scanning calorimeter (DSC). The results were evaluated using the equations of Ozawa and Kissinger with respect to the activation energies. Furthermore, the Ozawa method was used for the determination of Avrami parameters, which provides further information on the nucleation and crystallisation processes. Scanning electron microscopy including electron backscatter diffraction (EBSD) was used to characterise the microstructure, to determine the crystallite size and the crystal orientation. For the characterisation of the occurring crystalline phases, X-ray diffraction was used.

Effect of ZrO(2) additions on the crystallization, mechanical and biological properties of MgO-CaO-SiO(2)-P(2)O(5)-CaF(2) bioactive glass-ceramics.

Science.gov (United States)

Li, H C; Wang, D G; Meng, X G; Chen, C Z

2014-06-01

A series of ZrO(2) doped MgO-CaO-SiO(2)-P(2)O(5)-CaF(2) bioactive glass-ceramics were obtained by sintering method. The crystallization behavior, phase composition, morphology and structure of glass-ceramics were characterized. The bending strength, elastic modulus, fracture toughness, micro-hardness and thermal expansion coefficient (TEC) of glass-ceramics were investigated. The in vitro bioactivity and cytotoxicity tests were used to evaluate the bioactivity and biocompatibility of glass-ceramics. The sedimentation mechanism and growth process of apatites on sample surface were discussed. The results showed that the mainly crystalline phases of glass-ceramics were Ca(5)(PO4)3F (fluorapatite) and β-CaSiO(3). (β-wollastonite). m-ZrO(2) (monoclinic zirconia) declined the crystallization temperatures of glasses. t-ZrO(2) (tetragonal zirconia) increased the crystallization temperature of Ca(5)(PO4)(3)F and declined the crystallization temperature of β-CaSiO(3). t-ZrO(2) greatly increased the fracture toughness, bending strength and micro-hardness of glass-ceramics. The nanometer apatites were induced on the surface of glass-ceramic after soaking 28 days in SBF (simulated body fluid), indicating the glass-ceramic has good bioactivity. The in vitro cytotoxicity test demonstrated the glass-ceramic has no toxicity to cell. Copyright © 2014 Elsevier B.V. All rights reserved.

Glass-ceramic nuclear waste forms obtained by crystallization of SiO 2-Al 2O 3-CaO-ZrO 2-TiO 2 glasses containing lanthanides (Ce, Nd, Eu, Gd, Yb) and actinides (Th): Study of the crystallization from the surface

Science.gov (United States)

Loiseau, P.; Caurant, D.

2010-07-01

Glass-ceramic materials containing zirconolite (nominally CaZrTi 2O 7) crystals in their bulk can be envisaged as potential waste forms for minor actinides (Np, Am, Cm) and Pu immobilization. In this study such matrices are synthesized by crystallization of SiO 2-Al 2O 3-CaO-ZrO 2-TiO 2 glasses containing lanthanides (Ce, Nd, Eu, Gd, Yb) and actinides (Th) as surrogates. A thin partially crystallized layer containing titanite and anorthite (nominally CaTiSiO 5 and CaAl 2Si 2O 8, respectively) growing from glass surface is also observed. The effect of the nature and concentration of surrogates on the structure, the microstructure and the composition of the crystals formed in the surface layer is presented in this paper. Titanite is the only crystalline phase able to significantly incorporate trivalent lanthanides whereas ThO 2 precipitates in the layer. The crystal growth thermal treatment duration (2-300 h) at high temperature (1050-1200 °C) is shown to strongly affect glass-ceramics microstructure. For the system studied in this paper, it appears that zirconolite is not thermodynamically stable in comparison with titanite growing form glass surface. Nevertheless, for kinetic reasons, such transformation (i.e. zirconolite disappearance to the benefit of titanite) is not expected to occur during interim storage and disposal of the glass-ceramic waste forms because their temperature will never exceed a few hundred degrees.

A Novel SOFC/SOEC Sealing Glass with a Low SiO2 Content and a High Thermal Expansion Coefficient

DEFF Research Database (Denmark)

Kiebach, Wolff-Ragnar; Agersted, Karsten; Zielke, Philipp

2017-01-01

the amount of Si emission, a low Si containing sealing glass (chemical composition: 50 mol% CaO, 20 mol% ZnO, 20 mol% B2O3 and 10 mol% SiO2) was developed at DTU. In this work, the results from thermal characterization, the crystallization behavior of the glass and the long-term stability and adhesion......Solid oxide cells require seals that can function in harsh, elevated temperature environments. In addition, a low Si content can be advantageous, since Si impurities from the glass sealant can be transported to the active fuel electrode and poison the Ni-YSZ triple phase boundaries. To reduce...... behavior of the glass were studied under SOFC and SOEC relevant conditions. The glass-ceramic sealant performed well over 400 h, and no cell degradation or leakage related to the seal was found, indicating that the developed glass system is applicable for the use in SOFC/SOEC stacks....

First Measurements of Time-Dependent Nucleation as a Function of Composition in Na2O.2CaO.3SiO2 Glasses

Science.gov (United States)

Kelton, K. F.; Narayan, K. Lakshmi

1996-01-01

The first measurements in any system of the composition dependence of the time-dependent nucleation rate are presented Nucleation rates of the stoichiometric crystalline phase, Na2O.2CaO.3SiO2, from quenched glasses made with different SiO2 concentrations were determined as a function of temperature and glass composition. A strong compositional dependence of the nucleation rates and a weak dependence for the induction times are observed. Using measured values of the liquidus temperatures and growth velocities as a function of glass composition, these data are shown to be consistent with predictions from the classical theory of nucleation, assuming a composition-dependent interfacial energy.

Tunable Synthesis of SiC/SiO2 Heterojunctions via Temperature Modulation

Directory of Open Access Journals (Sweden)

Wei Li

2018-05-01

Full Text Available A large-scale production of necklace-like SiC/SiO2 heterojunctions was obtained by a molten salt-mediated chemical vapor reaction technique without a metallic catalyst or flowing gas. The effect of the firing temperature on the evolution of the phase composition, microstructure, and morphology of the SiC/SiO2 heterojunctions was studied. The necklace-like SiC/SiO2 nanochains, several centimeters in length, were composed of SiC/SiO2 core-shell chains and amorphous SiO2 beans. The morphologies of the as-prepared products could be tuned by adjusting the firing temperature. In fact, the diameter of the SiO2 beans decreased, whereas the diameter of the SiC fibers and the thickness of the SiO2 shell increased as the temperature increased. The growth mechanism of the necklace-like structure was controlled by the vapor-solid growth procedure and the modulation procedure via a molten salt-mediated chemical vapor reaction process.

Composition and crystallization kinetics of R2O-Al2O3-SiO2 glass-ceramics

International Nuclear Information System (INIS)

Xiong, Dehua; Cheng, Jinshu; Li, Hong

2010-01-01

The crystallization behavior and microstructure of R 2 O-Al 2 O 3 -SiO 2 (R means K, Na and Li) glass were investigated by means of differential scanning calorimeter (DSC), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The crystallization kinetic parameters including the crystallization apparent activation energy (E a ), the Avrami parameter (n), glass transition temperature (T g ) and the activity energy of glass transition (E t ) were also measured with different methods. The results have shown that: the DSC traces of composition A parent glass have two different precipitation crystallization peaks corresponding to E a1 (A) = 151.4 kJ/mol (Li 2 SiO 3 ) and E a2 (A) = 623.1 kJ/mol (Li 2 Si 2 O 5 ), the average value of n = 1.70 (Li 2 Si 2 O 5 ) for the surface crystallization and E t (A) = 202.8 kJ/mol. And E a (B) = 50.7 kJ/mol (Li 2 SiO 3 ), the average value of n = 3.89 (Li 2 SiO 3 ) for the bulk crystallization and E t (B) = 220.4 kJ/mol for the composition B parent glass. Because of the content of R 2 O is bigger than composition A, composition B parent glass has a lower E a , T g and a larger n, E t .

High temperature mechanical behaviour of glass-ceramics in the YSiAlON and ErSiAlON systems

Energy Technology Data Exchange (ETDEWEB)

Bondanini, A.; Massouras, G.; Besson, J.L. [ENSCI, Limoges (France). SPCTS

2002-07-01

The high temperature mechanical behaviour of oxynitride glass-ceramics in the YSiAlON and ErSiAlON systems was studied in the 950-1150 C temperature range under compressive stresses ranging from 20 to 100 MPa. The parent glass had a composition of 35 Y(or Er)-45 Si-20 Al-83 O-17 N in equivalent percent. Starting from these glasses, glass-ceramics were prepared using a two stage heat treatment: nucleation at the optimum nucleation temperature followed by crystal growth at 1050, 1150 or 1250 C. The two parent glasses had similar viscosities, with that of the Er-glass being slightly less than that of the Y-glass. After the devitrification treatment at 1050 C, B-phase (M{sub 2}SiAlO{sub 5}N) was the only crystalline phase formed in both systems. The creep behaviour was similar for the yttrium and the erbium materials. It was characterised by a long transient stage, due to the viscoelastic response of the residual glass, with recovered strain after unloading decreasing as loading time increased. The creep resistance was compared to that of the parent glasses in terms of apparent viscosity. The crystallisation of 75% of the glass resulted in an increase in viscosity such that a temperature some 100 C higher showed the same viscosity value. After heat treatment at 1150 C, the phase assemblage in the yttrium material changed with the formation of wollastonite and partial conversion of B-phase into Iw-phase. The apparent viscosity was 2 orders of magnitude higher than that of the samples heat treated at 1050 C and no strain recovery was observed upon unloading. In contrast, the erbium materials retained the same microstructure as after the heat treatment at 1050{sup b}C and there was no difference in the creep behaviour of the samples heat treated at 1050 or 1150 C. After a crystallisation treatment at 1250 C of the yttrium parent glass, the glass-ceramic consisted of yttrium aluminium garnet, N-apatite and {beta}-Y{sub 2}Si{sub 2}O{sub 7} and showed excellent creep

Preparation and Characterization of PbO-SrO-Na2O-Nb2O5-SiO2 Glass Ceramics Thin Film for High-Energy Storage Application

Science.gov (United States)

Tan, Feihu; Zhang, Qingmeng; Zhao, Hongbin; Wei, Feng; Du, Jun

2018-03-01

PbO-SrO-Na2O-Nb2O5-SiO2 (PSNNS) glass ceramic thin films were prepared by pulsed laser deposition technology on heavily doped silicon substrates. The influence of annealing temperatures on microstructures, dielectric properties and energy storage performances of the as-prepared films were investigated in detail. X-ray diffraction studies indicate that Pb2Nb2O7 crystallizes at 800°C and disappears at 900°C, while NaNbO3 and PbNb2O6 are formed at the higher temperature of 900°C. The dielectric properties of the glass ceramics thin films have a strong dependence on the phase assemblages that are developed during heat treatment. The maximum dielectric constant value of 171 was obtained for the film annealed at 800°C, owing to the high electric breakdown field strength, The energy storage densities of the PSNNS films annealed at 800°C were as large as 36.9 J/cm3, These results suggest that PSNNS thin films are promising for energy storage applications.

Effect of SiO2 addition and gamma irradiation on the lithium borate glasses

Science.gov (United States)

Raut, A. P.; Deshpande, V. K.

2018-01-01

The physical properties like density, glass transition temperature (Tg), and ionic conductivity of lithium borate (LB) glasses with SiO2 addition were measured before and after gamma irradiation. Remarkable changes in properties have been obtained in the physical properties of LB glasses with SiO2 addition and after gamma irradiation. The increase in density and glass transition temperature of LB glasses with SiO2 addition has been explained with the help of increase in density of cross linking due to SiO4 tetrahedra formation. The increase in ionic conductivity with SiO2 addition was explained with the help of ‘mixed glass former effect’. The increase in density and Tg of LB glasses with SiO2 addition after gamma irradiation has been attributed to fragmentation of bigger ring structure into smaller rings, which increases the density of cross linking and hence compaction. The exposure of gamma irradiation has lead to decrease in ionic conductivity of LB glasses with SiO2 addition. The atomic displacement caused by gamma irradiation resulted in filling of interstices and decrease in trapping sites. This explains the obtained decrease in ionic conductivity after gamma irradiation of glasses. The obtained results of effect of SiO2 addition and gamma irradiation on the density, Tg and ionic conductivity has been supported by FTIR results.

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.

Glass-ceramic materials of system MgO-Al{sub 2}O{sub 3}-SiO{sub 2} from rice husk ash; Materiales vitroceramicos del sistema MgO-Al2O3-SiO2 a partir de ceniza de cascara de arroz

Energy Technology Data Exchange (ETDEWEB)

Martin, M. I.; Rincon, J. M.; Andreola, F.; Barbieri, L.; Bondioli, F.; Lancellotti, I.; Romero, M.

2011-07-01

This wok shows the results of a valorisation study to use rice husk ash as raw material to develop glass-ceramic materials. An original glass has been formulated in the base system MgO-Al{sub 2}O{sub 3}-SiO{sub 2} with addition of B{sub 2}O{sub 3} and Na{sub 2}O to facilitate the melting and poring processes. Glass characterization was carried out by determining its chemical composition. Sintering behaviour has been examined by Hot Stage Microscopy (HSM). Thermal stability and crystallization mechanism have been studied by Differential Thermal Analysis (DTA). Mineralogy analyses of the glass-ceramic materials were carried out using X-ray Diffraction (XRD). Results show that it is possible to use ash rice husk to produce glass-ceramic materials by a sinter crystallization process, with nepheline (Na{sub 2}O-Al{sub 2}O{sub 3}-SiO{sub 2}) as major crystalline phase in the temperature interval 700-950 degree centigrade and forsterite (2MgO-SiO{sub 2}) at temperatures above 950 degree centigrade. (Author) 15 refs.

Silicon nitride and YMgSiAlON glass study by mechanical spectroscopy

International Nuclear Information System (INIS)

Doen, B.; Gadaud, P.

1996-01-01

Si 3 N 4 /TiN and YMgSiAlON/SiC composites have been studied by isothermal mechanical spectroscopy over a large frequency range. Internal friction curves obtained for the composite Si 3 N 4 -TiN(30% vol)-Al 2 O 3 , Y 2 O 3 (7.5% vol) exhibit a thermally activated pseudo peak superposed on a non purely exponential background. We can assume that this maximum is due to relaxations in the compressed intergranular glassy films. The apparent dynamical parameters deduced from its shift (11.2 eV and 3.10 -45 s) are unusual as observed in amorphous materials. YMgSiAlON glass has a composition very similar to the one of the intergranular phase of Si 3 N 4 /TiN composite. The damping curves obtained for YMgSiAlON/SiC composites above the glass transition temperature are pure exponential backgrounds. An original analysis of these curves allows to determine an activation energy of about 3.6 eV. This value is more realistic for an elementary diffusion mechanism in a glass near Tg. (orig.)

The influence of SiO2 Addition on 2MgO-Al2O3-3.3P2O5 Glass

DEFF Research Database (Denmark)

Larsen, P.H.; Poulsen, F.W.; Berg, Rolf W.

1999-01-01

2MgO-Al2O3-3.3P2O5 glasses with increasing amounts of SiO2 are considered for sealing applications in Solid Oxide Fuel Cells (SOFC). The change in chemical durability under SOFC anode conditions and the linear thermal expansion is measured as functions of the SiO2 concentration. Raman spectroscopy...... analysis of the glasses reveals no sign of important changes in the glass structure upon SiO2 addition. Some increase in glass durability with SiO2 concentration is reported and its cause is discussed....

Crystallization and magnetic properties of a 10Li{sub 2}O–9MnO{sub 2}–16Fe{sub 2}O{sub 3}–25CaO–5P{sub 2}O{sub 5}–35SiO{sub 2} glass

Energy Technology Data Exchange (ETDEWEB)

Wang, Moo-Chin, E-mail: mcwang@kmu.edu.tw [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80708, Taiwan (China); Cheng, Huy-Zu [Department of Materials Science and Engineering, I-Shou University, 1 123456789Hsueh-Cheng Road, Section 1, Ta-Hsu, Kaohsiung 84001, Taiwan (China); Lin, Huey-Jiuan [Department of Materials Science and Engineering, National United University, 1 Lien-Da Road, Kung-Ching Li, Miao-Li 36003, Taiwan (China); Wang, Chien-Fu [Department of Materials Science and Engineering, I-Shou University, 1 123456789Hsueh-Cheng Road, Section 1, Ta-Hsu, Kaohsiung 84001, Taiwan (China); Hsi, Chi-Shiung, E-mail: chsi@nuu.edu.tw [Department of Materials Science and Engineering, National United University, 1 Lien-Da Road, Kung-Ching Li, Miao-Li 36003, Taiwan (China)

2013-06-15

The crystallization behavior and magnetic properties of 10Li{sub 2}O–9MnO{sub 2}–16Fe{sub 2}O{sub 3}–25CaO–5P{sub 2}O{sub 5}–35SiO{sub 2} (10LFS) glass have been studied using differential thermal analysis (DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDS), transmission electron microscopy (TEM) and selected area electron diffraction (SAED) to observe the crystallization behavior and a superconducting quantum interference device (SQUID) for measurements of the magnetic properties. The DTA shows that the 10LFS glass has one broad exothermic peak at approximately 674 °C and one sharp (the highest) exothermic peak at 764 °C. When the 10LFS glass crystallized at 850 °C for 4 h, the crystalline phases identified by XRD were lithium silicate (Li{sub 2}SiO{sub 3}), β-wollastonite (β-CaSiO{sub 3}), lithium orthophosphate (Li{sub 3}PO{sub 4}), magnetite (FeFe{sub 2}O{sub 4}) and triphylite (Li(Mn{sub 0.5}Fe{sub 0.5})PO{sub 4}). The SEM surface analysis revealed that the β-wollastonite and lithium silicate have a lath morphology. The TEM microstructure examination showed that the largest FeFe{sub 2}O{sub 3} particles have a size of approximately 0.3 μm. When the 10LFS glass was heat treated at 850 °C for 16 h and a magnetic field of 1000 Oe was applied, a very small remnant magnetic induction of 0.01 emu g{sup −1} and a coercive force of 50 Oe were obtained, which revealed an inverse spinel structure. - Highlights: ► The phases formed at 850 °C in the 10LFS glass-ceramics are LiSiO{sub 3}, β-CaSiO{sub 3}, Li{sub 3}PO{sub 4}, FeFe{sub 2}O{sub 4} and Li(Mn{sub 0.5}Fe{sub 0.5})PO{sub 4}. ► The β-wollastonite and lithium silicate have a lath morphology. ► When 10LFS glass-ceramics applied magnetic field showing the ferromagnetic behavior of an inverse spinel structure.

The phase transformation and crystallization kinetics of (1 - x)Li{sub 2}O-xNa{sub 2}O-Al{sub 2}O{sub 3}-4SiO{sub 2} glasses

Energy Technology Data Exchange (ETDEWEB)

Wang, Moo-Chin [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 807, Taiwan (China); Li, Wang-Long [Institute of Nanotechnology and Microsystems Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Cheng, Chih-Wei [Department of Mechanical Engineering, National Kaohsiung University of Applied Sciences, 415 Chien-Kung Road, Kaohsiung 80782, Taiwan (China); Chang, Kuo-Ming; Chen, Yong-Feng [Department of Electrical Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Hsi, Chi-Shiung, E-mail: chsi@nuu.edu.tw [Department of Materials Science and Engineering, National United University, 1 Lein-Da, Kung-Ching Li, Miaoli 36003, Taiwan (China)

2010-09-01

The phase transformation and crystallization kinetics of (1 - x)Li{sub 2}O-xNa{sub 2}O-Al{sub 2}O{sub 3}-4SiO{sub 2} glasses have been studied by using differential thermal analysis (DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron diffraction (ED) analysis. The crystallization temperature at the exothermic peak increases from 1171 to 1212 K when the Na{sub 2}O content increases from 0 to 0.6 mol. The crystalline phase is composed of spodumene crystallization when the Na{sub 2}O content increases from 0 to 0.6 mol. The activation energy of spodumene crystallization decreases from 444.0 {+-} 22.2 to 284.0 {+-} 10.8 kJ mol{sup -1} when the Na{sub 2}O content increases from 0 to 0.4 mol. Moreover, the activation energy increases from 284.0 {+-} 10.8 to 446.0 {+-} 23.2 kJ mol{sup -1} when the Na{sub 2}O content increases from 0.4 to 0.6 mol. The crystallization parameters m and n approach 2, indicating that the surface nucleation and two-dimensional growth are dominant in (1 - x)Li{sub 2}O-xNa{sub 2}O-Al{sub 2}O{sub 3}-4SiO{sub 2} glasses.

Oxidation of BN-coated SiC fibers in ceramic matrix composites

International Nuclear Information System (INIS)

Sheldon, B.W.; Sun, E.Y.

1996-01-01

Thermodynamic calculations were performed to analyze the simultaneous oxidation of BN and SiC. The results show that, with limited amounts of oxygen present, the formation of SiO 2 should occur prior to the formation of B 2 O 3 . This agrees with experimental observations of oxidation in glass-ceramic matrix composites with BN-coated SiC fibers, where a solid SiO 2 reaction product containing little or no boron has been observed. The thermodynamic calculations suggest that this will occur when the amount of oxygen available is restricted. One possible explanation for this behavior is that SiO 2 formation near the external surfaces of the composite closes off cracks or pores, such that vapor phase O 2 diffusion into the composite occurs only for a limited time. This indicates that BN-coated SiC fibers will not always oxidize to form significant amounts of a low-melting, borosilicate glass

Crystallization and chemical durability of glasses in the system Bi2O3-SiO2

International Nuclear Information System (INIS)

Fredericci, C.

2011-01-01

The crystallization of the Bi 2 O 3 -SiO 2 -TiO 2 -Al 2 O 3 -Na 2 O-K 2 O and Bi 2 O 3 -SiO 2 -ZnO-Al 2 O 3 -B 2 O 3 -Na 2 O glasses was studied using glass samples prepared by traditional melt-quench method. Differential thermal analysis (DTA) curves suggested that surface crystallization played a major role in the crystallization of the glass samples. X-ray diffraction (XRD) analysis revealed the crystallization of bismuth silicate for both glasses and bismuth silicate and zinc silicate for the glass containing ZnO. Through scanning electron microscopy (MEV) and energy dispersive spectroscopy (EDS), it was possible to observe that the crystals of zinc silicate (Zn 2 SiO 4 ) were readily attacked by hot 0,1 N sulfuric acid, whereas bismuth silicate crystals were more resistant to acidic attack etching. (author)

The role of Sr2+ on the structure and reactivity of SrO-CaO-ZnO-SiO2 ionomer glasses.

Science.gov (United States)

Boyd, Daniel; Towler, Mark R; Watts, Sally; Hill, Robert G; Wren, Anthony W; Clarkin, Owen M

2008-02-01

The suitability of Glass Polyalkenoate Cements (GPCs) for use in orthopaedics is retarded by the presence in the glass phase of aluminium, a neurotoxin. Unfortunately, the aluminium ion plays an integral role in the setting process of GPCs and its absence is likely to hinder cement formation. However, the authors have previously shown that aluminium free GPCs may be formulated based on calcium zinc silicate glasses and these novel materials exhibit significant potential as hard tissue biomaterials. To further improve their potential, and given that Strontium (Sr) based drugs have had success in the treatment of osteoporosis, the authors have substituted Calcium (Ca) with Sr in the glass phase of a series of aluminium free GPCs. However to date little data exists on the effect SrO has on the structure and reactivity of SrO-CaO-ZnO-SiO(2) glasses. The objective of this work was to characterise the effect of the Ca/Sr substitution on the structure of such glasses, and evaluate the subsequent reactivity of these glasses with an aqueous solution of Polyacrylic acid (PAA). To this end (29)Si MAS-NMR, differential scanning calorimetry (DSC), X-ray diffraction, and network connectivity calculations, were used to characterize the structure of four strontium calcium zinc silicate glasses. Following glass characterization, GPCs were produced from each glass using a 40 wt% solution of PAA (powder:liquid = 2:1.5). The working times and setting times of the GPCs were recorded as per International standard ISO9917. The results acquired as part of this research indicate that the substitution of Ca for Sr in the glasses examined did not appear to significantly affect the structure of the glasses investigated. However it was noted that increasing the amount of Ca substituted for Sr did result in a concomitant increase in setting times, a feature that may be attributable to the higher basicity of SrO over CaO.

Structure and crystallization of B{sub 2}O{sub 3}-Al{sub 2}O{sub 3}-SiO{sub 2} glasses

Energy Technology Data Exchange (ETDEWEB)

Cheng Yin, E-mail: zjbcy@126.co [College of Physics and Electronic Science, Changsha University of Science and Technology, Changsha 410114 (China); Xiao Hanning [College of Physics and Electronic Science, Changsha University of Science and Technology, Changsha 410114 (China); College of Materials Science and Engineering, Hunan University, Changsha 410082 (China); Shuguang Chen; Tang Bingzhong [College of Physics and Electronic Science, Changsha University of Science and Technology, Changsha 410114 (China)

2009-05-01

B{sub 2}O{sub 3}-Al{sub 2}O{sub 3}-SiO{sub 2} glasses with different B{sub 2}O{sub 3}/Al{sub 2}O{sub 3} ratios of 0.4-1.3 were prepared by the melting-quenching method at 1500-1600 deg. C for 2 h. Fragility index F was used to estimate the glass-forming ability. The infrared (IR) absorption curves and differential scanning calorimetry (DSC) curves of the glasses have been investigated for estimating the influence of the B{sub 2}O{sub 3}/Al{sub 2}O{sub 3} ratio on glass structure and crystallization of the B{sub 2}O{sub 3}-Al{sub 2}O{sub 3}-SiO{sub 2} glass system. The crystallization kinetics of the glasses were described by activation energy (E) for crystallization and calculated by the Kissinger method. X-ray diffraction (XRD) and SEM analyses were also used to describe the types and morphologies of the crystals precipitated from the B{sub 2}O{sub 3}-Al{sub 2}O{sub 3}-SiO{sub 2} glasses. The results show that with the increase of B{sub 2}O{sub 3}/Al{sub 2}O{sub 3} ratio, glass stability improves and the trend of crystallization decreases relatively. However, when the B{sub 2}O{sub 3}/Al{sub 2}O{sub 3} ratio reaches 1.3, boron-abnormal phenomenon appears and results in the raising trend of crystallization. Rod-like crystals of Al{sub 4}B{sub 2}O{sub 9} and Al{sub 20}B{sub 4}O{sub 36} were observed in the crystallized samples.

Thermal shock behaviour of SiC-fibre-reinforced glasses

International Nuclear Information System (INIS)

Klug, T.; Reichert, J.; Brueckner, R.

1992-01-01

The preparation of two SiC-fibre-reinforced glasses with very different thermal expansion coefficients and glass transition temperatures is described and the influence of long-time temperature and thermal shock behaviour of these composites on the mechanical properties is investigated by means of bending test experiments before and after thermal treatments. It will be shown from experiments and calculations on stresses due to thermal expansion mismatch between fibre and glass matrix that not only best mechanical properties but also best thermal shock behaviour are connected with low tensile intrinsic stresses produced by thermal expansion mismatch during preparation. The thermal shock resistance of the best composite (SiC fibre/DURAN glass) does not show a significant decrease of flexural strength even after 60 shocks from 550 to 25deg C in water, while the bulk glass sample of the same dimension was destroyed by one thermal shock from 350deg C. (orig.) [de

Adsorption of uranyl in SiO2 porous glass

International Nuclear Information System (INIS)

Benedetto, F. E.; Prado, M. O.

2013-01-01

Vitreous SiO 2 porous matrices can be used in many applications involving the uptake of chemical species on its solid surface. In this work, vitreous silica sponges were prepared from a sodium borosilicate glass manufactured in our laboratory. The product obtained was then separated into phases with subsequent leaching of the soluble phase rich in B and Na. The resulting porous matrices have a specific surface of 35 m2/gr. Adsorption of uranyl ions onto the SiO 2 porous surface was studied to evaluate the use of this material as a filter for treatment of uranium containing water. The effects of contact time, adsorbent mass and equilibrium concentration of solution were studied. The porous adsorbent exhibits a pseudo-second-order kinetic behavior. The sponges with adsorbed uranium were thermally sealed as a way of U immobilization. Retention of uranium was confirmed during the matrix sealing by TGA. Uranium concentration before and after adsorption tests were made by means of ICP-OES. For uranium concentration of 800 ppm, 72 hours contact time and pH of 3.5, the amount of uranium adsorbed was 21.06 ± 0.02 mg U per gram of vitreous porous SiO 2 . (author)

Synthesis of nanocrystals in KNb(Ge,Si)O5 glasses and chemical etching of nanocrystallized glass fibers

International Nuclear Information System (INIS)

Enomoto, Itaru; Benino, Yasuhiko; Fujiwara, Takumi; Komatsu, Takayuki

2006-01-01

The nanocrystallization behavior of 25K 2 O-25Nb 2 O 5 -(50-x)GeO 2 -xSiO 2 glasses with x=0,25,and50 (i.e., KNb(Ge,Si)O 5 glasses) and the chemical etching behavior of transparent nanocrystallized glass fibers have been examined. All glasses show nanocrystallization, and the degree of transparency of the glasses studied depends on the heat treatment temperature. Transparent nanocrystallized glasses can be obtained if the glasses are heat treated at the first crystallization peak temperature. Transparent nanocrystallized glass fibers with a diameter of about 100μm in 25K 2 O-25Nb 2 O 5 -50GeO 2 are fabricated, and fibers with sharpened tips (e.g., the taper length is about 450μm and the tip angle is about 12 o ) are obtained using a meniscus chemical etching method, in which etching solutions of 10wt%-HF/hexane and 10M-NaOH/hexane are used. Although the tip (aperture size) has not a nanoscaled size, the present study suggests that KNb(Ge,Si)O 5 nanocrystallized glass fibers have a potential for new near-field optical fiber probes with high refractive indices of around n=1.8 and high dielectric constants of around ε=58 (1kHz, room temperature)

Understanding the magnetic behavior of heat treated CaO-P2O5-Na2O-Fe2O3-SiO2 bioactive glass using electron paramagnetic resonance studies

Science.gov (United States)

Shankhwar, Nisha; Kothiyal, G. P.; Srinivasan, A.

2014-09-01

Bioactive glass of composition 41CaO-44SiO2-4P2O5-8Fe2O3-3Na2O has been heat treated in the temperature (TA) range of 750-1150 °C for time periods (tA) ranging from 1 h to 3 h to yield magnetic bioactive glass ceramics (MBCs). X-ray diffraction studies indicate the presence of bone mineral (hydroxyapatite and wollastonite) and magnetic (magnetite and α-hematite) phases in nanocrystalline form in the MBCs. Electron paramagnetic resonance (EPR) study was carried out to understand the variation in saturation magnetization and coercivity of the MBCs with TA and tA. These studies reveal the nature and amount of iron ions present in the MBCs and their interaction in the glassy oxide matrix as a function of annealing parameters. The deterioration in the magnetic properties of the glass heat treated above 1050 °C is attributed to the crystallization of the non-magnetic α-hematite phase. These results are expected to be useful in the application of these MBCs as thermoseeds in hyperthermia treatment of cancer.

Materiales vitrocerámicos del sistema MgO-Al2O3-SiO2 a partir de ceniza de cáscara de arroz

Directory of Open Access Journals (Sweden)

Romero, M.

2011-08-01

Full Text Available This wok shows the results of a valorisation study to use rice husk ash as raw material to develop glass-ceramic materials. An original glass has been formulated in the base system MgO-Al2O3-SiO2 with addition of B2O3 and Na2O to facilitate the melting and poring processes. Glass characterization was carried out by determining its chemical composition. Sintering behaviour has been examined by Hot Stage Microscopy (HSM. Thermal stability and crystallization mechanism have been studied by Differential Thermal Analysis (DTA. Mineralogy analyses of the glass-ceramic materials were carried out using X-ray Diffraction (XRD. Results show that it is possible to use ash rice husk to produce glass-ceramic materials by a sintercrystallization process, with nepheline (Na2O·Al2O3 · SiO2 as major crystalline phase in the temperature interval 700-950ºC and forsterite (2MgO·SiO2 at temperatures above 950ºC.En este trabajo se muestran los resultados de un estudio de valorización de la ceniza de cáscara de arroz como materia prima en la obtención de materiales vitrocerámicos. Se ha formulado un vidrio en el sistema base MgO-Al2O3-SiO2 incorporando B2O3 y Na2O para facilitar los procesos de fusión y colado del vidrio. El vidrio se ha caracterizado mediante la determinación de su composición química. Su comportamiento frente a la sinterización se ha llevado a cabo mediante Microscopía de Calefacción (MC. La estabilidad térmica de las muestras y el mecanismo de cristalización preferente se ha estudiado mediante Análisis Térmico Diferencial (ATD. La mineralogía de los materiales vitrocerámicos se ha llevado a cabo por Difracción de rayos-X (DRX. Los resultados obtenidos muestran que es posible utilizar ceniza de cáscara de arroz para producir materiales vitrocerámicos mediante un proceso de sinterización seguido de cristalización, con nefelina (Na2O·Al2O3·2SiO2 como fase cristalina mayoritaria en el intervalo de temperatura 700º-950ºC y

Nano-phase separation and structural ordering in silica-rich mixed network former glasses.

Science.gov (United States)

Liu, Hao; Youngman, Randall E; Kapoor, Saurabh; Jensen, Lars R; Smedskjaer, Morten M; Yue, Yuanzheng

2018-06-13

We investigate the structure, phase separation, glass transition, and crystallization in a mixed network former glass series, i.e., B2O3-Al2O3-SiO2-P2O5 glasses with varying SiO2/B2O3 molar ratio. All the studied glasses exhibit two separate glassy phases: droplet phase (G1) with the size of 50-100 nm and matrix phase (G2), corresponding to a lower calorimetric glass transition temperature (Tg1) and a higher one (Tg2), respectively. Both Tg values decrease linearly with the substitution of B2O3 for SiO2, but the magnitude of the decrease is larger for Tg1. Based on nuclear magnetic resonance and Raman spectroscopy results, we infer that the G1 phase is rich in boroxol rings, while the G2 phase mainly involves the B-O-Si network. Both phases contain BPO4- and AlPO4-like units. Ordered domains occur in G2 upon isothermal and dynamic heating, driven by the structural heterogeneity in the as-prepared glasses. The structural ordering lowers the activation energy of crystal growth, thus promoting partial crystallization of G2. These findings are useful for understanding glass formation and phase separation in mixed network former oxide systems, and for tailoring their properties.

Bioactive SrO-SiO2 glass with well-ordered mesopores: characterization, physiochemistry and biological properties.

Science.gov (United States)

Wu, Chengtie; Fan, Wei; Gelinsky, Michael; Xiao, Yin; Simon, Paul; Schulze, Renate; Doert, Thomas; Luo, Yongxiang; Cuniberti, Gianaurelio

2011-04-01

For a biomaterial to be considered suitable for bone repair it should ideally be both bioactive and have a capacity for controllable drug delivery; as such, mesoporous SiO(2) glass has been proposed as a new class of bone regeneration material by virtue of its high drug-loading ability and generally good biocompatibility. It does, however, have less than optimum bioactivity and controllable drug delivery properties. In this study, we incorporated strontium (Sr) into mesoporous SiO(2) in an effort to develop a bioactive mesoporous SrO-SiO(2) (Sr-Si) glass with the capacity to deliver Sr(2+) ions, as well as a drug, at a controlled rate, thereby producing a material better suited for bone repair. The effects of Sr(2+) on the structure, physiochemistry, drug delivery and biological properties of mesoporous Sr-Si glass were investigated. The prepared mesoporous Sr-Si glass was found to have an excellent release profile of bioactive Sr(2+) ions and dexamethasone, and the incorporation of Sr(2+) improved structural properties, such as mesopore size, pore volume and specific surface area, as well as rate of dissolution and protein adsorption. The mesoporous Sr-Si glass had no cytotoxic effects and its release of Sr(2+) and SiO(4)(4-) ions enhanced alkaline phosphatase activity - a marker of osteogenic cell differentiation - in human bone mesenchymal stem cells. Mesoporous Sr-Si glasses can be prepared to porous scaffolds which show a more sustained drug release. This study suggests that incorporating Sr(2+) into mesoporous SiO(2) glass produces a material with a more optimal drug delivery profile coupled with improved bioactivity, making it an excellent material for bone repair applications. Copyright © 2010 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Sintering of SiC ceramics, via liquid phase, with Al{sub 2}O{sub 3}-Yb{sub 2}O{sub 3} additives; Sinterizacao de ceramicas de SiC, via fase liquida, com aditivos de Al{sub 2}O{sub 3}-Yb{sub 2}O{sub 3}

Energy Technology Data Exchange (ETDEWEB)

Atilio, I.; Oliveira, M.R.; Garcia, G.C.R.; Ribeiro, S., E-mail: isabelaatilio@hotmail.com [Universidade de Sao Paulo (USP/EEL), Lorena, SP (Brazil). Escola de Engenharia. Dept. de Engenharia de Materiais

2012-07-01

The objective of this work was to study the sintering of SiC, through liquid phase, using the additive system Al{sub 2}O{sub 3} and Yb{sub 2}O{sub 3} for the first time. The samples were sintered at temperatures of 1900, 1950 and 2000 deg C for 60 minutes. The melting point of the system was determined according to DIN 51730. It has been found the ability of wetting of SiC in the system. The densification results were: 86,36% at 1900 deg C, 88,25% at 1950 deg C and 82,09% at 2000 deg C. The average linear shrinkage was approximately 17%. There was a conversion of β-SiC in α-SiC at all temperatures and sintering phase formation Yb{sub 3}Al{sub 5}O{sub 12}. The melting temperature was 1850 deg C for de system, consistent with the value in the phase diagram, and the wetting angle of 20 deg. The system (Yb{sub 2}O{sub 3}-Al{sub 2}O{sub 3}) is promising to make liquid phase sintering of SiC, for presenting a good result of wettability. (author)

450 {sup o}C isothermal section of the Fe-Zn-Si ternary phase diagram

Energy Technology Data Exchange (ETDEWEB)

Su, Xuping [Inst. of Materials Research, School of Mechanical Engineering, Xiangtan Univ., Xiangtan, Hunan (China); Univ. of Toronto, Dept. of Materials Science and Engineering, Toronto, Ontario (Canada); Tang, Nai-Yong [Cominco Ltd., Product Technology Centre, Mississauga, Ontario (Canada); Toguri, J.M. [Univ. of Toronto, Dept. of Materials Science and Engineering, Toronto, Ontario (Canada)

2001-07-01

The 450 {sup o}C isothermal section of the Fe-Zn-Si ternary phase diagram has been determined experimentally using optical microscopy, scanning electron microscopy (SEM) coupled with energy dispersive X-ray spectroscopy (EDS) and X-ray diffractometry. The focus of the work has been concentrated on the Zn-rich corner which is relevant to general galvanizing. The present study has confirmed the existence of the equilibrium state between the liquid, the {zeta} phase and the FeSi phase. This three phase equilibrium state prevents the equilibrium between the liquid and the {delta} phase suggested by some researchers. Experimental results indicate that Si solubility in all four binary Zn-Fe compounds is limited. The Fe solubility in molten Zn was found to decrease with increasing Si content in the melt. The liquid phase boundary was determined using a model based phenomenological approach. (author)

Liquid phase sintered SiC. Processing and transformation controlled microstructure tailoring

Directory of Open Access Journals (Sweden)

V.A. Izhevskyi

2000-10-01

Full Text Available Microstructure development and phase formation processes during sintering of silicon carbide based materials with AlN-Y2O3, AlN-Yb2O3, and AlN-La2O3 sintering additives were investigated. Densification of the materials occurred by liquid-phase sintering mechanism. Proportion of alpha- and beta-SiC powders in the initial mixtures was a variable parameter, while the molar ratio of AlN/RE2O3, and the total amount of additives (10 vol. % were kept constant. Shrinkage behavior during sintering in interrelation with the starting composition of the material and the sintering atmosphere was investigated by high temperature dilatometry. Kinetics of b-SiC to a-SiC phase transformation during post-sintering heat treatment at temperatures 1900-1950 °C was studied, the degree of phase transformation being determined by quantitative x-ray analysis using internal standard technique. Evolution of microstructure resulting from beta-SiC to alpha-SiC transformation was followed up by scanning electron microscopy on polished and chemically etched samples. Transformation-controlled grain growth mechanism similar to the one observed for silicon nitride based ceramics was established. Possibility of in-situ platelet reinforced dense SiC-based ceramics fabrication with improved mechanical properties by means of sintering was shown.

Phase separation in an ionomer glass

DEFF Research Database (Denmark)

Pedersen, Malene Thostrup; Tian, K.V.; Dobó-Nagy, C.

2015-01-01

The G338 ionomer glass is a fluoro-alumino-silicate system, which is used as the powder component of glass ionomer cements (GICs) in dental applications. However, despite progress in understanding the nature of this glass, chemical identity of its separated amorphous phases has not yet been...... amorphous phases in G388 are Ca/Na-Al-Si-O, Ca-Al-F and Ca-P-O-F phases, respectively. However, the exact chemical compositions of the three phases still require further exploration. The results of this work are important for understanding the impact of phase separation within ionomer glasses on the setting...... conclusively determined. In this work, we identify these phases by performing differential scanning calorimetry (DSC) and X-ray diffraction (XRD) analyses on both the as-received glass and heat-treated samples. We detected three glass transitions in the as-received G338 glass during DSC upscaning, implying...

Characterization of SiCf/SiC and CNT/SiC composite materials produced by liquid phase sintering

International Nuclear Information System (INIS)

Lee, J.K.; Lee, S.P.; Cho, K.S.; Byun, J.H.; Bae, D.S.

2011-01-01

This paper dealt with the microstructure and mechanical properties of SiC based composites reinforced with different reinforcing materials. The composites were fabricated using reinforcing materials of carbon nanotubes (CNT) and Tyranno Lox-M SiC chopped fibers. The volume fraction of carbon nanotubes was also varied in this composite system. An Al 2 O 3 -Y 2 O 3 powder mixture was used as a sintering additive in the consolidation of the SiC matrix. The characterization of the composites was investigated by means of SEM and three point bending tests. These composites showed a dense morphology of the matrix region, by the creation of a secondary phase. The composites reinforced with SiC chopped fibers possessed a flexural strength of about 400 MPa at room temperature. The flexural strength of the carbon nanotubes composites had a tendency to decrease with increased volume fraction of the reinforcing material.

Study of phase separation and crystallization phenomena in soda-lime borosilicate glass enriched in MoO3

International Nuclear Information System (INIS)

Magnin, M.

2009-09-01

Molybdenum oxide immobilization (MoO 3 , as fission product) is one of the major challenges in the nuclear glass formulation issues for high level waste solutions conditioning since many years, these solutions arising from spent nuclear fuel reprocessing. Phase separation and crystallisation processes may arise in molten glass when the MoO 3 content is higher than its solubility limit that may depend on glass composition. Molybdenum combined with other elements such as alkali and alkaline-earth may form crystalline molybdates, known as 'yellow phases' in nuclear glasses which may decrease the glass durability. In order to confine high level wastes (HLW) such as the fission product solutions arising from the reprocessing of high burn-up UOX-type nuclear spent fuels, a new glass composition (HLW glass) is being optimized. This work is devoted to the study of the origin and the mechanism of phase separation and crystallization phenomena induced by molybdenum oxide incorporation in the HLW glass. From microstructural and structural point of view, the molybdenum oxide behavior was studied in glass compositions belonging to the SiO 2 -B 2 O 3 - Na 2 O-CaO simplified system which constituted basis for the HLW glass formulation. The structural role of molybdenum oxide in borosilicate network explaining the phase separation and crystallization tendency was studied through the coupling of structural ( 95 Mo, 29 Si, 11 B, 23 Na MAS NMR, XRD) and microstructural (SEM, HRTEM) analysis techniques. The determination of phase separation (critical temperature) and crystallization (liquidus temperature) appearance temperatures by in situ viscosimetry and Raman spectroscopy experiments allowed us to propose a transformation scenario during melt cooling. These processes and the nature of the crystalline phases formed (CaMoO 4 , Na 2 MoO 4 ) that depend on the evolution of MoO 3 , CaO and B 2 O 3 contents were correlated with changes of sodium and calcium cations proportions in the

Making MgO/SiO2 Glasses By The Sol-Gel Process

Science.gov (United States)

Bansal, Narottam P.

1989-01-01

Silicon dioxide glasses containing 15 mole percent magnesium oxide prepared by sol-gel process. Not made by conventional melting because ingredients immiscible liquids. Synthesis of MgO/SiO2 glass starts with mixing of magnesium nitrate hexahydrate with silicon tetraethoxide, both in alcohol. Water added, and transparent gel forms. Subsequent processing converts gel into glass. Besides producing glasses of new composition at lower processing temperatures, sol-gel method leads to improved homogeneity and higher purity.

Elemental and isotopic (Si-{sup 29} and O-{sup 18}) tracing of glass alteration mechanisms

Energy Technology Data Exchange (ETDEWEB)

Verney-Carron, A.; Libourel, G.; Deloule, E. [CNRS, Ctr Rech Petrog and Geochim, UPR 2300, F-54501 Vandoeuvre Les Nancy (France); Valle, N. [Ctr Rech Publ Gabriel Lippmann, Dept Sci and Anal Mat, L-4422 Belvaux (Luxembourg); Sterpenich, J. [Univ H Poincare, G2R, CNRS, UMR 7566, F-54501 Vandoeuvre Les Nancy (France); Jollivet, P. [CEA Marcoule, DEN, Lab Comportement Long Terme, F-30207 Bagnols Sur Ceze (France)

2010-07-01

To better understand glass alteration mechanisms, especially alteration layers formation, leaching experiments of a borosilicate glass (SON68) doped with a different rare earth element (La, Ce, or Nd) with solutions rich in {sup 29}Si and {sup 18}O were carried out. The coupled analyses of glass, alteration products, and solution led to a complete elemental and isotopic ({sup 29}Si and {sup 18}O) budget. They revealed different behaviours of elements that depend not only on their structural role in the glass, but also on their affinity for alteration products (gel, phyllosilicates, phosphates). However, analyses of both glass and solution are not sufficient to describe the real exchanges occurring between glass and solution. The use of {sup 29}Si and {sup 18}O tracers gives new insights on the formation of alteration layers. During alteration the phyllosilicates records the isotopic variations of the leaching solution. Their isotopic signatures highlight a mechanism of dissolution/precipitation, which implies equilibrium between the secondary phases and the solution. On the other hand the gel isotopic signature, that is intermediate between the glass and the solution, substantiates the hypothesis that the gel is formed by hydrolysis/condensation reactions. This mechanism can thus explain the influence of the gel formation conditions (alteration conditions, solution saturation) on the structure (reorganisation) and texture (porosity) of this layer and on its protective effect. These hydrolysis/condensation reactions are also certainly involved in the aluminosilicate glass alteration and in the formation of palagonite. (authors)

Extremely improved InP template and GaInAsP system growth on directly-bonded InP/SiO2-Si and InP/glass substrate

International Nuclear Information System (INIS)

Matsumoto, Keiichi; Makino, Tatsunori; Kimura, Katsuya; Shimomura, Kazuhiko

2013-01-01

We have developed an ultrathin InP template with low defect density on SiO 2 -Si and glass substrate by employing wet etching and wafer direct bonding technique. We have demonstrated epitaxial growth on these substrates and GaInAs/InP multiple quantum well layers were grown by low pressure metal-organic vapor-phase epitaxy. Photoluminescence measurements of the layers show that they are optically active and we have obtained almost the same intensity from these substrates compared to the InP substrate. These results may be attributed to improvement of InP template quality and should provide further improvements in device performance realized on SiO 2 -Si and glass substrate. And, these are promising results in terms of integration of InP-based several functional optical devices on SiO 2 -Si and glass substrate. (copyright 2013 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

Study on spectroscopic properties and effects of tungsten ions in 2Bi2O3-3GeO2/SiO2 glasses.

Science.gov (United States)

Yu, Pingsheng; Su, Liangbi; Cheng, Junhua; Zhang, Xia; Xu, Jun

2017-04-01

The 2Bi 2 O 3 -3GeO 2 /SiO 2 glass samples have been prepared by the conventional melt quenching technique. XRD patterns, absorption spectra, excitation-emission spectra and Raman measurements were utilized to characterize the synthesized glasses. When substitute SiO 2 for GeO 2 , the 0.4Bi 2 O 3 -(0.4-0.1)GeO 2 -(0.2-0.5)SiO 2 glasses exhibit strong emission centered at about 475nm (under 300nm excitation), and the decay constants are within the scope of 20-40ns. W doping into 2Bi 2 O 3 -3SiO 2 glass could increase the emission intensity of 470nm, and the W-doped 2Bi 2 O 3 -3SiO 2 glass has shown another emission at about 433nm with much shorter decay time (near 10ns). The 2Bi 2 O 3 -3GeO 2 /SiO 2 glass system could be the possible candidate for scintillator in high energy physics applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

Crystallization behavior of (1 - x)Li{sub 2}O.xNa{sub 2}O.Al{sub 2}O{sub 3}.4SiO{sub 2} glasses

Energy Technology Data Exchange (ETDEWEB)

Wang, Moo-Chin [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 807, Taiwan (China); Cheng, Chih-Wei; Chang, Kuo-Ming [Department of Mechanical Engineering, National Kaohsiung University of Applied Sciences, 415 Chien-Kung Road, Kaohsiung 80782, Taiwan (China); Hsi, Chi-Shiung, E-mail: chsi@nuu.edu.t [Department of Materials Science and Engineering, National United University, 1 Lien-Da, Kung-Ching Li, Miao-Li 36003, Taiwan (China)

2010-07-02

The crystallization behavior of the (1 - x)Li{sub 2}O.xNa{sub 2}O.Al{sub 2}O{sub 3}.4SiO{sub 2} glasses has been investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), electron diffraction (ED) and energy dispersive spectroscopy (EDS). The crystalline phase was composed of {beta}-spodumene. The isothermal crystallization kinetics of {beta}-spodumene from the (1 - x)Li{sub 2}O.xNa{sub 2}O.Al{sub 2}O{sub 3}.4SiO{sub 2} glasses has also been studied by a quantitative X-ray diffraction method. The activation energy of {beta}-spodumene formation decreases from 359.2 to 317.8 kJ/mol when the Na{sub 2}O content increases from 0 to 0.4 mol and it increases from 317.8 to 376.9 kJ/mol when the Na{sub 2}O content increases from 0.4 to 0.6 mol. The surface nucleation and plate-like growth were dominant in the crystallization of the (1 - x)Li{sub 2}O.xNa{sub 2}O.Al{sub 2}O{sub 3}.4SiO{sub 2} glasses.

Glass-ceramic enamels derived from the Li2O-Na2O-Al2O3-TiO2-SiO2 system

Directory of Open Access Journals (Sweden)

SNEZANA R. GRUJIC

2002-02-01

Full Text Available The results of research on the conditions for obtaining model glass-ceramic enamels, derived from the basic Li2O-Na2O-Al2O3-TiO2-SiO2 system, by varying the initial composition and thermal treatment conditions, are presented in this paper. Segregation of the crystal phases in the glassy-matrix was carried out during subsequent thermal treatment. The formation of different crystal phases was evidenced through the results of differential-thermal analysis and X-ray powder diffraction analysis.

The structure of MgO-SiO2 glasses at elevated pressure.

Science.gov (United States)

Wilding, Martin; Guthrie, Malcolm; Kohara, Shinji; Bull, Craig L; Akola, Jaakko; Tucker, Matt G

2012-06-06

The magnesium silicate system is an important geophysical analogue and neutron diffraction data from glasses formed in this system may also provide an initial framework for understanding the structure-dependent properties of related liquids that are important during planetary formation. Neutron diffraction data collected in situ for a single composition (38 mol% SiO(2)) magnesium silicate glass sample shows local changes in structure as pressure is increased from ambient conditions to 8.6 GPa at ambient temperature. A method for obtaining the fully corrected, total structure factor, S(Q), has been developed that allows accurate structural characterization as this weakly scattering glass sample is compressed. The measured S(Q) data indicate changes in chemical ordering with pressure and the real-space transforms show an increase in Mg-O coordination number and a distortion of the local environment around magnesium ions. We have used reverse Monte Carlo methods to compare the high pressure and ambient pressure structures and also compare the high pressure form with a more silica-poor glass (Mg(2)SiO(4)) that represents the approach to a more dense, void-free and topologically ordered structure. The Mg-O coordination number increases with pressure and we also find that the degree of continuous connectivity of Si-O bonds increases via a collapse of interstices.

Bioactivity and cell proliferation in radiopaque gel-derived CaO-P2O5-SiO2-ZrO2 glass and glass-ceramic powders.

Science.gov (United States)

Montazerian, Maziar; Yekta, Bijan Eftekhari; Marghussian, Vahak Kaspari; Bellani, Caroline Faria; Siqueira, Renato Luiz; Zanotto, Edgar Dutra

2015-10-01

In this study, 10 mol% ZrO2 was added to a 27CaO-5P2O5-68SiO2 (mol%) base composition synthesized via a simple sol-gel method. This composition is similar to that of a frequently investigated bioactive gel-glass. The effects of ZrO2 on the in vitro bioactivity and MG-63 cell proliferation of the glass and its derivative polycrystalline (glass-ceramic) powder were investigated. The samples were characterized using thermo-gravimetric and differential thermal analysis (TG/DTA), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM) coupled to energy dispersive X-ray spectroscopy (EDS). Release of Si, Ca, P and Zr into simulated body fluid (SBF) was determined by inductively coupled plasma (ICP). Upon heat treatment at 1000 °C, the glass powder crystallized into an apatite-wollastonite-zirconia glass-ceramic powder. Hydroxycarbonate apatite (HCA) formation on the surface of the glass and glass-ceramic particles containing ZrO2 was confirmed by FTIR and SEM. Addition of ZrO2 to the base glass composition decreased the rate of HCA formation in vitro from one day to three days, and hence, ZrO2 could be employed to control the rate of apatite formation. However, the rate of HCA formation on the glass-ceramic powder containing ZrO2 crystal was equal to that in the base glassy powder. Tests with a cultured human osteoblast-like MG-63 cells revealed that the glass and glass-ceramic materials stimulated cell proliferation, indicating that they are biocompatible and are not cytotoxic in vitro. Moreover, zirconia clearly increased osteoblast proliferation over that of the Zr-free samples. This increase is likely associated with the lower solubility of these samples and, consequently, a smaller variation in the media pH. Despite the low solubility of these materials, bioactivity was maintained, indicating that these glassy and polycrystalline powders are potential candidates for bone graft substitutes and bone cements with

Structural variations and dielectric properties of (Bi1-xL ax ) 2Si O5 (0 ≤x ≤0.1 ): Polycrystallines synthesized by crystallization of Bi-Si-O and Bi-La-Si-O glasses

Science.gov (United States)

Taniguchi, Hiroki; Tatewaki, Shingo; Yasui, Shintaro; Fujii, Yasuhiro; Yamaura, Jun-ichi; Terasaki, Ichiro

2018-04-01

This paper focuses on effects of isovalent La substitution on the crystal structure and dielectric properties of ferroelectric B i2Si O5 . Polycrystalline samples of (Bi1-xL ax ) 2Si O5 are synthesized by crystallization of Bi-Si-O and Bi-La-Si-O glasses with a composition range of 0 ≤x ≤0.1 . The crystal structure changes from monoclinic to tetragonal with increasing La-substitution rate x at room temperature. This structural variation stems from the change in orientation of Si O4 tetrahedra that form one-dimensional chains when they are in the ordered configuration, thus suggesting that lone-pair electrons play an important role in sustaining one-dimensional chains of Si O4 tetrahedra. Synchronizing with the disordering of Si O4 chains, ferroelectric phase transition temperature of (Bi1-xL ax ) 2Si O5 sharply decreases as x increases, and ferroelectricity finally vanishes at around x =0.03 . The present results demonstrate that lone-pair electrons of Bi play an important role in the ferroelectricity of B i2Si O5 through propping the ordered structure of one-dimensional Si O4 chains with stereochemical activity. Furthermore, an additional phase transition has been first discovered in the low-temperature region of (Bi1-xL ax ) 2Si O5 with x ≤0.01 , where the ordered one-dimensional Si O4 chains remain.

Effect of SiO2/B2O3 Ratio on the Crystallization Behavior and Dielectric Properties of Barium Strontium Titanate Glass-Ceramics Prepared by Sol-Gel Process

Science.gov (United States)

Chen, Yongzhou; Zhang, Yong; Song, Xiaozhen; Shen, Ziqin; Zhang, Tianyuan

2018-05-01

Ferroelectric glass-ceramics, with a basic composition 90 wt.% (Ba0.65Sr0.35)TiO3-10 wt.% (B2O3-nSiO2) (n = 0.5, 1, 3, 5) were synthesized by the sol-gel method and their phase development and dielectric properties were investigated by differential thermal analysis, x-ray diffraction, field emission scanning electron microscopy, dielectric temperature curves and impedance spectroscopy. From the differential thermal analysis, glass transition and crystallization behavior can be observed. From the x-ray diffraction study, two crystalline phases (Ba,Sr)TiO3 and Ba2TiSi2O8 were formed over the entire composition range of the glass-ceramics. In addition, the main crystal phase has undergone a transformation from (Ba,Sr)TiO3 to Ba2TiSi2O8 with the increase of n. A typical structure in which the crystal phase was surrounded by a glassy matrix has been observed in the scanning electron microscope images. As a result of temperature dependent dielectric property measurements, the dielectric constant increased obviously with the increase of n from 0.5 to 1. Further increasing n led to a reduction of the dielectric constant, which is in coincidence with the variation of the intensity of (Ba,Sr)TiO3 phase with n. According to the impedance spectroscopy analysis and the activation energy calculation, the relaxation peak in both Z″ and M″ data should be attributed to the crystal-glass interface, and the change of conduction mechanism with the increase of SiO2/B2O3 ratio may be attributed to the corresponding transition of the main crystal phase.

Electronic states of SiO2-MxOy (MxOy=P205, TiO2 and ZrO2) glasses

Energy Technology Data Exchange (ETDEWEB)

Kowada, Y [Hyogo Univ. of Teacher Education, Hyogo (Japan); Adachi, H [Kyoto Univ. (Japan). Faculty of Engineering; Minami, T [Univ. of Osaka Prefecture, Osaka (Japan). Faculty of Engineering

1993-12-01

Using the sol-gel method the surface of metal and glass substrates can be modified. For example, stainless steel sheets coated with the SiO2-ZrO2 glass films have higher resistance to corrosion and oxidation. The coating films contain high concentration of alkali ions diffusing from the glass substrates. It suggests that the sodium ions are trapped strongly within the coating films and are blocked to further diffuse to the surface. This behavior must be associated with the chemical bonding around the sodium ions in the SiO2-TiO2 and SiO2-ZrO2 films. For better understanding of the chemical bonding in the glasses, the electronic states of the SiO2-MxOy glasses were calculated by means of the DV-Xa cluster method. In this paper, the calculation method is explained, the results are discussed and the conclusion is stated. 17 refs., 6 figs.

Raman and optical absorption spectroscopic investigation of Yb-Er codoped phosphate glasses containing SiO2

Institute of Scientific and Technical Information of China (English)

Youkuo Chen; Lei Wen; Lili Hu; Wei Chen; Y. Guyot; G. Boulon

2009-01-01

Yb-Er codoped Na2O-Al2O3-P2Os-xSiO2 glasses containing 0 鈥? 20 mol% SiO2 were prepared successfully. The addition of SiO2 to the phosphate glass not only lengthens the bond between P5+ and non-bridging oxygen but also reduces the number of P=O bond. In contrast with silicate glass in which there is only four-fold coordinated Si4+, most probably there coexist [SiO4] tetrahedron and [SiO6] octahedron in our glasses. Within the range of 0 鈥? 20 mol% SiO2 addition, the stimulated emission cross-section of Er3+ ion only decreases no more than 10%. The Judd-Ofelt intensity parameters of Er3+, 惟.2 does not change greatly, but 惟74 and 惟6 decrease obviously with increasing SiO2 addition, because the bond between Er + and O2- is more strongly covalently bonded.

Doping of low-T{sub g} phosphate glass with Al{sub 2}O{sub 3}, B{sub 2}O{sub 3} and SiO{sub 2}: Part I- effect on glass property and stability

Energy Technology Data Exchange (ETDEWEB)

Rajbhandari, P., E-mail: p.rajbhandari@sheffield.ac.uk [UCCS UMR-CNRS 8181, Universite de Lille1, Villeneuve d' Ascq (France); Montagne, L. [UCCS UMR-CNRS 8181, Universite de Lille1, Villeneuve d' Ascq (France); Tricot, G. [UCCS UMR-CNRS 8181, Universite de Lille1, Villeneuve d' Ascq (France); LASIR UMR-CNRS 8516, Universite de Lille1, Villeneuve d' Ascq (France)

2016-11-01

A zinc alkali pyrophosphate system 46.6ZnO-20Na{sub 2}O-33.5P{sub 2}O{sub 5} presenting low-T{sub g} (339 °C) and good thermal stability has been doped with (1–4) mol% of Al{sub 2}O{sub 3}, B{sub 2}O{sub 3} and SiO{sub 2} to improve the stability of the glass with a minimal increase in glass transition temperature (T{sub g}). XRD and 1D {sup 31}P solid state NMR were used to monitor the isothermal crystallization process occurring at 130 °C above T{sub g}. If the Al{sub 2}O{sub 3} and B{sub 2}O{sub 3} doping significantly improved thermal stability, this property was marginally affected by SiO{sub 2} doping. Viscosity measurements were performed to observe the crystallization effects induced by the doping. It is noteworthy that the T{sub g} values of all the doped compositions with improved stability presented in this work are below 400 °C. Raman spectroscopy, 1D {sup 31}P, {sup 27}Al, {sup 11}B and {sup 29}Si solid state NMR were carried out to determine the structural modifications and coordination states of the doping elements all along the composition line. - Highlights: • Low-Tg phosphate glasses doped with Al{sub 2}O{sub 3}, B{sub 2}O{sub 3} and SiO{sub 2} have been formulated. • Thermal stability of the glass has been improved significantly. • The structural modification induced by doping elements has been studied by employing solid state NMR technique.

Vibrational mode frequencies of silica species in SiO2-H2O liquids and glasses from ab initio molecular dynamics.

Science.gov (United States)

Spiekermann, Georg; Steele-MacInnis, Matthew; Schmidt, Christian; Jahn, Sandro

2012-04-21

Vibrational spectroscopy techniques are commonly used to probe the atomic-scale structure of silica species in aqueous solution and hydrous silica glasses. However, unequivocal assignment of individual spectroscopic features to specific vibrational modes is challenging. In this contribution, we establish a connection between experimentally observed vibrational bands and ab initio molecular dynamics (MD) of silica species in solution and in hydrous silica glass. Using the mode-projection approach, we decompose the vibrations of silica species into subspectra resulting from several fundamental structural subunits: The SiO(4) tetrahedron of symmetry T(d), the bridging oxygen (BO) Si-O-Si of symmetry C(2v), the geminal oxygen O-Si-O of symmetry C(2v), the individual Si-OH stretching, and the specific ethane-like symmetric stretching contribution of the H(6)Si(2)O(7) dimer. This allows us to study relevant vibrations of these subunits in any degree of polymerization, from the Q(0) monomer up to the fully polymerized Q(4) tetrahedra. Demonstrating the potential of this approach for supplementing the interpretation of experimental spectra, we compare the calculated frequencies to those extracted from experimental Raman spectra of hydrous silica glasses and silica species in aqueous solution. We discuss observed features such as the double-peaked contribution of the Q(2) tetrahedral symmetric stretch, the individual Si-OH stretching vibrations, the origin of the experimentally observed band at 970 cm(-1) and the ethane-like vibrational contribution of the H(6)Si(2)O(7) dimer at 870 cm(-1).

SAW propagation characteristics of TeO3/3C-SiC/LiNbO3 layered structure

Science.gov (United States)

Soni, Namrata D.

2018-04-01

Surface acoustic wave (SAW) devices based on Lithium Niobate (LiNbO3) single crystal are advantageous because of its high SAW phase velocity, electromechanical coupling coefficient and cost effectiveness. In the present work a new multi-layered TeO3/3C-SiC/128° Y-X LiNbO3 SAW device has been proposed. SAW propagation properties such as phase velocity, coupling coefficient and temperature coefficient of delay (TCD) of the TeO3/SiC/128° Y-X LiNbO3 multi layered structure is examined using theoretical calculations. It is found that the integration of 0.09λ thick 3C-SiC over layer on 128° Y-X LiNbO3 increases its electromechanical coupling coefficient from 5.3% to 9.77% and SAW velocity from 3800 ms‑1 to 4394 ms‑1. The SiC/128° Y-X LiNbO3 bilayer SAW structure exhibits a high positive TCD value. A temperature stable layered SAW device could be obtained with introduction of 0.007λ TeO3 over layer on SiC/128° Y-X LiNbO3 bilayer structure without sacrificing the efficiency of the device. The proposed TeO3/3C-SiC/128° Y-X LiNbO3 multi-layered SAW structure is found to be cost effective, efficient, temperature stable and suitable for high frequency application in harsh environment.

The influence of glass composition on crystalline phase stability in glass-ceramic wasteforms

International Nuclear Information System (INIS)

Maddrell, Ewan; Thornber, Stephanie; Hyatt, Neil C.

2015-01-01

Highlights: • Crystalline phase formation shown to depend on glass matrix composition. • Zirconolite forms as the sole crystalline phase only for most aluminous glasses. • Thermodynamics indicate that low silica activity glasses stabilise zirconolite. - Abstract: Zirconolite glass-ceramic wasteforms were prepared using a suite of Na 2 O–Al 2 O 3 –B 2 O 3 –SiO 2 glass matrices with variable Al:B ratios. Zirconolite was the dominant crystalline phase only for the most alumina rich glass compositions. As the Al:B ratio decreased zirconolite was replaced by sphene, zircon and rutile. Thermodynamic data were used to calculate a silica activity in the glass melt below which zirconolite is the favoured crystalline phase. The concept of the crystalline reference state of glass melts is then utilised to provide a physical basis for why silica activity varies with the Al:B ratio

Internal Friction of (SiO2)1-x (GeO2)x Glasses

OpenAIRE

Kosugi , T.; Kobayashi , H.; Kogure , Y.

1996-01-01

Internal friction of (SiO2)1-x (GeO2)x glasses (x = 0, 5, 10, 24 and 100 mole%) is measured at temperatures between 1.6 and 280 K. The data are filted with the equations for thermally activated relaxation with distributing activation energies in symmetrical double-well potentials. From the determined relaxation strength spectra for each sample, the contributions from each type of microscopic structural units are calculated assuming that transverse motion of the bridging O atom in Si-O-Si, Si-...

Influence of heat treatments upon the mechanical properties and in vitro bioactivity of ZrO2-toughened MgO-CaO-SiO2-P2O5-CaF2 glass-ceramics.

Science.gov (United States)

Li, Huan-Cai; Wang, Dian-Gang; Meng, Xiang-Guo; Chen, Chuan-Zhong

2014-09-01

Zirconia-toughened MgO-CaO-SiO2-P2O5-CaF2 glass-ceramics are prepared using sintering techniques, and a series of heat treatment procedures are designed to obtain a glass-ceramic with improved properties. The crystallization behavior, phase composition, and morphology of the glass-ceramics are characterized. The bending strength, elastic modulus, fracture toughness, and microhardness of the glass-ceramics are investigated, and the effect mechanism of heat treatments upon the mechanical properties is discussed. The bioactivity of glass-ceramics is then evaluated using the in vitro simulated body fluid (SBF) soaking test, and the mechanism whereby apatite forms on the glass-ceramic surfaces in the SBF solution is discussed. The results indicate that the main crystal phase of the G-24 sample undergoing two heat treatment procedures is Ca5(PO4)3F (fluorapatite), and those of the G-2444 sample undergoing four heat treatment procedures are Ca5(PO4)3F and β-CaSiO3 (β-wollastonite). The heat treatment procedures are found to greatly influence the mechanical properties of the glass-ceramic, and an apatite layer is induced on the glass-ceramic surface after soaking in the SBF solution.

Densification of MgSiO3 glass with pressure and temperature

DEFF Research Database (Denmark)

Yamada, A; Gaudio, Sarah; Lesher, Charles

2010-01-01

The density and structure of MgSiO3 glass (v-En) recovered from a series of annealing experiments up to 1000°C at 2.0, 5.5 and 8.5 GPa have been investigated using Archimedes' method and Raman spectroscopy, respectively. The densities of recovered glasses are found to be a complex function...... of pressure and temperature. At room temperature, compression up to 8.5 GPa, followed by decompression, yields a glass with a density within 0.6 % of the 1-atm value. Likewise, the 1-atm density is fully recovered in glass heated up to ~500°C at 2.0 GPa at higher pressures. A sharp increase in recovered...... density is observed between 500°C and 800°C at 2.0 GPa, 200°C and 500°C at 5.5 GPa and from room-T and 300°C at 8.5 GPa. At higher annealing temperatures the changes in density are more modest. This break in slope occurs for a glass density of 2.89 g/cm3 at 2.0 GPa and 2.95 g/cm3 at 5.5 and 8.5 GPa. Above...

B2O3/SiO2 substitution effect on structure and properties of Na2O-CaO-SrO-P2O5-SiO2 bioactive glasses from molecular dynamics simulations.

Science.gov (United States)

Ren, Mengguo; Lu, Xiaonan; Deng, Lu; Kuo, Po-Hsuen; Du, Jincheng

2018-05-23

The effect of B2O3/SiO2 substitution in SrO-containing 55S4.3 bioactive glasses on glass structure and properties, such as ionic diffusion and glass transition temperature, was investigated by combining experiments and molecular dynamics simulations with newly developed potentials. Both short-range (such as bond length and bond angle) and medium-range (such as polyhedral connection and ring size distribution) structures were determined as a function of glass composition. The simulation results were used to explain the experimental results for glass properties such as glass transition temperature and bioactivity. The fraction of bridging oxygen increased linearly with increasing B2O3 content, resulting in an increase in overall glass network connectivity. Ion diffusion behavior was found to be sensitive to changes in glass composition and the trend of the change with the level of substitution is also temperature dependent. The differential scanning calorimetry (DSC) results show a decrease in glass transition temperature (Tg) with increasing B2O3 content. This is explained by the increase in ion diffusion coefficient and decrease in ion diffusion energy barrier in glass melts, as suggested by high-temperature range (above Tg) ion diffusion calculations as B2O3/SiO2 substitution increases. In the low-temperature range (below Tg), the Ea for modifier ions increased with B2O3/SiO2 substitution, which can be explained by the increase in glass network connectivity. Vibrational density of states (VDOS) were calculated and show spectral feature changes as a result of the substitution. The change in bioactivity with B2O3/SiO2 substitution is discussed with the change in pH value and release of boric acid into the solution.

Phase selection and microstructure in directional solidification of glass forming Pd-Si-Cu alloys

Science.gov (United States)

Huo, Yang

Phase selection and microstructure formation during the rapid solidification of alloy melts has been a topic of substantial interest over the last several decades, attributed mainly to the access to novel structures involving metastable crystalline and non-crystalline phases. In this work, Bridgeman type directional solidification was conducted in Pd-Si-Cu glass forming system to study such cooling rate dependent phase transition and microstructure formation. The equilibrium state for Pd-Si-Cu ternary system was investigated through three different works. First of all, phase stabilities for Pd-Si binary system was accessed with respects of first-principles and experiments, showing Pd5Si, Pd9Si2, Pd3Si and Pd 2Si phase are stable all way to zero Kevin while PdSi phase is a high temperature stable phase, and Pd2Si phase with Fe2P is a non-stoichiometry phase. A thermodynamic database was developed for Pd-Si system. Second, crystal structures for compounds with ternary compositions were studied by XRD, SEM and TEM, showing ordered and disordered B2/bcc phases are stable in Pd-rich part. At last, based on many phase equilibria and phase transitions data, a comprehensive thermodynamic discrption for Pd-Si-Cu ternary system was first time to be developed, from which different phase diagrams and driving force for kinetics can be calculated. Phase selection and microstructure formation in directional solidification of the best glass forming composition, Pd 77.5Si16.5Cu6, in this system with growth velocities from 0.005 to 7.5mm/s was systematically studied and the solidification pathways at different conditions were interpreted from thermodynamic simulation. The results show that for growth velocities are smaller than 0.1mm/s Pd 3Si phase is primary phase and Pd9Si2 phase is secondary phase, the difficulty for Pd9Si2 phase nucleation gives rise to the formation of two different eutectic structure. For growth velocities between 0.4 and 1mm/s, instead of Pd3Si phase, Pd9Si2

Comparative study of gamma ray shielding and some properties of PbO–SiO2–Al2O3 and Bi2O3–SiO2–Al2O3 glass systems

International Nuclear Information System (INIS)

Singh, K.J.; Kaur, Sandeep; Kaundal, R.S.

2014-01-01

Gamma-ray shielding properties have been estimated in terms of mass attenuation coefficient, half value layer and mean free path values, whereas, structural studies have been performed in terms of density, optical band gap, glass transition temperature and longitudinal ultrasonic velocity parameters. X-ray diffraction, UV–visible, DSC and ultrasonic techniques have been used to explore the structural properties of PbO–SiO 2 –Al 2 O 3 and Bi 2 O 3 –SiO 2 –Al 2 O 3 glass systems. - Highlights: • Bi 2 O 3 –SiO 2 –Al 2 O 3 and PbO–SiO 2 –Al 2 O 3 glasses can replace conventional concretes as gamma-ray shielding materials. • Gamma-ray shielding properties improve with the addition of heavy metals. • Rigidity deteriorates with the increase in the content of heavy metals. • Bi 2 O 3 –SiO 2 –Al 2 O 3 glass system is better than PbO–SiO 2 –Al 2 O 3 glass system in terms of gamma-ray shielding as well as structural properties

The effect of TiO2 on nucleation and crystallization of a Li2O-Al2O3-SiO2 glass investigated by XANES and STEM.

Science.gov (United States)

Kleebusch, Enrico; Patzig, Christian; Krause, Michael; Hu, Yongfeng; Höche, Thomas; Rüssel, Christian

2018-02-13

Glass ceramics based on Li 2 O/Al 2 O 3 /SiO 2 are of high economic importance, as they often show very low coefficients of thermal expansion. This enables a number of challenging applications, such as cooktop panels, furnace windows or telescope mirror blanks. Usually, the crystallization of the desired LAS crystal phases within the glasses must be tailored by a careful choice of crystallization schedule and type of nucleation agents to be used. The present work describes the formation of nanocrystalline TiO 2 within an LAS base composition that contains solely TiO 2 as nucleating agent. Using a combination of scanning transmission electron microscopy as well as X-ray absorption spectroscopy, it is found that a mixture of four- and six-fold coordinated Ti 4+ ions exists already within the glass. Heating of the glass to 740 °C immediately changes this ratio towards a high content of six-fold coordinated Ti, which accumulates in liquid-liquid phase-separation droplets. During the course of thermal treatment, these droplets eventually evolve into nanocrystalline TiO 2 precipitations, in which Ti 4+ is six-fold coordinated. Thus, it is shown that the nucleation of nanocrystalline TiO 2 is initiated by a gradual re-arrangement of the Ti ions in the amorphous, glassy matrix, from a four-fold towards a six-fold coordination.

Synthesis, bioactivity and preliminary biocompatibility studies of glasses in the system CaO-MgO-SiO2-Na2O-P2O5-CaF2.

Science.gov (United States)

Tulyaganov, D U; Agathopoulos, S; Valerio, P; Balamurugan, A; Saranti, A; Karakassides, M A; Ferreira, J M F

2011-02-01

New compositions of bioactive glasses are proposed in the CaO-MgO-SiO(2)-Na(2)O-P(2)O(5)-CaF(2) system. Mineralization tests with immersion of the investigated glasses in simulated body fluid (SBF) at 37°C showed that the glasses favour the surface formation of hydroxyapatite (HA) from the early stages of the experiments. In the case of daily renewable SBF, monetite (CaHPO(4)) formation competed with the formation of HA. The influence of structural features of the glasses on their mineralization (bioactivity) performance is discussed. Preliminary in vitro experiments with osteoblasts' cell-cultures showed that the glasses are biocompatible and there is no evidence of toxicity. Sintering and devitrification studies of glass powder compacts were also performed. Glass-ceramics with attractive properties were obtained after heat treatment of the glasses at relatively low temperatures (up to 850°C).

Dy3+-doped nano-glass ceramics comprising NaAlSiO4 and NaY9Si6O26 nanocrystals for white light generation

International Nuclear Information System (INIS)

Bagga, Ruchika; Achanta, Venu Gopal; Goel, Ashutosh; Ferreira, José M.F.; Singh, Narinder Pal; Singh, Davinder Paul; Falconieri, Mauro; Sharma, Gopi

2013-01-01

Highlights: ► Environment safe glass ceramics were fabricated via heat treatment. ► Optical and structural properties were studied before and after heat treatment. ► White light generation with single RE 3+ ion-doping was observed under UV excitation. ► Emission color temperature was between fluorescent tube and daylight values. - Abstract: The radiative emission properties of the Dy 3+ ions in oxyfluoride glasses and glass ceramics have been investigated for the generation of white light. The X-ray diffraction pattern of the glass ceramics reveals the presence of NaAlSiO 4 nanocrystals along with secondary phase of NaY 9 Si 6 O 26 in the glass matrix after a suitable thermal treatment of the pristine glasses. Intense white light emission has been observed when the samples are excited with 350 nm light. Yellow to blue emission intensity ratios and chromaticity color coordinates have been determined from the visible luminescence spectra. All color coordinates are found to lie in the white region of the chromaticity color diagram proposing the suitability of the present studied materials for color display devices.

Thermal phase separation of ZrSiO4 thin films and frequency- dependent electrical characteristics of the Al/ZrSiO4/p-Si/Al MOS capacitors

Science.gov (United States)

Lok, R.; Kaya, S.; Yilmaz, E.

2018-05-01

In this work, the thermal phase separation and annealing optimization of ZrSiO4 thin films have been carried out. Following annealing optimization, the frequency-dependent electrical characteristics of the Al/ZrSiO4/p-Si/Al MOS capacitors were investigated in detail. The chemical evolution of the films under various annealing temperatures was determined by Fourier transform infrared spectroscopy (FTIR) measurements. The phase separation was determined by x-ray diffraction (XRD) measurements. The electrical parameters were determined via the capacitance–voltage (C–V), conductance–voltage (G/ω) and leakage-current–voltage (Ig–Vg ). The results demonstrate that zirconium silicate formations are present at 1000 °C annealing with the SiO2 interfacial layer. The film was in amorphous form after annealing at 250 °C. The tetragonal phases of ZrO2 were obtained after annealing at 500 °C. When the temperature approaches 750 °C, transitions from the tetragonal phase to the monoclinic phase were observed. The obtained XRD peaks after 1000 °C annealing matched the crystalline peaks of ZrSiO4. This means that the crystalline zirconium dioxide in the structure has been converted into a crystalline silicate phase. The interface states increased to 5.71 × 1010 and the number of border traps decreased to 7.18 × 1010 cm‑2 with the increasing temperature. These results indicate that an excellent ZrSiO4/Si interface has been fabricated. The order of the leakage current varied from 10‑9 Acm‑2 to 10‑6 Acm‑2. The MOS capacitor fabricated with the films annealed at 1000 °C shows better behavior in terms of its structural, chemical and electrical properties. Hence, detailed frequency-dependent electrical characteristics were performed for the ZrSiO4 thin film annealed at 1000 °C. Very slight capacitance variations were observed under the frequency variations. This shows that the density of frequency-dependent charges is very low at the ZrSiO4/Si interface. The

Si-to-Si wafer bonding using evaporated glass

DEFF Research Database (Denmark)

Reus, Roger De; Lindahl, M.

1997-01-01

Anodic bonding of Si to Si four inch wafers using evaporated glass was performed in air at temperatures ranging from 300°C to 450°C. Although annealing of Si/glass structures around 340°C for 15 minutes eliminates stress, the bonded wafer pairs exhibit compressive stress. Pull testing revealed...

Thermal properties and crystallization of lithium–mica glass and glass-ceramics

International Nuclear Information System (INIS)

Nia, A. Faeghi

2013-01-01

Highlights: • Two groups of Li–mica glass-ceramics, have been compared. • By controlling the glass composition, crystalline lepidolite was obtained. • The T p of Li–mica was through the previous virgilite and eucryptite phase. - Abstract: The purpose of this study was the synthesis of two groups of Li–mica glass-ceramics denoted by lepidolite (Al 2.5 F 2 KLi 1.5 O 10 Si 3 ) and Li-phlogopite (LiMg 3 AlSi 3 O 10 F 2 ). The studied system was SiO 2 –Al 2 O 3 –MgO–K 2 O–Li 2 O. A total of 3 compositions were prepared. Bulk casted glasses and sintered glass-ceramics of Li-phlogopite and lepidolite systems, were prepared. Eucryptite and virgilite were two prior phases of lepidolite and Li-phlogopite crystallization. It was shown that the obtained glass-ceramics have lower TEC than corresponding glasses. Sinterability of lepidolite glass-ceramic was shown that improved by increasing the Al 2 O 3 content in glass composition. TEC and microhardness values were α = 6.08 × 10 −6 /°C, 755 ± 11.1, α = 7.86 × 10 −6 /°C, 739 ± 7.4 and α = 5.05 × 10 −6 /°C, 658 ± 6.2 HV for Li-lep, Klep1 and Klep2 glasses, respectively

Homogeneity of peraluminous SiO2-B2O3-Al2O3-Na2O-CaO-Nd2O3 glasses: Effect of neodymium content

International Nuclear Information System (INIS)

Gasnier, E.; Bardez-Giboire, I.; Massoni, N.; Montouillout, V.; Pellerin, N.; Allix, M.; Ory, S.; Cabie, M.; Poissonnet, S.; Massiot, D.

2014-01-01

Considering the interest of developing new glass matrices able to immobilize higher concentration of high level nuclear wastes than currently used nuclear borosilicate compositions, glasses containing high rare earth contents are of particular interest. This study focuses on a peraluminous alumino borosilicate system SiO 2 -B 2 O 3 -Al 2 O 3 -Na 2 O-CaO-Nd 2 O 3 defined by a per-alkaline/peraluminous ratio RP = ([Na 2 O] + [CaO])/ ([Na 2 O] + [CaO] + [Al 2 O 3 ]) ≤ 0.5. Samples with various contents of Nd 2 O 3 from 0 to 10 mol% were studied using DSC, XRD, SEM, TEM, STEM and EMPA methods. The glasses present a high thermal stability even after a slow cooling treatment from the melt. Only a slight mullite crystallization is detected for low Nd 2 O 3 content (≤2.3 mol%) and crystallization of a neodymium borosilicate crystalline phase combined to a phase separation occurred at high Nd 2 O 3 content (≥8 mol%). The solubility of neodymium in the presence of aluminum is demonstrated, with higher neodymium incorporation amounts than in per-alkaline glasses. (authors)

Bioactivity and cytotoxicity of glass and glass-ceramics based on the 3CaO·P₂O₅--SiO₂--MgO system.

Science.gov (United States)

Daguano, Juliana K M F; Rogero, Sizue O; Crovace, Murilo C; Peitl, Oscar; Strecker, Kurt; Dos Santos, Claudinei

2013-09-01

The mechanical strength of bioactive glasses can be improved by controlled crystallization, turning its use as bulk bone implants viable. However, crystallization may affect the bioactivity of the material. The aim of this study was to develop glass-ceramics of the nominal composition (wt%) 52.75(3CaO·P₂O₅)-30SiO₂-17.25MgO, with different crystallized fractions and to evaluate their in vitro cytotoxicity and bioactivity. Specimens were heat-treated at 700, 775 and 975 °C, for 4 h. The major crystalline phase identified was whitlockite, an Mg-substituted tricalcium phosphate. The evaluation of the cytotoxicity was carried out by the neutral red uptake methodology. Ionic exchanges with the simulated body fluid SBF-K9 acellular solution during the in vitro bioactivity tests highlight the differences in terms of chemical reactivity between the glass and the glass-ceramics. The effect of crystallinity on the rates of hydroxycarbonate apatite (HCA) formation was followed by Fourier transformed infrared spectroscopy. Although all glass-ceramics can be considered bioactive, the glass-ceramic heat-treated at 775 °C (V775-4) presented the most interesting result, because the onset for HCA formation is at about 24 h and after 7 days the HCA layer dominates completely the spectrum. This occurs probably due to the presence of the whitlockite phase (3(Ca,Mg)O·P₂O₅). All samples were considered not cytotoxic.

Reaction mechanisms at 4H-SiC/SiO2 interface during wet SiC oxidation

Science.gov (United States)

Akiyama, Toru; Hori, Shinsuke; Nakamura, Kohji; Ito, Tomonori; Kageshima, Hiroyuki; Uematsu, Masashi; Shiraishi, Kenji

2018-04-01

The reaction processes at the interface between SiC with 4H structure (4H-SiC) and SiO2 during wet oxidation are investigated by electronic structure calculations within the density functional theory. Our calculations for 4H-SiC/SiO2 interfaces with various orientations demonstrate characteristic features of the reaction depending on the crystal orientation of SiC: On the Si-face, the H2O molecule is stable in SiO2 and hardly reacts with the SiC substrate, while the O atom of H2O can form Si-O bonds at the C-face interface. Two OH groups are found to be at least necessary for forming new Si-O bonds at the Si-face interface, indicating that the oxidation rate on the Si-face is very low compared with that on the C-face. On the other hand, both the H2O molecule and the OH group are incorporated into the C-face interface, and the energy barrier for OH is similar to that for H2O. By comparing the calculated energy barriers for these reactants with the activation energies of oxide growth rate, we suggest the orientation-dependent rate-limiting processes during wet SiC oxidation.

Phase diagram study for the PbO-ZnO-CaO-SiO_2 -“Fe_2O_3 ” system in air with CaO/SiO_2 in 1.1 and PbO/(CaO+SiO_2) in 2.4 weight ratios

International Nuclear Information System (INIS)

Lopez-Rodriguez, Josue; Romero-Serrano, Antonio; Hernandez-Ramirez, Aurelio; Cruz-Ramirez, Alejandro; Almaguer-Guzman, Isaias; Benavides-Perez, Ricardo; Flores-Favela, Manuel

2017-01-01

An experimental study on the phase equilibrium and the liquidus isotherms for the PbO-ZnO-CaO-SiO_2 -“Fe_2O_3 ” system with CaO/SiO_2 in 1.1 and PbO/(CaO+SiO_2) in 2.4 weight ratios, respectively, was carried out in the temperature range 1100-1300 deg C (1373-1573 K). High temperature phases were determined by the equilibrium-quenching method. Results are presented in the form of pseudo-ternary sections “Fe_2O_3 ”-ZnO-(PbO+CaO+SiO_2). X-Ray diffraction (XRD) and SEM-EDS results showed that the phase equilibria in this system are dominated by the high melting temperature spinel and zincite phases. It was observed that if the system is at a temperature below 1300 deg C and the total (Fe_2O_3 + ZnO) is greater than 20 wt%, spinel and/or zincite will be present in the slag system. As an application of the phase diagram, the liquid phase compositions below the liquidus surface were estimated, then their viscosities were calculated using FACTSage software. (author)

Investigating the solubility and cytocompatibility of CaO-Na2 O-SiO2 /TiO2 bioactive glasses.

Science.gov (United States)

Wren, Anthony W; Coughlan, Aisling; Smith, Courtney M; Hudson, Sarah P; Laffir, Fathima R; Towler, Mark R

2015-02-01

This study aims to investigate the solubility of a series of titanium (TiO2 )-containing bioactive glasses and their subsequent effect on cell viability. Five glasses were synthesized in the composition range SiO2 -Na2 O-CaO with 5 mol % of increments TiO2 substituted for SiO2 . Glass solubility was investigated with respect to (1) exposed surface area, (2) particle size, (3) incubation time, and (4) compositional effects. Ion release profiles showed that sodium (Na(+) ) presented high release rates after 1 day and were unchanged between 7 and 14 days. Calcium (Ca(2+) ) release presented a significant change at each time period and was also composition dependent, where a reduction in Ca(2+) release is observed with an increase in TiO2 concentration. Silica (Si(4+) ) release did not present any clear trends while no titanium (Ti(4+) ) was released. Cell numbers were found to increase up to 44%, compared to the growing control population, with a reduction in particle size and with the inclusion of TiO2 in the glass composition. © 2014 Wiley Periodicals, Inc.

Room Temperature Imprint Using Crack-Free Monolithic SiO2-PVA Nanocomposite for Fabricating Microhole Array on Silica Glass

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Shigeru Fujino

2015-01-01

Full Text Available This paper aims to fabricate microhole arrays onto a silica glass via a room temperature imprint and subsequent sintering by using a monolithic SiO2-poly(vinyl alcohol (PVA nanocomposite as the silica glass precursor. The SiO2-PVA suspension was prepared from fumed silica particles and PVA, followed by drying to obtain tailored SiO2-PVA nanocomposites. The dependence of particle size of the fumed silica particles on pore size of the nanocomposite was examined. Nanocomposites prepared from 7 nm silica particles possessed suitable mesopores, whereas the corresponding nanocomposites prepared from 30 nm silica particles hardly possessed mesopores. The pore size of the nanocomposites increased as a function of decreasing pH of the SiO2-PVA suspension. As a consequence, the crack-free monolithic SiO2-PVA nanocomposite was obtained using 7 nm silica particles via the suspension at pH 3. Micropatterns were imprinted on the monolithic SiO2-PVA nanocomposite at room temperature. The imprinted nanocomposite was sintered to a transparent silica glass at 1200°C in air. The fabricated sintered glass possessed the microhole array on their surface with aspect ratios identical to the mold.

Structure-Dependent Spectroscopic Properties of Yb3+-Doped Phosphosilicate Glasses Modified by SiO2

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Ling Wang

2017-02-01

Full Text Available Yb3+-doped phosphate glasses containing different amounts of SiO2 were successfully synthesized by the conventional melt-quenching method. The influence mechanism of SiO2 on the structural and spectroscopic properties was investigated systematically using the micro-Raman technique. It was worth noting that the glass with 26.7 mol % SiO2 possessed the longest fluorescence lifetime (1.51 ms, the highest gain coefficient (1.10 ms·pm2, the maximum Stark splitting manifold of 2F7/2 level (781 cm−1, and the largest scalar crystal-field NJ and Yb3+ asymmetry degree. Micro-Raman spectra revealed that introducing SiO2 promoted the formation of P=O linkages, but broke the P=O linkages when the SiO2 content was greater than 26.7 mol %. Based on the previous 29Si MAS NMR experimental results, these findings further demonstrated that the formation of [SiO6] may significantly affect the formation of P=O linkages, and thus influences the spectroscopic properties of the glass. These results indicate that phosphosilicate glasses may have potential applications as a Yb3+-doped gain medium for solid-state lasers and optical fiber amplifiers.

Structure-Dependent Spectroscopic Properties of Yb3+-Doped Phosphosilicate Glasses Modified by SiO2

Science.gov (United States)

Wang, Ling; Zeng, Huidan; Yang, Bin; Ye, Feng; Chen, Jianding; Chen, Guorong; Smith, Andew T.; Sun, Luyi

2017-01-01

Yb3+-doped phosphate glasses containing different amounts of SiO2 were successfully synthesized by the conventional melt-quenching method. The influence mechanism of SiO2 on the structural and spectroscopic properties was investigated systematically using the micro-Raman technique. It was worth noting that the glass with 26.7 mol % SiO2 possessed the longest fluorescence lifetime (1.51 ms), the highest gain coefficient (1.10 ms·pm2), the maximum Stark splitting manifold of 2F7/2 level (781 cm−1), and the largest scalar crystal-field NJ and Yb3+ asymmetry degree. Micro-Raman spectra revealed that introducing SiO2 promoted the formation of P=O linkages, but broke the P=O linkages when the SiO2 content was greater than 26.7 mol %. Based on the previous 29Si MAS NMR experimental results, these findings further demonstrated that the formation of [SiO6] may significantly affect the formation of P=O linkages, and thus influences the spectroscopic properties of the glass. These results indicate that phosphosilicate glasses may have potential applications as a Yb3+-doped gain medium for solid-state lasers and optical fiber amplifiers. PMID:28772601

Commercial alkaline earth boroaluminosilicate glasses for sealing solid oxide cell stacks Part II: Characterization of devitrification and glass-ceramic phase assemblages

DEFF Research Database (Denmark)

Agersted, Karsten; Balic-Zunic, T.

2018-01-01

The devitrification process and formation of crystalline phases from commercial alkaline earth boroaluminosilicate glasses containing 48-61 mol% SiO2, 18-28 mol% CaO, 1-7 mol% MgO, 7-10 mol% Al2O3, 1-11 mol% B2O3 plus minor amounts of Na2O, K2O, FeO and TiO2 were quantified through analysis...... of phase assemblages as function of heat treatments above the glass transition temperatures using the electron microprobe and powder X-ray diffraction. Treatments at 800 °C and 850 °C lasted up to 6 weeks. Results indicate that devitrification was strongly activated through presence of heterogeneous...... nucleation, and that the growth mechanism gradually changed from three-dimensional growth at the onset of devitrification towards one-dimensional growth in later stages, when heterogeneous nucleation was absent or less dominating. Most glasses developed entangled and fibrous microstructures with little...

Stability analysis of SiO2/SiC multilayer coatings

International Nuclear Information System (INIS)

Fu Zhiqiang; Jean-Charles, R.

2006-01-01

The stability behaviours of SiC coatings and SiO 2 /SiC coatings in helium with little impurities are studied by HSC Chemistry 4.1, the software for analysis of Chemical reaction and equilibrium in multi-component complex system. It is found that in helium with a low partial pressure of oxidative impurities under different total pressure, the key influence factor controlling T cp of SiC depends is the partial pressure of oxidative impurities; T cp of SiC increases with the partial pressure of oxidative impurities. In helium with a low partial pressure of different impurities, the key influence factor of T cs of SiO 2 are both the partial pressure of impurities and the amount of impurities for l mol SiO 2 ; T cs of SiO 2 increases with the partial pressure of oxidative impurities at the same amount of the impurities for 1 mol SiO 2 while it decreases with the amount of the impurities for 1 mm SiO 2 at the same partial pressure of the impurities. The influence of other impurities on T cp of SiC in He-O 2 is studied and it is found that CO 2 , H 2 O and N-2 increase T cp of SiC in He-O 2 while H 2 , CO and CH 4 decrease T cp of SiC He-O 2 . When there exist both oxidative impurities and reductive impurities, their effect on T cs of SiO 2 can be suppressed by the other. In HTR-10 operation atmosphere, SiO 2 /SiC coatings can keep stable status at higher temperature than SiC coatings, so SiO 2 /SiC coatings is more suitable to improve the oxidation resistance of graphite in HTR-10 operation atmosphere compared with SiC coatings. (authors)

Properties of Desert Sand and CMAS Glass

Science.gov (United States)

Bansal, Narottam P.; Choi, Sung R.

2014-01-01

As-received desert sand from a Middle East country has been characterized for its phase composition and thermal stability. X-ray diffraction analysis showed the presence of quartz (SiO2), calcite (CaCO3), gypsum (CaSO4.2H2O), and NaAlSi3O8 phases in as-received desert sand and showed weight loss of approx. 35 percent due to decomposition of CaCO3 and CaSO4.2H2O when heated to 1400 C. A batch of as-received desert sand was melted into calcium magnesium aluminosilicate (CMAS) glass at approx. 1500 C. From inductively coupled plasma-atomic emission spectrometry, chemical composition of the CMAS glass was analyzed to be 27.8CaO-4MgO-5Al2O3-61.6SiO2-0.6Fe2O3-1K2O (mole percent). Various physical, thermal and mechanical properties of the glass have been evaluated. Bulk density of CMAS glass was 2.69 g/cc, Young's modulus 92 GPa, Shear modulus 36 GPa, Poisson's ratio 0.28, dilatometric glass transition temperature (T (sub g)) 706 C, softening point (T (sub d)) 764 C, Vickers microhardness 6.3 +/- 0.4 GPa, indentation fracture toughness 0.75 +/- 0.15 MPa.m (sup 1/2), and coefficient of thermal expansion (CTE) 9.8 x 10 (exp -6)/degC in the temperature range 25 to 700 C. Temperature dependence of viscosity has also been estimated from various reference points of the CMAS glass using the Vogel-Fulcher-Tamman (VFT) equation. The glass remained amorphous after heat treating at 850 C for 10 hr but crystallized into CaSiO3 and Ca-Mg-Al silicate phases at 900 C or higher temperatures. Crystallization kinetics of the CMAS glass has also been investigated by differential thermal analysis (DTA). Activation energies for the crystallization of two different phases in the glass were calculated to be 403 and 483 kJ/mol, respectively.

Apatite formation on organic polymers by biomimetic process using Na2O-SiO2 glasses as nucleating agent

Energy Technology Data Exchange (ETDEWEB)

Tanahashi, M; Yao, t; Kokubo, T [Kyoto University, Kyoto (Japan). Faculty of Engineering; Minoda, M; Miyamoto, T [Kyoto University, Kyoto (Japan). Institute for Chemical Research; Nakamura, T [Kyoto University, Kyoto (Japan). Research Center for Biomedical Engineering; Yamamuro, T [Kyoto University, Kyoto (Japan). Faculty of Medicine

1994-09-01

In this investigation, CaO-SiO2-based glass, which was previously used as the nucleating agent, was replaced by Na2O-SiO2 glasses, SiO2 glass, and SiO2 gel. The induction period for the apatite nucleation on various organic polymer substrates and the adhesive strength of the apatite layer to the substrates were examined. It was considered that the short induction period for the glasses with high Na2O contents was attributed to high dissolution rates of sodium and silicate ions from them. It was also considered that highly polar carboxyl or sulfinyl groups were formed on the polymer surfaces by the hydrolysis of their ester, amide or sulfonyl group in simulated body fluid with its pH increased by the Na{sup +} dissolution from the glass, and that these polar groups formed a strong bond with the apatite. It is suggested that thus formed apatite-organic polymer composites are useful as the bone-repairing as well as soft tissue-repairing materials. 11 refs., 13 figs., 3 tabs.

Obtenção de substratos cerâmicos no sistema Si-Al-O-N-C empregando polissiloxanos e carga de Si e Al2O3 Ceramic tapes of Si-Al-O-N-C compounds using mixtures of polyssiloxane and Si-Al2O3 fillers

Directory of Open Access Journals (Sweden)

R. M. Rocha

2005-03-01

heat exchanger. In this work the conventional tape casting technique was adapted to utilize the active filler controlled polymer pyrolysis process making use of polyssiloxanes and fillers in the initial suspension. Suspensions were prepared with 60 vol. % of polymeric phase (polyssiloxanes and methyl-trietoxy-silane and 40 vol. % of fillers (Si and Al2O3 with different contents of polymer and fillers. The cured tapes were pyrolysed In nitrogen atmosphere at 1400 ºC/2 h and 1500 ºC/2 h, converting the material to ceramic tapes in the Si-Al-O-N-C system. The pyrolysis process was characterized by thermogravimetry up to 1000 ºC and pyrolyzed tapes were characterized according to phase formation, microstructure, density and thermal conductivity. The converted tapes showed relatively high porosity (between 12 and 22% and low thermal conductivity (between 3 and 8 W/m.K.. The tapes are mainly composed by crystalline phases of beta-SiC, Si2ON2, O'SiAlON, Al2O3 and mullite and a SiOC amorphous phase; Si was observed in tapes pyrolysed at 1400 ºC.

Raman and infrared investigations of glass and glass-ceramics with composition 2Na2O·1CaO·3SiO2

OpenAIRE

Ziemath, Ervino C.; Aegerter, Michel A.

1994-01-01

Precursor glass and glass-ceramics with molar composition 2Na2O·1CaO·3SiO2 are studied by infrared, conventional, and microprobe Raman techniques. The Gaussian deconvoluted Raman spectrum of the glass presents bands at 625 and 660 cm-1, attributed to bending vibrations of Si-O-Si bonds, and at 860, 920, 975 and 1030 cm-1, attributed to symmetric stretching vibrations of SiO4 tetrahedra with 4, 3, 2, and 1 nonbridging oxygens, respectively. The Raman microprobe spectrum of a highly crystalliz...

Surface crystallization in a Li{sub 2}O-ZrO{sub 2}-SiO{sub 2}-Al{sub 2}O{sub 3} glass; Cristalizacao de superficie em vidro do sistema Li{sub 2}O-ZrO{sub 2}-SiO{sub 2}-Al{sub 2}O{sub 3}

Energy Technology Data Exchange (ETDEWEB)

Oliveira, Antonio Pedro Novaes de; Teixeira, Alexandre Henrique Bortolotto; Venturelli, Hugo Henrique, E-mail: bortolotto_teixeira@yahoo.com.br, E-mail: venturellihugo@gmail.com, E-mail: antonio.pedro@ufsc.br [Universidade Federal de Santa Catarina (VITROCER/PGMAT/UFSC), Florianopolis, SC (Brazil). Laboratorio de Materiais Vitroceramicos; Montedo, Oscar Rubem Klegues, E-mail: oscar.rkm@gmail.com [Universidade do Extremo Sul Catarinense (CERTEC/PPGCEM/UNESC), Criciuma, SC (Brazil). Grupo de Pesquisa em Ceramica Tecnica

2017-04-15

Growth kinetics of crystallized surface layer in a LZSA glass composition, 11.7Li{sub 2}O·12.6ZrO{sub 2}·68.6SiO{sub 2}·7.1Al{sub 2}O{sub 3} (wt%), was studied. For the production of the LZSA glass, it was used commercial raw materials (Li{sub 2}CO{sub 3}, ZrSiO{sub 4}, SiO{sub 2}, Al{sub 2}O{sub 3}) which were mixed and melted at 1550 °C for 120 min and then poured into a metallic mold. Samples of the obtained glass were cut and subjected to heat treatments at different temperatures (825 - 925 °C) and times (30 - 150 min) for formation and growth of crystalline layer. Cross-sections of the heat-treated samples were ground and polished such that images of the formed crystallized layers could be visualized and measured by microscopy. Results showed that it is possible to obtain LZSA glasses with crystallized layers formed by β-spodumene, zircon and lithium silicate, which present thicknesses between 13 and 665 μ and grow at rates varying from 0.4 to 4.8 μm/min in the studied temperature range. (author)

Phase transitions and glass transition in a hyperquenched silica–alumina glass

DEFF Research Database (Denmark)

Zhang, Y.F.; Zhao, D.H.; Yue, Yuanzheng

2017-01-01

We investigate phase transitions, glass transition, and dynamic behavior in the hyperquenched 69SiO2–31Al2O3 (mol%) glass (SA glass). Upon reheating, the SA glass exhibits a series of thermal responses. Subsequent to the sub-Tg enthalpy release, the glass undergoes a large jump in isobaric heat...... capacity (ΔCp) during glass transition, implying the fragile nature of the SA glass. The mullite starts to form before the end of glass transition, indicating that the SA glass is extremely unstable against crystallization. After the mullite formation, the remaining glass phase exhibits an increased Tg...... and a suppressed ΔCp. The formation of cristobalite at 1553 K indicates the dominance of silica in the remaining glass matrix. The cristobalite gradually re-melts as the isothermal heat-treatment temperature is raised from 1823 to 1853 K, which is well below the melting point of cristobalite, while the amount...

CRYSTALLIZATION AND THERMAL EXPANSION CHARACTERISTICS OF In2O3-CONTAINING LITHIUM IRON SILICATE-DIOPSIDE GLASSES

Directory of Open Access Journals (Sweden)

S.M. SALMAN

2011-06-01

Full Text Available The crystallization characteristics of glasses based on lithium iron silicate (LiFeSi2O6-diopside (CaMgSi2O6 composition with addition of Al2O3 at the expense of Fe2O3 were described. The effect of LiInSi2O6/CaMgSi2O6 replacements was also investigated. The thermal treatment, the crystal phases, and the micro-structural properties of (LiFeSi2O6–CaMgSi2O6 glasses, replacing partial Fe2O3 with Al2O3 and partial CaMgSi2O6 with LiInSi2O6, have been studied by a differential thermal analysis, an X-ray diffraction, and a scanning electron microscopy. The glasses show the intense uniform bulkcrystallization with the fine grained microstructure by increasing the replacement of Al2O3/Fe2O3 and LiInSi2O6/CaMgSi2O6. The crystallizing phases of Ca(Fe,Mg(SiO32, a-LiFe5O8, Li2SiO3, a-SiO2 and CaMgSi2O6 are mostly formed together, in most case, with Li0.6Al0.6Si2.4O6, β-eucryptite solid solution, LiInSi2O6, In2Si2O7, and LiFeSi2O6. The Al2O3 partial replacement increases the transformation temperature (Tg and softening one (Ts for the glasses and the glass-ceramics, and decreases the thermal expansion coefficient (a-value for the glasses. The LiInSi2O6 partial replacement decreases Tg and Ts and increases the a-value for the glasses, while the Al2O3 and LiInSi2O6 partial replacements decrease the a-value for the glassceramics. The crystallization characters of the glasses are correlated to the internal structure, as well as role played by the glass-forming cations. However, the one of the glass-ceramics are mainly attributed to the crystalline phases formed in the material.

Effect of magnesia on the degradability and bioactivity of sol-gel derived SiO2-CaO-MgO-P2O5 system glasses.

Science.gov (United States)

Ma, J; Chen, C Z; Wang, D G; Jiao, Y; Shi, J Z

2010-11-01

Mesoporous 58SiO(2)-(38-x)CaO-xMgO-4P(2)O(5) glasses (where x=0, 5, 10 and 20 mol%) have been prepared by the sol-gel synthesis route. The effects of the substitution of MgO for CaO on glass degradation and bioactivity were studied in tris-(hydroxymethyl)-aminomethane and hydrochloric acid buffer solution (Tris-HCl) and simulated body fluid (SBF), respectively. It is observed that the synthesized glasses with various MgO contents possess the similar textural properties. The studies of in vitro degradability and bioactivity show that the rate of glass degradation gradually decreases with the increase of MgO and the formation of apatite layer on glass surface is retarded. The influences of the composition upon glass properties are explained in terms of their internal structures. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Thermal stability of SiO{sub 2}–B{sub 2}O{sub 3}–Al{sub 2}O{sub 3}–Na{sub 2}O–CaO glasses with high Nd{sub 2}O{sub 3} and MoO{sub 3} concentrations

Energy Technology Data Exchange (ETDEWEB)

Chouard, Nolwenn [Chimie ParisTech, PSL Research University, CNRS, Institut de Recherche de Chimie Paris (IRCP), 75005, Paris (France); Laboratoire d' Etude et Développement des Matrices de Conditionnement, CEA/DEN/DTCD/SECM, Marcoule, 30207, Bagnols-sur-Cèze (France); Caurant, Daniel, E-mail: daniel.caurant@chimie-paristech.fr [Chimie ParisTech, PSL Research University, CNRS, Institut de Recherche de Chimie Paris (IRCP), 75005, Paris (France); Majérus, Odile; Guezi-Hasni, Nadia [Chimie ParisTech, PSL Research University, CNRS, Institut de Recherche de Chimie Paris (IRCP), 75005, Paris (France); Dussossoy, Jean-Luc [Laboratoire des Matériaux et Procédés Actifs, CEA/DEN/DTCD/SECM/LMPA, Marcoule, 30207, Bagnols-sur-Cèze (France); Baddour-Hadjean, Rita; Pereira-Ramos, Jean-Pierre [Groupe Electrochimie et Spectroscopie des Matériaux (UMR CNRS 7182), Institut de Chimie et des Matériaux Paris-Est, 94320, Thiais (France)

2016-06-25

The incorporation of high MoO{sub 3} amounts in borosilicate glasses developed for the immobilization of radioactive waste may lead to the crystallization of Mo-rich phases that may induce a decrease of the long term performances of glasses. It is thus essential to understand their crystallization mechanisms and the possible effect of other abundant fission products present in the wastes (such as rare earths) in order to control or to avoid their formation during glass preparation. This paper presents a study, performed by X-ray diffraction, scanning electron microscopy, Raman and optical absorption spectroscopies of the stability as a function of the thermal treatment temperature T{sub C} of a simplified Mo-rich nuclear waste glass. The impact of the addition of a high amount of Nd{sub 2}O{sub 3} on the thermal stability of this glass is studied. For comparison, the thermal stability of a Nd{sub 2}O{sub 3}-rich glass without Mo is also presented. The crystallization range of all phases formed in these glasses (CaMoO{sub 4}, Na{sub 2}MoO{sub 4}, Ca{sub 2}Nd{sub 8}(SiO{sub 4}){sub 6}O{sub 2} (apatite)) and the evolution of their structure and microstructure as a function of T{sub C} are presented. The introduction of Nd{sub 2}O{sub 3} in the MoO{sub 3}-rich glass inhibits the crystallization of molybdates (increase of Mo solubility), as long as apatite does not form which suggests that [MoO{sub 4}]{sup 2-} entities and Nd{sup 3+} cations are close to each other in the glass structure. Besides, when a high density of apatite crystals form, for instance from glass surface, small Mo-rich partially crystallized globular heterogeneities are observed between these crystals that exacerbate the nucleation of new apatite crystals (nucleating effect). - Highlights: • Effect of MoO{sub 3} and Nd{sub 2}O{sub 3} separately or together on glass crystallization is studied. • The crystallization range of molybdates and apatite (Ca{sub 2}Nd{sub 8}(SiO{sub 4}){sub 6}O{sub 2}) was

Structural analysis and thermal behavior of diopside-fluorapatite-wollastonite-based glasses and glass-ceramics.

Science.gov (United States)

Kansal, Ishu; Tulyaganov, Dilshat U; Goel, Ashutosh; Pascual, Maria J; Ferreira, José M F

2010-11-01

Glass-ceramics in the diopside (CaMgSi2O6)-fluorapatite (Ca5(PO4)3F)-wollastonite (CaSiO3) system are potential candidates for restorative dental and bone implant materials. The present study describes the influence of varying SiO2/CaO and CaF2/P2O5 molar ratio on the structure and thermal behavior of glass compositions in the CaO-MgO-SiO2-P2O5-Na2O-CaF2 system. The structural features and properties of the glasses were investigated by nuclear magnetic resonance (NMR), infrared spectroscopy, density measurements and dilatometry. Sintering and crystallization behavior of the glass powders were studied by hot-stage microscopy and differential thermal analysis, respectively. The microstructure and crystalline phase assemblage in the sintered glass powder compacts were studied under non-isothermal heating conditions at 825 °C. X-ray diffraction studies combined with the Rietveld-reference intensity ratio (R.I.R) method were employed to quantify the amount of amorphous and crystalline phases in the glass-ceramics, while scanning electron microscopy was used to shed some light on the microstructure of resultant glass-ceramics. An increase in CaO/SiO2 ratio degraded the sinterability of the glass powder compacts, resulting in the formation of akermanite as the major crystalline phase. On the other hand, an increase in P2O5/CaF2 ratio improved the sintering behavior of the glass-ceramics, while varying the amount of crystalline phases, i.e. diopside, fluorapatite and wollastonite. Copyright © 2010. Published by Elsevier Ltd.

Physical and thermal behaviour of Sr-La-Al-B-Si based SOFC glass sealants as function of SrO content and B2O3/SiO2 ratio in the matrix

Science.gov (United States)

Ojha, Prasanta Kumar; Rath, S. K.; Chongdar, T. K.; Gokhale, N. M.; Kulkarni, A. R.

2011-05-01

A series of SOFC glass sealants with composition SrO (x), La2O3 (15), Al2O3 (15), B2O3 (40 - x), and SiO2 (30) [x = 10, 15, 20, 25 and 30] (wt.%) [SLABS] are investigated for their structure property correlations at different compositions. Quantitative Fourier transform infrared spectroscopy shows structural rigidity with increasing SrO content, as demonstrate by an increase in the Si-O-Si/O-Si-O bending and B-O-B stretching frequencies. The role of SrO as a modifier dominates the control of the structure and behaviour of glasses compared with the effect of network formers, i.e., the B2O3/SiO2 ratio. Consequent to the structural changes, increasing substitution of B2O3 by SrO the glasses causes increases in the density, glass transition temperature and dilatometric softening point. On the other hand, the crystallization temperatures show a decreasing trend and the coefficient of thermal expansion increases with increase in substitution.

Preparation, structural characterization, and in vitro cell studies of three-dimensional SiO2-CaO binary glass scaffolds built ofultra-small nanofibers.

Science.gov (United States)

Luo, Honglin; Li, Wei; Ao, Haiyong; Li, Gen; Tu, Junpin; Xiong, Guangyao; Zhu, Yong; Wan, Yizao

2017-07-01

Three-dimensional (3D) nanofibrous scaffolds hold great promises in tissue engineering and regenerative medicine. In this work, for the first time, 3D SiO 2 -CaO binary glass nanofibrous scaffolds have been fabricated via a combined method of template-assisted sol-gel and calcination by using bacterial cellulose as the template. SEM with EDS, TEM, and AFM confirm that the molar ratio of Ca to Si and fiber diameter of the resultant SiO 2 -CaO nanofibers can be controlled by immersion time in the solution of tetraethyl orthosilicate and ethanol. The optimal immersion time was 6h which produced the SiO 2 -CaO binary glass containing 60at.% Si and 40at.% Ca (named 60S40C). The fiber diameter of 60S40C scaffold is as small as 29nm. In addition, the scaffold has highly porous 3D nanostructure with dominant mesopores at 10.6nm and macropores at 20μm as well as a large BET surface area (240.9m 2 g -1 ), which endow the 60S40C scaffold excellent biocompatibility and high ALP activity as revealed by cell studies using osteoblast cells. These results suggest that the 60S40C scaffold has great potential in bone tissue regeneration. Copyright © 2017 Elsevier B.V. All rights reserved.

Alkali passivation mechanism of sol-gel derived TiO2-SiO2 films coated on soda-lime-silica glass substrates

Energy Technology Data Exchange (ETDEWEB)

Matsuda, A; Matsuno, Y; Katayama, S; Tsuno, T [Nippon Steel Glass Co. Ltd., Tokyo (Japan); Toge, N; Minami, T [University of Osaka Prefecture, Osaka (Japan). College of Engineering

1992-09-01

TiO2-SiO2 films prepared by the sol-gel method serves as an effective alkali passivation layer on a soda-lime-silica glass substrate and the film is superior to a sol-gel derived pure SiO2 film from the view point of weathering resistance improvement. To clarify the reason, alkali passivation mechanism of sol-gel derived TiO2-SiO2 glass films with different TiO2 contents coated on a soda-lime-silica glass substrate was studied by SIMS (secondary ion mass spectroscopy) and XPS (X-ray photoelectron spectroscopy) analyses, and compared with the results of a sol-gel derived pure SiO2 film. As a result, the following conclusions were obtained: An increase in TiO2 content in the TiO2 SiO2 film increases the sodium concentration in the film, which was induced by sodium migration from the glass substrate during the heat-treatment. Because of the presence of sodium the TiO2 -SiO2 films serve not as a barrier but as an effective getter of alkali ions and thereby effectively improve the weathering resistance Of the glass substrate. 10 refs., 6 figs.

Crystallization and properties of Sr-Ba aluminosilicate glass-ceramic matrices

Science.gov (United States)

Bansal, Narottam P.; Hyatt, Mark J.; Drummond, Charles H., III

1991-01-01

Powders of roller quenched (Sr,Ba)O-Al2O3-2SiO2 glasses of various compositions were uniaxially pressed into bars and hot isostatically pressed at 1350 C for 4 hours or cold isostatically pressed and sintered at different temperatures between 800 to 1500 C for 10 or 20 hours. Densities, flexural strengths, and linear thermal expansion were measured for three compositions. The glass transition and crystallization temperatures were determined by Differential Scanning Calorimetry (DSC). The liquidus and crystallization temperature from the melt were measured using high temperature Differential Thermal Analysis (DTA). Crystalline phases formed on heat treatment of the glasses were identified by powder X ray diffraction. In Sr containing glasses, the monoclinic celsian phase always crystallized at temperatures above 1000 C. At lower temperatures, the hexagonal analog formed. The temperature for orthorhombic to hexagonal structural transformation increased monotonically with SrO content, from 327 C for BaO-Al2O3-2SiO2 to 758 C for SrO-Al2O3-2SiO2. These glass powders can be sintered to almost full densities and monoclinic celsian phase at a relatively low temperature of 1100 C.

Phonon spectra in SiO2 glasses

International Nuclear Information System (INIS)

Perez R, J.F.; Jimenez S, S.; Gonzalez H, J.; Vorobiev, Y.V.; Hernandez L, M.A.; Parga T, J.R.

1999-01-01

Phonon spectra in SiO 2 sol-gel made glasses annealed under different conditions are investigated using infrared absorption and Raman scattering. These data are compared with those obtained in commercial optical-quality quartz. All the materials exhibit the same phonon bands, the exact position and the intensity depend on the measuring technique and on the sample preparation method. The phonon spectra in this material are interpreted on the basis of a simple quasi-linear description of elastic waves in an O-Si-O chain. It is shown that the main features observed in the range 400-1400 cm -1 can be predicted using a quasi-linear chain model in which the band at 1070 cm -1 is assigned to the longitudinal optical waves in the O-Si-O chain with the smallest possible wavelength at the Brillouin zone boundary, the band located around 450 cm -1 is assigned to the transversal optical waves and the band at 800 cm -1 to the longitudinal acoustical waves with the same wavelength. The degree of structural disorder can be also deduced within the framework of the proposed model. (Author)

Development and characterization of glass-ceramic sealants in the (CaO-Al2O3-SiO2-B2O3) system for Solid Oxide Electrolyzer Cells

International Nuclear Information System (INIS)

Khedim, Hichem; Nonnet, Helene; Mear, Francois O.

2012-01-01

The efficiency of glass-ceramic sealants plays a crucial role in Solid Oxide Electrolyzer Cell performance and durability. In order to develop suitable sealants, operating around 800 degrees C, two parent glass compositions, CAS1B and CAS2B, from the CaO-Al 2 O 3 -SiO 2 -B 2 O 3 system were prepared and explored. The thermal and physicochemical properties of the glass ceramics and their crystallization behavior were investigated by HSM. DTA and XRD analyses. The microstructure and chemical compositions of the crystalline phases were investigated by microprobe analysis. Bonding characteristic as well as chemical interactions of the parent glass with yttria-stabilized zirconia (YSZ) electrolyte and ferritic steel-based interconnect (Crofere (R)) were also investigated. The preliminary results revealed the superiority of CAS2B glass for sealing application in SOECs. The effect of minor additions of V 2 O 5 , K 2 O and TiO 2 on the thermal properties was also studied and again demonstrated the advantages of the CAS2B glass composition. Examining the influence of heat treatment on the seal behavior showed that the choice of the heating rate is a compromise between delaying the crystallization process and delaying the viscosity drop. The thermal Expansion Coefficients (TEC) obtained for the selected glass ceramic are within the desired range after the heat treatment of crystallization. The crystallization kinetic parameters of the selected glass composition were also determined under non-isothermal conditions by means of differential thermal analysis (DTA) and using the formal theory of transformations for heterogeneous nucleation. (authors)

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.

Lithium conductivity in glasses of the Li2O-Al2O3-SiO2 system.

Science.gov (United States)

Ross, Sebastian; Welsch, Anna-Maria; Behrens, Harald

2015-01-07

To improve the understanding of Li-dynamics in oxide glasses, i.e. the effect of [AlO4](-) tetrahedra and non-bridging oxygens on the potential landscape, electrical conductivity of seven fully polymerized and partly depolymerized lithium aluminosilicate glasses was investigated using impedance spectroscopy (IS). Lithium is the only mobile particle in these materials. Data derived from IS, i.e. activation energies, pre-exponential factors and diffusivities for lithium, are interpreted in light of Raman spectroscopic analyses of local structures in order to identify building units, which are crucial for lithium dynamics and migration. In polymerized glasses (compositional join LiAlSiO4-LiAlSi4O10) the direct current (DC) electrical conductivity continuously increases with increasing lithium content while lithium diffusivity is not affected by the Al/Si ratio in the glasses. Hence, the increase in electrical conductivity can be solely assigned to lithium concentration in the glasses. An excess of Li with respect to Al, i.e. the introduction of non-bridging oxygen into the network, causes a decrease in lithium mobility in the glasses. Activation energies in polymerized glasses (66 to 70 kJ mol(-1)) are significantly lower than those in depolymerized networks (76 to 78 kJ mol(-1)) while pre-exponential factors are nearly constant across all compositions. Comparison of the data with results for lithium silicates from the literature indicates a minimum in lithium diffusivity for glasses containing both aluminium tetrahedra and non-bridging oxygens. The findings allow a prediction of DC conductivity for a large variety of lithium aluminosilicate glass compositions.

Microstructural dependence on relevant physical-mechanical properties on SiO2-Na2O-CaO-P2O5 biological glasses.

Science.gov (United States)

Rajendran, V; Begum, A Nishara; Azooz, M A; el Batal, F H

2002-11-01

Bioactive glasses of the system SiO2-Na2O-CaO-P2O5 have been prepared by the normal melting and annealing technique. The elastic moduli, attenuation, Vickers hardness, fracture toughness and fracture surface energy have been obtained using the known method at room temperature. The temperature dependence of elastic moduli and attenuation measurements have been extended over a wide range of temperature from 150 to 500 K. The SiO2 content dependence of velocities, attenuation, elastic moduli, and other parameters show an interesting observation at 45 wt% of SiO2 by exhibiting an anomalous behaviour. A linear relation is developed for Tg, which explores the influence of Na2O on SiO2-Na2O-CaO-P2O5 bioactive glasses. The measured hardness, fracture toughness and fracture surface energy show a linear relation with Young's modulus. It is also interesting to note that the observed results are functions of polymerisation and the number of non-bridging oxygens (NBO) prevailing in the network with change in SiO2 content. The temperature dependence of velocities, attenuation and elastic moduli show the existence of softening in the glass network structure as temperature increases.

Preparation and characterization of new glasses from the TeO2-CdO-Al2O3-SiO2 system

OpenAIRE

Zayas, Mª. E.; Espinoza-Beltrán, F. J.; Romero, Maximina; Rincón López, Jesús María

1998-01-01

A new family of glasses from the TeO2-CdO-Al2O3-SiO2 system obtained from CdS-TeO2 mixtures melted in fireclay crucibles have been prepared and characterized. The density values of these glasses are in the 3.30-3.46 gcm-3 range. The viscosity-temperature variation shows that glasses with high TeO2 content depict the typical variation of `short glasses' for a molding operation. Microstructural observations by TEM (replica method) and SEM microscopies have shown that these glasses contain very ...

Compositional and microstructural design of highly bioactive P2O5-Na2O-CaO-SiO2 glass-ceramics.

Science.gov (United States)

Peitl, Oscar; Zanotto, Edgar D; Serbena, Francisco C; Hench, Larry L

2012-01-01

Bioactive glasses having chemical compositions between 1Na(2)O-2CaO-3SiO(2) (1N2C3S) and 1.5Na(2)O-1.5CaO-3SiO(2) (1N1C2S) containing 0, 4 and 6 wt.% P(2)O(5) were crystallized through two stage thermal treatments. By carefully controlling these treatments we separately studied the effects on the mechanical properties of two important microstructural features not studied before, crystallized volume fraction and crystal size. Fracture strength, elastic modulus and indentation fracture toughness were measured as a function of crystallized volume fraction for a constant crystal size. Glass-ceramics with a crystalline volume fraction between 34% and 60% exhibited a three-fold improvement in fracture strength and an increase of 40% in indentation fracture toughness compared with the parent glass. For the optimal crystalline concentration (34% and 60%) these mechanical properties were then measured for different grain sizes, from 5 to 21 μm. The glass-ceramic with the highest fracture strength and indentation fracture toughness was that with 34% crystallized volume fracture and 13 μm crystals. Compared with the parent glass, the average fracture strength of this glass-ceramic was increased from 80 to 210 MPa, and the fracture toughness from 0.60 to 0.95 MPa.m(1/2). The increase in indentation fracture toughness was analyzed using different theoretical models, which demonstrated that it is due to crack deflection. Fortunately, the elastic modulus E increased only slightly; from 60 to 70 GPa (the elastic modulus of biomaterials should be as close as possible to that of cortical bone). In summary, the flexural strength of our best material (215 MPa) is significantly greater than that of cortical bone and comparable with that of apatite-wollastonite (A/W) bioglass ceramics, with the advantage that it shows a much lower elastic modulus. These results thus provide a relevant guide for the design of bioactive glass-ceramics with improved microstructure. Copyright © 2011 Acta

Temperature stability of c-axis oriented LiNbO3/SiO2/Si thin film layered structures

International Nuclear Information System (INIS)

Tomar, Monika; Gupta, Vinay; Mansingh, Abhai; Sreenivas, K.

2001-01-01

Theoretical calculations have been performed for the temperature stability of the c-axis oriented LiNbO 3 thin film layered structures on passivated silicon (SiO 2 /Si) substrate with and without a non-piezoelectric SiO 2 overlayer. The phase velocity, electromechanical coupling coefficient and temperature coefficient of delay (TCD) have been calculated. The thicknesses of various layers have been determined for optimum SAW performance with zero TCD. The presence of a non-piezoelectric SiO 2 overlayer on LiNbO 3 film is found to significantly enhance the coupling coefficient. The optimized results reveal that a high coupling coefficient of K 2 =3.45% and a zero TCD can be obtained in the SiO 2 /LiNbO 3 /SiO 2 /Si structure with a 0.235λ thick LiNbO 3 layer sandwiched between 0.1λ thick SiO 2 layers. (author)

CHARACTERIZATION OF COMMERCIALLY AVAILABLE ALKALI RESISTANT GLASS FIBER FOR CONCRETE REINFORCEMENT AND CHEMICAL DURABILITY COMPARISON WITH SrO-Mn2O3-Fe2O3-MgO-ZrO2-SiO2 (SMFMZS SYSTEM GLASSES

Directory of Open Access Journals (Sweden)

Göktuğ GÜNKAYA

2012-12-01

Full Text Available According to the relevant literature, the utilization of different kind of glass fibers in concrete introduces positive effect on the mechanical behavior, especially toughness. There are many glassfibers available to reinforce concretes. Glass fiber composition is so important because it may change the properties such as strength, elastic modulus and alkali resistance. Its most important property to be used in concrete is the alkali resistance. Some glasses of SrO–MgO–ZrO2–SiO2 (SMZS quaternary system, such as 26SrO, 20MgO, 14ZrO2, 40SiO2 (Zrn glass, have been found to be highly alkali resistant thanks to their high ZrO2 and MgO contents. Previous researches on these glasses with MnO and/or Fe2O3 partially replacing SrO have been made with the aim of improving the chemical resistance and decreasing the production cost.The main target of the present study, first of all, was to characterize commercially available alkali resistant glass fiber for concrete reinforcement and then to compare its alkali durability with those of the SrO-Mn2O3-Fe2O3-MgO-ZrO2-SiO2 (SMFMZS system glasses. For such purposes, XRF, Tg-DTA, alkali resistance tests and SEM analysis conducted with EDX were employed. According tothe alkali endurance test results it was revealed that some of the SMFMZS system glass powders are 10 times resistant to alkali environments than the commercial glass fibers used in this study.Therefore, they can be considered as alternative filling materials on the evolution of chemically resistant concrete structures.

Investigating the effect of V{sub 2}O{sub 5} addition on sodium barium borosilicate glasses

Energy Technology Data Exchange (ETDEWEB)

Halder, Rumu, E-mail: rumuhalder24feb@gmail.com; Sengupta, Pranesh; Dey, G. K. [Materials Science Division, Bhabha Atomic Research Centre, Mumbai-700 085 (India); Sudarsan, V. [Chemistry Division, Bhabha Atomic Research Centre, Mumbai-700 085 (India); Kaushik, C. P. [Waste Management Division, Bhabha Atomic Research Centre, Mumbai-700 085 (India)

2016-05-23

V{sub 2}O{sub 5} doped sodium barium borosilicate glasses were characterized by photoluminescence spectroscopy and electron probe microanalyzer (EPMA). The glass remains homogeneous for lower concentration of V{sub 2}O{sub 5} but a phase separation is observed when V{sub 2}O{sub 5} doping is increased beyond 5 mol%. Detailed microanalysis reveals that the phase separated glass consists of a phase containing V, Ba and Si and a separate Si rich phase within the glass matrix. The luminescence study demonstrated that at low concentration the vanadium mainly interacts with the structural units of B/Si while at higher concentrations, V-O-V/ V-O{sup −} Na{sup +}/Ba{sup 2+} linkages are formed.

A simple transferable adaptive potential to study phase separation in large-scale xMgO-(1-x)SiO2 binary glasses.

Science.gov (United States)

Bidault, Xavier; Chaussedent, Stéphane; Blanc, Wilfried

2015-10-21

A simple transferable adaptive model is developed and it allows for the first time to simulate by molecular dynamics the separation of large phases in the MgO-SiO2 binary system, as experimentally observed and as predicted by the phase diagram, meaning that separated phases have various compositions. This is a real improvement over fixed-charge models, which are often limited to an interpretation involving the formation of pure clusters, or involving the modified random network model. Our adaptive model, efficient to reproduce known crystalline and glassy structures, allows us to track the formation of large amorphous Mg-rich Si-poor nanoparticles in an Mg-poor Si-rich matrix from a 0.1MgO-0.9SiO2 melt.

The influence of Al2O3, MgO and ZnO on the crystallization characteristics and properties of lithium calcium silicate glasses and glass-ceramics

International Nuclear Information System (INIS)

Salman, S.M.; Darwish, H.; Mahdy, E.A.

2008-01-01

The crystallization characteristics of glasses based on the Li 2 O-CaO-SiO 2 eutectic (954 ± 4 deg. C) system containing Al 2 O 3 , MgO and ZnO has been investigated by differential thermal analysis (DTA), X-ray diffraction analysis (XRD), and scanning electron microscopy (SEM). The partial replacement of Li 2 O by Al 2 O 3 and CaO by MgO or ZnO in the studied glass-ceramics led to the development of different crystalline phase assemblages, including lithium meta- and di-silicates, lithium calcium silicates, α-quartz, diopside, clinoenstatite, wollastonite, β-eucryptite ss, β-spodumene, α-tridymite, lithium zinc orthosilicate, hardystonite and willemite using various heat-treatment processes. The dilatometric thermal expansion of the glasses and their corresponding glass-ceramics were determined. A wide range of thermal expansion coefficient values were obtained for the investigated glasses and their corresponding crystalline products. The thermal expansion coefficients of the investigated glasses were decreased by Al 2 O 3 , MgO or ZnO additions. The α-values of the investigated glasses were ranged from (+18) to (+108) x 10 -7 K -1 (25-300 deg. C), while those of the glass-ceramics were (+3) to (+135) x 10 -7 K -1 (25-700 deg. C). The chemical durability of the glass-ceramics, towards the attack of 0.1N HCl solution, was markedly improved by Al 2 O 3 with MgO replacements. The composition containing 11.5 mol% Al 2 O 3 and 6.00 mol% MgO exhibited low thermal expansion values and good chemical durability

SiC-SiC and C-SiC Honeycomb for Advanced Flight Structures, Phase II

Data.gov (United States)

National Aeronautics and Space Administration — The proposed project builds upon the work done in Phase I with the development of a C-SiC CMC honeycomb material that was successfully tested for mechanical...

Characterisation and Properties of Lithium Disilicate Glass Ceramics in the SiO2-Li2O-K2O-Al2O3 System for Dental Applications

Directory of Open Access Journals (Sweden)

Naruporn Monmaturapoj

2013-01-01

Full Text Available This work proposes four different glass formulas derived from the SiO2-Li2O-K2O-Al2O3 system to investigate the effect of glass composition on their crystal formations and properties. Glass LD1 was SiO2-Li2O-K2O-Al2O3 system with the addition of P2O5 and CaF2 as nucleating agents. In Glass LD2, a slight amount of MgO was mixed in order to increase the viscosity of the melting glass. Finally, the important factor of Si : Li ratio was increased in Glasses LD3 and LD4 with compositions otherwise the same as LD1 and LD2. The results found that P2O5 and CaF2 served as a nucleating site for lithium phosphate and fluorapatite to encourage heterogenous nucleation and produce a fine-grained interlocking microstructure of lithium disilicate glass ceramics. MgO content in this system seemed to increase the viscosity of the melting glass and thermal expansion coefficient including the chemical solubility. Increasing the Si : Li ratio in glass compositions resulted in the change of the microstructure of Li2Si2O5 crystals.

Wearing mechanisms of Al{sub 2} O{sub 3}-Si C-C for torpedo car; Mecanismos de desgate dos refratarios de Al{sub 2}O{sub 3}-SiC-C para carro-torpedo

Energy Technology Data Exchange (ETDEWEB)

Quintela, Marco Antonio; Correa Filho, Gerson [USIMINAS, Ipatinga, MG (Brazil). Centro de Pesquisa e Desenvolvimento; Correa Filho, Joao Rodrigues [USIMINAS, Ipatinga, MG (Brazil). Gerencia de Manutencao de Refratarios e Civil

1995-12-31

Recently, with the improvement in the hot metal pretreatment practice in the torpedo car at USIMINAS, refractory linings were subjected to severe working conditions resulting in a considerable change in the performance of Al{sub 2} O{sub 3}-Si C-C bricks. A Post Mortem study of the torpedo car linings was carried out using ceramographic analysis and scanning electron microscopy. It was found that the wear mechanisms of Al{sub 2} O{sub 3}-Si C-C bricks comprise mainly the development of dense and secondary phases around Al{sub 2} O{sub 3} particles, together with the formation of low refractoriness phases on the slag and refractory interface. (author) 5 figs.

Phase diagram study for the PbO-ZnO-CaO-SiO{sub 2} -“Fe{sub 2}O{sub 3} ” system in air with CaO/SiO{sub 2} in 1.1 and PbO/(CaO+SiO{sub 2}) in 2.4 weight ratios

Energy Technology Data Exchange (ETDEWEB)

Lopez-Rodriguez, Josue; Romero-Serrano, Antonio; Hernandez-Ramirez, Aurelio; Cruz-Ramirez, Alejandro, E-mail: romeroipn@hotmail.com [Instituto Politecnico Nacional-ESIQIE, Zacatenco, Mexico City (Mexico); Almaguer-Guzman, Isaias; Benavides-Perez, Ricardo; Flores-Favela, Manuel [Servicios Administrativos Penoles S.A de C.V., Torreon, Coahuila (Mexico)

2017-07-15

An experimental study on the phase equilibrium and the liquidus isotherms for the PbO-ZnO-CaO-SiO{sub 2} -“Fe{sub 2}O{sub 3} ” system with CaO/SiO{sub 2} in 1.1 and PbO/(CaO+SiO{sub 2}) in 2.4 weight ratios, respectively, was carried out in the temperature range 1100-1300 deg C (1373-1573 K). High temperature phases were determined by the equilibrium-quenching method. Results are presented in the form of pseudo-ternary sections “Fe{sub 2}O{sub 3} ”-ZnO-(PbO+CaO+SiO{sub 2}). X-Ray diffraction (XRD) and SEM-EDS results showed that the phase equilibria in this system are dominated by the high melting temperature spinel and zincite phases. It was observed that if the system is at a temperature below 1300 deg C and the total (Fe{sub 2}O{sub 3} + ZnO) is greater than 20 wt%, spinel and/or zincite will be present in the slag system. As an application of the phase diagram, the liquid phase compositions below the liquidus surface were estimated, then their viscosities were calculated using FACTSage software. (author)

Characterization of μc-Si:H/a-Si:H tandem solar cell structures by spectroscopic ellipsometry

International Nuclear Information System (INIS)

Murata, Daisuke; Yuguchi, Tetsuya; Fujiwara, Hiroyuki

2014-01-01

In order to perform the structural characterization of Si thin-film solar cells having submicron-size rough textured surfaces, we have developed an optical model that can be utilized for the spectroscopic ellipsometry (SE) analysis of a multilayer solar cell structure consisting of hydrogenated amorphous silicon (a-Si:H) and microcrystalline silicon (μc-Si:H) layers fabricated on textured SnO 2 :F substrates. To represent the structural non-uniformity in the textured structure, the optical response has been calculated from two regions with different thicknesses of the Si layers. Moreover, in the optical model, the interface layers are modeled by multilayer structures assuming two-phase composites and the volume fractions of the phases in the layers are controlled by the structural curvature factor. The polarized reflection from the μc-Si:H layer that shows extensive surface roughening during the growth has also been modeled. In this study, a state-of-the-art solar cell structure with the textured μc-Si:H (2000 nm)/ZnO (100 nm)/a-Si:H (200 nm)/SnO 2 :F/glass substrate structure has been characterized. The μc-Si:H/a-Si:H textured structure deduced from our SE analysis shows remarkable agreement with that observed by transmission electron microscopy. From the above results, we have demonstrated the high-precision characterization of highly-textured μc-Si:H/a-Si:H solar cell structures. - Highlights: • Characterization of textured μc-Si:H/a-Si:H solar cell structures by ellipsometry • A new optical model using surface area and multilayer models • High precision characterization of submicron-range rough interface structures

Crystallization studies and dielectric properties of (Ba0.7Sr0.3)TiO3 in bariumaluminosilicate glass

Science.gov (United States)

Divya, P. V.; Vignesh, G.; Kumar, V.

2007-12-01

Ferroelectric glass-ceramics with a basic composition (1 - y)(Ba0.70Sr0.30)TiO3 : y(BaO : Al2O3 : 2SiO2) have been synthesized by the sol-gel method. The major crystalline phase is the perovskite. The crystallization of the ferroelectric phase in the glass matrix have been studied using differential thermal analysis and x-ray diffraction and the kinetic parameters characterizing the crystallization have been determined using an Arrhenius model. Glass contents <= 5 mol% promoted liquid phase sintering, which reduced the sintering temperature to 1250 °C. The dielectric permittivity of the glass-ceramic samples decreased and the ferroelectric-paraelectric phase transition became more diffuse with increasing glass content. The dielectric connectivity of the ferroelectric phase in the composite have also been investigated and are reported.

Glass-ceramic materials of system MgO-Al2O3-SiO2 from rice husk ash

OpenAIRE

Martín Hernández, María Isabel; Rincón López, Jesús María; Andreola, F.; Barbieri, L.; Bondioli, F.; Lancellotti, I.; Romero, Maximina

2011-01-01

This wok shows the results of a valorisation study to use rice husk ash as raw material to develop glass-ceramic materials. An original glass has been formulated in the base system MgO-Al2O3-SiO2 with addition of B2O3 and Na2O to facilitate the melting and poring processes. Glass characterization was carried out by determining its chemical composition. Sintering behaviour has been examined by Hot Stage Microscopy (HSM). Thermal stability and crystallization mechanism have been studied by Diff...

Microstructural characterization of an opal glass in the Na/sub 2/O-CdO-SiO/sub 2/ system

Energy Technology Data Exchange (ETDEWEB)

Rivera, E; Celaya, L E; Rincon, J M

1987-05-01

The microstructure of an opal glass formulated in the ternary system Na/sub 2/O-CdO-SiO/sub 2/ has been determined by scanning electron microscopy (SEM) and energy dispersive X-ray microanalysis (EDX). This type of glass shows tridymite devitrification with a high level of liquid-liquid immiscibility.

Quantifying Silica Reactivity in Subsurface Environments: Reaction Affinity and Solute Matrix Controls on Quartz and SiO2 Glass Dissolution Kinetics

International Nuclear Information System (INIS)

Dove, Patricia M.

1999-01-01

Our goal is to develop a quantitative and mechanistic understanding of amorphous silica, SiO2(am), dissolution kinetics in aqueous solutions. A knowledge of fundamental controls on the reactivity of simple Si-O bonded phases is the baseline of behavior for understanding highly complex silica phases. In the Earth, silicate minerals comprise >70% of the crust and dominate virtually every subsurface system. More importantly for the objectives of this EMSP project, the silicates are important because compositionally complex glasses will become the front line of defense in containing radioactive wastes in the nation's long term and interim storage strategies. To date, the behavior of SiO2(am) is largely inferred from studies of the better known crystalline polymorphs (e.g. alpha-quartz). In the first step towards constructing a general model for amorphous silica reactivity in the complex fluid compositions of natural waters, we are determining the dissolution behavior as a function of temperature, solution pH and cation concentration. With these data we are determining relationships between SiO2 glass structure and dissolution rates in aqueous solutions, as described below

Superconducting phase of YBa2Cu3O7-δ films in high magnetic fields: Vortex glass or Bose glass

International Nuclear Information System (INIS)

Woeltgens, P.J.M.; Dekker, C.; Swueste, J.; de Wijn, H.W.

1993-01-01

Nonlinear current-voltage (I-V) curves are measured in laser-ablated YBa 2 Cu 3 O 7-δ films deposited onto SrTiO 3 . The measurements are performed near the glass phase transition in a magnetic field of 5 T at various angles from the c axis. From a critical scaling analysis, the angular dependencies of the glass transition temperature and the critical glass exponents are extracted. At small angles, these results distinguish between a vortex glass, caused by random pointlike disorder, and a Bose glass, caused by linelike disorder. The results can be understood in terms of the vortex-glass model only. No evidence is found for the existence of a Bose-glass phase

Nanoindentation Analysis of Elastic/Mechanical Behaviour of Surface of Transparent Glass Ceramics with Fresnoite Ba2TiSi2O8 Nanocrystals

International Nuclear Information System (INIS)

Shinozaki, K; Honma, T; Komatsu, T

2011-01-01

Transparent glass-ceramics containing Ba 2 TiSi 2 O 8 (BTS) nanocrystals with sizes of ∼200 nm were obtained by heat treatment of 40BaO-20TiO 2 -40SiO 2 glass. Their elastic/mechanical properties were evaluated using the cube-resonance method and the Berkovich nanoindentation technique under standard and 'continuous stiffness measurement' (CSM) modes, and the relation between these properties and the volume fraction (f) of BTS nanocrystals was clarified. The glass-ceramics were obtained by 1-h heat treatments at 760-790 deg. C of the precursor glass, resulting in the formation of BTS nanocrystals with f=2.7-54.5%, with a corresponding Young's modulus of 84-107 GPa. The CSM nanoindentation measurements gave an indentation modulus of 90 GPa for the glass and 110 GPa for the glass-ceramic heat-treated at 790 deg. C, for indentation depths of 200-1500 nm. The results suggest that the BTS nanocrystals confer a high resistance to deformation during indenter loading.

Heat treatment of Na2O-CaO-P2O5-SiO2 bioactive glasses: densification processes and postsintering bioactivity.

Science.gov (United States)

Sola, A; Bellucci, D; Raucci, M G; Zeppetelli, S; Ambrosio, L; Cannillo, V

2012-02-01

Because of their excellent bioactivity, bioactive glasses are increasingly diffused to produce biomedical devices for bone prostheses, to face the dysfunctions that may be caused by traumatic events, diseases, or even natural aging. However, several processing routes, such as the production of scaffolds or the deposition of coatings, include a thermal treatment to apply or sinter the glass. The exposure to high temperature may induce a devetrification phenomenon, altering the properties and, in particular, the bioactivity of the glass. The present contribution offers an overview of the thermal behavior and properties of two glasses belonging to the Na2O-CaO-P2O5-SiO2 system, to be compared to the standard 45S5 Bioglass(®). The basic goal is to understand the effect of both the original composition and the thermal treatment on the performance of the sintered glasses. The new glasses, the one (BG_Na) with a high content of Na2O, the other (BG_Ca) with a high content of CaO, were fully characterized and sintering tests were performed to define the most interesting firing cycles. The sintered samples, treated at 880°C and 800°C respectively, were investigated from a microstructural point of view and their mechanical properties were compared to those of the bulk (not sintered) glass counterparts. The effect of sintering was especially striking on the BG_Ca material, whose Vickers hardness increased from 598.9 ± 46.7 HV to 1053.4 ± 35.0 HV. The in vitro tests confirmed the ability of the glasses, both in bulk and sintered form, of generating a hydroxyapatite surface layer when immersed in a simulated body fluid. More accurate biological tests performed on the sintered glasses proved the high bioactivity of the CaO-rich composition even after a heat treatment. Copyright © 2011 Wiley Periodicals, Inc.

Cat-CVD-prepared oxygen-rich μc-Si:H for wide-bandgap material

International Nuclear Information System (INIS)

Matsumoto, Yasuhiro; Ortega, Mauricio; Peza, Juan-Manuel; Reyes, Mario-Alfredo; Escobosa, Arturo

2005-01-01

Microcrystalline phase-involved oxygen-rich a-Si:H (hydrogenated amorphous silicon) films have been obtained using catalytic chemical vapor deposition (Cat-CVD) process. Pure SiH 4 (silane), H 2 (hydrogen), and O 2 (oxygen) gases were introduced in the chamber by maintaining a pressure of 0.1 Torr. A tungsten catalyzer was fixed at temperatures of 1750 and 1950 deg. C for film deposition on glass and crystalline silicon substrates at 200 deg. C. As revealed from X-ray diffraction spectra, the microcrystalline phase appears for oxygen-rich a-Si:H samples deposited at a catalyzer temperature of 1950 deg. C. However, this microcrystalline phase tends to disappear for further oxygen incorporation. The oxygen content in the deposited films was corroborated by FTIR analysis revealing Si-O-Si bonds and typical Si-H bonding structures. The optical bandgap of the sample increases from 2.0 to 2.7 eV with oxygen gas flow and oxygen incorporation to the deposited films. In the present thin film deposition conditions, no strong tungsten filament degradation was observed after a number of sample preparations

ZnO epitaxy on SiC(0001-bar) substrate: Comparison with ZnO/SiC(0 0 0 1) heterostructure

International Nuclear Information System (INIS)

Ashrafi, Almamun; Aminuzzaman, Mohammod

2011-01-01

ZnO thin layers deposited on 6H-SiC substrates showed six-fold crystal symmetry with an epitaxial relationship of (0 0 0 2) ZnO ||(0 0 0 6) SiC and [112-bar 0] ZnO ||[112-bar 0] SiC . Despite the different 6H-SiC substrate surface orientations for the ZnO epitaxy, the orientation relationship of ZnO/6H-SiC heterostructures is identical, as confirmed by X-ray diffraction studies. In these ZnO/6H-SiC(0 0 0 1) and ZnO/6H-SiC(0001-bar) heterostructures, the valence band offsets are measured to be 1.12 eV and 1.09 eV, leading to the conduction band offset values of 0.75 eV and 0.72 eV, respectively. These slightly different band-offset values in ZnO/6H-SiC heterojunctions are attributed to the variation of valence band maximums and the different interface charge compensation mechanisms.

Investigating the Effect of Glass Ion Release on the Cytocompatibility, Antibacterial Eflcacy and Antioxidant Activity of Y2O3 / CeO2 doped SiO2-SrO-Na2O glasses

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Placek L. M.

2018-02-01

Full Text Available The effect on ion release and cytocompatibility of Yttrium (Y and Cerium (Ce are investigated when substituted for Sodium (Na in a 0.52SiO2-0.24SrO-0.24-Na2OMOglass series (where MO= Y2O3 or CeO2. Glass leaching was evaluated through pH measurements and Inductive Coupled Plasma-Optical Emission Spectrometry (ICP-OES analysiswhere the extract pH increased during incubation (11.2 - 12.5. Ion release of Silicon (Si, Na and Strontium (Sr from the Con glass was at higher than that of glasses containing Y or Ce, and reached a limit after 1 day. Ion release from Y and Ce containing glasses reached a maximum of 1800 μg/mL, 1800 μg/mL, and 10 μg/mL for Si, Na, and Sr, respectively. Release of Y and Cewas below the ICP- OES detection limit 75% of bacteria at a 9% extract concentration. Antioxidant capacity (mechanism for neuroprotection was evaluated using the ABTS assay. All glasses had inherent radical oxygen species (ROS scavenging capability with Con reaching 9.5 mMTE.

Effect of heat treatment on the properties of SiO2-CaO-MgO-P 2O 5 bioactive glasses.

Science.gov (United States)

Zhou, Yue; Li, Hongying; Lin, Kaili; Zhai, Wanying; Gu, Weiming; Chang, Jiang

2012-09-01

Since the invention of 45S5 Bioglass, researchers never stopped exploring new generation bioactive glass (BG) materials for wider applications in regenerative medicine, among which a novel SiO(2)-CaO-MgO-P(2)O(5) bioactive glass (BG20) is an excellent candidate. However, apart from their biocompatibility and bioactivity, a porous structure is also a must for a tissue engineering scaffold in successfully fixing bone defect. The porosity is the outcome of the high temperature (500-1,000 °C) treatment in the fabricating process of the bioglass scaffold. Under the high temperature, the amorphous glass material will become crystallized at certain percentage in the glass matrix, and possibly leading to consequent changes in the mechanical strength, biodegradability and bioactivity. To elucidate the effect of phase transition on the change of the properties of BG20, the experiments in this report were designed to fine-tuning the heat treating temperatures to fabricate a series of BG20 powders with different crystallization structures. X-ray diffraction revealed a positive correlation between the heating temperature and the crystallization, as well as the compressive strength of the materials. In vitro degradation and ion analysis by ICP-AES demonstrated a similar releasing behavior of different ions including Mg(2+), Ca(2+) and Si(4+), which in common is the tendency of decreasing of the ion concentration along with the increasing of the treating temperature. Cell proliferation assay using both mouse fibroblasts (NIH3T3) and bone marrow stromal cells (BMSCs) showed little toxicity of the ionic extract of the BG20 powders at all the treating temperatures, while fibroblasts demonstrated a significant promoting in the percentage of proliferation. Furthermore, reverse-transcription and polymerase chain reaction analysis on two representative marker genes for early osteogenesis and endochondral ossification, respectively, type I collagen alpha 1 and Indian Hedge-hog, showed

Crystallization Mechanism and Kinetics of BaO-Li2O-ZrO2-SiO2 Glasses

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Cristian Berto da Silveira

2002-03-01

Full Text Available Differential thermal analysis and scanning electron microscopy were used to determine the influence of the addition of BaO on the crystallization mechanism of Li2O-ZrO2-SiO2 systems. As the concentration of BaO in the samples increased, a transition occurred in the predominant crystallization mechanism, which passed from superficial to volumetric. To determine the maximum nucleation rate, the crystallization kinetics of the sample containing 20 mole % BaO, which showed the most uniform crystallization, was studied by counting the nuclei with an image analyzer. The first nuclei appeared at the first endothermic inflection point (at the start of Tg, at 440 °C, while the maximum number of nuclei was counted at the midpoint of the glass transition region (446 °C. These results are similar to those observed for other materials that crystallize in volume, and confirm scanning electron microscopy data.

Preparation of anti-oxidative SiC/SiO2 coating on carbon fibers from vinyltriethoxysilane by sol–gel method

International Nuclear Information System (INIS)

Xia Kedong; Lu Chunxiang; Yang Yu

2013-01-01

Highlights: ► The SiC/SiO 2 coating was prepared on carbon fibers by the sol–gel method. ► Nano-crystallites with an average diameter of 130 nm were aligned along the fiber axis uniformly. ► The oxidation resistant property of coated carbon fiber was increased with the increase of sol concentration and the heat treatment temperature. ► The oxidation activation energy of the coated carbon fiber was increased by 23% in comparison with uncoated carbon fiber. - Abstract: The anti-oxidative SiC/SiO 2 coating was prepared on carbon fibers by a sol–gel process using vinyltriethoxysilane (VTES) as the single source precursor. The derived coating was characterized by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES). The oxidation resistant properties of the carbon fiber with and without coating were studied by isothermal oxidation. The results indicated that the carbothermal reduction reaction led to the decrease of SiO 2 phase and the increase of SiC phase at 1500 °C. The uniform SiC/SiO 2 coating prepared from a sol concentration of 4 wt% and heat treated at 1500 °C showed the optimal oxidation resistant property. The oxidation resistance of the carbon fiber was improved by the SiC/SiO 2 coating, and the oxidation activation energy was increased by about 23% as compared with uncoated carbon fiber.

Electrochemical and optical properties of CeO2-SnO2 and CeO2-SnO2:X (X = Li, C, Si films

Directory of Open Access Journals (Sweden)

Berton Marcos A.C.

2001-01-01

Full Text Available Thin solid films of CeO2-SnO2 (17 mol% Sn and CeO2-SnO2:X (X = Li, C and Si were prepared by the sol-gel route, using an aqueous-based process. The addition of Li, C and Si to the precursor solution leads to films with different electrochemical performances. The films were deposited by the dip-coating technique on ITO coated glass (Donnelly Glass at a speed of 10 cm/min and submitted to a final thermal treatment at 450 °C during 10 min in air. The electrochemical and optical properties of the films were determined from the cyclic voltammetry and chronoamperometry measurements using 0.1 M LiOH as supporting electrolyte. The ion storage capacity of the films was investigated using in situ spectroelectrochemical method and during the insertion/extraction process the films remained transparent. The powders were characterized by thermal analysis (DSC/TGA and X-ray diffraction.

ZnO epitaxy on SiC(0001-bar) substrate: Comparison with ZnO/SiC(0 0 0 1) heterostructure

Energy Technology Data Exchange (ETDEWEB)

Ashrafi, Almamun, E-mail: ash2phy@gmail.com [Department of Physics, University of Vermont, VT 05405 (United States); Aminuzzaman, Mohammod [Department of Chemical Science, Universiti Tunku Abdul Rahman, Perak (Malaysia)

2011-05-01

ZnO thin layers deposited on 6H-SiC substrates showed six-fold crystal symmetry with an epitaxial relationship of (0 0 0 2){sub ZnO}||(0 0 0 6){sub SiC} and [112-bar 0]{sub ZnO}||[112-bar 0]{sub SiC}. Despite the different 6H-SiC substrate surface orientations for the ZnO epitaxy, the orientation relationship of ZnO/6H-SiC heterostructures is identical, as confirmed by X-ray diffraction studies. In these ZnO/6H-SiC(0 0 0 1) and ZnO/6H-SiC(0001-bar) heterostructures, the valence band offsets are measured to be 1.12 eV and 1.09 eV, leading to the conduction band offset values of 0.75 eV and 0.72 eV, respectively. These slightly different band-offset values in ZnO/6H-SiC heterojunctions are attributed to the variation of valence band maximums and the different interface charge compensation mechanisms.

Synthesis of Zr-Si-O-N phases by carbonitriding reaction. Characterization of crystalline phases using the Rietveld method

Directory of Open Access Journals (Sweden)

Mazzoni A.D.

2001-01-01

Full Text Available Zirconium compounds are of great interest for ceramic application due to their excellent thermal and mechanical properties. Zirconium phases of the system Zr-O-C-N were obtained using carbonitriding reactions of zircon mineral (ZrO2.SiO2, under different reaction conditions. The reaction products were studied by X-ray diffraction (XRD using the Rietveld method. Silicon was employed as internal standard. Zirconium compounds formed were m-ZrO2 (monoclinic, beta"-zirconium oxynitride and a cubic Zr(C,N,O phase whose lattice parameter a o depends on the composition. The crystallite sizes of the three zirconium phases were determined also by XRD. The minority phases present are the ones of the Si-O-N-C system. The reaction conditions employed allows to obtain reaction products with low or without silicon content.

WxC-β-SiC Nanocomposite Catalysts Used in Aqueous Phase Hydrogenation of Furfural

Directory of Open Access Journals (Sweden)

Jacek Rogowski

2017-11-01

Full Text Available This study investigates the effects of the addition of tungsten on the structure, phase composition, textural properties and activities of β-SiC-based catalysts in the aqueous phase hydrogenation of furfural. Carbothermal reduction of SiO2 in the presence of WO3 at 1550 °C in argon resulted in the formation of WxC-β-SiC nanocomposite powders with significant variations in particle morphology and content of WxC-tipped β-SiC nano-whiskers, as revealed by TEM and SEM-EDS. The specific surface area (SSA of the nanocomposite strongly depended on the amount of tungsten and had a notable impact on its catalytic properties for the production of furfuryl alcohol (FA and tetrahydrofurfuryl alcohol (THFA. Nanocomposite WxC-β-SiC catalysts with 10 wt % W in the starting mixture had the highest SSA and the smallest WxC crystallites. Some 10 wt % W nanocomposite catalysts demonstrated up to 90% yield of THFA, in particular in the reduction of furfural derived from biomass, although the reproducible performance of such catalysts has yet to be achieved.

Synthesis of nucleated glass-ceramics using oil shale fly ash

International Nuclear Information System (INIS)

Luan Jingde; Li Aimin; Su Tong; Cui Xiaobo

2010-01-01

Nucleated glass-ceramics materials were produced from oil shale fly ash obtained from Huadian thermal power plant in China with the addition of analytic reagent CaO. On basis of differential thermal analysis (DTA) results, the nucleation and crystallization temperature of two parent glass samples with different alkalinity (Ak=m CaO /m SiO 2 ) were identified as Tn 1 = 810 deg. C, Tc 1 = 956 deg. C and Tn 2 = 824 o C, Tc 2 = 966 deg. C, respectively. X-ray diffraction (XRD) analysis of the produced nucleated glass-ceramics materials revealed that there was a coexistence phenomenon of multi-crystalline phase and the main crystalline phase was anorthite ([Ca,Na][AI,Si] 2 Si 2 O 8 ). The microstructure of the glass-ceramics materials was examined by scanning electron microscope (SEM). SEM observation indicated that there was an increase in the quantity of sphere-shaped crystals when crystallization time increased. Furthermore, the increase of alkalinity caused more amorphous phase occurring in glass-ceramics materials. Through the tests of physical and mechanical properties, the glass-ceramics materials with more crystalline phase and fine microstructure had high density, fine performance of resisting compression (328.92 MPa) and negligible water absorption. Through chemical resistance tests, the glass-ceramics samples showed strong corrosion resistance. Overall results indicated that it was a feasible attempt to produce nucleated glass-ceramics materials for building and decorative materials from oil shale fly ash.

Crystallization and sintering characteristics of CaO-Al2O3-SiO2 glasses in the presence of TiO2, CaF2 and ZrO2

International Nuclear Information System (INIS)

Banijamali, S.; Eftekhari Yekta, B.; Rezaie, H.R.; Marghussian, V.K.

2009-01-01

In this study, the effects of different amounts of TiO 2 , ZrO 2 and CaF 2 nucleating agents on sinterability, crystallization, mechanical properties and chemical resistance of glass-ceramics belonging to the CaO-Al 2 O 3 -SiO 2 system were investigated, using differential thermal analysis (DTA), X-ray diffractometry (XRD), scanning electron microscopy (SEM), mechanical and chemical resistance measurements. It was found that in CaF 2 containing samples, the sinterability, crystallization and mechanical properties were improved by increasing of CaF 2 amount. However, addition of ZrO 2 and TiO 2 increases the firing temperature required for complete densification of specimens. Our experiments showed that fluctuations of chemical composition of the residual glass phases during sintering were responsible for these dissimilar trends and greatly influenced mechanical and chemical properties. According to the obtained results, appropriate sinterability, acceptable mechanical and chemical properties, as well as desirable whiteness of the most promising specimens make them suitable choices for floor tile applications. The main crystallization phases in all fully sintered glass-ceramics were wollastonite, anorthite and calcium aluminum silicate.

Fabrication and characterization of Er+3 doped SiO2/SnO2 glass-ceramic thin films for planar waveguide applications

Science.gov (United States)

Guddala, S.; Chiappini, A.; Armellini, C.; Turell, S.; Righini, G. C.; Ferrari, M.; Narayana Rao, D.

2015-02-01

Glass-ceramics are a kind of two-phase materials constituted by nanocrystals embedded in a glass matrix and the respective volume fractions of crystalline and amorphous phase determine the properties of the glass-ceramics. Among these properties transparency is crucial in particular when confined structures, such as, dielectric optical waveguides, are considered. Moreover, the segregation of dopant rare-earth ions, like erbium, in low phonon energy crystalline medium makes these structures more promising in the development of waveguide amplifiers. Here we are proposing a new class of low phonon energy tin oxide semiconductor medium doped silicate based planar waveguides. Er3+ doped (100-x) SiO2-xSnO2 (x= 10, 20, 25 and 30mol%), glass-ceramic planar waveguide thin films were fabricated by a simple sol-gel processing and dip coating technique. XRD and HRTEM studies indicates the glass-ceramic phase of the film and the dispersion of ~4nm diameter of tin oxide nanocrystals in the amorphous phase of silica. The spectroscopic assessment indicates the distribution of the dopant erbium ions in the crystalline medium of tin oxide. The observed low losses, 0.5±0.2 dB/cm, at 1.54 μm communication wavelength makes them a quite promising material for the development of high gain integrated optical amplifiers.

Phase evolution and dielectric properties of MgTi2O5 ceramic sintered with lithium borosilicate glass

International Nuclear Information System (INIS)

Shin, Hyunho; Shin, Hee-Kyun; Jung, Hyun Suk; Cho, Seo-Yong; Hong, Kug Sun

2005-01-01

Phase evolution, densification, and dielectric properties of MgTi 2 O 5 dielectric ceramic, sintered with lithium borosilicate (LBS) glass, were studied. Reaction between LBS glass and MgTi 2 O 5 was significant in forming secondary phases such as TiO 2 and (Mg,Ti) 2 (BO 3 )O. The glass addition was not necessarily deleterious to the dielectric properties due to the formation of TiO 2 : permittivity increased and temperature coefficient of resonance frequency could be tuned to zero with the addition of LBS glass, although the inevitable glass-induced decrease of quality factor was not retarded by the formation of TiO 2 . The sintered specimen with 10 wt% LBS fired at 950 deg. C for 2 h showed permittivity of 19.3, quality factor of 6800 GHz, and τ f of -16 ppm/ deg. C

Ferromagnetic glass ceramics and glass fibers based on the composition of SiO{sub 2}-CaO-Al{sub 2}O{sub 3}-B{sub 2}O{sub 3}-Fe{sub 2}O{sub 3} glass system

Energy Technology Data Exchange (ETDEWEB)

Liu, Jianan, E-mail: lja@qlu.edu.cn; Zhu, Chaofeng; Zhang, Meimei; Zhang, Yanfei; Yang, Xuena

2017-03-15

Ferromagnetic glass-ceramics and glass fibers were obtained by the melt-method from the glass system SiO{sub 2}-CaO-Al{sub 2}O{sub 3}-B{sub 2}O{sub 3}-Fe{sub 2}O{sub 3} without performing any nucleation and crystallization heat treatments. Glass-ceramics and glass fibers were characterized by x-ray diffraction, scanning and transmission electron microscopy, magnetic measurements, and thermal expansion instrument. The influence of alumina content on the spontaneous crystallization of magnetite, magnetism properties and thermal expansion performances in glass were investigated. We examined the crystallization behavior of the glasses and found that the spontaneous crystallization capacity of magnetite and magnetism properties in base glass increases with increasing the content of alumina. The ferromagnetic glass fibers containing magnetite nano-crystals are also obtained. - Highlights: • Magnetite nano-crystals are formed spontaneously in the investigated glass systems. • The crystallization behavior of the glasses with the alumina content is examined. • Ferromagnetic glass fibers containing magnetite nano-crystals are obtained.

Cordierite Glass-Ceramics for Dielectric Materials

International Nuclear Information System (INIS)

Siti Mazatul Azwa Saiyed Mohd Nurddin; Selamat, Malek; Ismail, Abdullah

2007-01-01

The objective of this project is to examine the potential of using Malaysian silica sand deposit as SiO2 raw material in producing cordierite glass-ceramics (2MgO-2Al2O3-5SiO2) for dielectric materials. Upgraded silica sands from Terengganu and ex-mining land in Perak were used in the test-works. The glass batch of the present work has a composition of 45.00% SiO2, 24.00% Al2O3, 15.00% MgO and 8.50% TiO2 as nucleation agent. From the differential thermal analysis results, the crystallization temperature was found to start around 900 deg. C. The glass samples were heat-treated at 900 deg. C and 1000 deg. C. The X-ray diffraction analysis (XRD) results showed glass-ceramics from Terengganu samples containing mainly cordierite and minor β-quartz crystals. However, glass-ceramics from ex-mining land samples contained mainly α-quartz and minor cordierite crystals. Glass-ceramics with different crystal phases exhibit different mechanical, dielectric and thermal properties. Based on the test works, both silica sand deposits, can be potentially used to produce dielectric material component

Temperature stability of c-axis oriented LiNbO{sub 3}/SiO{sub 2}/Si thin film layered structures

Energy Technology Data Exchange (ETDEWEB)

Tomar, Monika [Department of Physics and Astrophysics, University of Delhi, Delhi (India)]. E-mail: mtomar@physics.du.ac.in; monikatomar@rediffmail.com; Gupta, Vinay; Mansingh, Abhai; Sreenivas, K. [Department of Physics and Astrophysics, University of Delhi, Delhi (India)

2001-08-07

Theoretical calculations have been performed for the temperature stability of the c-axis oriented LiNbO{sub 3} thin film layered structures on passivated silicon (SiO{sub 2}/Si) substrate with and without a non-piezoelectric SiO{sub 2} overlayer. The phase velocity, electromechanical coupling coefficient and temperature coefficient of delay (TCD) have been calculated. The thicknesses of various layers have been determined for optimum SAW performance with zero TCD. The presence of a non-piezoelectric SiO{sub 2} overlayer on LiNbO{sub 3} film is found to significantly enhance the coupling coefficient. The optimized results reveal that a high coupling coefficient of K{sup 2}=3.45% and a zero TCD can be obtained in the SiO{sub 2}/LiNbO{sub 3}/SiO{sub 2}/Si structure with a 0.235{lambda} thick LiNbO{sub 3} layer sandwiched between 0.1{lambda} thick SiO{sub 2} layers. (author)

Luminescence of MnS in glasses: spectroscopic probe for the study of thermal phase separation

Energy Technology Data Exchange (ETDEWEB)

Menassa, P E

1984-01-01

A new approach for studying thermal phase separation in sodium borosilicate glasses using MnS as a luminescent probe is investigated. Seventy-one samples of glasses activated by MnS inside and around the Na2O.B2O3.SiO2 miscibility gaps were prepared. These samples were then phase separated by dry thermal treatment. It is shown that on addition of MnO, the ternary Na2O.B2O3.SiO2 system behaved like other quaternary systems of the type X2O.MO.B2O3.SiO2 (X = Na, K; M = Mg, Ca, Ba, Zn). Scanning electron microscopy and X-ray microanalysis demonstrated that manganese concentrates preferentially in the boron-rich phase. This, analysis, in conjuction with a comparison of MnS emission spectra of upheated and heat treated glasses shows that the glasses are submicroscopically phase separated when prepared. The decay-time analysis of MnS luminescence indicates that the low energy emission band arises from MnS in the boron-rich phase while the high energy emission is due to MnS in the silica-rich phase. The difference in the crystal field parameters obtained from the excitation spectra of the two emission bands shows that the high energy emission band is from MnS in tetrahedral sites while the low energy emission band is from MnS in an octahedral environment.

Photochemical process of divalent germanium responsible for photorefractive index change in GeO2-SiO2 glasses.

Science.gov (United States)

Sakoh, Akifumi; Takahashi, Masahide; Yoko, Toshinobu; Nishii, Junji; Nishiyama, Hiroaki; Miyamoto, Isamu

2003-10-20

The photoluminescence spectra of the divalent Ge (Ge2+) center in GeO2-SiO2 glasses with different photosensitivities were investigated by means of excitation-emission energy mapping. The ultraviolet light induced photorefractivity has been correlated with the local structure around the Ge2+ centers. The glasses with a larger photorefractivity tended to exhibit a greater band broadening of the singlet-singlet transition on the higher excitation energy side accompanied by an increase in the Stokes shifts. This strongly suggests the existence of highly photosensitive Ge2+ centers with higher excitation energies. It is also found that the introduction of a hydroxyl group or boron species in GeO2-SiO2 glasses under appropriate conditions modifies the local environment of Ge2+ leading to an enhanced photorefractivity.

Effect of Y2O3-Al2O3 ratio on inter-granular phases and films in tape-casting α-SiC with high toughness

International Nuclear Information System (INIS)

Huang Rong; Gu Hui; Zhang Jingxian; Jiang Dongliang

2005-01-01

Silicon carbide (SiC) ceramics prepared from liquid phase sintering after aqueous-tape-casting can yield high toughness when appropriate amount of Y 2 O 3 -Al 2 O 3 are added, even though no elongated grains are present. Grain boundaries (GB), second-phases and hetero-phase boundaries (HB) in 2 samples with additive mole ratios of 3:5 and 3:7 are investigated using high-resolution and analytical electron microscopy (HREM and AEM). The meta-stable YAlO 3 (YAP) was nucleated from SiC surfaces in the sample with Y/Al = 3:5 as revealed by crystallographic relations across the HB, whilst relatively thick amorphous films were found at GB. In contrary, the higher level of Al 2 O 3 additives decreases the GB film thickness in the sample with Y/Al = 3:7, and the homogeneous nucleation of Y 3 Al 5 O 12 (YAG) occurs at triple pockets accompanying with thick HB films. The strong variation of GB widths is a result of GB wetting in the sample with Y/Al = 3:5 and HB wetting in the sample of Y/Al = 3:7, both by liquid Al 2 O 3 . The energy of GB in the former sample is higher than the energy of HB as exhibited by the preferential nucleation of meta-stable YAP on SiC surfaces, which results in wetting of GB by the liquid; the situation is opposite in the latter sample as the wetting of HB occurs, leading to de-wetting of GB. The thermal mismatch between SiC and YAP or YAG as well as the presence of amorphous films facilitate the creation of micro-crack to promote inter-granular fracture and result in high toughness in both SiC ceramics

Network structure and thermal stability study of high temperature seal glass

Science.gov (United States)

Lu, K.; Mahapatra, M. K.

2008-10-01

High temperature seal glass has stringent requirement on glass thermal stability, which is dictated by glass network structures. In this study, a SrO-La2O3-Al2O3-B2O3-SiO2 based glass system was studied using nuclear magnetic resonance, Raman spectroscopy, and x-ray diffraction for solid oxide cell application purpose. Glass structural unit neighboring environment and local ordering were evaluated. Glass network connectivity as well as silicon and boron glass former coordination were calculated for different B2O3:SiO2 ratios. Thermal stability of the borosilicate glasses was studied after thermal treatment at 850 °C. The study shows that high B2O3 content induces BO4 and SiO4 structural unit ordering, increases glass localized inhomogeneity, decreases glass network connectivity, and causes devitrification. Glass modifiers interact with either silicon- or boron-containing structural units and form different devitrified phases at different B2O3:SiO2 ratios. B2O3-free glass shows the best thermal stability among the studied compositions, remaining stable after thermal treatment for 200 h at 850 °C.

Network rigidity and properties of SiO2 and GeO2 glasses under pressure.

Science.gov (United States)

Trachenko, Kostya; Dove, Martin T; Brazhkin, Vadim; El'kin, F S

2004-09-24

We report in situ studies of SiO2 glass under pressure and find that temperature-induced densification takes place in a pressure window. To explain this effect, we study how rigidity of glasses changes under pressure, with rigidity percolation affecting the dynamics of local relaxation events. We link rigidity percolation in glasses to other effects, including a large increase of crystallization temperature and logarithmic relaxation under pressure.

Experimental Determination of the Effect of the Ratio of B/Al on Glass Dissolution along the Nepheline (NaAlSiO₄) – Malinkoite (NaBSiO₄) Join

Energy Technology Data Exchange (ETDEWEB)

Pierce, Eric M; Reed, Lunde R; Shaw, Wendy J; McGrail, B Peter; Icenhower, Jonathan P; Windisch, Charles F; Cordova, Elsa A; Broady, Johnathan W

2010-03-27

The dissolution kinetics of five glasses along the NaAlSiO₄-NaBSiO₄ join were used to evaluate how the structural variations associated with boron-aluminum substitution affect the rate of dissolution. The composition of each glass varied inversely in mol% of Al₂O₃ (5 to 25 mol%) and B₂O₃ (20 to 0 mol%) with Na₂O (25 mol%) and SiO₂ (50 mol%) making up the remaining amount, in every case Na/(Al+B) = 1.0. Single-pass flow-through experiments (SPFT) were conducted under dilute conditions as a function of solution pH (from 7.0 to 12.0) and temperature (from 23° to 90°C). Analysis by ²⁷Al and ²⁹Si MAS-NMR suggests Al (~98% ^[4]Al) and Si atoms (~100% ^[4]Si) occupy a tetrahedral coordination whereas, B atoms occupy both tetrahedral ([4]B) and trigonal (^[3]B) coordination. The distribution of [3]B fractionated between ^[3]B(ring) and ^[3]B(non-ring) moieties, with the ^[3]B(ring)/^[3]B(non-ring) ratio increases with the B/Al ratio. The MAS-NMR results also indicated an increase in the fraction of ^[4]B with an increase in the B/Al ratio. But despite the changes in the B/Al ratio and B coordination, the ²⁹Si spectra maintain a chemical shift between -88 to -84 ppm for each glass. Unlike the ²⁹Si spectra, the ²⁷Al resonances shift to more positive values with an increase in the B/Al ratio which suggests mixing between the ^[4]Al and ^[3]B sites, assuming avoidance between tetrahedral trivalent cations (^[4]Al-O-^[4]B avoidance). Raman spectroscopy was use to augment the results collected from MAS-NMR and demonstrated that NeB4 (glass sample with the highest B content) was glass-glass phase separated (e.g., heterogeneous glass). Results from SPFT experiments suggest a forward rate of reaction and pH power law

Investigating the influence of Na+ and Sr2+ on the structure and solubility of SiO2-TiO2-CaO-Na2O/SrO bioactive glass.

Science.gov (United States)

Li, Y; Placek, L M; Coughlan, A; Laffir, F R; Pradhan, D; Mellott, N P; Wren, A W

2015-02-01

This study was conducted to determine the influence that network modifiers, sodium (Na+) and strontium (Sr2+), have on the solubility of a SiO2-TiO2-CaO-Na2O/SrO bioactive glass. Glass characterization determined each composition had a similar structure, i.e. bridging to non-bridging oxygen ratio determined by X-ray photoelectron spectroscopy. Magic angle spinning nuclear magnetic resonance (MAS-NMR) confirmed structural similarities as each glass presented spectral shifts between -84 and -85 ppm. Differential thermal analysis and hardness testing revealed higher glass transition temperatures (Tg 591-760 °C) and hardness values (2.4-6.1 GPa) for the Sr2+ containing glasses. Additionally the Sr2+ (~250 mg/L) containing glasses displayed much lower ion release rates than the Na+ (~1,200 mg/L) containing glass analogues. With the reduction in ion release there was an associated reduction in solution pH. Cytotoxicity and cell adhesion studies were conducted using MC3T3 Osteoblasts. Each glass did not significantly reduce cell numbers and osteoblasts were found to adhere to each glass surface.

Optical properties of the Al2O3/SiO2 and Al2O3/HfO2/SiO2 antireflective coatings

Science.gov (United States)

Marszałek, Konstanty; Winkowski, Paweł; Jaglarz, Janusz

2014-01-01

Investigations of bilayer and trilayer Al2O3/SiO2 and Al2O3/HfO2/SiO2 antireflective coatings are presented in this paper. The oxide films were deposited on a heated quartz glass by e-gun evaporation in a vacuum of 5 × 10-3 [Pa] in the presence of oxygen. Depositions were performed at three different temperatures of the substrates: 100 °C, 200 °C and 300 °C. The coatings were deposited onto optical quartz glass (Corning HPFS). The thickness and deposition rate were controlled with Inficon XTC/2 thickness measuring system. Deposition rate was equal to 0.6 nm/s for Al2O3, 0.6 nm - 0.8 nm/s for HfO2 and 0.6 nm/s for SiO2. Simulations leading to optimization of the thin film thickness and the experimental results of optical measurements, which were carried out during and after the deposition process, have been presented. The optical thickness values, obtained from the measurements performed during the deposition process were as follows: 78 nm/78 nm for Al2O3/SiO2 and 78 nm/156 nm/78 nm for Al2O3/HfO2/SiO2. The results were then checked by ellipsometric technique. Reflectance of the films depended on the substrate temperature during the deposition process. Starting from 240 nm to the beginning of visible region, the average reflectance of the trilayer system was below 1 % and for the bilayer, minima of the reflectance were equal to 1.6 %, 1.15 % and 0.8 % for deposition temperatures of 100 °C, 200 °C and 300 °C, respectively.

Nitric acid oxidation of Si (NAOS) method for low temperature fabrication of SiO{sub 2}/Si and SiO{sub 2}/SiC structures

Energy Technology Data Exchange (ETDEWEB)

Kobayashi, H., E-mail: koba771@ybb.ne.jp [Institute of Scientific and Industrial Research, Osaka University, and CREST, Japan Science and Technology Agency, 8-1 Mihogaoka, Ibaraki, Osaka 567-0047 (Japan); Imamura, K.; Kim, W.-B.; Im, S.-S.; Asuha [Institute of Scientific and Industrial Research, Osaka University, and CREST, Japan Science and Technology Agency, 8-1 Mihogaoka, Ibaraki, Osaka 567-0047 (Japan)

2010-07-15

We have developed low temperature formation methods of SiO{sub 2}/Si and SiO{sub 2}/SiC structures by use of nitric acid, i.e., nitric acid oxidation of Si (or SiC) (NAOS) methods. By use of the azeotropic NAOS method (i.e., immersion in 68 wt% HNO{sub 3} aqueous solutions at 120 deg. C), an ultrathin (i.e., 1.3-1.4 nm) SiO{sub 2} layer with a low leakage current density can be formed on Si. The leakage current density can be further decreased by post-metallization anneal (PMA) at 200 deg. C in hydrogen atmosphere, and consequently the leakage current density at the gate bias voltage of 1 V becomes 1/4-1/20 of that of an ultrathin (i.e., 1.5 nm) thermal oxide layer usually formed at temperatures between 800 and 900 deg. C. The low leakage current density is attributable to (i) low interface state density, (ii) low SiO{sub 2} gap-state density, and (iii) high band discontinuity energy at the SiO{sub 2}/Si interface arising from the high atomic density of the NAOS SiO{sub 2} layer. For the formation of a relatively thick (i.e., {>=}10 nm) SiO{sub 2} layer, we have developed the two-step NAOS method in which the initial and subsequent oxidation is performed by immersion in {approx}40 wt% HNO{sub 3} and azeotropic HNO{sub 3} aqueous solutions, respectively. In this case, the SiO{sub 2} formation rate does not depend on the Si surface orientation. Using the two-step NAOS method, a uniform thickness SiO{sub 2} layer can be formed even on the rough surface of poly-crystalline Si thin films. The atomic density of the two-step NAOS SiO{sub 2} layer is slightly higher than that for thermal oxide. When PMA at 250 deg. C in hydrogen is performed on the two-step NAOS SiO{sub 2} layer, the current-voltage and capacitance-voltage characteristics become as good as those for thermal oxide formed at 900 deg. C. A relatively thick (i.e., {>=}10 nm) SiO{sub 2} layer can also be formed on SiC at 120 deg. C by use of the two-step NAOS method. With no treatment before the NAOS method

Production of Al2O3–SiC nano-composites by spark plasma sintering

International Nuclear Information System (INIS)

Mansour Razavi; Ali Reza Farajipour; Mohammad Zakeri; Mohammad Reza Rahimipour; Ali Reza Firouzbakht

2017-01-01

In this paper, Al2O3–SiC composites were produced by SPS at temperatures of 1600°C for 10min under vacuum atmosphere. For preparing samples, Al2O3 with the second phase including of micro and nano-sized SiC powder were milled for 5h. The milled powders were sintered in a SPS machine. After sintering process, phase studies, densification and mechanical properties of Al2O3–SiC composites were examined. Results showed that the specimens containing micro-sized SiC have an important effect on bulk density, hardness and strength. The highest relative density, hardness and strength were 99.7%, 324.6 HV and 2329MPa, respectively, in Al2O3–20wt% SiCmicro composite. Due to short time sintering, the growth was limited and grains still remained in nano-meter scale. [es

Fracture and subcritical crack-growth behavior of Y-Si-Al-O-N glasses and Si3N4 ceramics

International Nuclear Information System (INIS)

Bhatnagar, A.; Hoffman, M.J.; Dauskardt, R.H.

2000-01-01

Fracture and environmentally assisted subcritical crack-growth processes are examined in bulk Y-Si-Al-O-N oxynitride glasses with compositions typical of the grain boundary phase of silicon nitride ceramics. Both long-crack (in compact tension specimens) as well as short-crack behavior (using indentation techniques) were investigated to establish a reliable fracture toughness and to elucidate the anomalous densification behavior of the oxynitride glass. Environmentally assisted subcritical crack-growth processes were studied in inert, moist, and wet environments under both cyclic and static loading conditions. Behavior is discussed in terms of the interaction of the environment with the crack tip. Likely mechanisms for environmentally assisted crack growth are discussed and related to the subcritical crack-growth behavior of silicon nitride ceramics

Properties of sodium borosilicate glasses/Al2O3 sintered composites containing fluorides. Gan Fukkabutsu hokei san natoriumu garasu to alumina fukugo shoketsutai no bussei

Energy Technology Data Exchange (ETDEWEB)

Ryu, Bonggi; Yasui, I [The Univ. of Tokyo, Tokyo (Japan). Inst. of Industrial Science

1993-06-01

Glass/alumina sintered composites were synthesized from sodium borosilicate glass powder containing fluorides like AlF3 and NaF3, and Al2O3, and change in material properties was examined. Glass compositions of B2O3 and Na2O greatly affected the crystal phase and material properties. Nephelin crystal phase was extracted by the reaction of Na2O, NaF2, SiO2 and Al2O3 when B/Na<1. Coefficient of thermal expansion increased with the increase of Na/Si ratio. The residual amount of fluorides of sintered materials in nitrogen atmosphere was higher than that of air, and differed with the type of fluoride. The F[sup -] of NaF is bonded with Si of glass network and forms quiet stable glass structure, whereas, F[sup -] of AlF3 reacts with Si[sup 4+] forming SiF4 which is vaporized. Sintering temperature and dielectric constant of sintered materials containing fluoride was lower than the sintered materials without fluorides addition, however, at a sintering temperature range of 100 to 150[degree]C, it was inferred that this was because of the increase in voids due to SiF4 formed in the reaction. 16 refs., 17 figs., 3 tabs.

Study on crystallization kinetics and phase evolution in Li2O-Al2O3-GeO2-P2O5 glass-ceramics system

Science.gov (United States)

Das, Anurup; Dixit, Anupam; Goswami, Madhumita; Mythili, R.; Hajra, R. N.

2018-04-01

To address the safety issues related to liquid electrolyte and improve the battery performance, Solid State Electrolytes (SSEs) are now in frontier area of research interest. We report here synthesis of Li-SSE based on Li2O-Al2O3-GeO2-P2O5 (LAGP) system with NASICON structure. Glass sample with nominal composition Li1.5Al0.5Ge1.5P2.5Si0.5O12 was prepared by melt-quenching technique. Non-isothermal crystallization kinetics was studied using DSC and activation energy of crystallisation was calculated to be ˜ 246 kJ/mol using Kissinger's equation. XRD of heat treated samples show the formation of required LiGe2(PO4)3 phase along with other minor phases. Compositional analysis using SEM-EDX confirms enrichment of Ge and Si along the grain boundaries.

Luminescence and energy transfer of Tb3+-doped BaO-Gd2O3-Al2O3-B2O3-SiO2 glasses.

Science.gov (United States)

Zuo, Chenggang; Huang, Jinze; Liu, Shaoyou; Xiao, Anguo; Shen, Youming; Zhang, Xiangyang; Zhou, Zhihua; Zhu, Ligang

2017-12-05

Transparent Tb 3+ -doped BaO-Gd 2 O 3 -Al 2 O 3 -B 2 O 3 -SiO 2 glasses with the greater than 4g/cm 3 were prepared by high temperature melting method and its luminescent properties have been investigated by measured UV-vis transmission, excitation, emission and luminescence decay spectra. The transmission spectrum shows there are three weak absorption bands locate at about 312, 378 and 484nm in the glasses and it has good transmittance in the visible spectrum region. Intense green emission can be observed under UV excitation. The effective energy transfer from Gd 3+ ion to Tb 3+ ion could occur and sensitize the luminescence of Tb 3+ ion. The green emission intensity of Tb 3+ ion could change with the increasing SiO 2 /B 2 O 3 ratio in the borosilicate glass matrix. With the increasing concentration of Tb 3+ ion, 5 D 4 → 7 F J transitions could be enhanced through the cross relaxation between the two nearby Tb 3+ ions. Luminescence decay time of 2.12ms from 546nm emission is obtained. The results indicate that Tb 3+ -doped BaO-Gd 2 O 3 -Al 2 O 3 -B 2 O 3 -SiO 2 glasses would be potential scintillating material for applications in X-ray imaging. Copyright © 2017 Elsevier B.V. All rights reserved.

On the relations between ISE and structure in some RE(Mg)SiAlO(N) glasses

DEFF Research Database (Denmark)

Keding, Ralf; Dauce, Rachel; Sangleboeuf, J. C.

2008-01-01

silicate units and SiO3N and SiO2N2 units are created when nitrogen is introduced into the glass network. The average number of rigid bonds per network former was calculated from the glasses’ composition. A discrepancy between and the Raman spectra of the glasses suggests that parts of the magnesium...... Six oxide and oxynitride glasses were synthesized in the Y–Mg–Si–Al–O–N, Nd–Mg–Si–Al–O–N and La–Mg–Si–Al–O–N systems. As already known, nitrogen introduction increases the T g, packing factor and mechanical properties of the glasses. Cationic substitution also has an influence on the glasses......’ behavior, particularly in terms of sensitivity to indentation load/size effect (ISE). The structure of the yttrium-containing glasses was investigated by mean of 27Al and 29Si MAS-NMR. Al is found to occur for 2/3 as a network former and for 1/3 as a modifier. The oxide glass mainly contains Q2 and Q3...

Structure of Mg2SiO4 glass up to 140 GPa

Science.gov (United States)

Prescher, C.; Prakapenka, V.; Wang, Y.; Skinner, L. B.

2014-12-01

The physical properties of melts at temperature and pressure conditions of the Earth's mantle have a fundamental influence on the chemical and thermal evolution of the Earth. However, direct investigations of melt structures at these conditions are experimentally very difficult or even impossible with current capabilities. In order to still be able to obtain an estimate of the structural behavior of melts at high pressures and temperatures, amorphous materials have been widely used as analogue materials. In particular the investigation of sound wave velocities of amorphous SiO2 and MgSiO3 as analogues for silicate melts indicate structural changes at about ~30-40 GPa and ~130-140 GPa [1]. The transition pressures are lower for MgSiO3 than for SiO2 indicating that these transitions are affected by the degree of polymerization of the SiO2 network of the glasses. Nevertheless, these measurements only give a hint about the occurrence of structural transitions but lack information on the actual structural changes accompanied by the sound wave velocity discontinuities. The pressure of the second structural transition at ~130-140 GPa is of vital importance for geophysics. If it causes silicate melts to become denser than the surrounding solid material, it would result in negatively buoyant melts close to the core-mantle boundary, which could be a major factor affecting the chemical stratification of the Earth's mantle during an early magma ocean after the moon forming impact. In order to resolve the structural transition and estimate the effect of a different degree of polymerization further, we studied the structural behavior of Mg2SiO4 glass up to 140 GPa using X-ray total scattering and pair distribution function analysis. The measurements were performed at the GSECARS 13-IDD beamline at the APS employing the newly developed multichannel collimator (MCC) setup. The MCC effectively removes unwanted Compton scattering of the diamond anvils and enables easy extraction of

Optical and dielectric properties of isothermally crystallized nano-KNbO3 in Er3+-doped K2O-Nb2O5-SiO2 glasses.

Science.gov (United States)

Chaliha, Reenamoni Saikia; Annapurna, K; Tarafder, Anal; Tiwari, V S; Gupta, P K; Karmakar, Basudeb

2010-01-01

Precursor glass of composition 25K(2)O-25Nb(2)O(5)-50SiO(2) (mol%) doped with Er(2)O(3) (0.5 wt% in excess) was isothermally crystallized at 800 degrees C for 0-100 h to obtain transparent KNbO(3) nanostructured glass-ceramics. XRD, FESEM, TEM, FTIRRS, dielectric constant, refractive index, absorption and fluorescence measurements were carried out to analyze the morphology, dielectric, structure and optical properties of the glass-ceramics. The crystallite size of KNbO(3) estimated from XRD and TEM is found to vary in the range 7-23 nm. A steep rise in the dielectric constant of glass-ceramics with heat-treatment time reveals the formation of ferroelectric nanocrystalline KNbO(3) phase. The measured visible photoluminescence spectra have exhibited green emission transitions of (2)H(11/2), (4)S(3/2)-->(4)I(15/2) upon excitation at 377 nm ((4)I(15/2)-->(4)G(11/2)) absorption band of Er(3+) ions. The near infrared (NIR) emission transition (4)I(13/2)-->(4)I(15/2) is detected around 1550 nm on excitation at 980 nm ((4)I(15/2)-->(4)I(11/2)) of absorption bands of Er(3+) ions. It is observed that photoluminescent intensity at 526 nm ((2)H(11/2)-->(4)I(15/2)), 550 nm ((4)S(3/2)-->(4)I(15/2)) and 1550 nm ((4)I(13/2)-->(4)I(15/2)) initially decrease and then gradually increase with increase in heat-treatment time. The measured lifetime (tau(f)) of the (4)I(13/2)-->(4)I(15/2) transition also possesses a similar trend. The measured absorption and fluorescence spectra reveal that the Er(3+) ions gradually enter into the KNbO(3) nanocrystals. Copyright 2009 Elsevier B.V. All rights reserved.

Synthesis and structure of Na-Li-Si-Al-P-O-N glasses prepared by melt nitridation using NH3

International Nuclear Information System (INIS)

Kidar, A.; Pomeroy, M.J.; Hampshire, S.; Mercier, C.; Leriche, A.; Revel, B.

2012-01-01

Na-Li-Si-Al-P-O-N glasses have been prepared by nitridation of a pre-synthesized Na 2 O-Li 2 O-SiO 2 -P 2 O 5 -Al 2 O 3 glass under anhydrous ammonia. Nitrogen for oxygen substitution increases the network connectivity leading to increases in microhardness and glass transition temperature. Raman and 31 P MAS-NMR spectroscopy indicate sequential nitridation reactions forming PO 3 N and PO 2 N 2 species. The data collected so far show no evidence of N/O substitutions in the silicate sub-network. (authors)

Production of Al2O3–SiC nano-composites by spark plasma sintering

Directory of Open Access Journals (Sweden)

Mansour Razavi

2017-07-01

Full Text Available In this paper, Al2O3–SiC composites were produced by SPS at temperatures of 1600 °C for 10 min under vacuum atmosphere. For preparing samples, Al2O3 with the second phase including of micro and nano-sized SiC powder were milled for 5 h. The milled powders were sintered in a SPS machine. After sintering process, phase studies, densification and mechanical properties of Al2O3–SiC composites were examined. Results showed that the specimens containing micro-sized SiC have an important effect on bulk density, hardness and strength. The highest relative density, hardness and strength were 99.7%, 324.6 HV and 2329 MPa, respectively, in Al2O3–20 wt% SiCmicro composite. Due to short time sintering, the growth was limited and grains still remained in nano-meter scale.

Study of the optical properties of deposited thin films on glass of HMDSO(C6H18Si2O) plasma

International Nuclear Information System (INIS)

Saloum, S.; Naddaf, M.

2007-06-01

Deposition of amorphous silicone like (Si:Ox:Cy:Hz) thin films in a remote RF hollow cathode discharge plasma using HMDSO (C 6 H 1 8Si 2 O) as monomer and Ar as feed gas, has been investigated for films optical constants as a function of RF power (100-300 W) and precursor flow rate (1-10 sccm), using different substrates: Quartz, BK7, and Glass. The optical constants (refractive index, extinction coefficient and dielectric constant) have been obtained by reflection/transmission measurements in the range 300-700 nm. The optical energy-band gap Eg and the optical-absorption tail E have been estimated from optical absorption spectra. The results were interpreted using plasma diagnostic by optical emission spectroscopy.(author)

Solid-phase crystallization of amorphous silicon on ZnO:Al for thin-film solar cells

Energy Technology Data Exchange (ETDEWEB)

Becker, C.; Conrad, E.; Dogan, P.; Fenske, F.; Gorka, B.; Haenel, T.; Lee, K.Y.; Rau, B.; Ruske, F.; Weber, T.; Gall, S.; Rech, B. [Helmholtz-Zentrum Berlin fuer Materialien und Energie (formerly Hahn-Meitner-Institut Berlin), Kekulestr. 5, D-12489 Berlin (Germany); Berginski, M.; Huepkes, J. [Institute of Photovoltaics, Forschungszentrum Juelich GmbH, D-52425 Juelich (Germany)

2009-06-15

The suitability of ZnO:Al thin films for polycrystalline silicon (poly-Si) thin-film solar cell fabrication was investigated. The electrical and optical properties of 700 -nm-thick ZnO:Al films on glass were analyzed after typical annealing steps occurring during poly-Si film preparation. If the ZnO:Al layer is covered by a 30 nm thin silicon film, the initial sheet resistance of ZnO:Al drops from 4.2 to 2.2 {omega} after 22 h annealing at 600 C and only slightly increases for a 200 s heat treatment at 900 C. A thin-film solar cell concept consisting of poly-Si films on ZnO:Al coated glass is introduced. First solar cell results will be presented using absorber layers either prepared by solid-phase crystallization (SPC) or by direct deposition at 600 C. (author)

The far infrared radiation characteristics for Li2O.Al2O3.4SiO2(LAS) glass-ceramics and transition-metal oxide

International Nuclear Information System (INIS)

Huh, Nam Jung; Yang, Joong Sik

1991-01-01

The far infrared radiation characteristic for Li 2 O.Al 2 O 3 .4SiO 2 (LAS) glass, the LAS glass-ceramic and sintered transition metal oxides such as CuO, Fe 2 O 3 and Co 3 O 4 , were investigated. LAS glass and LAS glass-ceramic was higher than that of the LAS glass. Heat-treated CuO and Co 3 o 4 had radiation characteristic of high efficiency infrared radiant, and heat-treated Fe 2 O 3 had radiation characteristic that infrared emissivity decreased in higher was length above 15μm. (Author)

Phase transformations in lithium bearing sodiumborosilicate base glass melts for the solidification of HAW

International Nuclear Information System (INIS)

Goettlicher, J.

1994-10-01

Metastable phase separation has been observed in the Li-bearing basic glass SM58. This observation gave rise to examine the exsolution behaviour in model glasses by chemical substitution. It is impossible to produce metastable phase separation in the Li-free HAW-glasses VG98/12 and VG98/12.2. However, one can't exclude textural changes of Li-bearing glasses, because in a HAW-container the central temperature remains at about 300 C for more than 50 years. For the first time it has been tried to find a relationship between glass textures and structural parameters by combining textural investigations (electron microscopy) with structural determinations (NMR, WAXS). Modell glasses belong to the system (Li, Na) 2 O.B 2 O 3 , (Al 2 O 3 ).n(TO 2 ), with T=Si, Ge and n=2, 4, 6. Furthermore glasses from the KfK and from Mol (PAMELA) were investigated. A newly built apparatus was used to prepare glasses by replica technique (PtIrC oblique shadowing) for TEM investigations. This method turned out to be well suited to study glass textures with features down to 5 nm. Sometimes direct examinations of ion-thinned glasses showed that their textures were affected by radiation damage, caused by accelerated electrons. LVSE-(Low Voltage Scanning Electron)- and AF-(Atomic Force)- microscopy seems to be a promising method for studying glass surfaces and their textures directly. (orig./MM) [de

Phase Stability and Thermal Conductivity of Composite Environmental Barrier Coatings on SiC/SiC Ceramic Matrix Composites

Science.gov (United States)

Benkel, Samantha; Zhu, Dongming

2011-01-01

Advanced environmental barrier coatings are being developed to protect SiC/SiC ceramic matrix composites in harsh combustion environments. The current coating development emphasis has been placed on the significantly improved cyclic durability and combustion environment stability in high-heat-flux and high velocity gas turbine engine environments. Environmental barrier coating systems based on hafnia (HfO2) and ytterbium silicate, HfO2-Si nano-composite bond coat systems have been processed and their stability and thermal conductivity behavior have been evaluated in simulated turbine environments. The incorporation of Silicon Carbide Nanotubes (SiCNT) into high stability (HfO2) and/or HfO2-silicon composite bond coats, along with ZrO2, HfO2 and rare earth silicate composite top coat systems, showed promise as excellent environmental barriers to protect the SiC/SiC ceramic matrix composites.

Phase Separation and Crystallization in soda-lime borosilicate glass enriched in MoO{sub 3} studied by in situ Raman spectroscopy at high temperature

Energy Technology Data Exchange (ETDEWEB)

Magnin, M.; Schuller, S.; Advocat, T. [CEA Valrho, DEN/DTCD/SCDV, Laboratoire d' Etude de Base sur les Verres, BP 17171, 30207 Bagnols-sur-Ceze Cedex (France); Caurant, D.; Majerus, O. [Laboratoire de Chimie de la Matiere Condensee de Paris- LCMCP - UMR-CNRS 7574, Ecole Nationale Superieure de Chimie de Paris - ENSCP, Paristech, 75231 Paris (France); Ligny, D. de [Laboratoire de Physico-Chimie des Materiaux Luminescents- LPCML - UMR-CNRS 5620, Universite Claude Bernard Lyon1, 69622 Villeurbanne (France)

2008-07-01

Phase separation and crystallisation processes may arise in molten glass when the MoO{sub 3} content exceeds its solubility limit. Molybdenum combined with other elements such as alkali and alkaline-earth may form crystalline molybdates, known as 'yellow phases' in nuclear glasses. In order to establish the sequence of phase separation and crystallization processes occurring during the cooling of the melt, a non-radioactive simplified glass composition was chosen in the SiO{sub 2}-B{sub 2}O{sub 3}-Na{sub 2}O-CaO system, with 2 mol.% MoO{sub 3}. Various cooling scenarios were tested: cooling by air blowing, quenching between two copper plates and cooling on metallic plate. The resulting glass specimens were then characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and Raman spectroscopy in temperature. These observations made it possible to determine the sequence and the appearance temperature of phenomena upon cooling: first, a phase separation occurs, (small droplets dispersed in the molten glass) followed by molybdates crystallization inside the droplets. (authors)

On the origin of near-IR luminescence in SiO{sub 2} glass with bismuth as the single dopant. Formation of the photoluminescent univalent bismuth silanolate by SiO{sub 2} surface modification

Energy Technology Data Exchange (ETDEWEB)

Romanov, A.N., E-mail: alexey.romanov@list.ru; Haula, E.V.; Shashkin, D.P.; Vtyurina, D.N.; Korchak, V.N.

2017-03-15

Near infrared photoluminescent bismuth(I) silanolate centers ((≡Si-O){sub 3}Si–O-Bi) were prepared on the surface of SiO{sub 2} xerogel, by the treatment in the vapors of bismuth(I) chloride. The optical properties of these groups are almost identical to that of photoluminescent centers in the bulk SiO{sub 2} glasses with bismuth as the single dopant. - Highlights: • univalent bismuth silanolate can be prepared on SiO{sub 2} surface by treatment in BiCl vapors. • univalent bismuth silanolate is responsible for NIR photoluminescence in Bi-doped SiO{sub 2} glass. • univalent bismuth silanolate is the active center in laser, operating on Bi-doped SiO{sub 2} fiber.

Evaluation method of TiO2-SiO2 ultra-low-expansion glasses with periodic striae using the LFB ultrasonic material characterization system.

Science.gov (United States)

Kushibiki, Jun-ichi; Arakawa, Mototaka; Ohashi, Yuji; Suzuki, Kouji

2006-09-01

Experimental procedures and standard specimens for characterizing and evaluating TiO2-SiO2 ultra-low expansion glasses with periodic striae using the line-focus-beam (LFB) ultrasonic material characterization system are discussed. Two types of specimens were prepared, with specimen surfaces parallel and perpendicular to the striae plane using two different grades of glass ingots. The inhomogeneities of each of the specimens were evaluated at 225 MHz. It was clarified that parallel specimens are useful for accurately measuring velocity variations of leaky surface acoustic waves (LSAWs) excited on a water-loaded specimen surface associated with the striae. Perpendicular specimens are useful for obtaining periodicities in the striae for LSAW propagation perpendicular to the striae plane on a surface and for precisely measuring averaged velocities for LSAW propagation parallel to the striae plane. The standard velocity of Rayleigh-type LSAWs traveling parallel to the striae plane for the perpendicular specimens was numerically calculated using the measured velocities of longitudinal and shear waves and density. Consequently, a reliable standard specimen with an LSAW velocity of 3308.18 +/- 0.35 m/s at 23 degrees C and its temperature coefficient of 0.39 (m/s)/degrees C was obtained for a TiO2-SiO2 glass with a TiO2 concentration of 7.09 wt%. A basis for the striae analysis using this ultrasonic method was established.

Effects of Fiber Content on Mechanical Properties of CVD SiC Fiber-Reinforced Strontium Aluminosilicate Glass-Ceramic Composites

Science.gov (United States)

Bansal, Narottam P.

1996-01-01

Unidirectional CVD SiC(f)(SCS-6) fiber-reinforced strontium aluminosilicate (SAS) glass-ceramic matrix composites containing various volume fractions, approximately 16 to 40 volume %, of fibers were fabricated by hot pressing at 1400 C for 2 h under 27.6 MPa. Monoclinic celsian, SrAl2Si2O8, was the only crystalline phase formed, with complete absence of the undesired hexacelsian phase, in the matrix. Room temperature mechanical properties were measured in 3-point flexure. The matrix microcracking stress and the ultimate strength increased with increase in fiber volume fraction, reached maximum values for V(sub f) approximately equal to 0.35, and degraded at higher fiber loadings. This degradation in mechanical properties is related to the change in failure mode, from tensile at lower V(sub f) to interlaminar shear at higher fiber contents. The extent of fiber loading did not have noticeable effect on either fiber-matrix debonding stress, or frictional sliding stress at the interface. The applicability of micromechanical models in predicting the mechanical properties of the composites was also examined. The currently available theoretical models do not appear to be useful in predicting the values of the first matrix cracking stress, and the ultimate strength of the SCS-6/SAS composites.

SiC/SiC composites through transient eutectic-phase route for fusion applications

International Nuclear Information System (INIS)

Katoh, Y.; Kohyama, A.; Nozawa, T.; Sato, M.

2004-01-01

Factors that may limit attractiveness of silicon-carbide-based ceramic composites to fusion applications include thermal conductivity, applicable design stress, chemical compatibility, hermeticity, radiation stability and fabrication cost. A novel SiC/SiC composite, which has recently been developed through nano-infiltration and transient eutectic-phase (NITE) processing route, surpasses conventional materials in many of these properties. In this paper, the latest development, property evaluation and prospect of the NITE SiC/SiC composites are briefly reviewed. The topics range from fundamental aspects of process development to industrial process development. Elevated temperature strength, fracture behavior, and thermo-physical properties in various environments are summarized. Future directions of materials and application technology development are also discussed

Low temperature spin-glass-like phases in magnetic nano-granular composites

KAUST Repository

Zhang, Bei

2012-09-01

It is a common understanding that the dipole-dipole interaction among the magnetic nanoparticles may result in a low-temperature spin-glass phase, which has been evidenced by observation of aging effect and memory effect. However, several studies on the nano-particles systems showed that some of the observed spin-glass-like phenomena could be due to the existence of spin-glasslike shells surrounding the ferrimagnetic cores. Therefore, it is very important to understand that how the dipole-dipole interaction induce the spin-glass phase. In order to address this issue, we have fabricated Co-SiO 2 and Fe-SiO 2 nano-granular thin films and measured the memory effect for them. Spin-glass-like phase has been observed at low temperatures. We found that, after annealing, the size of the clusters increased significantly. Based on a simple model, the dipole-dipole interaction between the clusters must be increased accordingly for the annealed samples. Interestingly, the memory effect is greatly weakened in the annealed films, which strongly suggested that the dipole-dipole interaction may not be the major factor for the formation of the low-temperature spin-glass-like phase. Copyright © 2012 American Scientific Publishers All rights reserved.

Si-O-Si bond-angle distribution in vitreous silica from first-principles 29Si NMR analysis

International Nuclear Information System (INIS)

Mauri, Francesco; Pasquarello, Alfredo; Pfrommer, Bernd G.; Yoon, Young-Gui; Louie, Steven G.

2000-01-01

The correlation between 29 Si chemical shifts and Si-O-Si bond angles in SiO 2 is determined within density-functional theory for the full range of angles present in vitreous silica. This relation closely reproduces measured shifts of crystalline polymorphs. The knowledge of the correlation allows us to reliably extract from the experimental NMR spectrum the mean (151 degree sign ) and the standard deviation (11 degree sign ) of the Si-O-Si angular distribution of vitreous silica. In particular, we show that the Mozzi-Warren Si-O-Si angular distribution is not consistent with the NMR data. This analysis illustrates the potential of our approach for structural determinations of silicate glasses. (c) 2000 The American Physical Society

Comprehensive study of electronic polarizability and band gap of B2O3–Bi2O3–ZnO–SiO2 glass network

Directory of Open Access Journals (Sweden)

Iskandar Shahrim Mustafa

2017-10-01

Full Text Available Quaternary glasses were successfully fabricated using melt quenching technique based on the chemical compound composition (xBi2O3–(0.5−x ZnO–(0.2B2O3–(0.3SiO2, where (x=0.1, 0.2, 0.3, 0.4, 0.45 mole. The sources of SiO2 was produced from rice husk ash (RHA at 99.36% of SiO2. The Urbach energy was increased from 0.16eV to the 0.29eV as the mole of Bi2O3 increased in the glass structure. The indirect energy band gap is indicated in decrement pattern with 3.15eV towards 2.51eV. The results of Urbach energy and band gap energy that were obtained are due to the increment of Bi3+ ion in the glass network. The refractive indexes for the prepared glasses were evaluated at 2.36 to 2.54 based on the Lorentz–Lorentz formulation which correlated to the energy band gap. The calculated of molar polarizability, electronic polarizability and optical basicity exemplify fine complement to the Bi2O3 addition in the glass network. The glass sample was indicated in amorphous state.

Bonding Characteristics and Chemical Inertness of Zr–Si–N Coatings with a High Si Content in Glass Molding

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Li-Chun Chang

2018-05-01

Full Text Available High-Si-content transition metal nitride coatings, which exhibited an X-ray amorphous phase, were proposed as protective coatings on glass molding dies. In a previous study, the Zr–Si–N coatings with Si contents of 24–30 at.% exhibited the hardness of Si3N4, which was higher than those of the middle-Si-content (19 at.% coatings. In this study, the bonding characteristics of the constituent elements of Zr–Si–N coatings were evaluated through X-ray photoelectron spectroscopy. Results indicated that the Zr 3d5/2 levels were 179.14–180.22 and 180.75–181.61 eV for the Zr–N bonds in ZrN and Zr3N4 compounds, respectively. Moreover, the percentage of Zr–N bond in the Zr3N4 compound increased with increasing Si content in the Zr–Si–N coatings. The Zr–N bond of Zr3N4 dominated when the Si content was >24 at.%. Therefore, high Si content can stabilize the Zr–N compound in the M3N4 bonding structure. Furthermore, the thermal stability and chemical inertness of Zr–Si–N coatings were evaluated by conducting thermal cycle annealing at 270 °C and 600 °C in a 15-ppm O2–N2 atmosphere. The results indicated that a Zr22Si29N49/Ti/WC assembly was suitable as a protective coating against SiO2–B2O3–BaO-based glass for 450 thermal cycles.

Effect of TiO2 addition on reaction between SiC and Ni in SiC-Ni cermet spray coatings. Part 2. ; Development of SiC-based cermet spray coatings. SiC-Ni yosha himakuchu no SiC-Ni kaimen hanno ni oyobosu TiO2 tenka no koka. 2. ; SiC-ki sametto yosha himaku no kaihatsu

Energy Technology Data Exchange (ETDEWEB)

Nakamura, T [Kumano Technical College, Mie (Japan); Oki, S; Goda, S [Kinki Univ., Higashi-Osaka, Osaka (Japan). Faculty of Science and Technology

1992-09-30

The depression of the reaction between SiC and Ni, by adding TiO2 powder in spraying powder which has caused uniform dispersion in spray coating and reduction of TiO2 by the reaction during spraying, was studied. The mass ratio of the mixed components has been, SiC:Ni:TiO2=3:2:1. The spray coating was examined by electron prove microanalysis as well as X-ray diffractometry, centering mainly to the SiC-metal interface reaction. The formation of Ni-Si compounds have been depressed by the addition of TiO2 to spraying powder and by using plasma gas containing H2. Reason for this has been that the TiC formed in the SiC-Ni interface has depressed the reaction at the SiC-Ni interface. Further, TiO2 is reduced during spraying, and TiC is thought to be formed by the reaction between Ti and SiC or reaction between TiO2 and SiC. 8 refs., 6 figs., 1 tab.

Spectroscopic features of Ni(2+) ion in PbO-Bi2O3-SiO2 glass system.

Science.gov (United States)

Suresh, B; Srinivasa Reddy, M; Siva Sesha Reddy, A; Gandhi, Y; Ravi Kumar, V; Veeraiah, N

2015-04-15

Glasses of the composition (30-x)PbO-5Bi2O3-65SiO2: xNiO (with x ranging from 0 to 1.0 mol%) were synthesized. A variety of spectroscopic studies, viz., IR, Raman optical absorption and luminescence properties of these glasses have been carried out as a function of NiO concentration. The analysis of results of all these studies has indicated that the nickel ions occupy both octahedral and tetrahedral positions. However, with the increase of NiO concentration the octahedral occupancy of Ni(2+) ions prevailed over the tetrahedral ions. The luminescence spectra of these glasses have exhibited a broad NIR emission band in region 1100-1500 nm. This band is identified as being due to (3)T2(3F)→(3)A2(3F) octahedral transition of Ni(2+) ions. The luminescence efficiency and cross section have been found to be the highest for the glass containing the highest concentration of NiO. The reasons for such high luminescence efficiency have been discussed in the light of structural variations taking place in the host glass network. Copyright © 2015 Elsevier B.V. All rights reserved.

Crystallization Kinetics of Barium and Strontium Aluminosilicate Glasses of Feldspar Composition

Science.gov (United States)

Hyatt, Mark J.; Bansal, Narottam P.

1994-01-01

Crystallization kinetics of BaO.Al2O3.2SiO2 (BAS) and SrO.Al2O3.2SiO2 (SAS) glasses in bulk and powder forms have been studied by non-isothermal differential scanning calorimetry (DSC). The crystal growth activation energies were evaluated to be 473 and 451 kJ/mol for bulk samples and 560 and 534 kJ/mol for powder specimens in BAS and SAS glasses, respectively. Development of crystalline phases on thermal treatments of glasses at various temperatures has been followed by powder x-ray diffraction. Powder samples crystallized at lower temperatures than the bulk and the crystallization temperature was lower for SAS glass than BAS. Crystallization in both glasses appeared to be surface nucleated. The high temperature phase hexacelsian, MAl2Si2O8 (M = Ba or Sr), crystallized first by nucleating preferentially on the glass surface. Also, monoclinic celsian does not nucleate directly in the glass, but is formed at higher temperatures from the transformation of the metastable hexagonal phase. In SAS the transformation to monoclinic celsian occurred rapidly after 1 h at 1100 C. In contrast, in BAS this transformation is sluggish and difficult and did not go to completion even after 10 h heat treatment at 1400 C. The crystal growth morphologies in the glasses have been observed by optical microscopy. Some of the physical properties of the two glasses are also reported.

Structure of high alumina content Al2O3-SiO2 composition glasses.

Science.gov (United States)

Weber, Richard; Sen, Sabyasachi; Youngman, Randall E; Hart, Robert T; Benmore, Chris J

2008-12-25

The structure of binary aluminosilicate glasses containing 60-67 mol % Al2O3 were investigated using high-resolution 27Al NMR and X-ray and neutron diffraction. The glasses were made by aerodynamic levitation of molten oxides. The 67% alumina composition required a cooling rate of approximately 1600 degrees C s(1-) to form glass from submillimeter sized samples. NMR results show that the glasses contain aluminum in 4-, 5-, and 6-fold coordination in the approximate ratio 4:5:1. The average Al coordination increases from 4.57 to 4.73 as the fraction of octahedral Al increases with alumina content. The diffraction results on the 67% composition are consistent with a disordered Al framework with Al ions in a range of coordination environments that are substantially different from those found in the equilibrium crystalline phases. Analysis of the neutron and X-ray structure factors yields an average bond angle of 125 +/- 4 degrees between an Al ion and the adjoining cation via a bridging oxygen. We propose that the structure of the glass is a "transition state" between the alumina-rich liquid and the equilibrium mullite phase that are dominated by 4- and 6-coordinated aluminum ions, respectively.

Studies on Bi-Sr-Ca-Cu-O glasses and superconducting glass ceramics

International Nuclear Information System (INIS)

Singh, R.; Zacharias, E.

1991-01-01

Bi-Sr-Ca-Cu-O glasses and glass ceramics of various compositions were synthesised. The glass transition temperature varies from 396 to 422degC depending on the glass composition. The bulk glass ceramics of 4334, 4336, 2223 and 4246 compositions show superconductivity when the corresponding glass samples were heat-treated in air at 820degC for 3, 9, 12 and 24 h respectively. X-ray diffraction studies show that the superconducting phase present in all these compositions is Bi 2 Sr 2 Ca 1 Cu 2 O x . The 4334 glass ceramic is almost a single-phase material with a preferred orientation such that the c axis is normal to the sample surface. The 2223 glass ceramic has a higher T c (onset) than the other three compositions indicating the presence of high T c phase (110 K) also. ESR studies on the glass samples indicate the existence of Cu 2+ . The effect of heat treatment on ESR shows that the intensity of resonance decreases with increase in heat-treatment duration. This effect is more pronounced for the 4334 and 2223 compositions. The advantages of synthesizing superconducting materials by glass route are discussed in view of practical applications. (author). 9 refs., 6 figs

Influence of fluoride additions on biological and mechanical properties of Na2O-CaO-SiO2-P2O5 glass-ceramics.

Science.gov (United States)

Li, H C; Wang, D G; Hu, J H; Chen, C Z

2014-02-01

Two series of Na2O-CaO-SiO2-P2O5 glass-ceramics doped with NH4HF2 (G-NH4HF2) or CaF2 (G-CaF2) have been prepared by sol-gel method. The glass-ceramic phase composition and morphology were characterized by X-ray diffraction (XRD) and scanning electron microscopy coupled with energy dispersive spectroscopy (SEM-EDS). The mechanical properties and thermal expansion coefficient were measured by a microhardness tester, an electronic tensile machine and a thermal expansion coefficient tester. The structure difference between these two glass-ceramics was investigated by Fourier transform infrared spectroscopy (FTIR), and the in vitro bioactivity of the glass-ceramics was determined by in vitro simulated body fluid (SBF) immersion test. The hemolysis test, in vitro cytotoxicity test, systemic toxicity test and the implanted experiment in animals were used to evaluate the biocompatibility of the glass-ceramics. The mechanical properties of sample G-NH4HF2 are lower than that of sample G-CaF2, and the bioactivity of sample G-NH4HF2 is better than that of sample G-CaF2. The thermal expansion coefficients of these two glass-ceramics are all closer to that of Ti6Al4V. After 7 days of SBF immersion, apatites were induced on glass-ceramic surface, indicating that the glass-ceramics have bioactivity. The hemolysis test, in vitro cytotoxicity test and systemic toxicity test demonstrate that the glass-ceramics do not cause hemolysis reaction, and have no toxicity to cell and living animal. The implanted experiment in animals shows that bone tissue can form a good osseointegration with the implant after implantation for two months, indicating that the glass-ceramics are safe to serve as implants. Copyright © 2013 Elsevier B.V. All rights reserved.

Q(n) species distribution in K2O.2SiO2 glass by 29Si magic angle flipping NMR.

Science.gov (United States)

Davis, Michael C; Kaseman, Derrick C; Parvani, Sahar M; Sanders, Kevin J; Grandinetti, Philip J; Massiot, Dominique; Florian, Pierre

2010-05-06

Two-dimensional magic angle flipping (MAF) was employed to measure the Q((n)) distribution in a (29)Si-enriched potassium disilicate glass (K(2)O.2SiO(2)). Relative concentrations of [Q((4))] = 7.2 +/- 0.3%, [Q((3))] = 82.9 +/- 0.1%, and [Q((2))] = 9.8 +/- 0.6% were obtained. Using the thermodynamic model for Q((n)) species disproportionation, these relative concentrations yield an equilibrium constant k(3) = 0.0103 +/- 0.0008, indicating, as expected, that the Q((n)) species distribution is close to binary in the potassium disilicate glass. A Gaussian distribution of isotropic chemical shifts was observed for each Q((n)) species with mean values of -82.74 +/- 0.03, -91.32 +/- 0.01, and -101.67 +/- 0.02 ppm and standard deviations of 3.27 +/- 0.03, 4.19 +/- 0.01, and 5.09 +/- 0.03 ppm for Q((2)), Q((3)), and Q((4)), respectively. Additionally, nuclear shielding anisotropy values of zeta =-85.0 +/- 1.3 ppm, eta = 0.48 +/- 0.02 for Q((2)) and zeta = -74.9 +/- 0.2 ppm, eta = 0.03 +/- 0.01 for Q((3)) were observed in the potassium disilicate glass.

Chemical compatibility issues associated with use of SiC/SiC in advanced reactor concepts

Energy Technology Data Exchange (ETDEWEB)

Wilson, Dane F. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

2015-09-01

Silicon carbide/silicon carbide (SiC/SiC) composites are of interest for components that will experience high radiation fields in the High Temperature Gas Cooled Reactor (HTGR), the Very High Temperature Reactor (VHTR), the Sodium Fast Reactor (SFR), or the Fluoride-cooled High-temperature Reactor (FHR). In all of the reactor systems considered, reactions of SiC/SiC composites with the constituents of the coolant determine suitability of materials of construction. The material of interest is nuclear grade SiC/SiC composites, which consist of a SiC matrix [high-purity, chemical vapor deposition (CVD) SiC or liquid phase-sintered SiC that is crystalline beta-phase SiC containing small amounts of alumina-yttria impurity], a pyrolytic carbon interphase, and somewhat impure yet crystalline beta-phase SiC fibers. The interphase and fiber components may or may not be exposed, at least initially, to the reactor coolant. The chemical compatibility of SiC/SiC composites in the three reactor environments is highly dependent on thermodynamic stability with the pure coolant, and on reactions with impurities present in the environment including any ingress of oxygen and moisture. In general, there is a dearth of information on the performance of SiC in these environments. While there is little to no excess Si present in the new SiC/SiC composites, the reaction of Si with O₂ cannot be ignored, especially for the FHR, in which environment the product, SiO₂, can be readily removed by the fluoride salt. In all systems, reaction of the carbon interphase layer with oxygen is possible especially under abnormal conditions such as loss of coolant (resulting in increased temperature), and air and/ or steam ingress. A global outline of an approach to resolving SiC/SiC chemical compatibility concerns with the environments of the three reactors is presented along with ideas to quickly determine the baseline compatibility performance of SiC/SiC.

Evolution of 3C-SiC islands nucleated from a liquid phase on Si face α-SiC substrates

International Nuclear Information System (INIS)

Kim-Hak, Olivier; Ferro, Gabriel; Lorenzzi, Jean; Carole, Davy; Dazord, Jacques; Chaudouet, Patrick; Chaussende, Didier; Miele, Philippe

2010-01-01

The contact between α-SiC crystals and Si-Ge based melts provokes the nucleation of 3C-SiC islands on the crystal surface. Evolution of these islands as a function of various parameters was studied. On both 4H and 6H substrates, it was found that, after nucleation, 3C-SiC islands first enlarge and may form a complete 3C layer under certain conditions. The 3C deposit can then be dissolved by the liquid phase at high temperature or for prolonged contact at relatively moderate temperature. The graphite crucible is proposed to play a central role in these enlargement and dissolution mechanisms by providing extra carbon atoms on the seed surface (enlargement) or provoking thermal induced carbon transport toward the sidewall (dissolution). Several differences between the use of 4H and 6H substrates were also observed.

Scratch resistance of SiO2 and SiO2 - ZrO2 sol-gel coatings on glass-ceramic obtained by sintering

International Nuclear Information System (INIS)

Soares, V. O.; Soares, P.; Peitl, O.; Zanotto, E. D.; Duran, A.; Castro, Y.

2013-01-01

The sol-gel process is widely used to obtain coatings on glass-ceramic substrates in order to improve the scratch and abrasion resistance, also providing a bright and homogeneous appearance of a glaze avoiding expensive final polishing treatments. This paper describes the preparation of silica and silica / zirconia coatings by sol-gel method on Li 2 O-Al 2 O3-SiO 2 (LAS) glassceramic substrates produced by sintering. The coatings were deposited by dip-coating on LAS substrates and characterized by optical microscopy and spectral ellipsometry. On the other hand, hardness and elastic modulus, coefficient of friction and abrasion and scratch resistance of the coatings were determined and compared with the substrate properties. Coatings deposited on LAS glass-ceramic confere the substrate a bright and homogeneous aspect, similar to a glaze, improving the appearance and avoiding the final polishing. However these coatings do not increase the scratch resistance of the substrate only equaling the properties of the glass-ceramic. (Author)

Radiopaque Strontium Fluoroapatite Glass-Ceramics.

Science.gov (United States)

Höland, Wolfram; Schweiger, Marcel; Dittmer, Marc; Ritzberger, Christian

2015-01-01

The controlled precipitation of strontium fluoroapatite crystals was studied in four base glass compositions derived from the SiO2-Al2O3-Y2O3-SrO-Na2O-K2O/Rb2O/Cs2O-P2O5-F system. The crystal phase formation of these glasses and the main properties of the glass-ceramics, such as thermal and optical properties and radiopacity were compared with a fifth, a reference glass-ceramic. The reference glass-ceramic was characterized as Ca-fluoroapatite glass-ceramic. The four strontium fluoroapatite glass-ceramics showed the following crystal phases: (a) Sr5(PO4)3F - leucite, KAlSi2O6, (b) Sr5(PO4)3F - leucite, KAlSi2O6, and nano-sized NaSrPO4, (c) Sr5(PO4)3F - pollucite, CsAlSi2O6, and nano-sized NaSrPO4, and (d) Sr5(PO4)3F - Rb-leucite, RbAlSi2O6, and nano-sized NaSrPO4. The proof of crystal phase formation was possible by X-ray diffraction. The microstructures, which were studied using scanning electron microscopy, demonstrated a uniform distribution of the crystals in the glass matrix. The Sr-fluoroapatites were precipitated based on an internal crystallization process, and the crystals demonstrated a needle-like morphology. The study of the crystal growth of needle-like Sr-fluoroapatites gave a clear evidence of an Ostwald ripening mechanism. The formation of leucite, pollucite, and Rb-leucite was based on a surface crystallization mechanism. Therefore, a twofold crystallization mechanism was successfully applied to develop these types of glass-ceramics. The main focus of this study was the controlled development of glass-ceramics exhibiting high radiopacity in comparison to the reference glass-ceramic. This goal could be achieved with all four glass-ceramics with the preferred development of the Sr-fluoroapatite - pollucite-type glass-ceramic. In addition to this main development, it was possible to control the thermal properties. Especially the Rb-leucite containing glass-ceramic showed the highest coefficient of thermal expansion (CTE). These

Radiopaque strontium fluoroapatite glass-ceramics

Directory of Open Access Journals (Sweden)

Wolfram eHöland

2015-10-01

Full Text Available The controlled precipitation of strontium fluoroapatite crystals, was studied in four base glass compositions derived from the SiO2 – Al2O3 – Y2O3 – SrO – Na2O – K2O/Rb2O/Cs2O – P2O5 – F system. The crystal phase formation of these glasses and the main properties of the glass-ceramics, such as thermal and optical properties and radiopacity were compared with a fifth, a reference glass-ceramic. The reference glass-ceramic was characterized as Ca-fluoroapatite glass-ceramic. The four strontium fluoroapatite glass-ceramics showed the following crystal phases: a Sr5(PO43F – leucite, KAlSi2O6 , b Sr5(PO43F – leucite, KAlSi2O6, and nano-sized NaSrPO4 c Sr5(PO43F – pollucite, CsAlSiO4 , and nano-sized NaSrPO4, d Sr5(PO43F – Rb-leucite, RbAlSi2O6, and nano-sized NaSrPO4.The proof of crystal phase formation was possible by X-ray diffraction (XRD. The microstructures, which were studied using scanning electron microscopy (SEM demonstrated a uniform distribution of the crystals in the glass matrix. The Sr-fluoroapatites were precipitated based on an internal crystallization process, and the crystals demonstrated a needlelike morphology. The study of the crystal growth of needlelike Sr-fluoroapatites gave a clear evidence of an Ostwald ripening mechanism.The formation of leucite, pollucite and Rb-leucite was based on a surface crystallization mechanism. Therefore, a twofold crystallization mechanism was successfully applied to develop these types of glass-ceramics. The main focus of this study was the controlled development of glass-ceramics exhibiting high radiopacity in comparison to the reference glass-ceramic. This goal could be achieved with all four glass-ceramics with the preferred development of the Sr-fluoroapatite – pollucite-type glass-ceramic. In addition to this main development, it was possible to control the thermal properties. Especially the Rb-leucite containing glass-ceramic showed the highest coefficient of thermal

The hydrophobic and omnidirectional antireflection coating of SiO2 nanospheres with C18-TEOS

Science.gov (United States)

Hsu, Cheng-Chih; Lan, Wen-Lin; Chen, Nien-Po; Wu, Chyan-Chyi

2014-06-01

This paper demonstrates the antireflection coating of SiO2 nanospheres applied to cover glass by using the optimal spin-coating method. Because of the hydrolysis and condensation reactions between the SiO2 nanosphere antireflection (AR) coating and n-octadecyltriethoxysilane solution (C18-TEOS), the contact angle of the AR coating with hydrophobic treatment is improved approximately 38%, and the moisture-resistance remains unchanged, which preserved similar transmittance for six weeks. Furthermore, the AR coating with hydrophobic treatment exhibits approximately 3% and 7% improvement in the transmittance at normal and oblique incidence, respectively. The hydrophobic and omnidirectional AR coating with nanoscale SiO2 particles can be fabricated using the proposed simple and economical method.

The Effect of Dispersion Phases of SiC and Al2O3 on the Properties of Galvanic Nickel Coatings

OpenAIRE

Kozik A.; Nowak M.; Gawlik M.; Bigaj M.; Karaś M.

2016-01-01

In this study, Ni, Ni-SiC and Ni-Al2O3 coatings were electroplated on the 2xxx series aluminium alloy. The following parameters of the electroplating process were applied: current density - 4A/dm2, time - 60 minutes, and temperature - 60°C. Hard particles of submicrometric size were used. The results of the research showing the effect of the addition of hard particles (introduced into the nickel bath as a dispersed phase) on the properties of coatings, including the effect of the type (SiC or...

Influence of Y2O3 Addition on Crystallization, Thermal, Mechanical, and Electrical Properties of BaO-Al2O3-B2O3-SiO2 Glass-Ceramic for Ceramic Ball Grid Array Package

Science.gov (United States)

Li, Bo; Li, Wei; Zheng, Jingguo

2018-01-01

Y2O3 addition has a significant influence on the crystallization, thermal, mechanical, and electrical properties of BaO -Al2O3 -B2O3 -SiO2 (BABS) glass-ceramics. Semi-quantitative calculation based on x-ray diffraction demonstrated that with increasing Y2O3 content, both the crystallinity and the phase content of cristobalite gradually decreased. It is effective for the additive Y2O3 to inhibit the formation of cristobalite phase with a large coefficient of thermal expansion value. The flexural strength and the Young's modulus, thus, are remarkably increased from 140 MPa to 200 MPa and 56.5 GPa to 63.7 GPa, respectively. Also, the sintering kinetics of BABS glass-ceramics with various Y2O3 were investigated using the isothermal sintering shrinkage curve at different sintering temperatures. The sintering activation energy Q sharply decreased from 99.8 kJ/mol to 81.5 kJ/mol when 0.2% Y2O3 was added, which indicated that a small amount of Y2O3 could effectively promote the sintering procedure of BABS glass-ceramics.

Nanocomposite dielectrics in PbO-BaO-Na2O-Nb2O5-SiO2 system with high breakdown strength for high voltage capacitor applications.

Science.gov (United States)

Zhang, Qingmeng; Luo, Jun; Tang, Qun; Han, Dongfang; Zhou, Yi; Du, Jun

2012-11-01

Nanocomposite dielectrics in 6PbO-4BaO-20Na2O-40Nb2O5-30SiO2 system were prepared via melt-quenching followed by controlled crystallization. X-ray diffraction studies reveal that Pb2Nb2O7, Ba,NaNb5O15, NaNbO3 and PbNb2O6 phases are formed from the as-quenched glass annealed in temperature range from 700 degrees C to 850 degrees C. Ba2NaNb5O15, Pb2Nb2O7 crystallizes at 700 degrees C and then Pb2Nb2O7 disappears at 850 degrees C, while PbNb2O6 and NaNbO3 are formed at 850 degrees C. Microstructural observation shows that the crystallized particles are nanometer-sized and randomly distributed with glass matrix being often found at grain boundaries. The dielectric constant of the nanocomposites formed at different crystallization temperatures shows good frequency and electric field stability. The breakdown strength is slightly decreased when the glass-ceramics thickness is varied from 1 mm to 4 mm. The corresponding energy density could reach 2.96 J/cm3 with a breakdown strength of 58 kV/mm for thickness of 1 mm.

Optical Properties of Malachite Green Dye Doped SiO2 Glasses: Effect of Transition Metal (Fe-I Used as a Codopant

Directory of Open Access Journals (Sweden)

Dulen Bora

2014-01-01

Full Text Available Enhanced luminescence properties of Malachite Green (MG (oxalate in Fe-MG codoped SiO2 glasses compared to its values in MG doped SiO2 glasses are reported here. The enhancement is chiefly attributed to a resonance nonradiative energy transfer between Fe and MG. The quantum yield of Malachite Green (MG, in presence of Iron, trapped in sol-gel derived SiO2 glass increases by an order of ~103 compared to that in low viscous solvent while a lifetime of 3.29 ns is reported.

Self-sealing multilayer coating for SiC/SiC composites

International Nuclear Information System (INIS)

Ferraris, M.; Appendino Montorsi, M.; Salvo, M.; Isola, C.; Kohyama, A.

1997-01-01

A double layer coating for SiC/SiC for fusion applications is proposed: the first layer consists in a homogeneous, crack free, glass-ceramic with high characteristic temperatures and thermal expansion coefficient compatible to the composite one; the second layer is amorphous and shows self-sealing properties above 700degC. The glass and the glass-ceramic materials used for this double layer coating do not contain lithium and boron oxide, making them particularly interesting for thermonuclear fusion applications. The self-sealing property of the double layer coating was valued by inducing cracks on the coatings and observing their reparation after heating. (author)

Effect of Ti concentration on the structure and texture of SiTiOC glasses

International Nuclear Information System (INIS)

Tellez, L.; Rubio, J.; Valenzuela, M.A.; Rubio, F.; Oteo, J.L.

2009-01-01

Five different silicon-titanium organic-inorganic hybrid materials were prepared by the reaction of tetraethoxysilane, titanium tetrabutoxide and silanol-terminated polydimethylsiloxane. Si-Ti oxycarbide glasses were prepared by pyrolysis of the hybrid materials in nitrogen atmosphere in the range of 400 to 1500 deg. C. The obtained Si-Ti oxycarbide materials were characterized by Fourier Transform-Infra Red spectroscopy, X-ray-diffraction, mercury porosimetry and SEM. The study indicated that the reactivity towards water increases up to 1000 deg. C, at higher temperatures it decreases for all samples. During the pyrolysis, Ti atoms were incorporated into the silicate network leading to the formation of Si-Ti oxycarbide glasses, except with sample containing 7% of Ti which presented also the formation of β-SiC and TiC crystalline phases. The porosity was increased up to 600 deg. C and then decreased tending to disappear at 1500 deg. C. When the titanium concentration increased from 1 to 3% in the oxycarbide glass, the porosity decreased; for higher concentration, an increase in the porosity was observed.

Effect of Ti concentration on the structure and texture of SiTiOC glasses

Energy Technology Data Exchange (ETDEWEB)

Tellez, L. [Dpt. Ing. Metalurgica. ESIQIE-Instituto Politecnico Nacional. Zacatenco, 07738 Mexico D.F. (Mexico); Rubio, J. [Instituto de Ceramica y Vidrio. C.S.I.C. Campus de la Universidad Autonoma de Madrid, Canto Blanco 28049, Madrid (Spain); Valenzuela, M.A., E-mail: mavalenz@ipn.mx [Lab. Catalisis y Materiales, ESIQIE-Instituto Politecnico Nacional. Zacatenco, 07738 Mexico D.F. (Mexico); Rubio, F.; Oteo, J.L. [Instituto de Ceramica y Vidrio. C.S.I.C. Campus de la Universidad Autonoma de Madrid, Canto Blanco 28049, Madrid (Spain)

2009-06-15

Five different silicon-titanium organic-inorganic hybrid materials were prepared by the reaction of tetraethoxysilane, titanium tetrabutoxide and silanol-terminated polydimethylsiloxane. Si-Ti oxycarbide glasses were prepared by pyrolysis of the hybrid materials in nitrogen atmosphere in the range of 400 to 1500 deg. C. The obtained Si-Ti oxycarbide materials were characterized by Fourier Transform-Infra Red spectroscopy, X-ray-diffraction, mercury porosimetry and SEM. The study indicated that the reactivity towards water increases up to 1000 deg. C, at higher temperatures it decreases for all samples. During the pyrolysis, Ti atoms were incorporated into the silicate network leading to the formation of Si-Ti oxycarbide glasses, except with sample containing 7% of Ti which presented also the formation of {beta}-SiC and TiC crystalline phases. The porosity was increased up to 600 deg. C and then decreased tending to disappear at 1500 deg. C. When the titanium concentration increased from 1 to 3% in the oxycarbide glass, the porosity decreased; for higher concentration, an increase in the porosity was observed.

Structural and magnetic properties of SiO{sub 2}-CaO-Na{sub 2}O-P{sub 2}O{sub 5} containing BaO-Fe{sub 2}O{sub 3} glass-ceramics

Energy Technology Data Exchange (ETDEWEB)

Leenakul, W.; Kantha, P.; Pisitpipathsin, N. [Department of Physics and Materials Science, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Rujijanagul, G.; Eitssayeam, S. [Department of Physics and Materials Science, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Materials Science Research Center, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Pengpat, K., E-mail: kamonpan.p@cmu.ac.th [Department of Physics and Materials Science, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Materials Science Research Center, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand)

2013-01-15

The incorporation method was employed to produce bioactive glass-ceramics from the BaFe{sub 12}O{sub 19}-SiO{sub 2}-CaO-Na{sub 2}O-P{sub 2}O{sub 5} glass system. The ferrimagnetic BaFe{sub 12}O{sub 19} was first prepared using a simple mixed oxide method, where the oxide precursors of 45S5 bioglass were initially mixed and then melted to form glass. The devitrification of Na{sub 3}Ca{sub 6}(PO{sub 4}){sub 5} and Fe{sub 3}O{sub 4} was observed in all of the quenched glass samples. The glass samples were then subjected to a heat treatment schedule for further crystallization. It was found that the small traces of BaFe{sub 12}O{sub 19} phases started to crystallize in high BF content samples of 20 and 40 wt%. These samples also exhibited good magnetic properties comparable to that of other magnetic glass-ceramics. The bioactivity of the BF glass-ceramics improved with increasing BF content as was evident by the formation of bone-like apatite layers on the surface of all of the glass-ceramics after soaking in SBF for 14 days. The results support the use of these bioactive glass-ceramics for hyperthermia treatment within the human body. - Highlights: Black-Right-Pointing-Pointer BF addition improves the magnetic property and bioactivity of 45S5 bioglasses. Black-Right-Pointing-Pointer Bioglass-ceramics exhibited soft magnetic properties with Mr=14.850 emu/g. Black-Right-Pointing-Pointer Magnetic property can be enhanced by crystallization of BF in 45S5 bioglasses.

Broadband infrared luminescence from Li2O-Al2O3-ZnO-SiO2 glasses doped with Bi2O3.

Science.gov (United States)

Peng, Mingying; Qiu, Jianrong; Chen, Danping; Meng, Xiangeng; Zhu, Congshan

2005-09-05

The broadband emission in the 1.2~1.6mum region from Li2O-Al2O3-ZnO-SiO2 ( LAZS ) glass codoped with 0.01mol.%Cr2O3 and 1.0mol.%Bi2O3 when pumped by the 808nm laser at room temperature is not initiated from Cr4+ ions, but from bismuth, which is remarkably different from the results reported by Batchelor et al. The broad ~1300nm emission from Bi2O3-containing LAZS glasses possesses a FWHM ( Full Width at Half Maximum ) more than 250nm and a fluorescent lifetime longer than 500mus when excited by the 808nm laser. These glasses might have the potential applications in the broadly tunable lasers and the broadband fiber amplifiers.

Pd/CeO2/SiC Chemical Sensors

Science.gov (United States)

Lu, Weijie; Collins, W. Eugene

2005-01-01

The incorporation of nanostructured interfacial layers of CeO2 has been proposed to enhance the performances of Pd/SiC Schottky diodes used to sense hydrogen and hydrocarbons at high temperatures. If successful, this development could prove beneficial in numerous applications in which there are requirements to sense hydrogen and hydrocarbons at high temperatures: examples include monitoring of exhaust gases from engines and detecting fires. Sensitivity and thermal stability are major considerations affecting the development of high-temperature chemical sensors. In the case of a metal/SiC Schottky diode for a number of metals, the SiC becomes more chemically active in the presence of the thin metal film on the SiC surface at high temperature. This increase in chemical reactivity causes changes in chemical composition and structure of the metal/SiC interface. The practical effect of the changes is to alter the electronic and other properties of the device in such a manner as to degrade its performance as a chemical sensor. To delay or prevent these changes, it is necessary to limit operation to a temperature sensor structures. The present proposal to incorporate interfacial CeO2 films is based partly on the observation that nanostructured materials in general have potentially useful electrical properties, including an ability to enhance the transfer of electrons. In particular, nanostructured CeO2, that is CeO2 with nanosized grains, has shown promise for incorporation into hightemperature electronic devices. Nanostructured CeO2 films can be formed on SiC and have been shown to exhibit high thermal stability on SiC, characterized by the ability to withstand temperatures somewhat greater than 700 C for limited times. The exchanges of oxygen between CeO2 and SiC prevent the formation of carbon and other chemical species that are unfavorable for operation of a SiC-based Schottky diode as a chemical sensor. Consequently, it is anticipated that in a Pd/CeO2/SiC Schottky

Preparação e caracterização de materiais compósitos SiC/caulim/Al via "squeeze-casting" Preparation and characterization of SiC/kaolin/Al composite materials by squeeze- casting

Directory of Open Access Journals (Sweden)

M. Freitas

2009-09-01

Full Text Available Na busca de materiais com propriedades diferenciadas, vem aumentando nos últimos anos as pesquisas em materiais compósitos. Um dos importantes métodos de fabricação destes compósitos é o processo de infiltração sob pressão de metal fundido denominado "squeeze-casting". Este processo oferece algumas vantagens, tais como facilidade de produzir o compósito, baixo custo e capacidade de formação de estruturas em rede. Neste trabalho foram produzidos e caracterizados compósitos SiC-Al, com concentrações em caulim variando entre 10 e 50% em substituição a fase majoritária SiC. As pré-formas cerâmicas foram produzidas controlando-se a fração granulométrica do SiC/caulim para uma melhor infiltração. Estas pré-formas, após sinterização a 1100 ºC/1 h, resultaram altamente porosas, sendo a porosidade aumentada com o aumento do caulim em substituição ao SiC. Análises de DRX mostraram a existência de partículas de quartzo além da fase SiC como constituintes das pré-formas. Durante o processo de infiltração e tratamento térmico, o alumínio no estado líquido reagiu preferencialmente com o quartzo e outros aluminossilicatos da pré-forma reduzindo-os, precipitando alumina e silício na microestrutura, a qual apresentou também alumínio em excesso que não reagiu no processo. A sílica e os silicatos da pré-forma, ao reagirem preferencialmente com o alumínio, evitaram a reação do Al com o SiC, prevenindo a formação da fase Al4C3,, a qual é altamente higroscópica e causa a degradação do compósito. Dependendo da composição, os compósitos SiC-caulim-Al desenvolvidos neste trabalho, podem ser usados em aplicações que envolvam elevada resistência mecânica à flexão (240 a 300 MPa, baixa densidade e dureza superficial entre 180 e 380 kgf/mm².In search of materials with different properties, has been increasing the research on composite materials in recent years. One of the important methods of

Fluorescence of Pentavalent Chromium in SiO2 Sol-Gel Glasses

Science.gov (United States)

Jia, Weiyi; Castro, Lymari; Wang, Yanyun; Liu, Huimin

1998-01-01

Chromium ions are very attractive to optical spectroscopy and laser physics. It is well known that the first laser in the history is a ruby laser activated with Cr(3+). It was found in early nineties that Cr(4+) was also an interesting lasing ion in the near infrared, and various Cr(4+) lasers have been developed. Very recently, it was reported that Cr(2+) doped in CdSe crystals showed lasing action in the infrared. The above achievement have stimulated an interest in searching for Cr(5+) and investigating its optical properties. Cr(5+) is isoelectronic with Ti(3+) and V(4+), having electron configuration 3d1. Ti(3+) is the active center of commercial cw and femtosecond sapphire lasers, tunable in the range 680-1100 nm. V(4+) doped in YAlO3 and Al2O3 showed broad band emission near 635 nm. Although EPR results of Cr(5+) were reported, the optical properties were less studied. Herren et al. reported an observation of luminescence from Cr doped in SiO2 sol-gel glass. The luminescence spectrum was assigned to pentavalent ions in their first paper, and later it was identified to be the emission from the charge transfer transition of Cr(6+). The first observation of photoluminescence from octahedrally coordinated Cr(5+) in BaCaMg aluminate glasses was reported very recently. In this work, we report luminescence results of Cr doped SiO2 sol-gel glasses. The fluorescence spectra are very different from Herrens' results, and we believe it originates from pentavalent Cr.

High-pressure phase relations and thermodynamic properties of CaAl 4Si 2O 11 CAS phase

Science.gov (United States)

Akaogi, M.; Haraguchi, M.; Yaguchi, M.; Kojitani, H.

2009-03-01

Phase relations in CaAl4Si2O11 were examined at 12-23 GPa and 1000-1800 °C by multianvil experiments. A three-phase mixture of grossular, kyanite and corundum is stable below about 13 GPa at 1000-1800 °C. At higher pressure and at temperature below about 1200 °C, a mixture of grossular, stishovite and corundum is stable, indicating the decomposition of kyanite. Above about 1200 °C, CaAl4Si2O11 CAS phase is stable at pressure higher than about 13 GPa. The triple point is placed at 14.7 GPa and 1280 °C. The equilibrium boundary of formation of CAS phase from the mixture of grossular, kyanite and corundum has a small negative slope, and that from the mixture of grossular, stishovite and corundum has a strongly negative slope, while the decomposition boundary of kyanite has a small positive slope. Enthalpies of the transitions were measured by high-temperature drop-solution calorimetry. The enthalpy of formation of CaAl4Si2O11 CAS phase from the mixture of grossular, kyanite and corundum was 139.5 ± 15.6 kJ/mol, and that from the mixture of grossular, stishovite and corundum was 94.2 ± 15.4 kJ/mol. The transition boundaries calculated using the measured enthalpy data were consistent with those determined by the high-pressure experiments. The boundaries in this study are placed about 3 GPa higher in pressure and about 200 °C lower in temperature than those by Zhai and Ito [Zhai, S., Ito, E., 2008. Phase relations of CaAl4Si2O11 at high-pressure and high-temperature with implications for subducted continental crust into the deep mantle. Phys. Earth Planet. Inter. 167, 161-167]. Combining the thermodynamic data measured in this study with those in the literature, dissociation boundary of CAS phase into a mixture of Ca-perovskite, corundum and stishovite and that of grossular into Ca-perovskite plus corundum were calculated to further constrain the stability field of CAS phase. The result suggests that the stability of CAS phase would be limited at the bottom of

Oxide Structure Dependence of SiO2/SiOx/3C-SiC/n-Type Si Nonvolatile Resistive Memory on Memory Operation Characteristics

Science.gov (United States)

Yamaguchi, Yuichiro; Shouji, Masatsugu; Suda, Yoshiyuki

2012-11-01

We have investigated the dependence of the oxide layer structure of our previously proposed metal/SiO2/SiOx/3C-SiC/n-Si/metal metal-insulator-semiconductor (MIS) resistive memory device on the memory operation characteristics. The current-voltage (I-V) measurement and X-ray photoemission spectroscopy results suggest that SiOx defect states mainly caused by the oxidation of 3C-SiC at temperatures below 1000 °C are related to the hysteresis memory behavior in the I-V curve. By restricting the SiOx interface region, the number of switching cycles and the on/off current ratio are more enhanced. Compared with a memory device formed by one-step or two-step oxidation of 3C-SiC, a memory device formed by one-step oxidation of Si/3C-SiC exhibits a more restrictive SiOx interface with a more definitive SiO2 layer and higher memory performances for both the endurance switching cycle and on/off current ratio.

Microstructure, mechanical and tribological properties of CrSiC coatings sliding against SiC and Al{sub 2}O{sub 3} balls in water

Energy Technology Data Exchange (ETDEWEB)

Wu, Zhiwei [State Key Laboratory of Mechanics and Control of Mechanical Structures, Nanjing University of Aeronautics and Astronautics, Nanjing 210016 (China); College of Mechanical and Electrical Engineering, Nanjing University of Aeronautics and Astronautics and Jiangsu Key Laboratory of Precision and Micro-Manufacturing Technology, Nanjing 210016 (China); College of Mechanical and Electrical Engineering, Nanjing Forestry University, Nanjing 210037 (China); Zhou, Fei, E-mail: fzhou@nuaa.edu.cn [State Key Laboratory of Mechanics and Control of Mechanical Structures, Nanjing University of Aeronautics and Astronautics, Nanjing 210016 (China); College of Mechanical and Electrical Engineering, Nanjing University of Aeronautics and Astronautics and Jiangsu Key Laboratory of Precision and Micro-Manufacturing Technology, Nanjing 210016 (China); Chen, Kangmin [Center of Analysis, Jiangsu University, Zhenjiang 212013 (China); Wang, Qianzhi [Department of Mechanical Engineering, Keio University, Yokohama 2238522 (Japan); Zhou, Zhifeng [Advanced Coatings Applied Research Laboratory, Department of Mechanical and Biomedical Engineering, City University of Hong Kong, 83 Tat Chee Avenue, Kowloon, Hong Kong (China); Yan, Jiwang [Department of Mechanical Engineering, Keio University, Yokohama 2238522 (Japan); Li, Lawrence Kwok-Yan [Advanced Coatings Applied Research Laboratory, Department of Mechanical and Biomedical Engineering, City University of Hong Kong, 83 Tat Chee Avenue, Kowloon, Hong Kong (China)

2016-04-15

Graphical abstract: CrSiC coatings were speculated to be X-ray amorphous (A). Although the hardness of coatings fluctuated slightly (13.2–13.8 GPa), the CrSiC coatings showed poor wear resistance due to the decline of the crack resistance and toughness. Moreover, the friction coefficient (0.24–0.31) and the wear rate (2.97–7.66 × 10{sup −6} mm{sup 3}/Nm) of CrSiC/SiC trobopairs were lower than those of CrSiC/Al{sub 2}O{sub 3} tribopairs (B and C). - Highlights: • CrSiC coatings with Si content of 2.0–7.4 at.% were deposited via adjusting the TMS flow. • The amorphous structure in the CrSiC coatings was presented. • No obvious fluctuations of hardness (about 13 GPa) were observed with TMS flow. • CrSiC/SiC tribopairs showed better tribological performance than CrSiC/Al{sub 2}O{sub 3} tribopairs. - Abstract: CrSiC coatings with different silicon contents were prepared using unbalanced magnetron sputtering via adjusting trimethylsilane (Si(CH{sub 3}){sub 3}H) flows. Their phase structure, bonding structure, microstructure and hardness were characterized by X-ray diffraction (XRD), X-ray photoelectrons spectroscopy (XPS), a field emission scanning electron microscope (FESEM) and nano-indenter, respectively. The tribological properties of CrSiC coatings sliding against SiC and Al{sub 2}O{sub 3} balls were investigated in water. The results showed that the CrSiC coatings were speculated to be X-ray amorphous. Although the hardness of coatings fluctuated slightly (13.2–13.8 GPa), the coatings showed poor wear resistance due to the decline of the crack resistance and toughness. Moreover, the friction coefficient (0.24–0.31) and the wear rate (2.97–7.66 × 10{sup −6} mm{sup 3}/Nm) of CrSiC/SiC trobopairs were lower than those of CrSiC/Al{sub 2}O{sub 3} tribopairs.

Radiopaque Strontium Fluoroapatite Glass-Ceramics

Science.gov (United States)

Höland, Wolfram; Schweiger, Marcel; Dittmer, Marc; Ritzberger, Christian

2015-01-01

The controlled precipitation of strontium fluoroapatite crystals was studied in four base glass compositions derived from the SiO2–Al2O3–Y2O3–SrO–Na2O–K2O/Rb2O/Cs2O–P2O5–F system. The crystal phase formation of these glasses and the main properties of the glass-ceramics, such as thermal and optical properties and radiopacity were compared with a fifth, a reference glass-ceramic. The reference glass-ceramic was characterized as Ca-fluoroapatite glass-ceramic. The four strontium fluoroapatite glass-ceramics showed the following crystal phases: (a) Sr5(PO4)3F – leucite, KAlSi2O6, (b) Sr5(PO4)3F – leucite, KAlSi2O6, and nano-sized NaSrPO4, (c) Sr5(PO4)3F – pollucite, CsAlSi2O6, and nano-sized NaSrPO4, and (d) Sr5(PO4)3F – Rb-leucite, RbAlSi2O6, and nano-sized NaSrPO4. The proof of crystal phase formation was possible by X-ray diffraction. The microstructures, which were studied using scanning electron microscopy, demonstrated a uniform distribution of the crystals in the glass matrix. The Sr-fluoroapatites were precipitated based on an internal crystallization process, and the crystals demonstrated a needle-like morphology. The study of the crystal growth of needle-like Sr-fluoroapatites gave a clear evidence of an Ostwald ripening mechanism. The formation of leucite, pollucite, and Rb-leucite was based on a surface crystallization mechanism. Therefore, a twofold crystallization mechanism was successfully applied to develop these types of glass-ceramics. The main focus of this study was the controlled development of glass-ceramics exhibiting high radiopacity in comparison to the reference glass-ceramic. This goal could be achieved with all four glass-ceramics with the preferred development of the Sr-fluoroapatite – pollucite-type glass-ceramic. In addition to this main development, it was possible to control the thermal properties. Especially the Rb-leucite containing glass-ceramic showed the highest coefficient of thermal

Thermal shock properties of 2D-SiCf/SiC composites

International Nuclear Information System (INIS)

Lee, Sang Pill; Lee, Jin Kyung; Son, In Soo; Bae, Dong Su; Kohyama, Akira

2012-01-01

This paper dealt with the thermal shock properties of SiC f /SiC composites reinforced with two dimensional SiC fabrics. SiC f /SiC composites were fabricated by a liquid phase sintering process, using a commercial nano-size SiC powder and oxide additive materials. An Al 2 O 3 –Y 2 O 3 –SiO 2 powder mixture was used as a sintering additive for the consolidation of SiC matrix region. In this composite system, Tyranno SA SiC fabrics were also utilized as a reinforcing material. The thermal shock test for SiC f /SiC composites was carried out at the elevated temperature. Both mechanical strength and microstructure of SiC f /SiC composites were investigated by means of optical microscopy, SEM and three point bending test. SiC f /SiC composites represented a dense morphology with a porosity of about 8.2% and a flexural strength of about 160 MPs. The characterization of SiC f /SiC composites was greatly affected by the history of cyclic thermal shock. Especially, SiC f /SiC composites represented a reduction of flexural strength at the thermal shock temperature difference higher than 800 °C.

Structure of Na2O·MO·SiO2·CaF2 (M=Mg, Ca) oxyfluoride glasses

International Nuclear Information System (INIS)

Cheng Jinshu; Deng Wei; Wang Mitang

2012-01-01

(9-x)CaO·xMgO·15Na 2 O·60SiO 2 ·16CaF 2 (x=0, 2, 4, 6, and 9) oxyfluoride glasses were prepared. Utilizing the Raman scattering technique together with 29 Si and 19 F MAS NMR, the effect of alkaline metal oxides on the Q species of glass was characterized. Raman results show that as magnesia is added at the expense of calcium oxide, the disproportional reaction Q 3 →Q 4 +Q 2 (Q n is a SiO 4 tetrahedron with n bridging oxygens) prompted due to the high ionic field strength of magnesia, magnesium oxide entered into the silicate network as tetrahedral MgO 4 , and removed other modifying ions for charge compensation. This reaction was confirmed by 29 Si MAS NMR. 19 F MAS NMR results show that fluorine exists in the form of mixed calcium sodium fluoride species in all glasses and no Si-F bonds were formed. As CaO is gradually replaced by MgO (x=6, 9), a proportion of the magnesium ions combines with fluorine to form the MgF + species. Meanwhile, some part of Na + ions complex F - in the form of F-Na(6).

Use of a cobalt-based metallic glass for joining MoSi{sub 2} to stainless steel

Energy Technology Data Exchange (ETDEWEB)

Vaidya, R.U.; Rangaswamy, P.; Misra, A.; Gallegos, D.E.; Castro, R.G.; Petrovic, J.J. [Los Alamos National Lab., NM (United States). Materials Science and Technology Div.; Butt, D.P. [Florida Univ., Gainesville, FL (United States). Dept. of Materials Science and Engineering

2002-07-01

The successful use of a cobalt-based metallic glass in joining molybdenum disilicide (MoSi{sub 2}) to stainless steel 316L was demonstrated. Such joints are being investigated for sensor tube applications in glass melting operations. The cobalt-based metallic-glass (METGLAS{sup TM} 2714A) was found to wet the MoSi{sub 2} and stainless steel surfaces and provide high quality joints. Joining was completed at 1050 C for 60 minutes in two different ways; either by feeding excess braze into the braze gap upon heating or by constraining the MoSi{sub 2}/stainless steel assembly with an alumina (Al{sub 2}O{sub 3}) fixture during the heating cycle. These steps were necessary to ensure the production of a high quality void free joint. Post-brazing metallographic evaluations coupled with quantitative elemental analysis indicated the presence of a Co-Cr-Si ternary phase with CoSi and CoSi{sub 2} precipitates within the braze. The residual stresses in these molybdenum disilicide (MoSi{sub 2})/stainless steel 316 L joints were evaluated using X-ray diffraction and instrumented indentation techniques. These measurements revealed that significant differences are induced in the residual stresses in MoSi{sub 2} and stainless steel depending on the joining technique employed. Push-out tests were carried out on these joints to evaluate the joint strength. (orig.)

Influence of Gd2O3 on thermal and spectroscopic properties of aluminosilicate glasses

Science.gov (United States)

Kasprzyk, Marta; Środa, Marcin