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  • Articles  (22)
  • sintering  (22)
  • Springer  (22)
  • Nature Publishing Group
  • 1995-1999  (22)
  • 1960-1964
  • 1945-1949
  • 1997  (22)
  • Chemistry and Pharmacology  (22)
Collection
  • Articles  (22)
Publisher
  • Springer  (22)
  • Nature Publishing Group
Years
  • 1995-1999  (22)
  • 1960-1964
  • 1945-1949
Year
  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Journal of thermal analysis and calorimetry 49 (1997), S. 1297-1304 
    ISSN: 1572-8943
    Keywords: dilatometry ; rate-controlled-sintering ; RCS ; sintering ; ZnO
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A fast-firing shrinkage rate controlled dilatometer was developed as a tool for optimizing sintering of powder compacts. The instrument described in this work features an infrared imaging radiation furnace and a low thermal mass dilatometer assembly which allowed controlled heating and cooling rates of up to 500°C min−1. Shrinkage control was accomplished using a computer interfaced PID control algorithm. Adjustments were made to hardware and software which reduced specimen creep under dilatometer pushrod load, eliminated non-uniform pushrod expansion, fostered reproducible specimen temperature determination, accounted for thermal expansion during sintering, and generated instantaneous termination of sintering at the specified end of RCS. Tests performed on ZnO samples demonstrated very rapid thermal response and excellent shrinkage control.
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Journal of sol gel science and technology 8 (1997), S. 377-380 
    ISSN: 1573-4846
    Keywords: sol-gel thin film ; sintering ; FTIR
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Solution derived thin films of molar composition 90SiO2-10TiO2 deposited on c-Si substrates, for use as planar waveguides are characterized in terms of thickness and refractive index, by ellipsometry, as a function of isothermal heat treatments. The structural evolution of the films with thermal treatment is followed by infrared spectroscopy. The estimated average Si–O–Si intertetrahedral bond angle increases from 137°, at room temperature, to 144°, after heating at 900°C. The films should be annealed at T 〉 800°C, in order to release the residual stresses.
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Journal of sol gel science and technology 8 (1997), S. 261-268 
    ISSN: 1573-4846
    Keywords: SnO2 xerogel ; sintering ; Eu3+ spectroscopy ; XRD ; EXAFS
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The evolution of Eu3+ doped SnO2 xerogels to the cassiterite structure observed during sintering was studied by means of Eu3+ spectroscopy, XRD and EXAFS at the Sn K-edge. Eu3+ ions adsorbed at the surface of colloidal particles present a broad distribution of sites, typical of oxide glasses. With sintering at 300°C, this distribution is still broadened. Crystallization is clearly observed by the three techniques with increasing sintering temperature. It is found that the addition of Eu3+ limits the crystallite growth.
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  • 4
    Electronic Resource
    Electronic Resource
    Springer
    Journal of sol gel science and technology 8 (1997), S. 353-363 
    ISSN: 1573-4846
    Keywords: sintering ; stress ; constraint ; crystallization ; nucleation ; film ; substrate ; rapid thermal annealing
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The sintering of films differs from that of bulk gels in several ways. The initial state of a film is generally denser and less crosslinked than a bulk gel made from the same sol, and these factors enhance the densification rate of the film. The substrate constrains the shrinkage of the film, leading to high stresses that retard densification and can influence phase changes. The substrate is a site for heterogeneous nucleation, and crystallization makes densification more difficult, so the competition between sintering and crystallization is particularly important for films. Fast heating favors densification over crystallization, so rapid thermal annealing usually produces denser films. The high surface to volume ratio of a thin film makes it susceptible to degradation by reaction with the substrate and the atmosphere, so choosing compatible materials and avoiding over-firing is essential.
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  • 5
    Electronic Resource
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    Springer
    Journal of sol gel science and technology 8 (1997), S. 269-274 
    ISSN: 1573-4846
    Keywords: SnO2 xerogels ; sintering ; EXAFS ; XRD
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The formation of an ordered (crystalline) phase during isothermal sintering of SnO2 monolithic xerogels, at 200, 250, 300, 400, 500, 600 and 700°C, has been analyzed by the combined use of EXAFS and XRD techniques. For the desiccated gel (110°C), EXAFS results show the formation of small microcrystallites with the incipient cassiterite structure. Between 110 and 250°C, the dehydratation reaction leads to an amorphization evidenced by a decrease of the long and short range crystallographic order. It is due to fissure formation in the xerogel network. For higher temperatures, a continuous coagulation of the crystallites occurs, leading to grain growth. Grain and pore growth obeys the same kinetic relation, so that the microstructure grows by simple enlargement while its morphology is static.
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  • 6
    Electronic Resource
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    Springer
    Journal of sol gel science and technology 8 (1997), S. 397-402 
    ISSN: 1573-4846
    Keywords: silica glass ; monolith ; sub-critical drying ; chlorination ; sintering
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Over the last few years, the feasibility of fabricating near net shape silica glass components, using a sub-critical drying process for pure alkoxide gels, has been demonstrated in our laboratories. Cracking during drying, due to capillary forces generated in the gel body, was overcome through two particular innovations. The first was the development and optimization of a dual-catalyzed high strength gel. The second was a controlled atmosphere drying process that allowed the gel to dry utilizing a newly observed phenomenology, postulated to be due to cavitation of the pore fluid. Contrary to conventional wisdom, in this drying approach the smallest pore size gels are the easiest to dry. Details of the types of gels and the drying process are reported. Gels of small size were sintered into crack-free glasses, utilizing conventional sintering approaches. However, large size gels always developed visible surface cracks that formed above 800°C. To successfully dry and sinter large monolithic gels then required re-optimization of the entire process. A great number of micron-range defects were initially detected in these sintered bodies. After analyzing the defects, further steps were taken to improve glass quality to the level of optical glass produced by vapor deposition processes. This included mixing and filtering of sols in a clean room, varying the pore size distribution, and optimizing the pre-sintering and sintering processes. Data of relevant glass quality parameters attained so far in the laboratory are reported.
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  • 7
    Electronic Resource
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    Springer
    Journal of sol gel science and technology 8 (1997), S. 477-481 
    ISSN: 1573-4846
    Keywords: supported membrane ; SnO2 coating ; pore size distribution ; sintering
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract In this work, the effect of the substrate microstructure on the formation of SnO2 membranes and of the sintering conditions on their porosity have been analysed. Samples have been prepared by colloidal suspensions cast on alumina or kaolin substrates. Supported membranes have been characterized by Hg porosimetry, MEV, XRD and N2 adsorption-desorption isotherms. The results show that the narrower pore size distribution of alumina substrate allowed to prepare membranes more homogeneous and free of cracks than that supported on kaolin. The crystallite and pore sizes of the membranes could be controlled by adjusting the temperature of sintering, allowing materials with adequate microstructure with application for ultrafiltration process.
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  • 8
    Electronic Resource
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    Springer
    Journal of sol gel science and technology 8 (1997), S. 697-701 
    ISSN: 1573-4846
    Keywords: ZnO-varistor ; sintering ; grain growth ; solution routes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract We have investigated the preparation of ZnO varistors by different chemical solution routes with the aim of improving the homogeneity of the phases formed and to obtain a better control of microstructure. One conventional oxide mixing route and four solution chemical routes have been used to prepare the precursor materials. In all cases, the same composition (mol%) was used; ZnO (95.9), Bi2O3 (1), Sb2O3 (1), NiO (1), Co2O3 (0.5), MnO (0.5), Cr2O3 (0.1). The same sintering procedure was also applied. It was found that the precursor materials consisting of ZnO grains covered by a thin film of the additive oxides yielded smaller ZnO grains. Also the microstructure in the final compacts was improved, compared with that of compacts prepared from oxide mixing routes. The smaller ZnO grain size in the final compacts was attributed to the presence of spinel grains. The spinel grains are formed at lower temperatures and, when they reach a size of 1 μm, they hinder the growth of ZnO grains.
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  • 9
    Electronic Resource
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    Springer
    Journal of sol gel science and technology 8 (1997), S. 789-794 
    ISSN: 1573-4846
    Keywords: aerogels ; plasticity ; elasticity ; SAXS ; Hg porosimetry ; sintering
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract When gently stressed, aerogels show an elastic response. However it was found that under isostatic pressure aerogels display an irreversible shrinkage which may be attributed to plastic behaviour. As a consequence of this plastic shrinkage it is possible to densify and modify the elastic properties of aerogels at room temperature. The structural evolution is followed by Small Angle X ray Scattering and the increase of the connectivity is revealed by the evolution of the elastic properties of the material. The SAXS data show that the densification mechanism is different from that obtained by sintering at high temperature. The densification mechanism induces a textural change at the periphery of the constitutive clusters but not inside, conversely to a sintering effect. We also show that the elasticity of the material is strongly influenced by this structural transformation. The power law evolution of the elastic modulus as a function of the density, usually observed on as-prepared and sintered aerogels, is not valid for compressed material.
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  • 10
    Electronic Resource
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    Springer
    Journal of sol gel science and technology 8 (1997), S. 831-836 
    ISSN: 1573-4846
    Keywords: aerogel ; silica-zirconia ; synthesis ; sintering ; pore distribution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A solution of zirconium propoxide stabilized by methoxyethanol is mixed with silicon ethoxide in ethanol and hydrolyzed by small amounts of neutral, basified or acidified water. The obtained silica-zirconia gel is dried in supercritical conditions, yielding an aerogel. The modifications of the aerogel porous texture as a function of chemical composition and thermal treatment are investigated using adsorption-desorption isotherms analysis, mercury porosimetry, electron-microscopy and X-ray diffraction.
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  • 11
    Electronic Resource
    Electronic Resource
    Springer
    Journal of sol gel science and technology 8 (1997), S. 261-268 
    ISSN: 1573-4846
    Keywords: SnO2 xerogel ; sintering ; Eu3+ spectroscopy ; XRD ; EXAFS
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The evolution of Eu3+ doped SnO2 xerogels to the cassiterite structure observed during sintering was studied by means of Eu3+ spectroscopy, XRD and EXAFS at the Sn K-edge. Eu3+ ions adsorbed at the surface of colloidal particles present a broad distribution of sites, typical of oxide glasses. With sintering at 300°C, this distribution is still broadened. Crystallization is clearly observed by the three techniques with increasing sintering temperature. It is found that the addition of Eu3+ limits the crystallite growth.
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  • 12
    Electronic Resource
    Electronic Resource
    Springer
    Journal of sol gel science and technology 8 (1997), S. 269-274 
    ISSN: 1573-4846
    Keywords: SnO2 xerogels ; sintering ; EXAFS ; XRD
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The formation of an ordered (crystalline) phase during isothermal sintering of SnO2 monolithic xerogels, at 200, 250, 300, 400, 500, 600 and 700°C, has been analyzed by the combined use of EXAFS and XRD techniques. For the desiccated gel (110°C), EXAFS results show the formation of small microcrystallites with the incipient cassiterite structure. Between 110 and 250°C, the dehydratation reaction leads to an amorphization evidenced by a decrease of the long and short range crystallographic order. It is due to fissure formation in the xerogel network. For higher temperatures, a continuous coagulation of the crystallites occurs, leading to grain growth. Grain and pore growth obeys the same kinetic relation, so that the microstructure grows by simple enlargement while its morphology is static.
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  • 13
    Electronic Resource
    Electronic Resource
    Springer
    Journal of sol gel science and technology 8 (1997), S. 353-363 
    ISSN: 1573-4846
    Keywords: sintering ; stress ; constraint ; crystallization ; nucleation ; film ; substrate ; rapid thermal annealing
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The sintering of films differs from that of bulk gels in several ways. The initial state of a film is generally denser and less crosslinked than a bulk gel made from the same sol, and these factors enhance the densification rate of the film. The substrate constrains the shrinkage of the film, leading to high stresses that retard densification and can influence phase changes. The substrate is a site for heterogeneous nucleation, and crystallization makes densification more difficult, so the competition between sintering and crystallization is particularly important for films. Fast heating favors densification over crystallization, so rapid thermal annealing usually produces denser films. The high surface to volume ratio of a thin film makes it susceptible to degradation by reaction with the substrate and the atmosphere, so choosing compatible materials and avoiding over-firing is essential.
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  • 14
    Electronic Resource
    Electronic Resource
    Springer
    Journal of sol gel science and technology 8 (1997), S. 377-380 
    ISSN: 1573-4846
    Keywords: sol-gel thin film ; sintering ; FTIR
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Solution derived thin films of molar composition 90SiO2−10TiO2 deposited on c-Si substrates, for use as planar waveguides are characterized in terms of thickness and refractive index, by ellipsometry, as a function of isothermal heat treatments. The structural evolution of the films with thermal treatment is followed by infrared spectroscopy. The estimated average Si−O−Si intertetrahedral bond angle increases from 137°, at room temperature, to 144°, after heating at 900°C. The films should be annealed atT〉800°C, in order to release the residual stresses.
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  • 15
    Electronic Resource
    Electronic Resource
    Springer
    Journal of sol gel science and technology 8 (1997), S. 397-402 
    ISSN: 1573-4846
    Keywords: silica glass ; monolith ; sub-critical drying ; chlorination ; sintering
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Over the last few years, the feasibility of fabricating near net shape silica glass components, using a sub-critical drying process for pure alkoxide gels, has been demonstrated in our laboratories. Cracking during drying, due to capillary forces generated in the gel body, was overcome through two particular innovations. The first was the development and optimization of a dual-catalyzed high strength gel. The second was a controlled atmosphere drying process that allowed the gel to dry utilizing a newly observed phenomenology, postulated to be due to cavitation of the pore fluid. Contrary to conventional wisdom, in this drying approach the smallest pore size gels are the easiest to dry. Details of the types of gels and the drying process are reported. Gels of small size were sintered into crack-free glasses, utilizing conventional sintering approaches. However, large size gels always developed visible surface cracks that formed above 800°C. To successfully dry and sinter large monolithic gels then required re-optimization of the entire process. A great number of micron-range defects were initially detected in these sintered bodies. After analyzing the defects, further steps were taken to improve glass quality to the level of optical glass produced by vapor deposition processes. This included mixing and filtering of sols in a clean room, varying the pore size distribution, and optimizing the pre-sintering and sintering processes. Data of relevant glass quality parameters attained so far in the laboratory are reported.
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  • 16
    Electronic Resource
    Electronic Resource
    Springer
    Journal of sol gel science and technology 8 (1997), S. 477-481 
    ISSN: 1573-4846
    Keywords: supported membrane ; SnO2 coating ; pore size distribution ; sintering
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract In this work, the effect of the substrate microstructure on the formation of SnO2 membranes and of the sintering conditions on their porosity have been analysed. Samples have been prepared by colloidal suspensions cast on alumina or kaolin substrates. Supported membranes have been characterized by Hg porosimetry, MEV, XRD and N2 adsorption-desorption isotherms. The results show that the narrower pore size distribution of alumina substrate allowed to prepare membranes more homogeneous and free of cracks than that supported on kaolin. The crystallite and pore sizes of the membranes could be controlled by adjusting the temperature of sintering, allowing materials with adequate microstructure with application for ultrafiltration process.
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  • 17
    Electronic Resource
    Electronic Resource
    Springer
    Journal of sol gel science and technology 8 (1997), S. 697-701 
    ISSN: 1573-4846
    Keywords: ZnO-varistor ; sintering ; grain growth ; solution routes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract We have investigated the preparation of ZnO varistors by different chemical solution routes with the aim of improving the homogeneity of the phases formed and to obtain a better control of microstructure. One conventional oxide mixing route and four solution chemical routes have been used to prepare the precursor materials. In all cases, the same composition (mol%) was used; ZnO (95.9), Bi2O3 (1), Sb2O3 (1), NiO (1), Co2O3 (0.5), MnO (0.5), Cr2O3 (0.1). The same sintering procedure was also applied. It was found that the precursor materials consisting of ZnO grains covered by a thin film of the additive oxides yielded smaller ZnO grains. Also the microstructure in the final compacts was improved, compared with that of compacts prepared from oxide mixing routes. The smaller ZnO grain size in the final compacts was attributed to the presence of spinel grains. The spinel grains are formed at lower temperatures and, when they reach a size of 1 μm, they hinder the growth of ZnO grains.
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  • 18
    Electronic Resource
    Electronic Resource
    Springer
    Journal of sol gel science and technology 8 (1997), S. 789-794 
    ISSN: 1573-4846
    Keywords: aerogels ; plasticity ; elasticity ; SAXS ; Hg porosimetry ; sintering
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract When gently stressed, aerogels show an elastic response. However it was found that under isostatic pressure aerogels display an irreversible shrinkage which may be attributed to plastic behaviour. As a consequence of this plastic shrinkage it is possible to densify and modify the elastic properties of aerogels at room temperature. The structural evolution is followed by Small Angle X ray Scattering and the increase of the connectivity is revealed by the evolution of the elastic properties of the material. The SAXS data show that the densification mechanism is different from that obtained by sintering at high temperature. The densification mechanism induces a textural change at the periphery of the constitutive clusters but not inside, conversely to a sintering effect. We also show that the elasticity of the material is strongly influenced by this structural transformation. The power law evolution of the elastic modulus as a function of the density, usually observed on as-prepared and sintered aerogels, is not valid for compressed material.
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  • 19
    Electronic Resource
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    Springer
    Journal of sol gel science and technology 8 (1997), S. 831-836 
    ISSN: 1573-4846
    Keywords: aerogel ; silica-zirconia ; synthesis ; sintering ; pore distribution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A solution of zirconium propoxide stabilized by methoxyethanol is mixed with silicon ethoxide in ethanol and hydrolyzed by small amounts of neutral, basified or acidified water. The obtained silica-zirconia gel is dried in supercritical conditions, yielding an aerogel. The modifications of the aerogel porous texture as a function of chemical composition and thermal treatment are investigated using adsorption-desorption isotherms analysis, mercury porosimetry, electron-microscopy and X-ray diffraction.
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  • 20
    Electronic Resource
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    Springer
    Journal of sol gel science and technology 9 (1997), S. 53-64 
    ISSN: 1573-4846
    Keywords: boehmite gel ; agglomerates ; dry pressing ; sintering ; alumina
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract It is demonstrated that dense alpha alumina can be fabricated by pressing ethanol-dispersed, α-Al2O3 seeded boehmite. Green bodies were formed by uniaxially pressing either water or ethanol dispersed gel powder and then isostatically pressing the compacts at 280 MPa. Green microstructure and alumina densification are correlated with gel agglomerate size and dispersing medium. The ethanol-dispersed specimens showed better sinterability than the water-dispersed specimens, and sintered to more than 99% theoretical density at 1300°C. It is shown that softer gel agglomerates were obtained by alcohol dispersion and resulted in better green microstructure and higher sintered density.
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  • 21
    Electronic Resource
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    Springer
    Journal of sol gel science and technology 9 (1997), S. 53-64 
    ISSN: 1573-4846
    Keywords: boehmite gel ; agglomerates ; dry pressing ; sintering ; alumina
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract It is demonstrated that dense alpha alumina can be fabricated by pressing ethanol-dispersed, α-Al2O3 seeded boehmite. Green bodies were formed by uniaxially pressing either water or ethanol dispersed gel powder and then isostatically pressing the compacts at 280 MPa. Green microstructure and alumina densification are correlated with gel agglomerate size and dispersing medium. The ethanol-dispersed specimens showed better sinterability than the water-dispersed specimens, and sintered to more than 99% theoretical density at 1300°C. It is shown that softer gel agglomerates were obtained by alcohol dispersion and resulted in better green microstructure and higher sintered density.
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  • 22
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    Journal of porous materials 4 (1997), S. 211-217 
    ISSN: 1573-4854
    Keywords: aerogel ; mechanical properties ; sintering ; model
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract The mechanical strength of silica aerogels and partially densified silica aerogels are investigated. This material allows the study of properties over a great range of porosity (0–95%). The experiments are performed in tension using a bending test. The mechanical strength increases by a 4 orders of magnitude over the whole range of porosity. The results are analyzed using two geometrical models (spheres and cylinder models) which account for the mean porosity properties of the materials and allows the mechanical strength evolution from aerogels to silica glass to be modelled.
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