掺铝钕高硅氧玻璃的制备及光谱性能研究

采用分相酸溶工艺制备了Na2O-B2O3-SiO2体系纳米多孔玻璃,并以此为基质进行了钕铝掺杂的实验,制备了掺钕铝高硅氧玻璃,光谱分析表明,所制得的玻璃在1064 nm附近有明显的发射峰.研究了掺杂浓度、烧结气氛对玻璃光谱性能的影响,分析了铝离子在共掺杂玻璃中的作用.结果表明在浓度为0.2 mol/L的Nd(NO3)3溶液中制备的掺杂高硅氧玻璃发光强度最强,还原气氛下烧结的掺杂高硅氧玻璃光谱强度高于在空气中烧结得到的高硅氧玻璃,同时在还原条件下铝离子能够明显的提高玻璃的发光强度.     

含CaF2纳米晶的透明玻璃陶瓷的制备工艺分析

采用熔融冷却法制备了组分为55SiO2-20Al2O3-5CaO-20CaF2及45SiO2-20Al2O3-10CaO-25CaF2两组玻璃,并通过热分析测定了玻璃的转变温度、核化温度和晶化温度。采取等温热处理工艺在不同温度下对两组玻璃进行3h晶化热处理并对热处理后的试样进行物相结构、透光率和微观形貌的表征。结果表明,将玻璃进行等温晶化热处理能制备含CaF2纳米晶的透明玻璃陶瓷;增加组分中CaF2及CaO的含量能提高体系的玻璃转变温度及成核温度;提高热处理温度使析晶程度增大,透光率下降;CaF2和CaO在玻璃中可引起成分偏聚而产生分相,提高玻璃的析晶程度。     

Tb3+掺杂钼酸盐玻璃陶瓷的制备及发光性能表征

采用熔融-晶化法制备了Tb3+掺杂的CaMoO4为主晶相的透明钼酸盐玻璃陶瓷。利用DSC、XRD、SEM确定了该体系玻璃样品的最佳热处理制度：715℃保温2.5 h;随着热处理时间的增加,玻璃陶瓷中的晶粒尺寸逐渐变大;利用UV-Vis-NIR得到样品玻璃陶瓷在可见光区的透过率可达80%;并利用荧光光谱讨论了在相同热处理条件下,不同Tb3+掺杂浓度对玻璃陶瓷样品发光性能的影响,研究表明Tb3+掺杂浓度为7.0mol%时样品的荧光强度最大。     

基于正交试验的钡硼硅酸盐玻璃陶瓷的热处理制度研究

热处理是使玻璃陶瓷获得预定结晶相的关键工序.采用正交试验法研究了热处理制度(核化温度、晶化温度、保温时间)对钡硼硅酸盐玻璃陶瓷晶相结构和显微结构的影响.结果表明:采用一步法(核化、晶化同时进行)和二步法(核化、晶化分开进行)热处理时,样品的主晶相均为CaZrTi2O7-2M,还含有少量ZrO2相.对于两步法,在720℃核化2h、850℃晶化3h的条件下,钙钛锆石的晶相含量较高,晶粒为长条状,长约20～30 μm.当晶化温度较高(900～950℃)或晶化时间较长(2～3 h)时,都会出现CaTiSiO5晶相.各参数对玻璃陶瓷中晶相含量的影响顺序为:晶化温度＞核化温度＞晶化时间＞核化时间.一步法热处理温度变化对样品的晶相组成和显微结构变化较小.     

锌铝硅透明微晶玻璃的体视学研究

用熔融法制备ZnO-A12O3-SiO2玻璃,经两步热处理工艺控制成核及晶体生长制备出透明微晶玻璃.对锌铝硅透明微晶玻璃进行光透过率、场发射环境扫描电镜(field emission-environment scanning electron microscope,FE-ESEM)测量.用体视学分析方法根据不同光透过率对应的FE-ESEM照片,定量研究陶瓷三维结构参数和光透过率之间的关系.结果表明:尺寸为10 mm×10 mm1 mm的锌铝硅透明微晶玻璃在可见光区的光透过率约为87%;在近红外光区的为92%.随着入射光波长的增加,光透过率增加.随着三维球当径和晶粒平均比表面积的增加,锌铝硅透明微晶玻璃光透过率下降.随着单个晶粒平均比表面积和晶粒三维平均自由距离的增加,锌铝硅透明微晶玻璃光透过率增加.     

基于Er3+/Yb3+掺杂的上转换玻璃陶瓷材料的制备和性能

采用熔融-晶化法在ZnO-Al2 O3-SiO2系玻璃陶瓷的基础上,用GeO2取代部分SiO2成功制备出Er3+/Yb3+共掺ZnO-Al2 O3-GeO2-SiO2系玻璃陶瓷,并通过对样品的硬度及上转换荧光测试分析确定了GeO2的最佳取代量为7.5wt％.研究发现在980 nm波长光的激发下,样品产生了绿色(524 nm、546 nm)和红色(659 nm)上转换发光,且当Er3+/Yb3+掺杂比为2.5:6.5时样品上转换荧光强度最强.     

钒酸盐玻璃陶瓷封接材料的制备及应用

采取熔融-晶化法制备了主晶相为Ba3(VO4)2的玻璃陶瓷,研究了热处理制度对玻璃陶瓷样品析晶情况、热学及力学性质的影响.结果表明:在最佳热处理条件晶化540 ℃,保温2 h下,玻璃陶瓷的转变温度Tg、软化温度Tf、热膨胀系数及硬度均优于基质玻璃,且热膨胀系数为17.81 ×10 -6℃-1与金属铜的热膨胀系数值( 17.7 × 10-6℃-1)临近,能够与之直接封接,将有毒的含铅封接材料取而代之.     

水热法制备钕掺杂BaTiO3粉体及其介电性能研究

以BaCl2·2H2O、TiCl4和NdCl3为原料,采用水热法制备了掺钕的BaTiO3纳米粉体,并经高温烧结后得到瓷体。利用DTA、XRD、SEM等测试手段,分析了钕掺杂对钛酸钡粉体及其陶瓷电性能的影响。研究表明,掺杂后,钕固溶到了钛酸钡的晶格中并取代钡位或钛位。钕的掺杂有助于获得细晶高致密的陶瓷,当W(NdCl3)%为0.6时,致密度最高,常温下相对介电常数高达5650,击穿场强达到3.5kV/mm。     

添加CeO2的Li2O-Al2O3-SiO2系微晶玻璃的晶化和性能研究

采用差热分析,X射线衍射分析和扫描电镜等分析手段研究了添加质量分数为5%CeO2对Li2O-Al2O3-SiO2系微晶玻璃形核和晶化的影响.结果表明添加5%CeO2使该体系玻璃转变温度降低,晶化峰值温度降低,最佳成核温度从760 ℃降低到730℃.晶化过程中,β-石英固溶体首先从玻璃中析出,在较高温度,β-石英固溶体转变为β-锂辉石固溶体.通过计算发现,添加CeO2后,样品的晶化活化能E和晶化指数n从添加前(323±7)kJ/mol,2.8±0.2变为(282士7)kJ/mol,3.2±0.2.说明了添加CeO2在降低玻璃的粘度的同时促进了玻璃晶化,而对材料的透明性与热膨胀系数等影响很小.     

硅锂比对二硅酸锂玻璃陶瓷的结构与性能的影响

研究了硅锂摩尔比对二硅酸锂体系玻璃的结构与性能的影响,并在具有最佳性能的组分基础上,探究成核处理对玻璃的结构与力学性能的影响规律。结果表明:硅锂摩尔比n(SiO_2):n(Li_2O)从2.0增加到2.4,玻璃的结构和热性能及力学性能发生显著变化。其中,n(SiO_2):n(Li_2O)为2.2的组分最易析晶,具有最佳的力学性能[玻璃陶瓷三点弯曲强度(404±30) MPa]。同时研究了成核温度、时间对玻璃结构与力学性能的影响规律。n(SiO_2):n(Li_2O)为2.2的组分经优化晶化工艺处理后,一次热处理的主晶相为偏硅酸锂,二次热处理的主晶相为二硅酸锂,断裂韧性为3.58 MPa·m~(–1/2)。     

Phase diagram of the Al2O3-HfO2-Y2O3 system

The phase diagram of the Al₂O₃-HfO₂-Y₂O₃ system was first constructed in the temperature range 1200-2800 °C. The phase transformations in the system are completed in eutectic reactions. No ternary compounds or regions of appreciable solid solution were found in the components or binaries in this system. Four new ternary and three new quasibinary eutectics were found. The minimum melting temperature is 1755 °C and it corresponds to the ternary eutectic Al₂O₃ + HfO₂ + Y₃Al₅O₁₂. The solidus surface projection, the schematic of the alloy crystallization path and the vertical sections present the complete phase diagram of the Al₂O₃-HfO₂-Y₂O₃ system.     

Laser machining of Al2O3-ZrO2 (3%Y2O3) eutectic composite

In this work we present the study of the interaction between NIR pulsed laser and Al₂O₃-ZrO₂ (3%Y₂O₃) eutectic composite. The effect produced by modifying the reference position as well as the working conditions and laser beam features has been studied when the samples are processed by means of pulse bursts.The samples were obtained by the laser floating zone technique using a CO₂ laser system. The laser machining was carried out with a Q-switched Nd:YAG laser at its fundamental wavelength of 1064 nm with pulse-widths in the nanosecond range.Geometric dimensions, i.e. ablated depth, machined width and removed volume as well as ablation yield of the resulting holes have been studied. We have described and discussed the morphology, composition and microstructure of the processed samples.     

Synthesis and characterization of Y2O3-ZrO2 and Y2O3-CeO2-ZrO2 precursor powders

Thixotropic gels of the precursor powders of the titled compounds have been prepared by the addition of oxalic acid to the mixed solutions of metal salts at room temperature (≈ 27 °C). The clear sols of yttrium-zirconyl oxalate (YZO) and yttrium-cerium-zirconyl oxalate (YCZO) gelled within a few hours and were oven-dried at 40 °C. The various stages of gelation behaviour of the sols are explained on the basis of DLVO theory. By repeptizing the dried gel powders with water, concentrated sols were prepared. The gelation time as a function of chloride ion concentration is discussed for both sols. The nature of the temperature dependence of the dried gel powders was studied by means of thermogravimetric analysis and differential thermal analysis. Powder X-ray diffraction was used to study the crystallization behaviour of the dried amorphous gel powders. It is found that these powders crystallize in tetragonal phase when calcined at 850 °C for 1 h. Estimation of surface area and infra-red characterization have also been carried out for the prepared powders.     

Preparation and characterization of Cr2O3-TiO2-Al2O3-V2O5 green pigment

Green pigments with high near infrared reflectance based on a Cr₂O₃-TiO₂-Al₂O₃-V₂O₅ composition have been synthesized. Cr₂O₃ was used as the host component and mixtures of TiO₂, Al₂O₃ and V₂O₅ were used as the guest components. TiO₂, Al₂O₃, and V₂O₅ were mixed into 39 different compositions. The spectral reflectance and the distribution of pigment powder were determined using a spectrophotometer and a scanning electron microscope, respectively. It was found that a pigment powder sample S9 with a Cr₂O₃-TiO₂-Al₂O₃-V₂O₅ composition of 80, 4, 14 and 2 wt%, respectively, gives a maximum near infrared solar reflectance of 82.8% compared with 49.0% for pure Cr₂O₃. The dispersion of pigment powders in a ceramic glaze was also studied. The results show that the pigment powder sample S9 is suitable for use as a coating material for ceramic-based roofs.     

Fabrication and mechanical properties of Al2O3-Si3N4/ZrO2-Al2O3 laminated composites

In this paper, Al₂O₃-Si₃N₄/ZrO₂-Al₂O₃ laminated composites were fabricated by tape casting and hot press sintering, and the relationships between the process, microstructure, and mechanical properties of Al₂O₃-Si₃N₄/ZrO₂-Al₂O₃ laminated composites were determined. The SiAlON phase was found in the Al₂O₃-Si₃N₄ layer, and liquid-phase sintering was proposed. Nano-scratch tests were carried out to investigate the interface bonding strength of the laminates. The distribution of residual stresses, generated due to the different coefficients of thermal expansion between the different layers, was estimated according to lamination theory and confirmed using Vickers indentation. When the sintering temperature was 1550 °C, the sintered laminated ceramics had good mechanical properties, with a maximum strength and toughness of 413 MPa and 6.2 MPa m^1/2, respectively. The main toughness mechanics of laminated composites was residual stress.     

Effect of Al2O3 on mechanical properties of Ti3SiC2/Al2O3 composite

The effect of Al₂O₃ on mechanical properties of Ti₃SiC₂/Al₂O₃ composite fabricated by SPS was studied systematically. The results show that the hardness of the Ti₃SiC₂/Al₂O₃ composite can reach 10.28 GPa, 50% higher than that of pure Ti₃SiC₂. However, slight decrease in the other mechanical properties was observed with Al₂O₃ addition higher than 5–10 vol.%, which is believed to be due to the agglomeration of Al₂O₃ in the composite.     

Formation of alkoxy-derived 3Al2O3 · 2GeO2

Germanium-mullite (3Al₂O₃·2GeO₂) is formed directly as a single phase at lower temperatures from amorphous material with 50–66.7 mole% Al₂O₃ prepared by the alkoxy-method. The kinetic data of the 3Al₂O₃·GeO₂ crystallization with 50 and 60 mole% Al₂O₃ are represented by different solid-state equations. The difference of the crystallization mechanism is possibly explained in terms of the morphology of the 3Al₂O₃·GeO₂ particles.     

Preparation and properties of ceramic composites with oxygen ionic conductivity in the ZrO2-CeO2-Al2O3 and ZrO2-Sc2O3-Al2O3 systems

Powder precursors in the ZrO₂-CeO₂-Al₂O₃ and ZrO₂-Sc₂O₃-Al₂O₃ systems are prepared by the sol-gel synthesis. It is revealed that the electrical conductivity of the sample doped with scandium oxide is higher than the electrical conductivity of the sample doped with cerium oxide despite the higher content of the nonconducting phase Al₂O₃ (corundum). The thermal expansion coefficients are determined for all the ceramic samples under investigation. It is established that the Al₂O₃ dopant affects the thermal expansion coefficient. The ceramic materials studied can be used as solid-electrolyte sensors. Original Russian Text ? P.A. Tikhonov, M. Yu. Arsent’ev, M.V. Kalinina, L.I. Podzorova, A.A. Il’icheva, V.P. Popov, N.S. Andreeva, 2008, published in Fizika i Khimiya Stekla.     

Mechanical properties of Al2O3-Cr2O3/Cr3C2 nanocomposite fabricated by spark plasma sintering

The fine grains of Al₂O₃-Cr₂O₃/Cr-carbide nanocomposites were prepared by employing recently developed spark plasma sintering (SPS) technique. The initial materials were fabricated by a metal organic chemical vapor deposition (MOCVD) process, in which Cr(CO)₆ was used as a precursor and Al₂O₃ powders as matrix in a spouted chamber. The basic mechanical properties like hardness, fracture strength and toughness, and the nanoindentation characterization of nanocomposites such as Elastics modulus (E), elastic work (W_e) and plastic work (W_p) were analyzed. The microstructure of dislocation, transgranular and step-wise fracture surface were observed in the nanocomposites. The nanocomposites show fracture toughness of (4.8 MPa m^1/2) and facture strength (780 MPa), which is higher than monolithic alumina. The strengthening mechanism from the secondary phase and solid solution are also discussed in the present work. Nanoindentation characterization further illustrates the strengthening of nanocomposites.     

负载型K2CO3/Al2O3二氧化碳吸收剂的碳酸化反应特性

The carbonation characteristics of K₂CO₃/Al₂O₃ supported sorbent for CO₂ capture was investigated with thermogravimetric apparatus（TGA）,X-ray diffraction（XRD）,scanning electron microscopy analysis（SEM）and N₂ adsorption.The results showed that the carbonation rate of K₂CO₃ before being loaded on Al₂O₃ was slow.However,the K₂CO₃/Al₂O₃ upported sorbent showed excellent carbonation performance.The difference in carbonation behavior between K₂CO₃ nd K₂CO₃/Al₂O₃ supported sorbent was analyzed from the microscopic view.The analytical reagent K₂CO₃ sample was of monoclinic crystal structure and could react quickly with H₂O in the experimental carbonation environment to produce K₂CO₃•1.5H₂O,which was unfavorable to carbonation reaction.When K₂CO₃was loaded on Al₂O₃,the surface area and porosity of the sorbent was improved greatly.So the carbonation properties of the K₂CO₃/Al₂O₃ supported sorbent was also improved.