非化学计量比制备纯MgTiO_3和Mg_2SiO_4及其性能

纯MgTiO3和Mg2SiO4粉体在微波陶瓷工业中具有重要价值,本文将MgO-TiO2和MgO-SiO2按非化学计量比配料,采用传统固相法制备了纯MgTiO3和Mg2SiO4粉体。当MgO和TiO2或SiO2按照1∶1和2∶1的化学计量比配料时,分别得到了主晶相为MgTiO3和Mg2SiO4的粉体,但同时伴随有少量的TiO2或MgO残余。XRD分析表明,MgO过量可以抑制残余TiO2制备纯MgTiO3粉体,而MgO不足可以有效控制MgO残余量制备纯Mg2SiO4粉体。采用SEM表征所制备的纯MgTiO3和Mg2SiO4粉体的形貌和粒度。最终获得的MgTiO3陶瓷1MHz下的介电常数为17.3,损耗角正切1.3×10-4,Mg2SiO4陶瓷1MHz下的介电常数为6.9,损耗角正切2.5×10-4。     

Al2O3添加剂对合成MgTiO3陶瓷相组成及介电性能的影响

研究了添加剂Al2O3对MgO和TiO2合成MgTiO3陶瓷烧结性，物相组成和微波介电性能的影响。XRD分析结果表明，没有添加Al2O3是，合成的MgTiO3陶瓷中只含有MgTiO3和MgTi5相,加入Al2O3，MgTiO3陶瓷中除了MgTiO3和MgTi2O5相外，还出现了MgAl2O4相，这是上由于Al2O3和MgO发生固相反应，MgAl2O4的出现虽然阻碍材料的致密化并导致密度下降，但是可能降低反应烧结合成MgTiO3陶瓷的相对介电常数和介电损耗。     

水基流延制备BaTiO3基PTC片的研究

通过水基流延制备BaTiO3基PTC片,陶瓷粉体采用固相合成预烧BaTiO3基PTC粉体,平均粒径为1.0μm,粘合剂采用浓度为12%的PVA溶液和B-1070乳液,分散剂采用D-3019(Rohm-Hass),增塑剂分别采用化学纯的丙三醇、邻苯二甲酸二丁脂和聚乙二醇PEG400,消泡剂采用化学纯的正辛醇,溶剂为水.主要讨论了分散剂的用量和粘度的关系、浆料的固相含量和粘度的关系、不同粘合剂浆料的流变行为、不同粘合剂的热失重特性等,发现采用PAA乳液粘合剂无论是在固含量、粘度以及烧成后电性能都优于PVA粘合剂,因此更适合于BaTiO3水基流延,当分散剂用量为粉体0.50%(质量分数)时,浆可以获得固相含量高达86.0%左右粘度仅为490mPa·s的BaTiO3陶瓷浆料.     

SmFeO_3的制备及其多波段兼容隐身性能研究

采用固相法制得了SmFeO3粉体.借助XRD、SEM对SmFeO3粉体的物相组成和形貌进行了表征.此外,测试了SmFeO3的微波电磁特性及其吸波性能、红外辐射率以及1.06 μm波长处的反射率性能.结果表明,当煅烧温度为1250℃时,可以制得单一相的SmFeO3粉体;该粉体宏观呈现橙红色,微观颗粒尺寸大小为2～4μm的不规则块状.当单层SmFeO3材料的厚度为2.0mm时,反射损耗在15.8GHz左右出现约为-10dB的峰值,同时在14.3～16.8 GHz频率范围内反射损耗均达到-5dB.SmFeO3粉体在1.06μm波长处的反射率为0.31%,激光吸收性能强;红外辐射率为0.58,属于中低红外辐射率.     

红色发光材料MgTiO_3:Eu~(3+)的水热合成研究

以MgSO4、TiC4为镁源和钛源,以NaOH为矿化荆,向体系内添加Eu3+,在有聚四氟乙烯衬的高压反应釜内以60%的填充度、以220℃的反应温度通过90～200h的反应时间制得MgTiO3:Eu3+粉体.XRD分析表明相纯度较高.FS结果显示,产品有294nm和483nm2个激发峰;发射峰位于615nm,颜色较纯.该方法具有合成温度低,产物发光亮度好,不用焙烧和球磨就能得到优质粉体的特点.     

高能球磨Al-Y203粉体固相反应制备YAG陶瓷的研究

用高纯Al粉体和Y2O3粉体(Al-Y2O3粉体)为原料采用固相反应法制备了YAG陶瓷. Al-Y2O3粉体高能经过球磨,煅烧生成YAG粉体,再真空烧结制备高致密YAG陶瓷.采用DTA-TG对球磨Al-Y2O3粉体进行分析,采用XRD、SEM对球磨的Al-Y2O3粉体、YAG粉体及YAG陶瓷进行了表征.实验表明:Al-Y2O3粉体在～569℃时,Al粉强烈氧化,并与Y2O3粉反应,600℃煅烧出现YAM相,随煅烧温度升高出现YAP相,1200℃煅烧生成YAG粉体.成型YAG素坯在1750℃保温2h真空烧结出YAG相陶瓷,YAG陶瓷相对密度可达98.6%,晶粒生长均匀,晶粒尺寸为8～10μm.     

影响喷雾造粒Al2O3/nano-TiO2复合陶瓷粉体流动特性的流变学因素研究

本文研究了分散剂、粘结剂及固相含量等流变学因素对喷雾造粒粉体流动性的影响.结果表明,Al2O3/3wt.%nano-TiO2浆料具有剪切变稀的特性,有利于复合陶瓷粉体的喷雾造粒.当固相含量为浆料总质量的60%,分散剂和粘结剂分别为固相质量的0.3%和1.0%时,浆料具有合适的粘度和最佳的分散稳定性,喷雾造粒所得到的粉体形状为球形或近球形,具有较高的松装密度和良好的流动性,满足用于热喷涂的需要.     

固相剪切碾磨对聚偏氟乙烯结构和介电性能的影响

利用固相剪切碾磨技术(S~3M)制备了高β晶含量的聚偏氟乙烯(PVDF)微米级粉体,研究了PVDF粉体的结构形态、粒径及粒径分布,碾磨遍数对粉体结晶结构和介电性能的影响。结果表明,固相力化学反应器强大的挤压和剪切作用可使PVDF中α晶转变为晶,从而有效提高PVDF粉体中β晶相对含量;随碾磨遍数增加,PVDF粉体β晶含量逐渐提高,未碾磨PVDF中的β晶相对含量为37%,碾磨15遍后β晶相对含量达90%以上;同时,介电常数则由1.20增加至10.77,提高约1个数量级。固相剪切碾磨技术为高介电性能材料的制备提供了新途径。     

高能球磨Al-Y2O3粉体固相反应制备YAG陶瓷的研究

用高纯Al粉体和Y₂O₃粉体(Al-Y₂O₃粉体)为原料采用固相反应法制备了YAG陶瓷. Al-Y₂O₃粉体高能经过球磨, 煅烧生成YAG粉体, 再真空烧结制备高致密YAG陶瓷. 采用DTA-TG对球磨Al-Y₂O₃粉体进行分析, 采用XRD、SEM对球磨的Al-Y₂O₃粉体、YAG粉体及YAG陶瓷进行了表征. 实验表明: Al-Y₂O₃粉体在～569℃时, Al粉强烈氧化, 并与Y₂O₃粉反应, 600℃煅烧出现YAM相, 随煅烧温度升高出现YAP相, 1200℃煅烧生成YAG粉体. 成型YAG素坯在1750℃保温2h真空烧结出YAG相陶瓷, YAG陶瓷相对密度可达98.6%, 晶粒生长均匀, 晶粒尺寸为810μm.     

非水解和水解溶胶-凝胶法合成钛酸铝粉体的研究对比

分别采用非水解和水解溶胶-凝胶法合成钛酸铝粉体,利用FT-IR、DTA-TG、XRD、SEM等方法研究了溶胶-凝胶转变和合成相变化过程及粉体烧结性能.结果发现:水解凝胶过程中Al3+以网络外离子形式富集于Ti-O-Ti凝胶网络之间,凝胶依次晶化成金红石和刚玉,再通过固相扩散在1350℃时合成钛酸铝,粉体粒径为1～2μm,比表面积仅3.2m2/g,1400℃烧结后抗弯强度为7.2MPa.非水解凝胶化过程中Al3+和Ti4+通过聚合共同形成凝胶网络,其在网络结构中地位趋同,凝胶在 750℃已直接由无定型晶化为钛酸铝,粉体粒径为0.1～0.3μm,比表面积与抗弯强度分别为水解法样品的35倍和2.3倍,性能较好.     

电弧气化法制备纳米ITO粉末及高密度ITO靶的研制

以纯度为99．99％的纯金属In和Sn为原料,采用电弧气化法制备了单一立方In2O3结构的纳米ITO合金粉末,所制备的粉末以四方和类球形两种形貌存在,粒度主要位于30-70nm,分散性良好;并在此基础上采用常压烧结制备了相对密度高达99．74％,平均电阻率达到1．52×10^-4Ω·cm,结构成份均匀,晶粒尺寸5—10μm左右的超高密度ITO靶材。     

石英基复合导电粉末的制备与应用

传统的导电粉末存在性能不稳定、适用性差等问题。本文中以石英粉为基体 ,应用化学共沉淀技术 ,表面包覆掺杂的SnO2 制得了复合导电粉末。采用正交实验方法 ,确定了石英基复合导电粉末制备的最优化工艺条件 :水解pH值1.0 ,SnCl4·5H2 O/SbCl3 摩尔比 10∶1,SnCl4·5H2 O用量为2 0 % ,水解温度为 4 5℃ ,焙烧温度为 70 0℃。在该条件下 ,制得了平均粒径为 5 .7μm、电阻率为 2 5 3Ω·cm的复合导电粉末。用该导电粉末制得的导电涂料的体积电阻率仅为12 .6Ω·cm ,各项性能指标均达到国家标准     

Preparation and characterization of ceramic porous sheet composed of platelet (Cr, Al)2O3 crystals

A compact powder mixture consisting of 3Al2O3·2SiO2 (mullite) and Cr2O3, which was heated in a carbon powder bed, was cut into a 1 mm thickness sheet. The ceramic porous sheet composed of platelet (Cr, Al)2O3 crystals was prepared by leaching SiO2 contained in the sheet by hydrofluoric acid. The porous sheet produced from the 50 mass % mullite/50 mass % Cr2O3 compact, heated at 1500°C for 2 h, was composed of platelet crystals with 30 μm average length and 4.6 μm average thickness. Its relative density and specific surface area were 73 % and 4.4 m2 g-1 respectively. This revised version was published online in November 2006 with corrections to the Cover Date.     

ZnFe2O4 and ZnO-Zn1−xMxFe2O4+δ (M = Sm3+, Eu3+ and Ho3+): Synthesis,physical properties and high performance visible light induced photocatalytic degradation of malachite green

The present work reports the synthesis of ZnFe₂O₄ and ZnO-Zn_1-xM_xFe₂O_4+δ (Ln?=?Sm, Eu and Ho) nanomaterials by conventional solid state reactions between Ln₂O₃, Zn(NO₃)₂, Fe(NO₃)₃·9H₂O and/or FeCl₃·6H₂O raw materials at 800?°C for 10?h and 15?h. Stoichiometric and nonstoichiometric reactions were explored for the synthesis of ZnFe₂O₄. The two Fe sources (Fe(NO₃)₃ and FeCl₃) were used to study the proper raw material type for the synthesis of the ZnFe₂O₄. The synthesized nanomaterials were characterized by powder X-ray diffraction (PXRD) technique. Rietveld analysis showed that the obtained materials were crystallized well in cubic crystal system with the space group Fd3m and lattice parameters a?=?b?=?c?=?8.4?Å. The rietveld data showed that the purity of ZnFe₂O₄ was increased from 14% to 88% when the Fe source was changed from FeCl₃ to Fe(NO₃)₃ meanwhile the reaction time was changed from 10 to 15?h. However, the purity was increased to 96% when the stoichiometry of Zn:Fe was changed from 1:2 to 0.8:2 at 800?°C for 15?h. The PXRD data revealed that dopant ion type had a considerable influence on the crystal phase purity of the obtained materials. It was found that Yb₂O₃ decreased more the purity of the obtained target compared to the other dopant ions. Ultraviolet-visible spectra showed that the synthesized nanomaterials had strong light absorption in the visible light region. Photocatalytic performance of the as-synthesized ZnFe₂O₄ was investigated for the degradation of pollutant Malachite Green (MG) in aqueous solution under direct visible light irradiation. The degradation yield at the optimized condition (0.09?mL H₂O₂, 30?mg catalyst and 60?min) was 98%.     

High strain rate superplasticity of ultrafined Ti–10V–2Fe–3Al compact prepared by sintering and isothermal forging

Abstract

High strain rate superplasticity was obtained for powder Ti–10V–2Fe–3Al (Ti-1023) alloy prepared by powder sintering and isothermal forging technology. The selected powder was cold isostatic pressed, sintered and isothermal forged to prepare this powder alloy. Tensile testing was conducted at optimum superplastic temperaure of 1023 K with different initial strain rate, and the elongation to failure, the flow stress and the microstructure were analysed. The experiment results exhibited that the microstructure of this powder alloy is extraordinary uniform and fine, resulted in considerable enhancement of optimum initial strain rate increased from 3·3×10^?4 s^?1 of conventional cast and wrought Ti-1023 alloy to 3·3×10^?3 s^?1 of this powder alloy. The elongation to failure increased first and then decreased with initial strain rate from 3·3×10^?4 to 3·3×10^?2 s^?1. The strain rate sensitivity m is about 0·46 near initial strain rate of 3·3×10^?3 s^?1, larger than conventional cast and wrought Ti-1023 alloy. Microstructure observations showed that dynamic recrystallisation and grain growth were present during superplastic deforming.     

High rate performance of LiFePO<Subscript>4</Subscript> cathode materials co-doped with C and Ti<Superscript>4+</Superscript> by microwave synthesis

Nanostructured LiFePO₄ powder with a narrow particle size (ca. 100 nm) for high rate lithium-ion battery cathode application was obtained by microwave heating and using citric acid as carbon source. The microstructures and morphologies of the synthesized materials were investigated by X-ray diffraction and scanning electron microscope while the electrochemical performances were evaluated by galvanostatic charge-discharge. The carbon coating and Ti⁴⁺ could improve the conductivity both between the LiFePO₄ particles and the intrinsic electronic conductivity. The LiFePO₄ doped with 5% C and 1% Ti⁴⁺ resulted in a specific capacity of 114·95 mAh·g⁻¹ and 102·4 mAh·g⁻¹ at discharge rates of 0·3C and 1C, respectively, and the cycle performance is very good.     

Sintering Behavior and Microwave Dielectric Properties of MgTiO3 Ceramics Doped with B2O3 by Sol-Gel Method

The B2O3-doped MgTiO3 powders and ceramics have been prepared by sol-gel method using Mg(NO3)2·6H2O, Ti(C4H9O)4 and H3BO3 as the starting materials. The sintering behavior and microwave dielectric properties of ceramics prepared from powders with different particle sizes were investigated. The gels were calcined at 650, 700, 750, 800, 850 and 900 C and the derived particle sizes of powders were 20-30 nm, 30-40 nm, 40-60 nm, 60-90 nm, 90-120 nm and 120-150 nm, respectively. The nanoparticles with the size of 30-60 nm benefited the sintering process with high surface energy whereas nanoparticles with the size of 20-30 nm damaged the microwave dielectric properties due to the pores in the ceramics. The addition of B2O3 used as a liquid sintering aid reduced the sintering temperature of MgTiO3 ceramic, which was supposed to enter the MgTiO3 lattice and resulted in the formation of (MgTi)2(BO3)O phase. The B2O3-doped MgTiO3 ceramic sintered at 1100 C and prepared from the nanoparticles of 40-60 nm had compact structure and exhibited good microwave dielectric properties: εr=17.63, Q × f=33,768 GHz and τ f= 48×10 6 C 1.     

Synthesis of magnetite by coprecipitation and sintering and its characterization

Magnetite powder was synthesized via chemical co-precipitation method using FeCl₃?·?6H₂O and FeCl₂?·?4H₂O as salts and ammonium hydroxide (25% NH₄OH) solution as precipitating agent. The phases, composition and morphology of the magnetite was characterized by X-ray diffraction (XRD), micro laser Raman spectroscopy and scanning electron microscopy–energy dispersive X-ray spectroscopy. The XRD and Raman studies confirmed the formation of magnetite phase only. The results showed that the particles were properly crystallized with no other impurity. Very fine and non-uniform powder sizes were observed even after sieving operation. The magnetite particles were also characterized after sintering the powder at 1100°C, grinding and sieving. The resultant powder size in the range of 105–125?µm was obtained. After sintering, magnetite peaks got sharpened due to increase in the crystallite size. Raman peaks even at a higher laser power were observed for magnetite that were absent before sintering. Hematite peaks observed for the un-sintered powder at higher laser power was attributed to oxidation by laser radiation/heat. Efficiency of the co-precipitation process (before sintering) was established to be ～85%.     

Design of powder metallurgy aluminium alloys for applications at elevated temperatures Part 2 Tensile properties of extruded and Conformed gas atomised powders

Abstract

The effects of aging treatments on the tensile properties and microstructure of Al–Cr–Zr–Mn powder metallurgy aluminium alloys prepared from high pressure gas atomised powders were investigated. The alloy compositions were designed to give powders with or without Al₁₃Cr₂ intermetallics in the <45 μm size fraction. The Al–5·2Cr–1·4Zr–1·3Mn alloy is typical of the former (concentrated alloy) and the Al–3·3Cr–0·7Zr–0·7Mn alloy of the latter (dilute alloy). The alloys were prepared using a canning/degassing/extrusion sequence or the Conform consolidation process. Measurements of micro hardness and electron microscopy were used to correlate the microstructure with the tensile properties. The extruded powders of both alloys exhibited better properties than those of the Conformed powders. A large contribution to the strength of the extruded materials is made by their stabilised fine grain size. The dilute alloys had consistently better ductility. Neither alloy retained its strength after prolonged aging at 400°C, but the results indicate that a service temperature of 300°C may be possible.

MST/1247b     

低温共烧氧化铝/玻璃复合基板材料的研究

以低软化点的钙硼硅酸盐玻璃和氧化铝粉末为原料,制备了氧化铝/玻璃低温共烧复合基板材料。所需的玻璃粉体采用溶胶-凝胶法制备。研究了烧结温度和氧化铝含量对复合材料的烧结特性、介电性能以及力学性能的影响。结果表明,当氧化铝质量分数为50%,复合材料经950℃、保温2 h烧结后,其εr=5.92,tanδ=5.7×10-4,ρ=1012Ω.cm,抗弯强度σ=167.82 MPa,热膨胀系数α=4.86×10-6/℃,可望作为低温共烧多层陶瓷基板材料应用。