均匀沉淀法制备羟基磷灰石的研究

对以硝酸钙和磷酸作为反应物,采用均匀沉淀法制备的羟基磷灰石粉体进行了研究。研究发现,硝酸钙溶液的初始浓度和粉末的煅烧温度对所制备的羟基磷灰石(HAP)的粒径、比表面积有较大的影响。采用XRD射线衍射谱、BET比表面积测试、粒径测试等分析手段,探索出较好的工艺条件,进而探讨了在形成生物陶瓷过程中,煅烧温度对HAP密度及收缩率的影响。     

Gas- and Liquid-Phase Reactions on Sulphated Zirconia Prepared by Precipitation

Sulphated zirconia (SZ) was synthesized under different precipitation and ageing conditions. Catalysts were characterized by nitrogen adsorption–desorption, thermal analysis, FTIR and Raman spectroscopy. The catalytic performance of these SZ systems in both gas and liquid-phase reactions has been investigated. The effect of precipitation and ageing conditions has been studied and a correlation with catalytic activity has been tried.     

Crystal Structure of Zirconia Prepared with Alumina by Coprecipitation

Zirconia was prepared by firing the coprecipitate from ZrOCl₂and AlCl₃mixed aqueous solution with ammonia. When fired above 600°C, the products were fine crystalline tetragonal zirconia of crystallite size <10 nm. In previous studies, the tetragonal phase had been assumed to be a (Zr_{1− x} ⁴⁺Al _x ³⁺)O_{2− x /2}solid solution, where x ≤ 0.25. However, X-ray diffraction pattern simulation and Al K -edge XANES spectroscopy confirmed the present product to be a mixture of t -ZrO₂fine powder with a small amount of δ-Al₂O₃of very low crystallinity, even below the expected compositional range of x ≤ 0.25 in the (Zr_{1− x} ⁴⁺Al _x ³⁺)O_{2− x /2}solid solution.     

均相沉淀法制备掺钕钇铝石榴石纳米粉末的研究

掺钕钇铝石榴石（Nd：YAG）多晶透明陶瓷具有容易制造、成本低、光学性能好、热导率高等优点,是一种很有前途的激光工作物质。以AI（N03）·9H2O,Y2O3,Nd2O3,（NH4）2SO4和尿素为原料,正硅酸乙酯为添加剂,采用均相沉淀法制备出分散均匀、纯YAG立方晶相的Nd：YAG纳米前驱体粉末。采用XRD、FT-IR、TEM等测试手段对前驱体粉末进行表征。研究结果表明：Nd：YAG前驱体粉末在800℃时为无定型态,当温度达到890℃时析出大量的中间相YAlO3（Y=AP）和少量的Y3Al5O5（YAG）,当温度达到1000℃时就全部转化为YAG立方晶相。     

Nanocrystallization and Phase Transformation in Monodispersed Ultrafine Zirconia Particles from Various Homogeneous Precipitation Methods

Monodispersed ultrafine (nano- to micrometer) zirconia precursor powders were synthesized by three different physicochemical methods: (I) forced hydrolysis, (II) homogeneous precipitation in inorganic salt solutions, and (III) hydrolysis/condensation of alkoxide. The forced hydrolysis method produced monoclinic nanocrystalline particles (cube shaped) of nanometer scale, which depended largely on the initial salt concentration. Methods II and III, both involving the use of alcohol as a solvent, exhibited a faster particle formation rate and generated amorphous ultrafine (submicrometer) monodispersed microspheres, indicating that the presence of alcohol may have stimulated particle nucleation due to its low dielectric property (and, thus, the low solubility of nucleus species in mixed water-alcohol solutions). Nucleation and growth of the particles in solutions are discussed based on the measurements obtained by small-angle X-ray scattering (SAXS) and dynamic light scattering (DLS). High-temperature X-ray diffraction (HTXRD) and TGA/DTA studies elucidated the differences in phase transformation for different types of powders. The most interesting finding was the nonconventional monoclinic nanocrystal nucleation and growth that occurred prior to transformation to the tetragonal phase (at 1200°C) during the heat treatment of the nanocrystalline powders produced by the forced hydrolysis.     

均匀沉淀法制备纳米ZnO

硝酸锌和尿素的浓度、反应温度以及表面活性剂的种类都是影响均匀沉淀法制备纳米ZnO的重要因素。实验结果表明:均匀沉淀法制备纳米ZnO时,控制硝酸锌的浓度0.6~0.9mol/L,尿素的浓度2.6~2.8mol/L,反应温度95℃,加入表面活性剂能制备出粒径在40~70nmZnO。     

二氧化锆对低品位菱镁矿制备镁铝尖晶石材料组成结构的影响

以低品位菱镁矿与工业氧化铝为原料制备镁铝尖晶石材料,分析研究二氧化锆对以低品位菱镁矿为原料制备的镁铝尖晶石的组成、结晶度、晶胞参数和微观结构的影响,用XRD和SEM对烧后试样的相组成和显微结构进行研究.利用X'pert plus软件对试样中结晶相的相对结晶度进行计算,并对镁铝尖晶石相的晶胞参数进行分析.结果表明:适量引入二氧化锆有利于以低品位菱镁矿与工业氧化铝为原料制备镁铝尖晶石材料;材料中结晶相的结晶度随二氧化锆加入量的增加呈现出先增加后降低的现象;镁铝尖晶石材料中主晶相镁铝尖晶石的晶胞参数及晶胞体积受到锆离子的置换固溶作用的影响;当二氧化锆加入量为1.2％时,镁铝尖晶石的晶胞参数和晶胞体积最大,结构中镁铝尖晶石形成量最大,而玻璃相形成量最小.因此对于以低品位菱镁矿与工业氧化铝为原料制备的镁铝尖晶石材料,二氧化锆的最佳引入量为1.2％.     

不同工艺制备的水合氧化锆凝胶之特性

用水解沉淀法和中和沉淀法两种工艺制备了水合氧化锆凝胶，并与经乙醇脱水处理后的水合氧化锆凝胶的形貌、热性能、相态以及红外吸收光谱作了比较。     

Precipitation in Partially Stabilized Zirconia

Transmission electron microscopy was used to study the sub-structure of partially stabilized ZrO₂ (PSZ) samples, i.e. 2-phase "alloys" containing both cubic and monoclinic modifications of zirconia, after various heat treatments. Monoclinic ZrO₂ exists as (1) isolated grains within the polycrystalline aggregate (a grain-boundary phase) and (2) small plate-like particles within cubic grains. These intragranular precipitates are believed to contribute to the useful properties of PSZ via a form of precipitation hardening. These precipitates initially form as tetragonal ZrO₂, with a habit plane parallel to the {100} matrix planes. The orientation relations between the tetragonal precipitates and the cubic matrix are
and      

Sintering Behavior of Nanocrystalline Zirconia Prepared by Chemical Vapor Synthesis

Powder synthesis and ceramic processing methods have to be improved to take full advantages of new, improved properties of nanocrystalline ceramics. Sintered nanocrystalline ceramics of pure, undoped zirconia are formed from nanocrystalline powder of optimized quality obtained by the chemical vapor synthesis (CVS) method. The as-synthesized CVS ZrO₂ powder is nonagglomerated with a crystallite size of about 5 nm, narrow size distribution, and high crystallinity. On uniaxial compaction a transparent green body of ultrafine, uniform microstructure and narrow pore size distribution corresponding to the grain size distribution is formed, which is sintered under vacuum at 950°C into a transparent, fully dense ZrO₂ ceramic with a grain size of 60 nm.     

Synthesis and Characterization of ZnCr2O4 Nanospinel Prepared via Homogeneous Precipitation Using Urea Hydrolysis

In situ and homogeneous hydrolysis of urea was utilized to design a homogeneous precipitation method to synthesize the ZnCr₂O₄ functional material. The as‐prepared nanospinel was systematically studied in terms of crystal structure, morphology, texture, and light absorption. A well‐crystalline single phase of ZnCr₂O₄ nanospinel with a spongy network structure was obtained. Transmission electron microscopy and X‐ray diffraction observations confirmed the formation of monocrystalline nanoparticles of ZnCr₂O₄ with the nanosize of 13 nm. The synthesized nanospinel showed a low direct band gap value of 1.8 eV with appropriate absorption in the visible light region, which was a remarkable result for this route.     

Preparation of Lead Zirconate by Homogeneous Precipitation and Calcination

Antiferroelectric PbZrO₃ has been synthesized by homogeneous precipitation from aqueous solutions in the presence of urea (NH₂CONH₂) and calcination for 6 h at 700°C. SEM studies displayed the presence of submicrometer powder, with a significant degree of agglomeration.     

均匀沉淀法制备不同粒径的纳米氧化锌

由于纳米氧化锌的功能和用途不同,因而需要制备出不同平均粒径的纳米氧化锌。论文以六水硝酸锌为原料,尿素为沉淀剂,研究了均匀沉淀法制备不同平均粒径纳米氧化锌的工艺条件,讨论了工艺条件对其粒径和产率的影响规律。结果表明:通过均匀沉淀法制备的纳米氧化锌的前驱体为Zn5(OH)6(CO3)2;制备的纳米氧化锌为六方晶系的球形颗粒,平均粒径为20～50nm;纳米氧化锌的产率随反应物浓度的增大、反应温度的升高、反应配比(n尿素/nZn2+)的增大而增大;纳米氧化锌颗粒的平均粒径随反应物浓度的减小、反应温度和煅烧温度的降低而减小。     

Stabilized Zirconia Nanoceramics Prepared by Magnetic Pulsed Compaction of Nanosized Powders

Ceramic materials with a fine structure are synthesized from zirconia-based nanopowders through magnetic pulsed compaction and subsequent sintering under different temperature-time conditions. The kinetics of crystallite growth and polymorphic phase transformations are analyzed. Unstabilized zirconia ceramic materials with a density of 96% and a crystallite size of 50 nm are prepared. It is found that, in the case when the ceramic materials with a cubic or tetragonal yttrium-stabilized zirconia (YSZ) matrix are synthesized with small additives of alumina nanopowders, the temperatures of active shrinkage and the polymorphic transformation γ-Al₂O₃ → α-Al₂O₃ are shifted to the high-temperature range, the density and microhardness of the final ceramics slightly decrease, and the size of α -Al₂O₃ crystallites does not exceed 100 nm. It is also established that the alumina additives have no noticeable effect on the growth of crystallites of the YSZ matrixOriginal Russian Text Copyright © 2005 by Fizika i Khimiya Stekla, Ivanov, Khrustov, Paranin, Medvedev, Shtol’ts, Ivanova, Nozdrin.     

Precipitation During Controlled Cooling of Magnesia-Partially-Stabilized Zirconia

A study has been made of the precipitation and growth processes which occur during cooling from solution treatment and under isothermal hold conditions in a magnesia-partially-stabilized zirconia alloy. Three types of precipitate have been identified which develop during cooling or during isothermal hold treatments just above and below the eutectoid temperature. These precipitate forms are termed (i) primary, (ii) large random, and (iii) secondary. Further precipitation, slow growth of existing precipitates, and subeutectoid decomposition result when an additional 1100°C aging treatment is given to the previously cooled material. It is shown that type (iii) secondary precipitates form rapidly within the temperature range of 1300° to 1375°C. The secondary precipitates are largely responsible for the improved room-temperature strength properties of the heat-treated samples. The formation and effects on mechanical properties of each type of precipitate are discussed.     

对采用三种烧结技术制备的氧化锆的致密化和性能的研究

由氨基乙酸／硝酸盐闷烧方法制备了含8％Y2O3的纳米晶钇稳定氧化锆粉末,用火花等离子体烧结（SPS）、热压（HP）和传统烧结法（CS）研究了其致密性。SPS技术比其余烧结方法优异,能在较低温度和较短烧结时间获取具有均匀形态的致密化材料（≥96％）。经SiX5、热压和传统烧结方法制备的材料,其晶粒尺寸分别是0．21、0．37和12μm。材料的总电导率与晶粒尺寸并无明确关系,但SPS烧结材料的活化能比其余两种致密化方法的稍高。由Vickers压痕法测得的硬度与晶粒尺寸无关,而断裂韧性（由压痕法测得）随晶粒尺寸增大而轻微下降。     

均匀沉淀法制备纳米氧化镁粉体的试验研究

以六水氯化镁和尿素为原料,以聚乙二醇辛基苯基醚为分散剂,采用均匀沉淀法制备出颗粒直径约为20～30 nm的氧化镁粉体.通过四因素三水平正交试验确定了液相反应条件对纳米氧化镁晶粒直径的影响程度和最佳液相合成条件.结果表明,影响纳米氧化镁晶粒直径的液相反应因素主次顺序依次为:反应物(六水氯化镁)浓度、反应时间、反应物配比(尿素和六水氯化镁的物质的量比)及反应温度.以纳米氧化镁粉体晶粒直径为控制指标的最佳液相反应条件为:反应物浓度1.5 mol/L,反应时间3 h,反应物配比5:1,反应温度99℃.     

Formation of Zirconia Solid Solutions Containing Alumina Prepared by New Preparation Method

In the system ZrO₂–Al₂O₃, a new method for preparing ZrO₂ solid solutions from ZrCl₄ and AlCl₃ using hydrazine monohydrate is investigated. c -ZrO₂ solid solutions containing up to ∼40 mol% Al₂O₃ crystallize at low temperatures from amorphous materials. The formation mechanism is discussed from IR spectral data. The values of the lattice parameter α increase linearly from 0.5072 to 0.5105 nm with increasing Al₂O₃ content. At higher temperatures, transformation of the solid solutions proceeds as follows: c ( SS ) → t ( ss ) → t ( ss ) +α-Al₂O₃→ m +α-Al₂O₃. m -ZrO₂–α-Al₂O₃ composite ceramics are fabricated by hot isostatic pressing for 2 h at 1250°C and 196 MPa. Microstructures and mechanical properties are examined, in connection with increasing Al₂O₃ content.     

非均匀沉淀法制备黑色氧化锆陶瓷

以Y-TZP（氧化钇稳定四方多晶氧化锆）为原料、硝酸锰和硝酸铝为着色剂、PEG2000（聚乙二醇2000）为分散剂,采用非均匀沉淀法制备着色剂/氧化锆复合粉体,经成型、烧结后得到黑色氧化锆陶瓷。采用X射线衍射,扫描电子显微镜、X射线荧光分析和透射电子显微镜等对复合粉体和陶瓷的结构和性能进行表征,结果表明：着色剂/氧化锆...