Al2O3/Ni包裹粉体的制备、烧结行为及其显微结构研究

利用非均相沉淀包裹技术,在铝无机盐溶液中制备出氧化铝前驱体包裹纳米镍颗粒的复合粉体,并通过能量发射能谱（EDS）以及俄歇电子能谱（AES）研究包裹粉体的成分构成,发现镍纳米颗料表面均匀地包裹一层氧化铝的前驱体。燃烧后的包裹粉体在氩气氛中进行热压烧结。结果表明,与溶胶－凝胶法制备的粉体相比,包裹粉体可以在较低的温度下达到致密化,烧结后的材料其显微结构明显不同于环磨粉体烧成的材料,否认在氧化铝晶界或晶内,镍颗粒与氧化铝之间都有孔隙,这是由于镍的热膨胀系数与氧化铝的热膨胀系数大引起的,Al2O3/Ni复合材料的断裂方式以及沿晶断裂为主。     

Ni包裹Al2O3复合粉体的制备

采用非均相沉淀工艺在Al2O3颗粒表面均匀地包裹上镍盐前驱体,经煅烧、还原后得到纳米晶Ni包裹Al2O3复合粉体.相分析表明,非晶态的镍盐前驱体在550℃已转变为NiO,再经700℃氢气处理后,NiO还原为Ni,其晶粒尺寸约为20nm.结构分析表明,复合粉体在热处理过程中,包裹层由连续态变为非连续态.     

镍掺杂方式对Al2O3／Ni复合材料的结构及力学性能的影响

分别以Ni包裹氧化铝微球、氧化铝包裹Ni微球以及氧化铝／Ni共沉淀复合微球粉体为烧结原料，通过热压烧结法制备了Ni质量含量在0％～30％的氧化铝基金属陶瓷。利用SEM，TEM，XRD对烧结Al2O3／Ni金属陶瓷的微结构及前躯体、热还原粉体和金属陶瓷的晶相进行了分析，通过阿基米德法测量了金属陶瓷的相对密度，并分别利用三点弯曲法和单边切口横梁法对材料的抗弯强度和断裂韧性进行了评估。结果显示：3种粉体制备的金属陶瓷分别形成了晶间型、晶内型及晶间／晶内混合型结构，且在烧结过程中，Ni相在某种程度上降低了材料的致密化速率，也抑制了氧化铝晶粒的长大．同时，Ni掺杂方式的不同导致了氧化铝基质的断裂模式及力学性能的变化。     

Ni包裹Al2O3复合粉体的制备

采用非均相沉淀工艺在Al2O3颗粒表面均匀地包裹上镍盐前驱体，经煅烧，还原后得到纳米晶Ni包裹Al2O3复合粉体，相分析表明，非晶态的镍盐前驱体在550℃已转变为NiO，再经700℃氢气处理后，NiO还原为Ni，其晶粒尺寸约为20nm。结果分析表明，复合粉体在热处理过程中，包裹层由连续态变为非连续态。     

新型光致发光储能材料的制备及其光学性能的研究

研究了一种新型的光致发光储能材料ＳｒＡｌ２Ｏ４∶Ｅｕ,Ｄｙ的合成方法,首先利用软化学法制备出了该发光材料的前驱体ＳｒＣＯ３－Ａｌ２Ｏ３－ＲＥ（ＯＨ）３超细粉体,解决了固相混合中存在的纷分不均匀性。然后将此前驱体粉体在还原气氛下高温烧结,最终制得亮度高、余辉时间长的超细发光粉体材料。并对其发光性能进行了研究,发光粉体的发射光谱表明,通过软化学法工艺制备出的发光粉体,其发射光谱的主峰位置较固相法兰移了１２ｎｍ。     

用包裹纳米复合粉体制备ZTA陶瓷

用非均匀成核法和液相共沉淀法相结合的方法制得ZrO2(3Y)包裹Al2O3纳米复合粉体,经干压成型,常压烧结制备ZTA复相陶瓷.通过XRD、TEM对粉料的物相组成和显微形貌进行表征,研究了包裹粉体中煅烧温度和ZrO2含量对烧结体的烧结性能和力学性能的影响.结果表明:随着前驱体粉料煅烧温度的升高,包裹后的Al2O3-ZrO2(3Y)复合陶瓷粉体比表面积降低,粒径变大;ZrO2含量为20wt.%的Al2O3-ZrO2(3Y)复合陶瓷粉体,经过1000℃锻烧后,干压成型制备的烧结样品的抗弯强度和断裂韧性分别高达454.9MPa和11.6MPa·m1/2,SEM观察结果表明烧结体结构致密.     

NiO纳米晶的制备及结构研究

采用溶胶-凝胶（sol-gel）技术制备氧化镍粉体，考察烧结条件对NiO粉体的组成、结构和形貌的影响。研究结果表明，以醋酸镍、柠檬酸和水为原料在一定温度下合成了稳定的溶胶和凝胶，凝胶在400℃左右基本分解完全，逐渐形成NiO纳米晶，随着烧结温度的升高，纳米NiO晶粒尺寸逐渐增大，晶型趋于完整且晶粒大小分布均匀。600℃烧结2h获得NiO粉体的颗粒尺寸52nm，晶型较好且无杂相存在，有望成为高性能锂离子电池的阳极材料。     

Al2O3基复合材料中纳米SiC对微观结构的影响

本文从烧结温度、基体晶粒大小、断裂方式、SiC在基体中的分布等几个方面研究了纳米SiC颗粒的加入对Al2O3微观结构的影响．用非均相沉淀工艺制备的纳米SiC-Al2O3复合粉体，具有Al2O3颗粒包裹纳米SiC的特点，提高了烧结温度，明显使Al2O3晶粒变小，并且抑制晶粒异常长大，试样的断裂方式从以沿晶断裂为主转变到以穿晶断裂为主．SiC在Al2O3中分布均匀，大部分位于晶粒内，少部分位于晶界上．这种微观结构有利于力学性能的提高．     

脉冲电流烧结机理的研究进展

脉冲电流烧结（Ｐｕｌｓｅ ｅｌｅｃｔｒｉｃ ｃｕｒｒｅｎｔ ｓｉｎｔｅｒｉｎｇ,ＰＥＣＳ）是材料科学领域开发出的一种新型快速烧结技术,已广泛应用于金属与合金、结构陶瓷、氧化物超导体、复合材料、热电材料、高分子材料以及功能梯度材料的制备．本文简介脉冲电流烧结特征,结合ＰＥＣＳ烧结条件对铜粉末和氧化铝粉体致密化及显微结构影响的实验证据,就脉冲电流烧结过程和机理进行探讨．     

纳米LaAlO3粉体的制备与烧结

对共沉淀法制备纳米LaAlO3粉体及烧结进行了初步研究．采用La(NO3)3与Al(NO3)3为原料，控制pH=9左右，在室温下完成共沉淀，前驱体经800℃／2h的条件下煅烧后可获得纳米LaAlO3粉体，粉体颗粒约50nm．无压烧结的结果表明，这种纳米LaAl03粉体的烧结性能较好，通过选择适当的条件，在1500℃下烧结可获得密度达6．2g／cm^3的LaAlO3材料．     

Fabrication and characterization of NiTi shape memory alloy synthesized by Ni electroless plating of titanium powder

In this work NiTi shape memory alloy was fabricated from mixed elemental powders, Ni plated titanium powder and Ni heated/plated titanium powder by Ar-sintering. Electroless plating process was utilized to fabricate Ni plated titanium powder. For this purpose titanium powder was plated in an electroless Ni bath for 225?min and hydrazine hydrate was used as a reductant to deposit pure nickel on the titanium particles. Ni plated titanium powder was heat treated under an argon atmosphere at 1000?°C to prepare Ni heated/plated titanium powder. Finally, the three sample powders were pressed by CIP followed by sintering at 980?°C for 8?h to manufacture NiTi shape memory alloy. The prepared powders, as well as sintered samples, were characterized by scanning electronic microscopy (SEM), energy dispersive spectrometer analysis (EDS), X-ray fluorescence (XRF), X-ray diffraction (XRD) and differential scanning calorimetric (DSC). The results indicated the presence of NiTi phase and also non-transformable phases (NiTi₂ and Ni₃Ti) in the heated/plated Ti powder and sintered samples. NiTi compound was dominated phase in the heated/plated sintered sample. All three sintered samples, as well as heated/plated powder, showed one-step phase transformation (B2???B19′).     

Synthesis of WC hard materials using coated powders

Nickel and cobalt were used as binder materials for tungsten carbide powders (WC) hard materials. Ni and Co binder were added individually to the WC powder by two different methods namely, mechanical mixing and chemical electroless coating. In this study WC powders of grain sizes 0.3–1.0 μm were electroless coated with either nickel or cobalt. The loading of either Ni or Co coating was 13 wt.%. The electroless-coating method conditions of both Ni and Co on WC powders are described. The coated powders were cold compacted and sintered in vacuum at different sintering temperatures. For comparison, identical materials compositions were prepared by mixing the powders constituents mechanically, compacted and sintered under the same conditions.The prepared powders and sintered materials were investigated using X-ray diffraction (XRD) and scanning electron microscope (SEM). The results revealed that coated WC materials have smaller values of porosity and more homogeneous microstructure while other properties, such as transverse rupture strength, and hardness exhibit greater values than those produced using mixing elemental powders. It is possible to outline the benefits of coated powder approach in the following: high homogeneity and better distribution of binder materials within WC hard materials, higher density and good interfacial bonding, capability of using fine powders, and possibility of using small alloying and/or reinforcement additions in a more uniform manner.     

Fabrication of nanosized alumina powders by a simple polymer solution route

Nanosized alumina (Al2O3) powders had been successfully fabricated by a simple polymer solution route employing polyvinyl alcohol (PVA) as an organic carrier. The fabricated alumina powders had an average particle size of 6.1 nm with a high specific surface area of 99.5 m2/g. As well, the alumina powders were fully crystallized to alpha phase at a relatively low temperature of 1000 degrees C. The PVA polymer contributed to a soft and porous microstructure of the calcined alumina powders, and ball-milling process with the porous powders was effective in making nanosized alumina powders. In addition, the content and degree of polymerization of the PVA affected the development of crystallization and powder properties. In this study, the simple polymer technique and milling process for the fabrication of nanosized alumina powders are introduced, and the effects of PVA on the property of the synthesized alumina powders are observed. For the study, the characterizations of the synthesized powders are conducted by using XRD, TEM, particle size analyzer, and nitrogen gas adsorption.     

Alumina coating on dense tungsten powder by fluidized bed metal organic chemical vapour deposition

In order to study the feasibility of coating very dense powders by alumina using Fluidized Bed Metal Organic Chemical Vapour Deposition (FB-MOCVD), experiments were performed on a commercial tungsten powder, 75 microm in median volume diameter and 19,300 kg/m3 in grain density. The first part of the work was dedicated to the experimental study of the tungsten powder fluidization using argon as carrier gas at room temperature and at 400 degrees C. Due to the very high density of the tungsten powder, leading to low initial fixed bed heights and low bed expansions, different weights of powder were tested in order to reach satisfactory temperature profiles along the fluidized bed. Then, using argon as a fluidized bed former and aluminium acetylacetonate Al(C5O2H7)3 as a single source precursor, alumina thin films were deposited on tungsten particles at a low temperature range (e.g., 370-420 degrees C) by FB-MOCVD. The influence of the weight of powder, bed temperature and run duration was studied. Characterizations of the obtained samples were performed by various techniques including scanning electron microscopy (SEM) coupled with Energy Dispersive X-ray Spectroscopy (EDS) analyses, Field Emission Gun SEM (FEG-SEM) and Fourier Transform InfraRed (FT-IR) spectroscopy. The different analyses indicated that tungsten particles were uniformly coated by a continuous alumina thin film. The thickness of the film ranged between 25 and 80 nm, depending on the coating conditions. The alumina thin films were amorphous and contained carbon contamination. This latter may correspond to the adsorption of species resulting from incomplete decomposition of the precursor at so low deposition temperature.     

Plasma spraying of nanostructured partially yttria stabilized zirconia powders

Nanosized partially yttria stabilized zirconia particles, prepared using a co-precipitation method, were reprocessed into agglomerate powders using two methods for plasma spraying. The first method was to make micrometer-sized agglomerates directly following the grinding of the calcined yttria–zirconia agglomerates. The second method was to reconstitute the nanosized particles into micrometer agglomerates using spray drying. The deposition efficiency, porosity, microhardness and average grain size of the deposits made from these two reprocessed powders were studied. Distinct results related to the process parameters were obtained for the two types of powders. The second type of powder was more suitable for plasma spraying than the first one. Using the second type of powder, some unique results distinguished from those of the conventional partially yttria stabilized zirconia powders were observed and an optimized coating with a porosity of 3.8%, Hv_0.3 of 953 and mainly consisting of 1–3 μm columnar grains in the columnar direction and smaller than 100 nm in their cross-sections was achieved.     

Preparation of NixTiy compound via Ni plating followed by thermal treatment of Ti powder

In this research, Ni_xTi_y compound was prepared by thermal treatment of Ni-plated Ti powder. For this purpose, Ti powder was plated in an electroless Ni bath for various times (120, 225, 300, and 720?min). Hydrazine hydrate was used as a reductant for the deposition of pure Ni on the Ti particles. The plated powder (225?min) was heat treated under argon atmosphere to achieve Ni_xTi_y powder. Finally, the heated/plated powder was pressed by CIP followed by sintering at 980°C for prepare the Ni_xTi_y bulk sample. The plated powders as well as sintered one were characterized using scanning electron microscopy, energy dispersive spectrometer, X-ray fluorescence, X-ray diffraction and differential scanning calorimetric. The NiTi₂, NiTi, and Ni₃Ti phases were detected in the XRD patterns of heated/plated Ti powder. According to DSC data, the heated/plated Ti powder showed reversible martensitic transformation at temperature range of ?38.0°C to +38.1°C, while sintered/heated/plated Ti powder displayed reversible transformation at temperature range of 16.0°C–15.4°C.     

SURFACE CHARGE OF SOL-GEL DERIVED ALUMINAS AS A FUNCTION OF CALCINATION TEMPERATURE

The sol-gel route for preparing alumina is thought to yield a unique molecular structure. Thus the powder characteristics of sol-gel derived aluminas are expected to be different from alumina powders derived by traditional processing methods. In this study wet alumina gels, after the sol-gel reaction was completed, were dried and calcined at 25^°C, 300^°C, 500^°C, 800^°C, 1100^°C, and 1400^°C following the methods of Yoldas and Clark and Lannutti. The initial points of zeta potential reversal (PZR) of the calcined powders determined from electrophoretic mobilities are 9.4, 10.2, 8.6, 10.6, 4.2 and 8.3, respectively for the above calcination series. The PZR of the alumina powders increased with calcination temperature up to 800^°C, with the exception of the alumina calcined at 500^°C. The PZR's of powders calcined between 800-1400^°C decreased. The anomalous PZR of the alumina calcined at 500^°C is due to catalytically formed carboxylates from the residual sec-butano1. The general trend of PZR change for other phases of gel derived alumina was compared with previously reported electrolcinetic behavior of traditional alumina powders and no significant differences were found.     

纳米氧化钛陶瓷的烧结

将醇盐水解制备的纳米氧化钛粉体（～13nm）在500～800℃下煅烧,用XRD研究氧化钛相变过程中粉体的热稳定性,发现在加入0．4wt％的金红石相作为晶种后;晶粒生长受到较好的控制,同时分别在30、57和200MPa下对纳米氧化钛样品进行热压烧结,用密度仪、压汞仪和SEM对烧结前后的样品进行表征后表明,700℃的热压烧结样品已开始致密化,200MPa、800℃热压烧结样品的相对密度为97．2％,此时3～15nm的小气孔仍难以消除,这些小气孔的存在是纳米氧化钛陶瓷在较高的压力下难以完全致密的主要原因．     

Influence of calcination temperature on the properties of spray dried alumina-zirconia composite powders

Alumina-zirconia composite powders containing 10, 12.5, 15 or 20 wt% zirconia were prepared by spray-drying the hydroxide gels. These powders were calcined at 650 and 950 °C. The spray-dried as well as the calcined powders were characterized by means of Coulter counter, Sorptometer, infrared spectroscopy (i.r.), scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and X-ray diffraction (XRD). Initially the spray-dried powders are amorphous and spherical in shape with a diameter of 6 m and crystallize after calcination treatment at 950 °C. Sintered density of the 950 °C calcined powder compacts was higher than 650 °C calcined powder compacts. Compacts made from 650 °C treated powders retained 100% tetragonal phase after sintering irrespective of composition. Some amount of tetragonal phase is transformed into monoclinic phase in the composites containing higher amount of zirconia in the sintered compacts made from 950 °C calcined powders.