聚丙烯酰胺凝胶法制备纳米BeO粉体前驱体的热分解过程及结晶机理

采用聚丙烯酰胺凝胶法制备纳米BeO粉体,通过TG-DSC、XRD和SEM等测试手段研究凝胶前驱体的热分解过程和所得粉体的性能,并借助负离子配位多面体生长基元理论分析热分解过程中纳米BeO的结晶机理。结果表明:随着温度的升高,凝胶前驱体内的有机凝胶逐渐分解,同时凝胶前驱体内的硫酸铍盐脱除结晶水;当温度达到600℃左右时,有机凝胶完全分解,得到纳米级的无水硫酸铍;继续升高温度,纳米级的无水硫酸铍分解得到纳米BeO;热分解过程中,纳米硫酸铍通过生长基元Be(SO4)6断键形成纳米BeO,成核过程为受迫状态下的非均匀成核。     

不同锆源对聚丙烯酰胺凝胶法制备氧化锆纳米粉体的影响

采用聚丙烯酰胺凝胶法,分别以氧氯化锆、硫酸锆和硝酸氧锆为锆源制备ZrO2纳米粉体,利用热重-差热同步分析仪(TG-DSC)、X射线衍射仪(XRD)和扫描电子显微镜(SEM) 分别对凝胶的热分解过程及氧化锆粉体的物相组成和形貌进行分析和表征,研究了不同锆源对聚丙烯酰胺凝胶法所制备的ZrO2纳米粉体相转变、物相组成及粉体形貌的影响。结果表明,锆盐影响聚丙烯酰胺凝胶的热分解完全温度,以硝酸氧锆为前驱体制得的凝胶热分解完全温度最低,约为530 ℃,以硫酸锆和氧氯化锆为前驱体制得的凝胶热分解完全温度分别为573 ℃和580 ℃。锆盐影响氧化锆的晶化温度,但氧化锆的相转变过程相似,均是由无定型氧化锆转变为四方相氧化锆,并在900 ℃时完全转变为单斜相氧化锆。氧化锆的晶化温度越高,平均粒径越小,团聚程度越高,以上述三种锆源为前驱体均可制备出近似球形的纳米氧化锆粉体,粉体粒径分布在52~97.4 nm范围内。     

金属Co／聚丙烯酰胺复合粉体的γ射线辐照制备

从Ｃｏ＾２＋丙烯酰胺有机单体混合水溶液体系出发,采用γ射线辐照合成制备金属Ｃｏ粒子均匀分散在丙烯酰胺基质中的Ｃｏ／聚丙烯酰胺复合粒子和相应粉体,其中金属Ｃｏ粒子平均粒径小于１５ｎｍ。     

溶胶-凝胶法制备氧化锆粉体

以正丙醇锆为锆源,采用溶胶-凝胶法制备了ZrO2粉体。研究了硝酸含量对凝胶时间及热处理温度对ZrO2晶型的影响规律。通过控制硝酸含量可以有效改变凝胶时间;通过锆醇盐水解缩聚制备的ZrO2干凝胶,在低温下热处理首先形成ZrO2四方相,在较高温度热处理后才转变为单斜相;锆醇盐水解缩聚制备的氧化锆粉体在1200℃以后烧结过程明显加快。     

氧化锌铝陶瓷(AZO)靶材的制备及其电阻性能的测定

采用二步烧结技术制备AZO陶瓷靶材,并采用XRD、SEM和EDS对AZO陶瓷靶材进行表征,研究AZO靶材的电阻性能。结果表明:当Al的掺杂量w(Al2O3)为0.5%时,AZO靶材出现第二相ZnAl2O4;随Al掺杂浓度增加,ZnAl2O4的衍射峰强度逐渐增强,ZnO晶粒尺寸逐渐减小;随着第二步烧结温度θnd的升高,AZO靶材的晶粒尺寸逐渐增大,相对密度也随之增加。靶材的电阻率随θnd增加而降低,且随掺杂浓度升高而增加;在第一步烧结温度θst=1 400℃,升温速率vst=10℃/min,第二步烧结温度θnd=1 350℃和t nd=16 h烧结条件下,AZO陶瓷靶材(w(Al2O3)=1.5%)的电阻率仅为2.9×10-2Ω·cm。     

溶胶凝胶和化学镀法制备超细CoAl2O4粉体的研究

本研究用溶胶凝胶法和化学镀法两种方法制备超细CoAl2O4粉体，并且利用XRD，SEM，EDX，DTA等手段进行了检测。结果表明两种方法制备的粉体有相同的尖晶石转变温度；溶胶凝胶法制备的粉体成分严格符合化学计量比，化学镀法制备的粉体中Al是过量的。与溶胶凝胶法相比，用化学镀法来制备的粉体粒度小而且均匀一致，比表面积大，可以很好地控制粉体的粒度和组成。在化学镀制备工艺下，粉体催化剂的反应接触面积较大，有可能获得较高的催化效率；而且用便宜的Al2O3部分替代了昂贵的CoAl2O4，降低了成本，说明化学镀法是一种制备超细CoAl2O4粉体的高效方法。     

溶胶-凝胶法制备PTCR陶瓷

以钛酸丁酯和乙酸钡为主要原料,硝酸钇作为施主加入物,乙酸为溶剂,乙二醇为稳定剂,采用溶胶-凝胶方法制备了BaTiO3粉体,并用此粉体制得PTCR陶瓷.通过XRD分析物相、扫描电镜观察粉体颗粒的大小及陶瓷的显微结构.结果表明实验获得的PTCR陶瓷性能优良,具有室温电阻率29.9Ω·cm,升阻比在104以上,电阻温度系数为12%.     

溶胶一凝胶法制备掺铝氧化锌薄膜

采用溶胶-凝胶工艺在普通玻璃片上制备了掺铝氧化锌薄膜.通过X-射线衍射(XRD)、原子力显微镜(AFM)对薄膜的组织结构和形貌进行了表征,结果表明:用溶胶-凝胶法制得的掺铝氧化锌薄膜为纤锌矿型结构,呈c轴方向择优生长,表面均匀、致密.通过紫外-可见透射光谱(UV)和标准四探针法对薄膜的光电性能进行了研究.试验发现,当铝离子掺杂浓度为4%(摩尔分数)、溶胶物质的量浓度为0.6mol/L、前处理温度为300℃时,薄膜在可见光区的透过率超过80%,且具有较好的导电性,电阻率为8.0×10-4Ω·cm.     

溶胶凝胶法制备Co掺杂ZnO粉体及其磁性

Co掺杂ZnO(Zn1-xCoxO)是理论预测的具有室温铁磁性的少数稀磁半导体之一,在自旋电子器件领域有着重要应用前景。以醋酸锌和醋酸钴为原料,采用溶胶-凝胶法制备Zn0.95Co0.05O粉体,研究了煅烧温度对其物相组成、晶体结构和磁学性能的影响。结果表明:随着煅烧温度的升高,更多的Co2+进入ZnO晶格中,取代纤锌矿结构中的Zn2+进入四面体配位环境;煅烧温度为800℃时得到具有单一纤锌矿结构的Zn0.95Co0.05O粉体;所有的粉体均表现为顺磁性,随着煅烧温度的升高,顺磁性增强。     

溶胶凝胶法合成Dy~(3+)离子掺杂的二氧化锆及其发光特性(英文)

采用溶胶凝胶法合成 Dy3+离子掺杂的单斜与正交的二氧化锆晶体,研究了结晶温度、时间、Dy3+离子浓度对氧化锆结构的影响。比较研究了 Dy3+离子在不同结构二氧化锆中的光谱特性,从结果看出,Dy3+离子可作为荧光探针反映二氧化锆的晶体结构。     

Spark plasma sintering of ZrB2 powders synthesized by citrate gel method

The densification behavior of nanocrystalline zirconium diboride (ZrB₂) powders with nickel (5 vol%) is reported by spark plasma sintering (SPS) technique. SPS experiments were performed at 1600 and 1900 °C with 65 MPa pressure and 1 min holding time. A maximum relative density around 95% was obtained after SPS processing of ZrB₂ at 1900 °C while the density of ZrB₂ sample sintered at 1600 °C reached 88% of the theoretical density. Hardness and fracture toughness values are 11 GPa and 4.11 MPa m^1/2 for the sample sintered at 1600 °C and 13.7 GPa and 2.65 MPa m^1/2 for the sample sintered at 1900 °C, respectively.     

Preparation and characterization of yttrium iron garnet (YIG) nanocrystalline powders by auto-combustion of nitrate-citrate gel

The nitrate–citrate gel exhibits auto-catalytic behavior, which can be used to synthesize nanocrystalline YIG powders. In this study, yttrium iron garnet (Y₃Fe₅O₁₂) nanocrystalline powders were prepared by a sol–gel auto-combustion process. The influence of metal nitrates to citric acid molar ratio (MN/CA) of the precursor solution on the combustion behavior and crystallite size of synthesized powders was investigated by scanning electron microscopy (SEM), thermal analyses (DTA/TGA) and X-ray diffraction (XRD). The results show that with increasing MN/CA value, the combustion rate increases and the single-phase YIG forms at a higher temperature. The crystallite size of the single phase YIG prepared with different MN/CA values and calcined at 800 °C for 3 h are in the range of 38–70 nm. In addition, the crystallite size of the powders increased with increasing the calcination temperature.     

机械合金化制备Ni-W(B)非晶-纳米晶的粉末特性

利用机械合金化(MA)制备了Ni-20.7W和Ni-17.9W-27B(at%)非晶-纳米晶粉末,分别采用扫描电镜(SEM)和X射线衍射(XRD)仪分析了不同球磨时间粉末的微观形貌和结构参数,探讨了B的添加对非晶化过程的影响。研究结果表明:MA过程中,Ni-20.7W样品没有明显发生非晶化,而Ni-17.9W-27B样品在40 h时发生了非晶化,说明B提高了Ni-W合金体系的非晶化形成能力;非晶化过程为W/B首先固溶于Ni中生成Ni(W,B)过饱和固溶体,然后转变为非晶;Ni-20.7W样品球磨30 h后Ni的晶粒尺寸为32.9 nm,晶格畸变为0.48%,而Ni-17.9W-27B样品球磨10 h后的晶粒尺寸为9 nm,晶格畸变为0.62%。     

Crystallization, morphology and luminescent properties of YAG：Ce^3＋ phosphor powder prepared by polyacrylamide gel method

A novel synthesis process, based on the polyacrylamide gel method, was used to prepare Ce-doped YAG phosphor powders. Effects of heat treatment parameters, temperature and holding time, the fluxes, and atmosphere on microstructure and particle morphology as well as luminescent properties of YAG：Ce^3＋ phosphor powders were studied by X-ray powder diffractometry, scanning electron microscopy, and fluorescence spectrophotometry. The results show that the formation temperature （1 000 ℃） of pure YAG phase is significant low when being synthesized by the polyacrylamide gel method, compared with solid-state reaction. For luminescent properties, the intensity of emission of YAG：Ce^3＋ phosphor increases steadily with increasing temperature from 900 ℃ to 1 300 ℃ and prolonging holding time from 100 min to 400 min. But blue shift phenomenon is observed for 400 min calcination Fluxes as BaF2 and H3BO3 can enhance the intensity of emission of phosphor due to the improvement of crystallization of YAG and the stabilization of trivalence cerium ion in YAG host lattice at high temperature. Weak reduction atmosphere can contribute to improvement of the emission intensity of YAG：Ce^3＋ phosphor powders.     

Microstructure and mechanical properties of rapidly solidified Mg alloy powders compacted by magnetic pulsed compaction (MPC) method

Gas atomized Mg–Zn_4.3Y_0.7 (at%) alloy powders were consolidated by using a magnetic pulsed compaction (MPC) process, and obtained by rapid solidification not to lose the fine microstructure during the generally conducted thermal consolidation process. MPC is known as one of the most rapid pressing process with the GPa range. The effects of the discharging voltage and thermal pressure on the microstructure, hardness, density and compressive strength were investigated. The experimental results showed that the density increased with increasing the voltage although the sample MPCed still consists of pores especially between the powder boundaries even at the maximum pressure of this investigation. The density was improved further up to 96% to the cast value by the MPC at the maximum voltage. Uniform and fine microstructure formed in the alloy powders as atomized was almost maintained even after the thermal MPC.     

Microstructures of nanosized alumina powders synthesized by sol-gel method

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Precipitation of Cr-rich phases in rapidly solidified Ni–20Al–8Cr (at.%) powders

The evolution of the microstructure in rapidly solidified Ni–20.9Al–8Cr–0.49B (at.%) powders after different continuous and isothermal heat treatments at temperatures up to 1100 °C has been studied by electron microscopy and microanalysis. Powders in the rapidly solidified condition have a dendritic microstructure consisting of Ni₃Al dendrites and a NiAl phase in the interdendritic regions. Chromium is in solid solution in both phases. This microstructure is stable when heating at 10 K min⁻¹ up to 750 °C. When the powders are heated up to 950 °C, partial dissolution of the NiAl phase and the precipitation of very small chromium-rich particles take place.The microstructure of the powders after annealing at temperatures between 750 and 1100 °C for different times is characterised by the dissolution of the β-NiAl phase and the simultaneous precipitation of various Cr-rich phases. α-Chromium, the metastable X-phase, and dark polygonal Cr₅B₃ precipitates have been identified.The segregation of chromium and boron in the form of borides removes these elements from the intermetallic matrix, so the content of both elements should be optimised to preserve their beneficial influence on the ductility of the γ′-Ni₃Al phase.     

机械球磨Ti_(50)Al_(50)复合粉的压制特性

研究了机械球磨Ti50 Al50 复合粉的组织与压制特性。结果表明 ,球磨导致粉末硬度增加 ,压制特性变差 ,这是由于球磨使层片结构细化 ,Ti和Al组元晶体缺陷增加和晶粒细化造成的 ;但球磨 3h形成纳米晶复合粉后 ,尤其是在球磨 7.5h开始发生非晶转变后 ,进一步球磨 ,粉末压制特性变化并不明显     

配合-共沉淀法制备锑掺杂二氧化锡(ATO)粉

在充分回收含锡阳极泥有价金属的基础上,采用从锡锑二次资源中直接提取的高纯氯锡酸铵和氯氧锑为原料,合成了性能优良的纳米级锑掺杂二氧化锡(ATO)粉.针对液相共沉淀法制备ATO的过程中,锡和锑的水解不同步从而未能实现真正共沉淀掺杂的问题,以(NH4)2SnCl6和Sb4O5Cl2为原料,采用配合-共沉淀法,考察了反应过程中的pH、反应温度、掺锑浓度、煅烧温度、前驱体洗涤次数和分散剂种类等对ATO粒度和形貌的影响,确定了最优化条件,即:滴定终点pH=3,反应温度60℃,锑掺杂浓度10%(质量分数),热处理温度600℃,前驱体洗涤次数为6次,采用分散剂c,并进行了实验验证.