化学还原法制备微纳米银粉

采用液相化学还原法,以PVA(聚乙烯醇)作分散剂,硼氢化钠作还原剂,硝酸银为前驱体,制备分散性相对较好的微纳米级银粉。探究银离子浓度、还原剂浓度、分散剂用量和反应温度等因素对银粉品质的影响规律,通过调节上述因素对银粉粒径和分散性进行调控。并运用XRD(X射线衍射仪)、SEM(扫描电子显微镜)和UV-Vis(紫外可见分光广度计)对银颗粒的晶体物相结构、表面形貌和光学特性进行表征。结果表明,当反应温度为40℃、银离子浓度为0.2 mol/L、硼氢化钠浓度为0.2 mol/L、硝酸银与PVA质量比为0.6时,可以制备出分散性良好、纯度较高的银粉,银粒子平均粒径在120 nm左右。     

电子浆料用微米级银粉的分步还原制备及其晶体生长特征

在水溶液中以抗坏血酸为还原剂、PVP为分散剂,分步还原硝酸银制备出微米级银粉.采用SEM和XRD等表征手段,考察银粉颗粒随反应原料加入速度及硝酸银加入量的生长规律,并借助AFM对其生长机理进行了研究.结果表明,当反应原料滴加速度为1 mL/min时,可获得粒径为1.8 μm、形貌规则的单分散性球形银粉颗粒,且其粒径随硝酸银加入量呈近线性增长;银粉晶粒以层状方式生长、台阶簇方式推进,属Kossel-Stranski二维成核.     

采用硫酸作为稳定剂制备微米级球形银粉

采用抗坏血酸作为还原剂,硫酸作为稳定剂,在高速搅拌、室温的条件下还原硝酸银溶液制备微米级球形银粉.考查了硫酸用量、反应温度和添加高分子保护剂对银粉的微观形貌的影响.通过SEM、EDX和XRD对制备的银粉进行了表征分析,结果表明:制备的超细银粉为类球形,粒径较为均一,粒径范围为1~2.0μm可调;减小或增大硫酸用量都将导致银粉粒径变小;升高温度或者添加适量的N-甲基吡咯烷酮也可减小粒子粒径.     

化学还原法原位制备石墨烯/纳米银复合粉体及其导电性能

以水合肼为还原剂,PVP为分散剂,在反应温度为60℃,p H为6条件下同时还原氧化石墨烯和硝酸银,原位制备石墨烯/纳米银复合粉体。通过扫描电镜、X射线衍射、红外吸收光谱和拉曼光谱等手段研究溶液中硝酸银的质量浓度对石墨烯/纳米银复合粉体形貌与结构的影响。用石墨烯/纳米银复合粉体替代部分微米银粉制备低温固化导电浆料,对其导电性能进行研究。结果表明:银纳米粒子分布于石墨烯片层之间。当反应溶液中硝酸银的质量浓度为0.75 g/L,氧化石墨烯质量浓度为0.25 g/L时,获得分散性好,粒径均匀的石墨烯/纳米银复合粉体,且负载在石墨烯片层上的银纳米粒子的粒径集中在100 nm左右。用石墨烯/纳米银复合粉体替代4%微米银粉制备导电浆料,浆料的体积电阻率为1.8×10-5Ω·cm,与未添加石墨烯/纳米银复合粉体的导电浆料相比,电阻率降低61.7%。     

截断流管式反应器中亚微米球形银粉的制备

研究了以银氨溶液和抗坏血酸溶液为原料,在截断流管式反应器中制备亚微米球形银粉。试验验证了在截断流管式反应器中还原制备亚微米球形银粉的可控性,考察了反应物浓度、搅拌速度、反应时间、温度等条件对银粉颗粒及形貌的影响。结果表明:在适宜条件下,用银氨溶液和抗坏血酸溶液可制备亚微米级银粉,所得银粉分散性好,主要约0.3μm。该方法简单易操作,银粉颗粒均匀可控。     

电极银浆用微纳米银粉的制备与性能研究

以硝酸银为前驱体, 抗坏血酸为还原剂, 单宁为分散剂, 采用液相化学还原法制备了微纳米超细银颗粒。通过X射线衍射仪、扫描电子显微镜、激光粒度分析仪、振实密度仪及太阳能性能测试仪等设备研究了反应物浓度、分散剂剂量、pH值等工艺参数对银颗粒形貌、平均粒径及振实密度的影响。结果表明, 当硝酸银浓度为0.1mol·L-1, 抗坏血酸浓度为0.1mol·L-1, 单宁浓度为0.01mol·L-1, pH值为1, 反应温度为25℃时, 能够获得分散性良好的球状银颗粒; 将平均粒径为1.16μm和0.66μm的两种银粉按照一定质量比进行混合, 制备得到的混合银粉最高振实密度可达到6.1g·mL-1; 通过研究基于不同振实密度银粉的银电极表面形貌和电池性能, 可以得出基于振实密度6.1g·mL-1混合银粉所制的银电极相对密度最好, 太阳能电池的光电转换效率最高, 达到17.16%。     

分步还原法制备电子浆料用球形银粉及其形貌与粒径

采用分步还原法制备银粉,即以硝酸银为银源,硼氢化钠为还原剂制备出晶种,然后还原硝酸银制备银粉,通过扫描电镜(SEM)和X射线衍射分析,研究还原剂的种类、晶种数量、溶液体系中还原剂的浓度及硝酸银浓度对银粉形貌和粒径的影响。结果表明:采用强还原剂制备的银粉团聚严重,粒径不均匀;当体系中还原剂浓度太小(0.05 mol/L)或太大(0.25 mol/L)时,银粉粒径很小,团聚严重;当加入的晶种数量较少时(1 m L),银粉粒径不均匀,而当晶种数量较大(3 m L)时,银粉粒径很小,团聚严重;随硝酸银的浓度从0.05 mol/L增加到0.20 mol/L,银粉粒径先增大后减小。采用还原性较弱的抗坏血酸为还原剂,晶种体积为2 m L,体系中C6H8O6和Ag NO3的浓度均为0.15 mol/L时,制备出表面光滑、分散性较好、粒径均匀、粒度为1.5μm的球形银粉。     

工艺条件对硝酸银溶液雾化热分解制备超细银粉的影响

以AgNO₃溶液为原料、柠檬酸为添加剂,在空气气氛下采用溶液雾化热分解法制备超细银粉.采用扫描电镜、激光粒度仪、振实密度测试仪、X射线衍射仪等对银粉进行了表征,系统地研究了反应温度、硝酸银溶液浓度、硝酸银溶液pH值、压缩空气流量、柠檬酸用量等工艺条件对产物银粉形貌、振实密度和平均粒径的影响.结果表明:在反应温度为700 ℃、硝酸银溶液浓度为2.0 mol/L、柠檬酸的添加量为2.5 %（摩尔比）、压缩空气流量为1.0 m3/h、硝酸银溶液pH值为6.0的条件下,可制备得到物相单一、表面光滑、分散性好的球形银粉,银粉的振实密度为4.24 g/cm3,平均粒径为3.16 μm.      

六方片状银粉的合成

以硝酸银为前驱物,过氧化氢为还原剂,在乙二醇(或乙醇)介质中,有分散保护剂PVP存在的情况下,通过控制H2O2/NH3和NH3/Ag不同的比例(摩尔比,MR),合成分散的球状单颗粒和六方片状银粉。本文着重考察了NH3/Ag、H2O2/Ag以及H2PtCl6/Ag对片状六方晶体银粉形成的影响。结果表明,在NH3/Ag<3 5情况下,得到的是<1 0μm的球状银粉。当NH3/Ag>3 5,且H2O2/NH3≥1时,得到厚度<0 1μm、最大投影面的长度为0 2～0 5μm的六方片状单晶体银粉。H2PtCl6是形成片状银的必要与关键条件,但不是充分的条件,PVP是形成单分散粒子的决定性因素。     

化学还原制备太阳能电池正极浆料用超细银粉

采用化学还原法制备太阳能电池正极浆料用超细银粉,通过扫描电镜(SEM)、激光粒度分析仪和能谱仪分析银粉的形貌、粒度及纯度,研究还原剂和分散刺的种类和用量,以及反应温度、溶液pH值等工艺条件对银粉粒度及形貌的影响.结果表明,采用水合肼作还原剂、明胶作分散剂时,可以得到分散性好、粒度约0.3μm的球状超细银粉;明胶的最佳加入量m(gelatin)为硝酸银质量m(AgNO3)的0.02倍,水合肼溶液和硝酸银溶液的最佳浓度分别为1.5 mol/L和0.5 mol/L;还原温度和溶液pH值对银粉粒度影响较大,当反应温度为20℃,硝酸银溶液pH值7.5时得到粒度均匀、形状规则的超细银粉.将该银粉制成浆料,印刷在硅片上,使用四探针测试仪测得烧结膜的方阻小于5mΩ/□,可满足太阳能电池的电性能要求.     

Contact precipitation of silver on copper powder

The processing characteristics of articles made from copper powder can be improved by alloying the copper powder with additions of silver (up to 0.2%). The simplest and most economical method is deposition of silver onto copper powder particles by contact exchange. We have studied the effect of different types of electrolytes (nitrate, pyrophosphate, sulfosalicylate, sulfite, ferricyanide, cyanide thiocyanate, and thiocyanate) on the kinetic characteristics of the electrode processes. We have done structural studies of copper powder alloyed with silver. We have determined the bulk (as-poured) density of the powders after cementation, and also the density, shrinkage, electrical resistance, and hardness of specimens prepared by the traditional procedure from the alloyed powders. In most of the studied systems, the cementation process occurs with diffusion control of the cathode reaction. However, this does not lead to visible formation of growths and dendrites of silver on the surface of the copper particles. According to x-ray phase analysis results, during cementation a solid solution of copper in silver is formed on the surface of the particles. After sintering the green compacts, the alloy is homogenized with formation of a solid solution of silver in copper. The nature of the electrolyte markedly affects the properties of the Cu−Ag material. In some cases, the hardness and electrical conductance of the specimens increase simultaneously. Technological and economic considerations lead to choosing cyanide thiocyanate electrolyte as the best for alloying copper powder with silver. Urals State Technical University; Institute of High-Temperature Electrochemistry, Urals Branch, Russian Academy of Sciences, Ekaterinburg. Translated from Poroshkovaya Metallurgiya, Nos. 7–8(408), pp. 22–29, July–August, 1999.     

Mechanism of zeolite A nanocrystal growth from colloids at room temperature

The formation and growth of crystal nuclei of zeolite A from clear solutions at room temperature were studied with low-dose, high-resolution transmission electron microscopy in field emission mode and with in situ dynamic light scattering. Single zeolite A crystals nucleated in amorphous gel particles of 40 to 80 nanometers within 3 days at room temperature. The resulting nanoscale single crystals (10 to 30 nanometers) were embedded in the amorphous gel particles. The gel particles were consumed during further crystal growth at room temperature, forming a colloidal suspension of zeolite A nanocrystals of 40 to 80 nanometers. On heating this suspension at 80 degrees C, solution-mediated transport resulted in additional substantial crystal growth.     

Structural transformations taking place in the surface layers of very fine BaFe12O19 powder particles

Conclusions During the comminution of powders of the ferrite BaFe₁₂O₁₉ in an attritor mechanical energy is expended in the disintegration of particles, formation of defects, and plastic deformation of the crystal lattice. The comminution of powders in a vibratory mill is accompanied by the formation of well-developed surface layers on particles, which are characterized by a high degree of defectiveness and crystal lattice disorder. The hypothesis is advanced that during prolonged comminution of powders in a vibratory mill the surface layers of particles can undergo structural transformations, which promote the formation of stable oxygen-containing phases at crystallite boundaries.Translated from Poroshkovaya Metallurgiya, No. 6(258), pp. 50–55, June, 1984.     

Microstructural features and heat flow analysis of atomized and spray-formed Al-Fe-V-Si alloy

Microstructural features of rapidly solidified powders and preforms of Al₈₀Fe₁₀V₄Si₆ alloy produced by spray forming process have been studied. The atomization and spray deposition were carried out using a confined gas atomization process and the microstructural features were characterized using scanning electron microscopy and transmission electron microscopy (TEM) and X-ray diffraction (XRD) techniques. The microstructure of a wide size range of atomized powders invariably revealed cellular and dendritic morphology. The extent of dendritic region and the dendritic arm spacing were observed to increase with powder particle size. The TEM investigations indicated the presence of ultrafine second-phase particles in the intercellular or interdendritic regions. In contrast, the spray deposits of the alloy showed considerable variation in microstructure and size and dispersion of the second-phase particles at specific distances from the deposit-substrate interface and the exterior regions of the deposit. Nevertheless, considerable homogeneity was observed in the microstructure toward the center of the spray deposit. The formation and distribution of a cubic phase α-Al(Fe,V)Si has been characterized in both atomized powders and spray deposits. A one-dimensional heat flow model has been used to analyze the evolution of microstructure during atomization and also during spray deposition processing of this alloy. The results indicate that thermal history of droplets in the spray on deposition surface and their solidification behavior considerably influence the micro-structural features of the spray deposits.     

Electron microscope characterization of AgBr heterojunctions with silver carboxylates and their influence on the morphology of developed silver particles in thermally developed photomaterials

Silver halide crystals formed during in situ treatment of silver stearate crystals with various halidizing agents are observed by scanning and transmission electron microscopy to form on the lateral edges of the silver carboxylate crystals. The location of the silver halide phase on the crystal edge is dictated by the anisotropic structure of the silver stearate crystal lattice, specifically, the layered structure in which silver ion layers are separated by long-chain hydrocarbon groups. The formation of AgBr on the lateral faces of these crystals is proposed to be typical not only of the formation of silver halide on silver stearate but also for all silver carboxylates of the general formula [AgCnH2(n-1)O2]2 when the crystals of these silver carboxylates have anisotropic, layered structures. The silver bromide/silver carboxylate heterojunction in an in situ system has been clearly observed by transmission electron microscopy. The heterojunction is comprised of a distorted silver carboxylate lattice, which accommodates the misalignment between the AgBr and [Ag(O2CR)]2 crystal lattices. The nature of heterojunction between the AgBr and the silver carboxylate when the AgBr is prepared separately from the preparation of the silver carboxylate differs from the in situ heterojunction. In this case, a layered compound, proposed to have a Ag1-xNaxSt composition, forms between the AgBr and the silver stearate which is a unique feature of this interface. The differences in the structure of interfaces formed between the silver halide and the silver fatty acid complex result in different silver particle morphologies during thermal development of exposed photothermographic films. The developed silver is generally filamentary when the photothermographic material contains silver halide prepared by the in situ exchange reaction between silver carboxylate and a brominating agent. If the photothermographic material is prepared from previously synthesized silver halide crystals, the preformed AgBr route, the developed silver generally crystallizes as dendritic crystals.     

Growth direction of columnar crystals solidified in flowing melt

Aluminum-copper alloys containing 0.5–8.8 wt% Cu were unidirectionally solidified. Columnar crystals were grown in flowing melts at flow rates ranging from 4 to 90 cm/s, and the deflection angle of the crystal growth direction in the upstream direction was measured as functions of flow rate and copper content. The columnar crystals originated from nuclei or solid particles with the most suitable crystallographic orientation for growing in flowing melt. The growth direction of the columnar dendrites was nearly equal to that of the columnar grains comprising the columnar dendrites. The deflection angle for the columnar grains increased only slightly with an increase in flow rate or copper content within the ranges investigated, while the inclination angle of the growth direction of columnar dendrites from the [100] direction increased with an increase in flow rate and with a decrease in copper content.     

An analysis of the microstructure of rapidly solidified Al-8 wt pct Fe powder

Rapidly solidified powders of Al-8 wt pct Fe exhibit four distinct microstructures with increasing particle diameter in the size range of 5 μm to 45 μm: microcellular α-Al; cellular α-Al; a-Al + Al₆Fe eutectic; and Al₃Fe primary intermetallic structure. Small powder particles (~10 μm or less) undercool significantly prior to solidification and typically exhibit a two-zone microcellular-cellular structure in individual powder particles. In the two-zone microstructure, there is a transition from solidification dominated by internal heat flow during recalescence with high growth rates (microcellular) to solidification dominated by external heat flow and slower growth rates (cellular). The origin of the two-zone microstructure from an initially cellular or dendritic structure is interpreted on the basis of growth controlled primarily by solute redistribution. Larger particles experience little or no initial undercooling prior to solidification and do not exhibit the two-zone structure. The larger particles contain cellular, eutectic, or primary intermetallic structures that are consistent with growth rates controlled by heat extraction through the particle surface (external heat flow).     

铜电极表面电火花沉积TiB2/TiC复层涂层的微观结构及成因

采用电火花沉积工艺将烧结二硼化钛和碳化钛涂覆到铜电极表面形成TiB2/TiC复层涂层,通过扫描电镜(SEM)结合能谱分析研究涂层和界面的微观结构及成分。结果表明,涂层电极横截面分为多个区域,涂层内有裂纹,与基体无明显分层;基体热影响区出现细晶和柱状晶,主要化学成分为铜。细晶区的形成主要是电火花放电过程中快速冷凝时高的形核率所致,并可能与电火花放电的脉冲能量有关。柱状晶区主要是因单向散热引起晶体的定向生长而产生的。     

Influence of pH on Morphology and Formation Mechanism of CeO2 Nanocrystalline

Nanoparticles of cerium oxide were prepared by common precipitation method using cerium nitrate solution and ammonia reagent. Cerium oxide particles with different morphologies were synthesized through adjusting pH values of the solution. TEM and BET results showed that spherical crystal was gained in acid solution, with the specific surface of 148. 1944 m2·g^-1. The cerium oxide appeared in the form of spherical and rod-like grains under neutral condition, and the specific surface changed to 114.7975 m^2·g^-1. Moreover, in alkaline solution, cerium oxide powders were exhibited in rod-like form with the specific surface of 106.2465 m^2·g^-1. Precipitation formation mechanism of different morphologies was also discussed, which followed decomposition precipitation mechanism and topology reaction mechanism in acid and alkaline solution, respectively.     

氩气雾化高温合金粉末的凝固组织特征

为深入了解高温合金粉末粒度细化对粉末涡轮盘性能的影响,对不同尺寸氩气雾化高温合金粉末的凝固组织特点进行了分析和研究.结果表明:AA粉表面和内部凝固组织主要为树枝晶和胞状晶组织,晶界和枝晶间分布少量富Ti、Nb的MC型碳化物.随着粉末尺寸的减小,冷却速率增大,组织从树枝晶向胞状晶转变,基体γ相晶面间距和点阵常数增加.小尺...