氢还原法制备Mo60Cu40纳米复合粉

以(NH4)6Mo7O24·2H2O和CuSO4·5H2O(Mo:Cu=60:40,质量比,下同)为原料,采用化学共沉淀制备Mo-Cu复合氧化物粉末,再经过氢还原得到Mo-Cu复合物纳米粉末。结果表明:化学共沉淀的条件是反应温度为(50±5)°C,pH值为(5.1±0.1),陈化时间为(8±1)h;Mo-Cu复合氧化物粉末粒度为20nm;氢还原温度为650°C,Mo-Cu复合物纳米粉末粒度小于100nm。     

Preparation of fine nickel powders via reduction of nickel hydrazine complex precursors

Fine nickel(Ni) powders with controllable particle sizes were synthesized via the reduction of nickel hydrazine complex precursors of pure [Ni(N2H4)2]Cl2 and a mixture of [Ni(N2H4)2]Cl2 and [Ni(N2H4)3]Cl2 in aqueous solution. The mechanism of the formation of metallic Ni powders experiences the reduction of nickel hydroxide by hydrazine released from the ligand exchange reaction between nickel hydrazine complex and NaOH. In comparison with the method of preparing Ni powders from nickel salts, the method of making Ni powders via the reduction of nickel hydrazine complex precursors shows the advantages of using half dosage of hydrazine for complete reduction of nickel ions in solution, and the obtained Ni particles show less agglomeration and better dispersibility. Moreover, the average particle size of nickel powders can be controlled from 180 to 260 nm by adjusting the reaction molar ratio and concentration.     

钛基镍钴合金电极的制备及析氢性能

目的降低电极的析氢过电位,提高析氢性能,从而降低电解水制氢的成本,促进氢储能技术的发展。方法通过异相共沉积法,制备了镍钴合金电极。利用场发射扫描电镜(SEM)、电化学交流阻抗(EIS)对纯镍电极及镍钴合金电极进行表征,采用阴极极化曲线(LSV)探究了电沉积液中Ni/Co元素的比例、电沉积电位及电沉积时间对镍钴合金电极析氢性能的影响。结果 SEM结果揭示了纯镍电极及镍钴合金电极表面分别是粒径约为100 nm左右的镍颗粒和镍钴颗粒。EIS结果说明了镍钴合金电极的导电性能优于纯镍电极。此外,纯镍电极、镍钴合金电极的阴极极化曲线测试表明在电流密度为30 mA/cm~2时,镍钴合金电极的析氢过电位比纯镍电极降低55 mV,降低了近20%。结论通过异相共沉积法制备镍钴合金电极,制备方法简单、方便、快速,其析氢性能优于纯镍电极。镍钴合金电极的最优制备工艺条件为:NiSO_4·6H_2O 27 g/L,CoSO_4·7H_2O_3 g/L,H_3BO_3 10 g/L,Na_2SO_4 10 g/L,柠檬酸10 g/L,十二烷基硫酸钠0.1 g/L,pH值4.0,电沉积电位-1.3 V,电沉积时间10 s。     

镀液组成对碱性体系Zn-Ni合金镀层性能的影响

目的 发现最优工艺条件,了解Zn-Ni电沉积机理。方法 通过场发射电镜分析、能谱分析以及电化学分析等方法,研究以一种胺羧多官能团配体为Ni²⁺络合剂的碱性锌酸盐电解液体系中,锌/镍离子物质的量之比与锌镍离子总浓度对镀层的光泽度、镍含量、耐蚀性、表观质量和微观结构的影响。结果 锌/镍离子物质的量之比增加会使得镀层镍含量降低,最后稳定在15%~19%,镀层微观结构由晶粒细致平滑型转化为粗大疏松型。物质的量之比为1.9时,镀层的腐蚀电流最小。锌镍离子总浓度增加会使得镀层镍含量缓慢减小,镀层微观结构由晶粒细致疏松型转化为细致紧密型,最后又转变为粗大疏松型,镀层的腐蚀电流先减小后急剧增大,即镀层的耐蚀性先增加后急剧降低。结论 在锌/镍离子物质的量之比为1.9、锌镍离子总浓度为0.12 mol/L时,所得镀层的综合性能最好。镀层锌/镍含量变化趋势符合Brenner吸附膜理论。     

Thermodynamic analysis on preparation of fibrous NiO precursor powders with oxalate precipitation process

According to the principles of simultaneous equilibrium and mass balance, a series of thermodynamic equilibrium equations of Ni（ Ⅱ）-C2 O4^2--NH3-NH4^＋-H2O system at ambient temperature are deduced theoretically and the logarithm concentration versus pH value（lg[Ni^2＋ ]r-pH） diagrams at different solution compositions are drawn. The results show that when pH is above 8.0, nickel ions coordinate with ammonia, the precipitation proceeds slowly accompanying with the release of nickel ions from the multi-coordinated Ni（NH3）n^2＋ （n= 1, 2,…, 6） and the morphology of NiO powder precursor is fibrous; when pH is below 8.0, nickel ion directly reacts with C2O4^2- and the morphology of NiO powder precursor is of cubic-shape. Some experiments were made to confirm the relation between the total concentration of nickel ion and pH. It is shown that the thermodynamic mathematical model is correct and the calculated values are basically accurate.     

单分散近球形和片状金粉的制备及表征

以HAuCl4·4H2O为前驱体,抗坏血酸(VC)为还原剂,线性聚乙烯亚胺(L-PEI)为表面活性剂在水相中制备了单分散的近球形和片状金粉.采用SEM、XRD和激光粒度分析仪对金粉的形貌、粒径、结晶和分散性进行了测试和表征.研究了还原剂和金前驱体的摩尔比、L-PEI浓度、温度及反应溶液的pH对近球形和片状金粉的形貌和粒径大小的影响.给出了制备微米级近球形和片状金粉的反应条件,同时也提出了近球形和片状金粉的成核和晶核生长的可能解释.     

Preparation of Flower-Like Ni Particles by the Water-Ethanol-Ammonia Liquid Phase Synthesis and Thermal Decomposition Method

在水-醇-氨液相体系中,沉淀合成了酒石酸镍纳米晶片和花状酒石酸镍颗粒。以花状酒石酸镍颗粒为前驱体,在CO2气氛中,于380和420 °C条件下,通过热分解过程分别制备花状金属镍颗粒。实验样品采用IR,DSC-TG,XRD和SEM测试技术进行分析,测试结果表明:液相沉淀法制备的样品为纯相的酒石酸镍,在1.0 mol的酒石酸镍中含有约2.5 mol的结晶水,花状的酒石酸镍颗粒直径约40 μm,纳米晶片花瓣的厚度约0.1 μm;热分解制备的具有银白光泽的粉体为纯相的具有面心立方结构的金属镍粉,花状金属镍颗粒直径约10 μm,纳米晶片花瓣的厚度约0.3 μm。     

PS 微球的制备及表面镀镍工艺研究

以聚乙烯吡咯烷酮为分散剂,偶氮二异丁腈为引发剂,无水乙醇为分散介质,通过分散聚合,制备出表面光滑、分散均匀的聚苯乙烯(PS)微球。在PS微球表面化学镀Ni,制得具有较好导电性能的PS/Ni复合粒子。研究了PS微球表面镀Ni前后的表观形貌及晶相变化,并分析了制备工艺对复合粒子导电性能的影响。分析表明,PS微球表面镀Ni的优化工艺为:PS/NiCl2·6H2O质量比4∶7,络合剂用量2 g,NH3·H2O用量30mL。     

EFFECT OF PRECIPITANT ON THE PROPERTIES OF ULTRAFINE YTTRIA POW DER PRODUCED BY PRE CIPITATION METHOD

１．ＩｎｔｒｏｄｕｃｔｉｏｎＨｉｇｈｒｅａｃｔｉｖｉｔｙａｎｄｇｏｏｄｐｈｙｓｉｃａｌａｎｄｃｈｅｍｉｃａｌｈｏｍｏｇｅｎｅｉｔｙｏｆｕｌｔｒａｆｉｎｅｃｅｒａｍｉｃｐｏｗｄｅｒｓｅｎａｂｌｅｓｄｅｎｓｉｆｉｃａｔｉｏｎｏｆｔｈｅｍａｔｅｒｉａｌｓａｔｌｏｗｅｒｔｅｍｐｅｒａｔｕｒｅｓａｎｄｍｉｃｒｏｓｔｒｕｃｔｕｒｅｃｏｎｔｒｏｌｏｎａｌｅｖｅｌｏｆ１～１００ｎｍ〔１２〕．Ｙｔｔｒｉｕｍｏｘｉｄｅｉｓｏｎｅｏｆｔｈｅｍｏｓｔｉｍｐｏｒｔａｎｔｃｅｒａｍｉｃｍａｔｅｒｉａｌｓａｎｄｉｓｕｓｅ…     

微反应器中LaPO4:Ce3+, Tb3+纳米发光颗粒的制备及表征

以Ln(NO3)3·6H2O(Ln=Ce,Tb)及NaH2PO4·2H2O为原料,乙二醇为溶剂,在微反应器中合成了铈铽共掺杂磷酸镧(LaPO4:Ce3+,Tb2+)纳米发光颗粒.采用X射线衍射仪(XRD)、透射电子显微镜(TEM)和荧光光谱仪对LaPO4:Ce3+,Tb3+纳米发光颗粒的物相、微结构和荧光性能进行了表征.结果表明:LaPO4:Ce3+,Tb3+纳米发光颗粒具有六方晶系的晶体结构,形貌不规则,粒度为20 nm左右、窄的粒度分布的纳米颗粒,并且颗粒分散均匀,具有较强的荧光性能.     

Ni/Ti(C,N)包覆粉及其金属陶瓷的制备

采用非均相沉淀-热还原法制备Ni/Ti(C,N)包覆粉,并用该包覆粉经真空烧结制得金属陶瓷。利用扫描电镜、电子能谱、X-射线衍射等手段研究包覆粉的结构形貌及烧结后的微观组织与性能。结果表明:非均相沉淀过程中,非晶态的NiCO3·2Ni(OH)2·2H2O在Ti(C,N)颗粒表面成核并生长;经热还原过程后,NiCO3·2Ni(OH)2·2H2O分解并完全还原成Ni,Ni的平均晶粒尺寸约为50nm;采用包覆粉为原料制备金属陶瓷,有效改善了硬质相和粘结相的分布均匀性,但包覆粉烧结过程中存在晶粒长大现象;金属陶瓷的相成分为纯净的Ti(C,N)与Ni两相;金属陶瓷的综合性能相对于传统工艺制得的金属陶瓷有一定提高。     

复合金属掺杂的LiFePO4/C复合材料的制备与电化学性能研究

以超声波辅助沉淀法合成的纳米级球形FePO4·2H2O为原料,采用碳热还原法制备了复合金属掺杂的LiFePO4/C复合材料。通过X射线衍射(XRD),扫描电镜(SEM),恒电流充放电测试,循环伏安和交流阻抗测试表征了FePO4·2H2O和LiFePO4/C的物相、结构和电化学性能。结果表明,溶液浓度为0.1 mol/L时制备的FePO4·2H2O为分布均匀的纳米级球形颗粒。复合金属掺杂显著提高了LiFePO4的放电比容量,Ni和Nb复合掺杂的LiFePO4/C复合材料表现出了最佳的电化学性能,0.1 C倍率条件下首次放电容量158.8 mAh/g,1 C倍率下首次放电容量150.2 mAh/g,100次循环后容量保持率分别为98.30%和97.8%。Ni和Nb复合掺杂后提高了LiFePO4的锂离子扩散速率和电导率。     

Separation and Precipitation of Nickel from Acidic Sulfate Leaching Solution of Molybdenum-Nickel Black Shale by Potassium Nickel Sulfate Hexahydrate Crystallization

Nickel was separated and precipitated with potassium nickel sulfate hexahydrate [K₂Ni(SO₄)₂·6H₂O] from acidic sulfate solution, a leach solution from molybdenum-nickel black shale. The effects of the potassium sulfate (K₂SO₄) concentration, crystallization temperature, solution pH, and crystallization time on nickel(II) recovery and iron(III) precipitation were investigated, revealing that nickel and iron were separated effectively. The optimum parameters were K₂SO₄ concentration of 200 g/L, crystallization temperature of 10°C, solution pH of 0.5, and crystallization time of 24 h. Under these conditions, 97.6% nickel(II) was recovered as K₂Ni(SO₄)₂·6H₂O crystals while only 2.0% of the total iron(III) was precipitated. After recrystallization, 98.4% pure K₂Ni(SO₄)₂·6H₂O crystals were obtained in the solids. The mother liquor was purified by hydrolysis-precipitation followed by cooling, and more than 99.0% K₂SO₄ could be crystallized. A process flowsheet was developed to separate iron(III) and nickel(II) from acidic-sulfate solution.     

Synthesis and characterization of CoFe2O4 magnetic particles prepared by co-precipitation method: Effect of mixture procedures of initial solution

CoFe₂O₄ magnetic particles were prepared by co-precipitation method in 60 °C homogeneous aqueous solution without any subsequent heat treatment. It was found that the mixing procedure and Fe²⁺/Fe³⁺ ratio of initial solution were critical in the preparation of CoFe₂O₄ particles in particle size, magnetization characters, uniformity in particle size and even cation distribution in spinel structure. Two different procedures were used to precipitate CoFe₂O₄ magnetic particles. Evidenced by XRD, Mossbauer analyses and magnetization determination, particles in comparative uniformity average size were obtained in procedure A, denoted as normal pH regulation procedure, in which NaOH solution was dropped into the mixture solution of iron ions, and with the decreasing in Fe²⁺/Fe³⁺ ratio of initial solution, the particle size decreased, which followed the same rule of diversification in saturation magnetization. Uniformity in particle size lowered when procedure B, referred to as reverse pH regulation procedure, where ferrous and cobalt ions were dropped into alkaline solution, was used to precipitate CoFe₂O₄. In both procedures, with the decreasing in Fe²⁺/Fe³⁺ ratio of initial solution, the saturation magnetization decreased, while the magnetic coercivity decreased but increased sharply when Fe²⁺/Fe³⁺ ratio of initial solution was 0.     

改进型Fe_3O_4磁流体的研制及带膜磁畴观察

利用化学反应的方法研制了一种带膜观察磁畴结构的改进型磁流体—Ｆｅ３Ｏ４磁流体,并对其生成条件及影响其磁性的因素进行了分析．实验表明：当ＦｅＣｌ２·４Ｈ２Ｏ：ＦｅＣｌ３·６Ｈ２Ｏ：ＮａＯＨ＝１：１：６（摩尔比）时最容易生成稳定的Ｆｅ３Ｏ４．在反应过程中,水质的好坏及有无搅拌是影响 Ｆｅ３Ｏ４磁流体颗粒大小及磁性的主要因素．对Ｚ８牌号的硅钢片进行带膜磁畴观察表明,该磁流体能够实现带膜观察,成纹性及重现性较好,而且磁稳定性也较好,未经任何处理的Ｆｅ３Ｏ４磁流体可以放置一周左右而磁性不发生变化;用去离子水清洗至ｐＨ值为７并且隔绝空气后,可放置更长时间．     

白云母 / CeO2 复合粉体的制备及其摩擦学性能研究

目的研究白云母/CeO2复合粉体在500SN基础油中的抗磨减摩性能和抗磨减摩机理。方法以白云母、硝酸铈、草酸为原料,通过球磨固相法制备不同配比的白云母/CeO2复合粉体,用油酸改性,采用XRD,SEM等对粉体的结构特征和表面形貌进行表征,并通过四球磨损实验考察不同油样的摩擦学性能。结果添加了白云母/CeO2和单一白云母的润滑油,摩擦学性能均比无添加的基础油优越。其中,添加了白云母/10%CeO2复合粉体的润滑油抗磨减摩性能最好,摩擦系数比基础油降低了10.7%,磨斑直径比基础油减少了24.4%。结论白云母/CeO2复合粉体有较好的抗磨减摩能力,对磨损表面有修复作用,合理配比的白云母/CeO2能有效提高基础油的抗磨减摩性能。     

稀土Y掺杂非晶态纳米Ni(OH)2的结构及其电化学性能研究

以Tween-80/n-C4H9OH/c-C6H12/NiSO4水溶液体系,采用微乳液快速冷冻沉淀法制备出稀土Y掺杂非晶态纳米级氢氧化镍粉体材料.采用XRD、SAED、SEM、TEM、EDS、Raman、IR,粒度分析和比表面等测试方法对所制备的粉体进行了结构形态表征,并对其充放电性能和交流阻抗谱进行测试.结果发现,适量稀土元素Y的掺入使非晶态纳米氢氧化镍的结构缺陷增多、无序性增强,平均粒度减小、比表面积增大,有利于降低其溶液电阻、电荷转移电阻和Warburg阻抗,从而提高其放电比容量.样品作为MH-Ni电池正极材料以0.2 C充放电,终止电压为1.0 V,当掺杂Y的质量分数为4%时,放电比容量达到333.3 mAh/g.     

WCu复合粉体的溶胶-凝胶制备及其还原行为研究

以偏钨酸铵和硝酸铜为原料,柠檬酸为络合剂的溶胶-凝胶法制备WCu复合粉体。利用XRD和TEM对还原前后粉末的物相组成﹑形貌﹑粒度进行分析。TEM显示还原后WCu粉末粒度在100 nm左右,Cu相均匀包覆在W颗粒表面。对氧化物粉体的还原性能和机理进行了系统的分析。程序升温还原(TPR)确定了氧化物粉体最佳的两步还原温度分别为500和700 ℃。红外光谱(FT-IR)分析表明,铜通过氧与钨键合,削弱W-O-W键,使得钨铜复合氧化物还原性增强。     

THERMAL DECOMPOSITION BEHAVIOR OF AMMONIUM THIO TUNGSTATE in H_2

１．ＩｎｔｒｏｄｕｃｔｉｏｎＡｍｍｏｎｉｕｍｔｈｉｏｔｕｎｇｓｔａｔｅｉｓｕｓｅｄａｓｒａｗｍａｔｅｒｉａｌｆｏｒｐｒｅｐａｒｉｎｇＷＳ２〔１〕ｂｙｔｈｅｒｍａｌｄｅｃｏｍｐｏｓｉｔｉｏｎｍｅｔｈｏｄ．ＡｓＷＳ２ｈａｓｍａｎｙａｄｖａｎｔａｇｅｓｓｕｃｈａｓｃｏｒｒｏｓｉｏｎｒｅｓｉｓｔａｎｃｅ,ｎｏｐｏｉｓｏｎ,ｎｏｐｏｌｌｕｔｉｏｎ,ｗｉｄｅｔｅｍｐｅｒａｔｕｒｅｒａｎｇｅｆｏｒａｐｐｌｉｃａｔｉｏｎａｎｄｓｍａｌｌｆｒｉｃｔｉｏｎｃｏｅｆｆｉｃｉｅｎｔ,ｉｔｉｓｅｘｔｅｎｓｉｖｅｌｙｕｓ…     

柠檬酸法制备热障涂层用La2Ce2O7粉体

以ZrO(NO3)2·2H2O、Ce(NO3)·6H2O和La2O3为原料,采用柠檬酸法制备了La2Ce2O7粉体,研究了pH值、乙二醇及柠檬酸用量、煅烧温度等工艺参数对La2Ce2O7粉体的影响。结果表明,采用该方法能够制备纯净的La2Ce2O7粉体,最佳实验条件是pH值为5,乙二醇、柠檬酸与金属离子的摩尔比分别是1.8和2,煅烧温度为400℃。