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| 昆明贵金属研究所->《贵金属》杂志-> 2006年第1期摘要 |
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《贵金属》2006年第1期（总103期）摘要 1, 广西某锰银矿银的赋存状态研究 杨洪英1，巩恩普2，杨 立1（1. 东北大学 材料与冶金学院， 辽宁 沈阳 110004； 2. 东北大学 资源与土木工程学院，辽宁 沈阳 110004） Study on the Occurrence State of Silver in the Manganese-silver Concentrate
in Guangxi Abstract：The process mineralogy of manganese-silver concentrate in Guangxi province was studied in this paper, and the occurrence state of silver in the concentrate was found out. Main metallic minerals in the manganese-silver concentrate were psilomelane, pyrolusite, pyrite, limonite, and a few arsenopyrite, hematite and sphalerite. Main gangue minerals were quartz, calcite and clay minerals. The grain size distribution of the concentrate was 0.152～0.088mm accounting for 10.21%; 0.088～0.074mm for 11.45%；＜0.074mm for 60.95%. The main silver-bearing minerals were psilomelane, pyrolusite, limonite, galena, pyrite and sphalerite. Main silver minerals were nature silver, argentite and chaorargyrite. 摘 要：对广西某锰银浮选精矿进行了工艺矿物学的研究，查明了锰银浮选精矿的工艺矿物学性质。该锰银精矿的主要金属矿物为硬锰矿、软锰矿、黄铁矿、褐铁矿、少量毒砂、赤铁矿和闪锌矿；脉石矿物主要为石英、方解石及粘土矿物等。精矿的粒级分布：0.152～0.088mm粒级的颗粒占10.21%，0.088～0.074mm 的颗粒占11.45%；＜0.074mm 的颗粒最多，占60.95%。主要载银矿物有硬锰矿、软锰矿、褐铁矿、方铅矿、黄铁矿和闪锌矿。主要含银矿物是自然银、辉银矿、角银矿。
朱书全，张正红* （中国矿业大学(北京校区) 化学与环境工程学院，北京，100083） Extraction of Platinum from Waste Pt-Al2O3 Catalysts with NaClO3 Oxidation ZHU Shuquan, ZHANG Zhenghong* ( School of Chemical and Environmental
Engineering, Beijing Campus, Abstract: Selective leaching of Pt from waste Pt-Al2O3 catalysts was achieved through NaClO3 oxidation in HCl solution. Pt in leaching solution was reduced with Zn. Pd and other impurity elements can be separated from Pt by the processes of precipitation of Pd with dimethyl glyoxime and hydrolization through NaBrO3. This technology was effective with the features of high recovery and high purity of Pt. 摘 要：本文采用盐酸介质中加入氯酸钠的方法进行废氧化铝－铂催化剂中铂的选择性氧化浸出，浸出液用锌片还原得到粗铂，粗铂用丁二酮肟沉淀除钯，再结合溴酸钠水解法来分离其中的其它杂质元素，可得到产品海绵铂。该方法有效可行，分离效果好，金属回收率高，产品质量符合国家标准。
张康侯，李锦宏，陈亮维 （昆明贵金属研究所，云南 昆明 650221） An Investigation of the Gold-rich Alloys in Au-Ag-Zr Ternary System ZHANG Kanghou, LI Jinhong, CHEN Liangwei( Kunming Institute of Precious Metals, Kunming, Yunnan 650221, China ) Abstract: On the basis of Au-Ag, Au-Zr and Ag-Zr binary phase diagrams, the 700℃ isothermal section of the gold-rich field in Au-Ag-Zr ternary system was established by X-ray diffraction analysis, electron probe microanalyses (EPMA) and optical microscopy. It was found that there is the long single-phase region, Au(Ag) or Ag(Au), along the Au-Ag binary isomorphous system on the gold-silver-rich side of the 700℃ isothermal section. It was confirmed that the partial 700℃ isothermal section consists of four single-phase regions：solid solution Au(Ag) or Ag(Au)，Au4Zr, Au3Zr and Au2Zr; four binary-phase regions：Au4Zr + Au(Ag), Au3Zr + Au(Ag), Au4Zr +Au3Zr and Au3Zr + Au2Zr; and two ternary regions：Au4Zr +Au3Zr + Au(Ag) and Au3Zr + Au2Zr + Au(Ag). No new ternary compound was formed in the gold-rich field. 摘 要：在Au-Ag、Au-Zr和 Ag-Zr二元系相图研究的基础上，采用X射线衍射分析、电子探针(EPMA)和显微金相方法测定了Au-Ag-Zr三元系富金区域的700℃等温截面。发现在该等温截面上的富Au-Ag侧，沿着Au-Ag二元匀晶系存在一个长条形的单相区Au(Ag)或Ag(Au)，确定在该部分等温截面上共有4个单相区：固溶体Au(Ag) 或 Ag(Au)、Au4Zr、Au3Zr 和 Au2Zr; 4个二相区：Au4Zr + Au(Ag)、Au3Zr + Au(Ag)、Au4Zr +Au3Zr 和 Au3Zr + Au2Zr; 2个三相区：Au4Zr +Au3Zr + Au(Ag) 和 Au3Zr + Au2Zr + Au(Ag)；在该区域没有形成新的三元化合物。
崔大田，王志法，姜国圣，郑秋波，吴泓（中南大学 材料科学与工程学院, 湖南 长沙410083） Study of the Au-Ag-Ge Brazing Alloy CUI Datian, WANG Zhifa, JIANG Guosheng, ZHENG Qiubo, WU Hong( Department of Materials Engineering , Central South University, Changsha, Hunan 410083, China ) Abstract: The composition of Au-19.25Ag-12.8Ge brazing alloy was selected based on analysis of Au-Ag-Ge ternary phase diagram. The Au-19.25Ag-12.8Ge brazing alloy tapes of 0.1mm in thickness were manufactured through cladding hot-rolling and then cold-rolling. The melting characteristics and the wettability on Ni plate of the alloy were tested. It was showed that the liquidus and solidus temperatures of the alloy are 491.0℃ and 445.0℃, respectively, the wetting angles of the alloy on Ni plate are less than 15°under temperature≤ 550℃, and the spreading area on Ni plate is increased with increasing in temperature from 490℃ to 550℃. This alloy could be used for packaging brazing of electronic devices. 摘 要：通过对Au-Ag-Ge三元相图的分析确定了Au-19.25Ag-12.80Ge共晶钎料，采取包复热轧后再冷轧制备出厚度为0.1mm的钎料合金薄带，测试了该合金的熔化特性和对Ni板的浸润性。研究结果表明该钎料合金的液、固相线温度分别为490.1℃和445.0℃，合金在≤550℃下对Ni板的润湿角＜15°，在Ni板上的铺展面积随着温度从490℃升至550℃而逐渐增大。该合金可以满足电子器件封装焊接的要求。
戴姣燕1,2，胡昌义2，万吉高2，方 颖2，欧阳远良2，高文桂2，刘伟平2，杨家明3（1. 中南大学， Composition and Microstructure of Ir/C Clusters Prepared by MOCVD DAI Jiaoyan1,2, HU Changyi2, WAN Jigao2, FANG Ying2, OYANG Yuanliang2,
GAO Wengui2, Abstract: Ir/C cluster films were prepared by MOCVD (metal-organic chemical vapor deposition) on quartz plate substrates using iridium-acetylacetonate as the precursor. The effects of oxygen flow and deposition temperature on the composition and microstructure of Ir/C cluster films were studied. It was found that small amount of oxygen additions (4mL/min) to the source gas decreases drastically the carbon content of the films. The effects of deposition temperature on carbon content in Ir/C cluster films are related to the oxygen flow: the carbon content increases with increasing in deposition temperature in the films prepared without oxygen addition and increases first and then decreases with increasing in deposition temperature in the films prepared with some oxygen addition. The Ir/C films with higher carbon content showed wider and lower XRD spectrum of iridium peaks, which was the characteristic of diffraction spectrum of non-crystalline. Ir grains are about 3nm in diameter as deposited at 650℃ without oxygen addition. 摘 要：以乙酰丙酮铱为前驱体，采用金属有机化合物化学气相沉积(MOCVD)技术在石英片上沉积了Ir/C簇膜。研究了氧气流量及沉积温度对Ir/C簇膜成分和结构的影响。研究发现，少量氧气的加入(4mL/min)大幅度地降低了Ir/C簇膜中碳元素的含量；沉积温度对薄膜中碳含量的影响规律则比较复杂：未通氧气的情况下，在实验温度范围内碳含量随着温度的升高而增大，而在通入氧气的情况下碳含量呈现出先升后降的复杂变化趋势。大量碳的沉积宽化了Ir的衍射峰，使其具有非晶衍射的特征。当沉积温度为650℃，未通氧气沉积的Ir/C簇膜中铱晶粒粒经约为3nm。
郭家秀，龚茂初，袁书华，沈 美，王娟芸，陈耀强* （四川大学 化学学院，四川 成都 610064） Effects of the Ratio of Rh on Different Support Materials on Properties of Low-precious Metal Catalysts GUO Jiaxiu, GONG Maochu, YUAN Shuhua, SHEN Mei, WANG Juanyun, CHEN
Yaoqiang* Abstract: A series of low Pt-Rh catalysts for automobile exhaust purification was prepared by dipping method. The effect of distribution ratio of Rh on two different supports on catalytic per- formance of the low Pt-Rh three way catalysts was investigated and the light-off temperatures of hydrocarbon and carbon monoxide and nitrogen oxides were measured. The catalysts were characterized by means of the temperature-programmed reduction(TPR) and the temperature- programmed desorption(TPD). The results of the test showed that the light-off temperatures of hydrocarbon and carbon monoxide and nitrogen oxides have little difference for the fresh catalysts, but for the catalysts treated by the hydrothermal-ageing for 5 hours at 1000℃ the great differences in the light-off temperature are observed. The best ratio of Rh on different supports can improve the property of the catalysts, specially, the anti-aging property. 摘 要：采用浸渍法制备了一系列低Pt、Rh含量的Pt-Rh型汽车尾气净化催化剂。研究了在Pt、Rh含量一定以及其他条件不变的情况下，只改变铑在不同载体上的分配比对催化剂性能的影响，测定了催化剂对C3H8、CO、NO的起燃温度，并对催化剂样品进行了程序升温还原(H2-TPR)、程序升温脱附(O2-TPD)表征。结果表明：新鲜催化剂对C3H8、CO、NO的起燃温度相差不大，但经过1000℃ 、5h的水热老化后，催化剂性能发生了显著的变化，C3H8、CO、NO的起燃温度出现较大的差异，说明了铑在不同载体上的分配比对催化剂性能有一定影响，特别是对催化剂的抗老化性能影响较大。
张爱敏1,2，黄荣光2，宁 平1，赵云昆2，贺小昆2（1. 昆明理工大学，云南 昆明 650093； 2. 昆明贵金属研究所，云南 昆明 650221） Influences of Precious Metals Ratio on Catalytic Activities ZHANG Aimin1,2, HUANG Rongguang2, NING Ping1, ZHAO Yunkun2, HE Xiaokun2( 1. Kunming University of Science & Technology, Kunming, Yunnan 650093, China; 2. Kunming Institute of Precious Metals, Kunming, Yunnan 650221, China ) Abstract: A series of catalysts containing 0.5wt% precious metals(PMs) were prepared by using a new RE based complex material as coating, and different ratios of Pt, Pd, Rh as active components. And their activities changing with PMs, especially with Pt, Pd ratio were studied by engine bench test system. The results indicated that increasing Pd ratio is favorable for catalytic activities in containing Pt, Pd and Rh catalysts, but function decline exists in the catalyst containing same ratio of Pt and Pd; Pd/Rh catalyst is better than Pt/Rh catalyst distinctly with the same ratio, and the activity of Pd/Rh catalyst is the best of all. So the article suggested that when the effect of PMs ratio on the catalytic activities was studied, the simulative functions and decline functions between different PMs should be considered thoroughly to ensure their best promotion functions with the best ratio. 摘 要：以新开发的稀土基复合材料为负载涂层，不同比例的Pt、Pd、Rh为活性组分，平行制成贵金属总含量为0.5wt%的系列催化剂。并通过发动机台架测试系统研究了贵金属负载比例，尤其是Pt、Pd比例对催化剂活性的影响。结果表明：在Pt、Pd、Rh系列催化剂中，Pd比例的增加有利于提高催化剂的活性，但Pt、Pd比例相同时出现作用下降现象；相同比例的Pd/Rh催化剂明显优于Pt/Rh催化剂，且前者在系列催化剂中活性最高。作者建议，在研究贵金属比例变化对催化剂活性影响的同时，需充分考虑到不同贵金属组分间作用的相互促进和可能会出现的作用降低现象，从而以最佳的配比发挥最大的协同促进作用。
刘锡林，李 欣，寇宗燕 （甘肃联合大学 理工学院，甘肃 兰州 730010） Determination of Platinum Group Metals with Chlorophosphonazo-pI LIU Xilin, LI Xin, KOU Zongyan( The Science and Engineering College, Gansu Lianhe University, Lanzhou, Gansu 730000, China ) Abstract: In this paper, five catalytic spectrophotometric methods based on the catalytic effect of platinum group metals on the oxidations of chlorophosphonazo-pI with KIO4(KBrO3) in acidic medium were proposed for the determination of trace Ru, Rh, Os, Ir and Pt. At the same time, the colouration reaction between palladium and chlorophosphonazo-pI was studied, too. It was found that palladium reacts with chlorophosphonazo-pI to form a 1:1 blue complex in H2SO4 medium. The methods proposed in this paper have been applied to the determination of platinum group metals in ores and catalysts with satisfactory results. 摘 要：根据对碘偶氮氯膦在微量铂系元素Ru、Rh、Os、Ir、Pt等离子的存在下与氧化剂KIO4(KBrO3)之间的褪色反应建立了这5种铂系元素的催化光度分析新方法；而对碘偶氮氯膦在硝酸介质中能与钯形成稳定的蓝色络合物又建立了分光光度法测定微量钯的新方法。作者研究了此系列反应的最佳条件及用于各种铂系元素测定的方法和应用。
吕 玲1，刘根起1，程永清1，张 光2 Determination of Trace Amount of Palladium by Dual-wavelength Overlapping Spectrophotometry Lü Ling1, LIU Genqi1, CHENG Yongqing1, ZHANG Guang2 （1. Department of Applied Chemistry, Northwestern Polytechnical University, Xi'an, Shanxi 710072, China; 2. Department of Chemistry, Shanxi Normal University, Xi'an, Shanxi 710062, China） Abstract: A method for determination of trace amount of palladium with 2-(3,5-diclholor-2 -pyridylazo)-5-dimethylaminoaniline (3,5-diCl-PADMA) by dual-wavelength overlapping spectro- photometry was developed. It was shown that in the medium of 0.02～1.6mol/L H2SO4, Pd reacts with 3,5-diCl-PADMA to form a stable green-blue complex with two absorption peaks at 621nm and 574nm respectively, and the sum of absorbance at these two peaks shows good linearity with Pd concentration. The apparent molar absorptivity was 1.61×105 L?mol-1?cm-1, 52% higher than that of single-wavelength spectrophotometry. Beer’s law is obeyed in the range of 0～12μg/10mL for palladium. Relatively large amounts of co-existing elements, including other precious metal ions can be tolerated. The method was simple, highly sensitive and selective. It can be used to determine trace amount of Pd in alloys and molecular sieves with satisfactory results. 摘 要：研究了2-(3,5-二氯-2-吡啶偶氮)-5-二甲氨基苯胺(简称为3,5-diCl-PADMA)与钯的显色反应，在0.02～1.6mol/L的H2SO4介质中，钯与试剂形成稳定的1:1绿蓝色配合物，其在621nm和574nm有2个强弱不等吸收峰。2个峰的吸光度之和与钯浓度线性相关，据此建立了应用双波长叠加分光光度法测定微量钯的新方法。钯浓度在0～12μg/10mL范围内符合比尔定律，表观摩尔吸光系数高达1.61×105L?mol-1?cm-1，比单波长法提高52%。大量的有色金属及其它贵金属离子不干扰测定。所研究的方法操作简便，灵敏度高，选择性好，用于合金及含钯分子筛中微量钯的直接测定结果满意。
李 英1，张玉泉1，张 焱1，马东兰2，王玉炉2 （1. 河南科技学院 河南 新乡453003; 2. 河南师范大 Spectrophotometric Determination of Au(III) with N-allyl-N/-antipyryl Thiourea(AATu) LI Ying1, ZHANG Yuquan1, ZHANG Yan 1, MA Donglan2, WANG Yulu2 （1. Henan Institute of Science and Technology, Xinxiang, Henan 453003, China; 2. Henan Normal University, Xinxiang, Henan 453002, China ） Abstract: The coloration reaction of Au(III) and AATu was studied in the present paper. It was found that under conditions of pH = 4.0 HAc-NaAc buffer solution, a stable complex is formed, the maximum absorbance appears at 275.0nm and its apparent molar absorptivity is 2.39?104 L?mol-1?cm-1, Beer’s law is obeyed in the range of 0～24.0?g/25mL Au(III). The new reagent AATu has been applied to determine gold(III) in the ores with agreeable results. 摘 要：研究了新试剂N-烯丙基-N/-安替比林基硫脲与Au(III)的显色反应。结果表明在pH = 3.8～4.4的HAc-NaAc 缓冲体系中，Au(III)与该试剂形成1∶2的络合物，其最大吸收峰位于275.0nm，表观摩尔吸光系数ε275.0 =2.39×104L?mol-1?cm-1，Au(III)含量在0～24.0?g/25mL内服从比尔定律。方法操作简便，选择性高。用于金矿石中微量金的测定，结果令人满意。
宁远涛（昆明贵金属研究所，云南 昆明 650221） Achievements and Prospects of Composites Based on Precious Metals: (III) Properties, Applications and Prospects of Precious Metals Composites NING Yuantao ( Kunmng Institute of Precious Metals, Kunming, Yunnan 650221, China ) Abstract: This paper is third part of the series papers of “Achievements and Prospects of Composites Based on Precious Metals” published on this journal. In the present paper the main properties and applications of precious metals composites were reviewed briefly, and the prospective developments were forecasted. 摘 要：本文是作者发表的“贵金属复合材料的成就与展望”系列文章的第三部分，介绍了贵金属复合材料的综合性质、复合效应和主要应用，展望了贵金属复合材料的发展前景。
楚 广1,2，杨天足1，刘伟锋1，唐永建2，江名喜1，杜作娟1（1. 中南大学 冶金科学与工程学院，湖南 长沙 410083； 2. 中国工程物理研究院 激光聚变研究中心，四川 绵阳 621900） Developments on Preparation and Application of Nanometer Silver Powders CHU Guang1,2, YANG Tianzu1, LIU Weifeng1, TANG Yongjian2, JIANG Mingxi1, DU Zuojuan1（1. College of Metallurgical of Science and Engineering, Central South University, Changsha, Hunan 410083, China; 2. Research Center of Laser Fusion of CAEP, Mianyang, Sichuan 621900,China） Abstract：In this paper, the methods including the reduction ball-milling, the optical induction, the chemical reduction, the liquid phase reduction, the liquid-solid phase reduction, the spray pyrolysis, the evaporation and condensation, and the atomization et al. which have been used for preparation of nanometer silver flakes and nanometer spherical silver powders in China since the 1990s were summarized under categories, the features of each method were compared, the development of preparation technology was looked forward to, in the meantime, the present application and potential application of nanometer silver powders were expounded. 摘 要：本文分类总结了20世纪90年代以来国内纳米片状银粉和球形银粉的制备方法，包括还原球磨法、光诱导法、化学还原法、液相还原法、液-固相还原法、喷雾热分解法、蒸发冷凝法及雾化法等，比较了各种方法的优缺点，展望了纳米银粉制备技术的发展，同时，论述了纳米银粉现有的和潜在的用途。
谭富彬1，谭浩巍2 （1. 昆明贵金属研究所，云南 昆明 650031；2. 昆明学院，云南 昆明 650032） Development of Electronic Components and Its Requirements to Electronic Pastes TAN Fubin1 , TAN Haowei2 ( 1. Kunming Institute of Precious Metals, Kunming, Yunnan 650031, China; 2. Kunming College, Kunming, Yunnan 650032, China ) Abstract: The development of the chip ceramic capacitor, PDP(plasma displays), silicon solar cell and electronic package was reviewed in the present paper, and the requirements to electronic pastes and the growing trend of base metals electronic pastes were introduced. 摘 要：本文评述了我国多层片式陶瓷电容器、PDP平板显示器、硅太阳能电池、电子封装等的发展现状以及对电子浆料的要求，同时还评述了贱金属浆料的发展趋势。
章 青1，贺小昆2，黄荣光2，赵云昆2 ，李 兵1 （ 1. 昆明贵金属研究所， 云南 昆明 650221； 2. 昆明贵研催化剂有限责任公司，云南 昆明 650101） Actualities and Advance and Prospect in the Research on Palladium Automotive Catalysts ZHANG Qing1, HE Xiaokun2, HUANG Rongguang2, ZHAO Yunkun2, LI Bing1 ( 1. Kunming Institute of Precious Metals, Kunming, Yunnan 650221, China; 2. Kunming Sino-Platinum Metals Catalyst Co. Ltd., Kunming, Yunnan 650101, China ) Abstract：The features and actualities of palladium automotive catalysts technology were reviewed in this paper. The effects of alumina washcoat and rare earth oxides on catalytic activity of palladium automotive catalysts were analyzed systematically. Distinctness of different methods for preparation of catalysts was discussed. The price fluctuation of precious metals in the market and good catalytic activity of palladium immediately affect the future mainstream of palladium automotive catalysts. The feasibility and value of the application of palladium automotive catalysts were considered. The research direction and technology nodus and hot points of palladium automotive catalysts in the future were put forward. 摘 要：阐述了汽车尾气净化Pd 催化剂的技术特点、现状及展望，分析了Al2O3、稀土氧化物对汽车尾气净化Pd 催化剂性能的影响，对比了不同制备方法的优异性，讨论了单Pd
催化剂的可行性和实用价值，以及未来的研究方向、技术难点和热点。
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