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　　　　昆明贵金属研究所->《贵金属》杂志-> 2006年第3期摘要

《贵金属》2006年第3期（总105期）摘要

1, Cu-Ag合金原位纤维复合材料的形变特征

宁远涛，张晓辉，吴跃军（昆明贵金属研究所，云南昆明650221）

Deformation Characteristics of the Cu-Ag Alloy in situ Filamentary Composite

NING Yuantao, ZHANG Xiaohui, WU Yuejun( Kunming Institute of Precious Metals, Kunming, Yunnan 650221, China )

Abstract: The Cu-10Ag alloy and the in situ filamentary composite based on the alloy were prepared. The microstructures of the alloy as cast and formed were observed and studied. The structure of the cast alloy consists of Ag precipitate, (Cu + Ag) eutectic and Cu phase. Ag phase is transformed gradually into the nanometer scale Ag filaments through deformation. The average diameter(d) of Ag filaments can be fitted with an exponential function of the true strain η: d = d0?exp(-0.228η). The deformation process of the composite contains mechanisms of sliding, twining, dislocation increasing and migrating, and cooperating deformation between Cu phase and Ag filaments conditioned by a coherent orientation relationship between them.

摘要：制备了Cu-10Ag合金及其原位纤维复合材料，观察与研究了铸态和形变态合金及复合材料的显微结构。铸态合金由Ag沉淀、(Cu＋Ag)共晶和Cu基体组成，其Ag相通过变形逐步形成纳米尺度Ag纤维，其平均直径可用真实应变η的幂指数d = d0?exp(-0.228η) 拟合。复合材料的形变过程包含了滑移、孪生、位错增生与迁移以及 Ag纤维与Cu基体间形成的共格位相关系和立方-立方协同形变机制。

2, SnO2表面改性对Ag/SnO2复合粉末烧结组织及性能的影响

倪孟良，凌国平*，刘远廷（浙江大学金属材料研究所，浙江杭州 310027）

Influences of Tin Oxide Surface Modification on the Morphology and Performance of Sintered Ag/SnO2 Composite Powders

NI Mengliang，LING Guoping*，LIU Yuanting ( Institute of Metallic Materials, Zhejiang University, Hangzhou, Zhejiang 310027, China )

Abstract: Ag/SnO2 composite powders were prepared by electroless silver plating on SnO2 powders those were modified by the addition of WO3 and CuO+Bi2O3 and with the methods of precipitation and evaporation, respectively. The Ag/SnO2 composite powders were then sintered by the powder metallurgy process. The influences of modifying method and additive agent on the sintering behavior and morphology of Ag/SnO2 samples were investigated by means of optical microscopy and scanning electronic microscopy(SEM). The results indicated that the modifying method of precipitation is superior to evaporation on improving density and uniformity of SnO2 dispersion in the silver matrix. The net like distribution of SnO2 is improved by the combination of additives CuO and Bi2O3, while the surface morphology of AgSnO2 contact after arc erosion is obviously improved by the addition of WO3.

摘要：采用沉积法和蒸发法分别对SnO2粉末进行WO3、Bi2O3+CuO表面改性处理，并用化学镀方法制备Ag/SnO2复合粉末。通过粉末冶金的方法对Ag/SnO2复合粉末进行烧结实验，并通过光学显微镜、扫描电镜观察烧结体的金相组织及复合粉末的形貌，对SnO2表面改性方法及添加剂种类对Ag/SnO2烧结性能和组织的影响进行了研究。结果表明：沉积法改性使烧结体组织中的SnO2分布更均匀，且能明显提高烧结体Ag/SnO2的致密度。Bi2O3+CuO改性可消除SnO2的网络状分布，而WO3改性则显著改善电弧侵蚀后的表面组织。

3, 富硫高砷难浸金精矿的氰化浸出工艺研究

董岁明，姚坡 ( 长安大学环境科学与工程学院化工系，陕西西安 710054 )

The Cyanide Leaching Technology for Treatment of High-arsenic and High-sulphur Gold Concentrate

DONG Suiming, YAO Po ( Department of Chemical Engineering, Institute of Environment Science and Engineering, Chang，an University, Xi，an, Shanxi 710054, China )

Abstract: A new process for treatment of high-sulphur and high-arsenic gold concentrate was studied, with included the roasting at lower temperature with the addition of alkali fusion agent and the cyanidation leaching with the addition of active additive. The results indicated that the leaching of gold is raised from 30%～50% of traditional cyanidation process to 87%～93% of present study and the leaching rate is also improved.

摘要：研究富硫高砷金精矿在加入碱熔剂经低温焙烧预处理后，再加活性添加剂条件下的氰化工艺，结果表明，金的氰化浸出率从直接氰化或沸腾炉焙烧后的焙砂氰化的30%～50%提高到87%～93%，浸出速度也有很大提高。

4, 合成亚砜BSO萃取分离钯铂的性能研究

徐志广，古国榜*，刘海洋，陈柱慧( 华南理工大学化学科学学院，广东广州 510640 )

Study on Extraction and Separation of Palladium from Platinum with Synthetic Sulfoxide BSO

XU Zhiguang, GU Guobang*, LIU Haiyang, CHEN Zhuhui( Department of Chemistry, South China University of Technology, Guangzhou, Guangdong 510640, China )

Abstract: The experimental results showed that Pd(II) can be well extracted by solvent extraction with synthetic sulfoxide BSO in the concentration range of hydrochloric acid from 0.1mol/L to 4.0mol/L, and Pt(IV) can be well extracted only in high concentration hydrochloric acid solution. These properties were used for extraction separation of Pd(II) from Pt(IV) in low hydrochloric acid concentration solution; the largest separation coefficient is 223258.0. They were also used for coextraction of Pd(II) and Pt(IV) in high hydrochloric acid concentration solution, and then with a back-extraction by water, the Pt(IV) was stripped from organic phase, and the largest separation coefficient is 4960.0. It indicated sulfoxide BSO is a valuable extractant from Pt(IV) by solvent extraction.

摘要:对合成亚砜BSO萃取Pd(II)、Pt(IV)性能的研究表明，在不同酸度下BSO对Pd(II)均有优异的萃取性能，而只有在高酸度介质里BSO对Pt(IV)有较高的萃取能力。在低酸度下利用BSO对Pd(II)、Pt(IV)萃取性能的差异，能很好地萃取分离Pd(II)、Pt(IV)；也可以在高酸度下共萃Pd(II)、Pt(IV)，再利用水反萃Pt(IV)，达到分离Pd(II)、Pt(IV)的目的。

5, 乙二醇水热还原法制备纳米银

徐惠，曲晓丽，翟钧，王毅，史建新（兰州理工大学石油化工学院，甘肃兰州 730050）

Preparation of Silver Nanoparticles by Hydrothermal Reduction of Ethylene Glycol

XU Hui, QU Xiaoli, ZHAI Jun, WANG Yi, SHI Jianxin( College of Petrochemical Engineering, Lanzhou University of Technology, Lanzhou, Gansu 730050, China )

Abstract: Ethylene glycol was used as the solvent and reductant for preparation of silver nanoparticles with the method of hydrothermal reduction. The structure of the particles was characterized by X-ray diffraction(XRD), transmission electron microscopy(TEM) and UV-Vis adsorption spectrum. The results indicated that the silver nanoparticles have fcc polycrystalline structure and the mean diameter is about 30nm. The absorption peak is about 380nm. The influences of dispersant and water content on the size of silver particles were also studied.

摘要：利用乙二醇在高温下的还原特性，在水热条件下制备了纳米银粒子，并通过透射电镜、X射线衍射、紫外吸收光谱对其结构进行了表征。研究结果表明：所制备的纳米银具有面心立方相的多晶结构，平均粒径在30nm左右，紫外吸收峰的位置在380 nm左右。分散剂和体系中含水量对纳米银的粒径有一定影响。

6, 口服铂类抗癌药物赛特铂原料药的稳定性研究

刘祝东1，普绍平*1，2，刘洋1 （1. 昆明贵金属研究所，云南昆明 650221； 2. 昆明理工大学，云南昆明 650093）

Study on Stability of Oral Platinum Anticancer Drug-satraplatin

LIU Zhudong1, PU Shaoping2, LIU Yang1 ( 1. Kunming Institute of Precious Metals, Kunming, Yunnan 650221, China; 2. Kunming University of Science and Technology, Kunming, Yunnan 650093, China )

Abstract: The changes in appearance, color and content of satraplatin after laying up in a certain circumstance and for certain time in according to Chinese Pharmacopoeia were tested by HPLC. Experiment results showed that satraplatin is stable at 80℃ and at 25℃ RH 92.5％ for 10 days, or in DMSO system and in pure water for 8 hours; the content of satraplatin is slightly decreased in 0.01mol/L HCl for 8 hours, or at 40℃ RH 75％ for 6 months; the content of satraplatin is still ≥98％ at 25℃ RH 60％ for 3 years, or in 0.1mol/L HCl for 5 hours. it can be confirmed that the term of validity of satraplatin is 3 years. But it is very unstable against light, the content of it decreases to ＜80 at 45001x for 10 days, so it must be strictly kept away from light for storage. The results provide basis for preparation, package, storage and transportation of satraplatin.

摘要：根据中国药典要求，采用高速液相色谱法研究了口服铂类金属抗癌药物赛特铂在一定的环境中放置后其外观、色泽及含量的变化，以此表征赛特铂的稳定性。试验结果表明：赛特铂在80℃和在 25℃、RH 92.5%环境中放置10d，或在DMSO体系和纯水中放置8h含量是稳定的；在0.01mol/L HCl中放置8h或在40℃、RH 75%环境中放置6个月，含量略有降低；在25℃、RH 60%环境中放置3年，或在0.1mol/L HCl中放置5h，含量仍≥98％，可确定赛特铂的有效期为3年。赛特铂对光极不稳定，在45001x光照强度下放置10d，含量降低到＜80%，应严格避光储存。试验结果为赛特铂原料药的研究、生产、包装、储运提供了科学依据。

7, 电镀镍组合添加剂研究

冯拉俊，樊菊红，雷阿利（西安理工大学材料科学与工程学院，陕西西安 710048）

Study of Compound Additives for Nickel Electroplating

FENG Lajun, FAN Juhong, LEI Ali
( School of Materials Science and Engineering, Xi’an University of Technology, Xi’an, Shanxi 710048, China )

Abstract: The influences of the additives of para toluene sulfonate, butynediol, and sodium allyl sulfonate with different concentrations and process parameters on the quality of nickel electroplating were studied using L27(9×35) orthogonal table. The best additives were screened out with the index of the lightness of coating, the current efficiency, deposition rate and dispersing power of solution, they are para toluene sulfonate 0.1g/L, butynediol 0.2g/L and sodium allyl sulfonate 0.5g/L. The results indicated that besides the additives the process parameters should be chosen appropriately so that the best effects can be got.

摘要：采用L27(9×35)混合正交体系，系统地研究了对甲苯磺酰胺、1,4-丁炔二醇和烯丙基磺酸钠3种镀镍添加剂在不同工艺参数和不同添加配比情况下对镀镍质量的影响，以镀层的光亮度，镀液的电流效率、沉积速度和分散能力为评价指标，筛选出最佳的电镀镍添加剂为：对甲苯磺酰胺0.1g/L，1,4-丁炔二醇0.2g/L，烯丙基磺酸钠0.5g/L。研究结果表明，电镀镍除了添加较好的添加剂之外，还应选择较佳的电镀工艺参数，才可达到电镀过程沉积速度快、分散能力好、电流效率高、镀层光亮性好的效果。

8, 难溶金锆系列合金的微波消解及锆的滴定

朱利亚1，赵泽松2，陶赛祥1，2，谢宏潮1，陈海云2，金娅秋1 （1. 昆明贵金属研究所，云南昆明 650221；2. 云南民族大学化学与生物技术学院，云南昆明 650031）

Microwave-assisted Digestion of Difficultly Dissolved Gold-zirconium Series Alloys and the Titration of the Zirconium

ZHU Liya1, ZHAO Zesong2, TAO Saixiang1,2, XIE Hongchao1, CHEN Haiyun2, JIN Yaqiu1( 1. Kunming Institute of Precious Metals, Kunming, Yunnan 650221, China; 2. Department of Chemistry and Biology Technology, Yunnan Nationalities University, Kunming , Yunnan 650031, China )

Abstract: A novel method of microwave-assisted digestion with HCl-H2O2 for the difficultly dissolved gold-zirconium and gold-silver-zirconium alloys was developed. The conditions of sample pretreatment and determination of zirconium with EDTA titration were optimized. Effect of pretreatment with different acidities on zirconium valence was investigated. The proposed method was also compared with the traditional method. Research results showed that zirconium is always in the valence of +4 in 4.5%～6.0%HCl, and there is no significant difference between the two methods on accuracy (relative error -0.33%～+0.08%) for zirconium content from 3 to 20mg. But the proposed method is novel, rapid, economic and convenient leading to its widely apply.

摘要：提出了HCl-H2O2微波快速消解难溶AuZr、AuAgZr合金的新方法，优化了样品预处理及EDTA滴定以测定Zr(IV)含量的条件；考察了在不同HCl酸度下，预处理过程对Zr价态的影响；对比了本法与传统方法的分析结果。研究表明：在4.5%～6.0%HCl下，Zr以+4价状态存在，本法与传统方法测得Zr(IV)的结果吻合，但本法新颖，消解快速、节能，分析操作简便、易于掌握，测定3～20mg Zr(IV)量，相对误差-0.33%～+0.08%。本法明显优于传统方法，适宜推广应用。

9, 石墨炉原子吸收测定岩石样品中超痕量铂

孙爱琴1，姚文生1，王烨2，陈静2，钟莅湘2，李艳华2，王玉林3 （1. 河南省地质调查院，河南郑州 450007； 2. 河南省岩石矿物测试中心，河南郑州 450012； 3. 河南省地矿局第三地质调查队，河南信阳 464000）

Determination of Ultra-trace Platinum in Rock Samples by GF-AAS Method

SUN Aiqin1, YAO Wensheng1, WANG Ye2, CHEN Jing2, ZHONG Lixiang2, LI Yanhua2, WANG Yulin3( 1. Henan Institute for Geological Survey, Zhengzhou, Henan 450007, China; 2. Henan Geoanalysis Laboratory, Zhengzhou, Henan 450012; 3. 3rd Geological Survey Bridge of Hen an Bureau for Geological and Mineral Exploration, Xinyang, Henan 464000, China )

Abstract: After the rock sample was dissolved, the solution was adjusted to the volume fraction of 5%～10% HCl and the Pt in the solution was adsorbed by active carbon. The active carbon was ashed and the ash was re-dissolved by pure aqua regia, and Pt was determinated by GF-AAS using pyrolytically coated electrographite cuvettes produced by Thermo Elemental Corporation. The determination conditions, such as acidity, media and the GF-AAS ashing temperature and graphite furnace atomizing temperature and their effects on the determination were investigated in detail. The detection limit of the method is 0.11×10-9 for Pt with RSD of 5%～9% for 12 times determination. And the method was used to determine national standard substances with coincidence results.

摘要：样品分解后，用超低灰分活性炭吸附φ为5%～15%HCl溶液中的Pt，活性炭灰化，灰分用王水溶解后，在10％HCl溶液中用GF-AAS方法测定岩石样品中超痕量铂。作者研究了测定酸度、介质及石墨炉灰化温度、原子化温度等因素对吸光度的影响。在选定条件下测定方法的检出限达到0.1×10-9，精密度(SD，n=12)5%～9%，经国家一级标准物质分析验证，结果吻合。

10, Distribution Behaviors of Pd(II) in PrOH-(NH4)SO4 Aqueous Biphasic System and Its Application in Determination of Pd(II)

GAO Yuntao1 , WANG Wei2 ( 1. School of Chemistry and Bio- Science, Yunnan Nationalities University, Kunming, Yunnan 650031, China; 2. School of Chemistry and Material Science, Yunnan University, Kunming, Yunnan 650031, China )

钯(II)碘络合物在丙醇-硫酸铵双水相萃取体系中的分配行为及在钯测定中的应用

高云涛1，王伟2 ( 1. 云南民族大学化学与生物技术学院，云南昆明650031；2. 云南大学化学与材料科学学院，云南昆明 650031 )

摘要：研究了Pd(II)碘络合物在丙醇-硫酸铵双水相萃取体系中的分配行为，在HCl介质中，碘化铵存在下，Pd(II)能形成离子缔合物[PdI4２－?(PrOH2+)2]从而被萃入丙醇相。获得了最佳萃取条件，结果表明本方法能定量萃取Pd(II)，在最佳萃取条件下，Pd(II)的萃取率可达99.2%. 合成样的分离结果表明，本方法可应用于从大量基体金属如Fe2+、Ca2+、Mg2+、Mn2+、Al3+、Pb2+和Zn2+中分离Pd(II)。对从废碳钯催化剂中Pd的回收也进行了试验，结果与火试金法相符。

Abstract: The extraction of iodide complex of Pd(II) in the propyl-alcohol ammonium sulfate aqueous biphasic extraction system was investigated. Pd(II) is found to be extracted into the propyl- alcohol phase due to the ion pair formation as [PdI4２－?(PrOH2+)2] in the presence of NH4I and in HCl medium. And the related extraction conditions were optimized. The experimental results indicated that Pd(II) can be quantitatively extracted by proposed method, and an extraction rate of 99.2% for Pd(II) can be achieved under optimized conditions. The proposed method was applied to the separation of palladium from large amount of base metals such as Fe2+,Ca2+, Mg2+, Mn2+, Al3+, Pb2+ and Zn2+ in synthetic sample. Application of the method for separation of palladium from spent carbon palladium catalysts was also investigated and the results agree well with fire-assay method.

11, 容量法测定金合金中的金

袁文明，黄树茂（北京航空材料研究院，北京100095）

Volumetric Determination of Gold in Gold Alloys

YUAN Wenming, HUANG Shumao ( Beijing Institute of Aeronautical Materials, Beijing 100095, China )

Abstract: The main problems in determination of gold by the back titration for the excessive FeSO4 with potassium bichromate were discussed and experimented. A simple, accurate and easy to operate method was developed. When the content of gold is from 60% to 99%, the relative standard deviation of ＜0.2% can be achieved.

摘要：对重铬酸钾滴定过量硫酸亚铁返滴定法测定金合金中金的主要问题做了探讨和实验。拟定了简便、准确的测定方法，方法的重现性好，金含量为60%～99%时的相对标准偏差＜0.2%。

12, 池窑拉丝铂合金大漏板锥形嘴冷镦工艺及模具设计

杨兴无，纪周礼*（南京玻璃纤维研究设计院，江苏南京 210012）

Cold Upsetting Technology and Die Design for Manufacture of Conical Tip of Platinum Alloy Bushing in Fiberglass Production

YANG Xingwu, JI Zhouli* ( Nanjing Fiberglass Research and Design Institute, Nanjing, Jiangsu 210012, China )

Abstract：In this paper, the advantages of the manufacture of Pt-10Rh alloy conical tips for bushings with the cold upsetting technology instead of cutting were pointed out. The structure feature and formed technology of the Pt-10Rh alloy conical tips for bushings were analyzed and the formulating process of the cold upsetting technology was determined. The preparation and treatments of the tips blank and structure design of the cold upsetting die were introduced.

摘要：本文阐明了采用冷镦工艺代替切削加工生产Pt-10Rh合金漏板锥形嘴的优点，对Pt-10Rh合金漏板锥形嘴零件结构特点和成形工艺进行了分析，制订了冷镦工艺方案。介绍了漏嘴坯制备处理及冷镦模具结构设计。

13, 湿法制备纳米结构银研究进展

杨声海，陈永明，杨建广，巨少华，唐谟堂（中南大学冶金科学与工程学院, 湖南长沙 410083）

Some Advances in Silver Nanostructures Prepared by Hydro-processes

YANG Shenghai, CHEN Yongming, YANG Jianguang, JU Shaohua, TANG Motang( College of Metallurgical Science and Engineering, Central South University, Changsha, Hunan 410083, China )

Abstract：In this paper the synthesis methods of silver nanostructure materials, such as nanocubes, triangular nanoprisms, nanorods, nanowires, nanotubes, dentrites, flake, nanodisks, nanobelts, and so on, were introduced, the methods include reducing precipitation, photoinduced conversion, irradiation reduction, electrodeposition, template, microwave-assisted, ultrasonic-assisted, hydrothermal assemble, microemulsion, and so on. The questions existing in synthesis processes were also discussed.

摘要：介绍了纳米立方体、三角形纳米棱柱、纳米棒、纳米线、纳米管、树枝状、片状、纳米盘、纳米带等纳米结构银的制备方法，包括溶液还原沉淀法、光诱导转化法、辐射还原法、电化学沉积法、模板法、微波或超声波辅助法、水热法、微乳液法等。并对纳米结构银制备方法存在的问题进行了分析。