ICP-AES法检验含金基体多元素混合标准溶液的均匀性

为了消除黄金基体对部分被测(杂质)元素产生的干扰与抑制作用,采用基体匹配法,配制了含金基体混合多元素标准溶液。用ICP-AES法对该含金基体溶液中的Ag、Cu、Fe、Zn元素进行了均匀性检验。采用F和t检验法联用统计处理数据对该溶液进行了均匀性评价。检验结果表明瓶间和瓶内的均值和方差不存在显著性差异,证明该含金基体混合多元素标准溶液是均匀的。     

TBP萃取剂从铜阳极泥盐酸-氯气浸出液中选择性萃取金（英文）

铜阳极泥的盐酸-氯气氧化性浸出会导致大量杂质元素如Fe、Cu、Pd、Se等的溶解。以TBP作为萃取剂,采用标准的溶剂萃取实验方法,等体积有机相和水相来萃取分离Au、Pd、Pt、Fe、Cu和Se等元素,研究TPB浓度、HCl和氯离子浓度对杂质分离效果的影响。结果表明,在有机相中TBP浓度为0.25 mol/L、水相中HCl浓度为2.5 mol/L的条件下,可以得到高的金萃取率。同时,其他杂质元素的萃取可以忽略不计。对负载有机相采用蒸馏水进行洗涤,可以去除部分杂质元素。采用硫代硫酸钠溶液进行反萃,反萃液中不含任何杂质元素。在反萃液中加入硫酸,反应产生的SO_2气体可还原金离子。     

铝酸钠溶液中 Na2 S 对 Q235 钢腐蚀的影响

目的研究在含S2-的铝酸钠溶液中Q235钢的腐蚀行为。方法模拟生产条件配制种分母液,采用盐雾腐蚀实验与SEM和EDS分析技术,结合腐蚀质量损失动力学方程与极化曲线,研究Na2S质量浓度与时间对Q235钢腐蚀行为的影响。结果腐蚀产物元素主要为O,S,Al,Fe。在铝酸钠溶液中,基体的表面会覆盖一层Al2O3保护膜,可以阻碍溶液中的硫离子穿透到基体表面,对基体起到一定的保护作用。因此腐蚀初期及低质量浓度下,腐蚀速率缓慢;但随着质量浓度的增加、腐蚀时间的延长,保护膜被破坏,S2-穿过保护膜与基体反应,生成硫化物加速了腐蚀速率;当S2-质量浓度增加到6 g/L,腐蚀时间为9 d时,硫化物被氧化成具有较稳定结构的氧化物,腐蚀被抑制。结论在铝酸钠溶液中,S2-质量浓度及腐蚀时间对腐蚀有一定的促进作用,但当腐蚀时间及S2-质量浓度达到一定值时,腐蚀速率呈现减小的趋势,腐蚀被抑制。     

氯金酸的浓度对纳米金形态的影响

采用Zn置换HAuCl4溶液的方法制备了具有不同形貌的纳米金,并研究了HAuCl4溶液的浓度对纳米金形貌的影响.实验结果表明,纳米金的形貌主要取决于HAuCl4溶液的浓度.当HAuCl4溶液的浓度为0.01 mmol/L时,置换反应进行5 min后的产物是金纳米颗粒,其粒径为10～50 nm,24 h后金颗粒的粒径超过100 nm,金颗粒团聚成金花状.当HAuCl4溶液的浓度为1 mmol/L时,金颗粒的粒径为数百纳米,部分金颗粒团聚成金花状.当HAuCl4溶液的浓度为10 mmol/L时,在金颗粒中出现由纳米金片组成的多晶枝晶,多晶枝晶随后通过OA和OR机制转变成单晶枝晶.当HAuCl4溶液的浓度为30 mmol/L时,反应时直接生成金枝晶.因此,通过控制HAuCl4溶液的浓度,可制备具有不同形貌的纳米金.     

铝合金铬酸阳极氧化后表面缺陷分析

目的对铝合金铬酸阳极氧化后显现出的表面缺陷及原因进行分析。方法通过扫描电镜观察试样表面缺陷处的形貌,通过金相显微镜观察缺陷处的金相组织,通过能谱仪对缺陷处的腐蚀产物进行分析。结果铝合金通过铬酸阳极氧化后,基体的缺陷处会在铬酸溶液中产生沿晶界腐蚀。结论材料本身含有一定量的Cu,Ni,Mg,Fe等元素,在热处理过程中,这些元素在晶界处富集形成偏析相,从而造成金属基体在铬酸溶液中的腐蚀。     

用阳离子表面活性剂浮选盐酸溶液中的铂、钯和金离子

用阳离子表面活性剂研究了盐酸溶液中的1.1～96.9μg/ml 铂族元素和金(Ⅲ)的离子浮选情况。对盐酸浓度和共存离子的干扰进行探讨,并尝试在这些金属的分离—浓缩中的应用。还测定盐酸溶液中的铂(Ⅱ)、钯(Ⅱ)和金(Ⅲ)氯络合物的平均配位数,从而得出了溶解组成和浮选率之间的关系。     

电感耦合等离子体法测定锡青铜中Fe、Sb元素

用混合酸溶解一系列同基体有证标准物质后移入100 ml容量瓶中作为标准溶液,同时锡青铜试样以同样方法溶样处理,用ICP-AES测量锡青铜中Fe、Sb元素。使用该法分析标准样品,分析结果与标准值基本一致,均在允许误差范围内。     

乙酸乙酯萃取-ICP-MS测定高纯金中杂质元素含量

采用乙酸乙酯萃取分离金基体,用电感耦合等离子体质谱(ICP-MS)内标法测定高纯金中31种杂质元素。萃取酸度为1 mol/L HCl,用25 mL乙酸乙酯可去除金基体对待测元素的干扰,对金的萃取率大于99.9%。将31种元素用~(45)Sc、~(133)Cs、~(159)Tb、~(187)Re等4个内标元素分组测定。方法检出限为0.25μg/L,定量限为0.83μg/L,精密度(RSD,n=12)为0.31%～5.97%,加标回收率为95.3%～109.2%。可满足99.999%的高纯金样品中杂质元素含量的检测。     

不同基体材料TD法盐浴渗钒层的组织及硬度

通过对45、T10、T12、W6Mo5Cr4V2、GCr15、Cr12MoV钢六种不同的基体进行盐浴渗钒,并对渗钒层的组织、厚度、成分和硬度进行测试比较。结果表明,基体化学成分对覆层的厚度、成分和硬度均有影响。基体中的固溶碳含量能促进覆层的生长,增加覆层厚度,提高覆层中的C/V浓度比,改善覆层硬度。而且,对覆层的能谱分析结果表明在碳素钢基体上的覆层中只含有C、V、Fe三种元素,而在合金钢基体上的覆层中还探测到了少量的来自基体的合金元素,这些合金元素向覆层中的扩散可以显著提高覆层的显微硬度。     

临界光线折射角与溶液浓度关系的研究

提出用掠入射法测量溶液浓度的方法，该法不受光源强弱和波长变化的影响，测量环境宽松。利用溶液浓度与其掠入射临界光线折射角的关系，采用标准溶液进行测量和拟合标定，给出数学解析关系式。对已知浓度为5％～80％的蔗糖溶液进行实验测量，结果最大偏差为0．002％，具有工程应用的前景。     

金多孔纳米片的一锅法制备及其在SERS检测中的应用

设计并构建多样的金微纳米结构是实现表面增强拉曼光谱（SERS）信号放大的合理途径。利用氯金酸与聚乙二醇（PEG）的氧化还原反应,通过水热合成法制备出金多孔纳米片。PEG在制备过程中既是包裹剂又是还原剂。该制备方法反应温度比较温和,采用一锅法一步合成工艺,成本效益高且环境友好。所制备的金多孔片尺寸多为微米级,清洗后表面没有有机物污染。EDS分析进一步证实所制备的多孔片结构为金单质。结果表明,金多孔纳米片的形貌可通过反应时间、PEG浓度和金离子浓度等实验参数进行调整。金多孔纳米片制备的拉曼光谱基底具有优异的SERS光谱增强效果,并在检测中表现出良好的重现性。另外,所制备的金纳米多孔片基底实现了有机农药福美双和甲拌磷的快速灵敏分析检测。     

金饰品在佩戴过程中出现白色斑点的问题探究

针对金饰品在佩戴过程中形成白色斑点的问题进行了研究。将金片浸泡到不同浓度的汞离子溶液中,实验结果表明,单纯的汞离子无法令黄金变白;在加入还原剂,且汞离子达到一定浓度条件下,金片出现明显变色现象;研究了汞离子浓度和金片变白程度的关系。     

引线键合中材料参数对硅基板应力状态的影响

利用＂热—力—超声＂增量耦合有限元模型,对采用不同引线（金,铜）以及采用铜引线在不同银镀层厚度（48,1,6μm）条件下的键合过程进行了模拟.结果表明,在其它条件不变的情况下,金引线键合过程对硅基板内应力状态的影响远小于铜引线,且应力集中的位置更接近键合中心;随着镀层厚度的增加,基板所受到的压应力逐渐减小,但基板所受到的最大压应力在硅的抗压力范围之内;同时基板所受到的剪应力也逐渐减小,由于剪应力是硅基板损坏的决定性因素,因此采用厚度为16μm的镀层对减小基板损坏更有利.     

LEACHING OF PRECIOUS METALS FROM COMPLEX SULPHIDE ORES——2.DIRECT LEACHING OF Cu SULFIDE CONCENTRATE BY ACIDIC THIOUREA SOLUTIONS

Recovery of gold and silver from a sulphide concentrate by thiourea leaching was investigat-ed.The effects of various parameters on the process,such as oxidants,the initial concentrationof thiourea and acidity in solutions as well as reaction temperature,were systematically exam-ined.From the results it was confirmed that(a)oxidants had no significant influence on the dis-solution of gold and silver at a fixed initial concentration of thiourea;(b)the initial concentra-tion of thiourea and acidity affected the dissolution rate only in the earliest period of leaching;(c)the rate of the process was controlled by reagent diffusion.The optimum operations wereworked out for the thiourea leaching process of the concentrate.     

双辉多元共渗与电刷镀复合表面耐蚀渗镀层的研究

在20钢表面电刷镀快速Ni层作为过渡层，然后采用双层辉光离子技术将Ni-Cr-Mo-Cu合金进行多元共渗，对形成的复合镀层在5%HCl溶液中进行了电化学腐蚀性能测试，利用XRD，扫描电镀以及EDX对渗层的组织结构和合金元素及碳元素在渗层中的分布进行了分析，结果表明；预先刷镀快速Ni镀层再进行双层辉光多元渗Ni-Cr-Mo-Cu的复合渗镀层的耐蚀性能明显优于双辉多元渗Ni-Cr-Mo-Cu以及单独电刷镀Ni镀层的耐蚀性能，分析认为，由于双辉多元共渗中的温度效应，使层复合渗镀层具有较好的耐蚀性能。     

Synthesis, processing and forming gold structures from a 0.1 wt. % concentration solution

A very low concentration (≈0.1 wt. %) of spherical 15nm diameter gold nanoparticles were produced by the sodium citrate reduction method and later transferred to ethanol using poly vinyl pyrrolidone (PVP) as a stabilizing agent. The alcosol was then subjected to electrohydrodynamic atomisation to generate fine droplets with an average droplet diameter of < 30μm and deposited on substrates accordingly. With the assistance of various deposition methods, three different microstructures were produced. Firstly, the droplets produced by atomisation with the help of an electric field were deposited at various times on a substrate to fabricate gold films with a thickness range of ~500nm to 2000nm. Secondly, the droplets were deposited on a moving table which is computer controlled to form an array of inter-connected droplets, thus enabling us to pattern microstructures containing gold nanoparticles of different geometries (electrohydrodynamic atomisation printing). Thirdly, to reduce the track size as well as to form a dense assembly of particles in the microstructures templates were used in conjunction with electrohydrodynamic atomisation (templateassisted patterning). In order to encapsulate gold nanoparticles in a fibre a co-axial needle set-up was used with a polyethylene oxide (PEO) and polyethylene glycol (PEG) mixture as the encapsulating media. Lastly, a gold hydrosol was used to produce near-monodisperse gold microbubbles with the help of a T-junction device having an average diameter of ≈150μm. The ability to generate such a range of structures starting from a very low concentration of gold is a significant achievement.     

Fabrication of concave micro lens array using laser patterning and isotropic etching

Micro lens arrays are widely used in optical communication and laser-fiber coupling applications. In this paper, a technique to fabricate concave micro lens arrays on glass substrate using a third harmonic Nd:YAG laser direct patterning and followed by chemical wet isotropic etching is presented. The patterning process was done on gold film, which was coated on a glass substrate by using a NC controlled laser ablation tool paths. The glass substrate is then etched by using hydrofluoric acid (HF) solutions whereby the exposed area will be dissolved away by chemical reaction with HF. The type of etching process is an isotropic etching which the etching rate is equal at all direction thus produce hemispherical concave profile on glass. The optimum laser patterning parameters is obtained and the effect of different types of HF solutions on etching efficiency is studied. The surface morphology, 2D and 3D profiles are also measured. Various micro lens diameters are fabricated with different values of lens sag.     

Au Recovery Using an Activated Carbon Column

The feasibility of a process involving the use of activated carbon in a multistage column (NIMCIX contactor) for the recovery of gold from unclarified pregnant solutions was investigated on pilot-plant scale. It was found that satisfactory extractions, corresponding to a recovery of 99.6 percent, can be achieved with an average gold concentration of 0.0077 p.p.m. in the barren solutions from a feed averaging 1.89 p.p.m. The results show that excessive loading of CaCO₃ can be prevented by lowering of the pH of the feed to about 7.6. This obviates the need for the carbon to be treated with hydrochloric acid. The gold was eluted from the carbon by the Zadra procedure. The operating conditions of the elution and electrowinning circuits are reported, and the elution of the gold and other metals is discussed. The reactivation of the carbon, which was carried out in a vibrating-deck kiln, is described, and the effects of this reactivation on the activity of the carbon and its microstructure are also discussed. The consumption of reagents in the adsorption and elution circuits is presented in sufficient detail to allow the potential of the activated-carbon process as an alternative to the Merrill-Crowe process for the treatment of high-grade solutions to be evaluated. In addition, the results of parallel small-scale investigations on the effect of pH on the loading of CaCO₃, gold, and other metals on activated carbon are presented and discussed briefly.     

Environmentally Induced Failure of Gold Jewelry Alloys

Stress corrosion cracking (SCC) is an established form of environmental attack in low karatage gold jewelry alloys. The cause of failure is often attributed to exposure to chlorinated solutions. At a certain gold content (usually greater than 14K) the alloy is widely believed protected from SCC. In this study, three commercial 18K gold alloys (yellow gold, nickel white gold, and palladium white gold) were tested in combination with three different household solutions to determine relative corrosion rates. These rates were determined using polarization tests. Once the maximum corrosion rate had been established, SCC tests using the constant potential dead weight method were used to determine time to failure. The resultant failure surfaces were examined to determine mode of fracture, which in all cases was predominantly intergranular. It was found that corrosion rates depended upon both the alloy system and the test solution. SCC was clearly demonstrated in 18K gold alloys, although in all cases times to failure were significantly greater than has been reported for lower karatage alloys. Palladium white gold was far more resistant to SCC than the other systems studied.