导电陶瓷Ti3SiC2颗粒表面无敏化活化的化学镀铜

利用无敏化、活化的化学镀覆技术能成功地在Ti3SiC2颗粒表面均匀地化学镀铜。实验表明：镀前对陶瓷颗粒进行严格的粗化处理,使其表面具有很强的催化中心,通过采用合适的镀液配方和工艺,能成功地在Ti3SiC2颗粒表面镀覆一层铜,从而增强了陶瓷TisSiC2颗粒和铜基体之间的界面结合力,为Ti3SiC2在复合材料领域中的应用开辟了更广阔的前景。     

表面活性剂辅助制备Cu-Ti3SiC2包覆粉末的电化学机理和化学镀特性

为提高Cu-(Ti3SiC 2)p复合材料中铜与陶瓷的界面结合强度,以环境友好型抗坏血酸为还原剂,D-葡萄糖酸钠为络合剂,制备了Cu-Ti3SiC 2包覆粉末。研究了Ti3SiC 2粉末表面化学镀铜及其电化学性能,以及十二烷基硫酸钠(SDS)结合聚山梨酯80(Tween-80)表面活性剂对化学镀铜的改性效果。采用线性扫描伏安法和开路电位-时间法确定了该体系的电化学机理并进行参数优化。结果表明,提高反应温度,增加Cu(II)和抗坏血酸的浓度,可以提高极化电流密度,有利于加速化学镀。铜镀层新核从依附在(Ti3SiC 2)p粒子表面的银催化活化中心开始形成,表面具有较多Ag催化活性中心的微球会促进涂层的形成。采用复配改性剂SDS(6~22 g/L)+Tween-80 (8~12mL/L)对化学镀铜表面涂覆的效果优于单一改性剂。采用SM4 (SDS+Tween-80)改性剂达到最佳涂层效果的Cu与Ti3SiC 2的总摩尔比为1:0.54。静电效应和空间位阻效应对铜在(Ti3SiC 2)p表面的生长起着至关重要的协同控制作用。     

Comparative studies on the electroless deposition of Ni-P, Co-P and their composites with SiC particles

Electroless deposition of nickel and cobalt from alkaline baths as well as their codeposition with SiC particles were compared. It was found that despite similarity in properties of the metals their behavior in the electroless process was different. Maleic acid was used to stabilize plating baths, however the optimal concentration of the additive depended on the type of deposited metal. The electroless deposition characterized with low plating efficiency and it was higher for nickel than for cobalt. The composition as well as the morphology of Ni-P and Co-P deposits were also dissimilar. SiC particles inhibited the metal deposition, affected the plating potential, but did not alter the matrix composition. SiC entrapment was more preferential within the cobalt matrix than the nickel one. Some adsorption phenomena on SiC powder were also studied.     

碳纤维增强Cu-Ti3SiC2复合材料的研究

采用电镀Cu碳纤维（Cf）与化学镀Cu的Ti3SiC2粉及Cu粉进行湿混,通过真空热压烧结法制备Cf增强的Cu-Ti3SiC2复合材料。研究了其致密度、电阻率、维氏硬度随Cf,Ti3SiC2含量变化的规律。实验结果表明,Ti3SiC2体积含量为20％,Cf体积含量为8％时,制备的Cf增强Cu-Ti3SiC2复合材料综合性能最好。Cf镀Cu和Ti3SiC2镀Cu改善了它们和Cu的润湿性,从而提高了相互之间的结合强度是复合材料获得良好综合性能的基本原因。     

Catalysts characteristics of Ni/YSZ core-shell according to plating conditions using electroless plating

This study aims to develop an anode catalyst for a solid oxide fuel cell (SOFC) using electroless nickel plating. We have proposed a new method for electroless plating of Ni metal on yttria-stabilized zirconia (YSZ) particles. We examine the uniformity of the Ni layer on the plated core-shell powder, in addition to the content of Ni and the reproducibility of the plating. We have also evaluated the carbon deposition rate and characteristics of the SOFC anode catalyst. To synthesize Ni-plated YSZ particles, the plated powder is heat-treated at 1200 °C. The resultant particles, which have an average size of 50 μm, were subsequently used in the experiment. The size of the Ni particles and the Ni content both increase with increasing plating temperature and plating time. The X-ray diffraction pattern reveals the growth of Ni particles. After heat-treatment, Ni is oxidized to NiO, leading to the co-existence of Ni and NiO; Ni₃P is also observed due to the presence of phosphorous in the plating solution. Following heat treatment for 1 h at 1200 °C, Ni is mostly oxidized to NiO. The carbon deposition rate of the reference YSZ powder is ~135%, while that of the Ni-plated YSZ is 1%-6%.     

不同形状钨粉化学镀铜的研究

通过化学镀法制备铜包钨复合粉末,研究不规则形状的钨粉以及经等离子球化处理的球形钨粉的化学镀铜。结果表明,对于颗粒形貌不规则棱角分明的破碎钨粉,经化学镀包覆后粉末没有明显的棱角,表面粗糙。而经等离子球化处理后球形度较高的球形粉,颗粒表面存在缺陷,化学镀后粉末的球形度没有明显的变化,化学镀层在其表面沉积均匀,且钨粉表面质量得到改善,不存在表面缺陷。化学镀后复合粉末在600℃下进行氢气退火处理后,镀层上的粗糙的表面变得平滑,镀层中的空隙明显减少,形成了一层均匀致密的铜层包覆在钨颗粒表面。     

SiC_p表面化学镀铜工艺研究

Si Cp 因其高强度、高模量、耐热、耐磨、耐高温等性能而被作为颗粒增强体制备金属基复合材料。本文用正交法优化了 Si Cp 表面化学镀铜工艺 ,获得了 Cu包覆 Si Cp,测定了 Si Cp 的增重百分率及镀液的 p H值随时间的变化规律 ,并对镀覆层形貌进行了 SEM考察。结果表明 ,镀液的 p H值及 Ni2 浓度对镀速影响最为显著 ;粒子分散很好、镀层均匀     

表面活性剂在陶瓷化学镀铜工艺中的作用

通过研究在镀液中添加十六烷基三甲基溴化铵(CTAB)、十二烷基硫酸钠(SDS)和吐温-80三种表面活性剂对化学镀铜沉积速率和镀液稳定性的影响,确定出三种添加剂的最优添加浓度。通过扫描电镜、能谱分析仪和X射线衍射仪,对镀层表面形貌、组成成分以及晶体结构分别进行研究。并通过线性伏安扫描法,研究了添加不同表面活性剂镀液的电化学行为。结果表明:表面活性剂可以提高化学镀铜的沉积速率和镀液稳定性。CTAB、SDS和吐温-80的最优添加浓度分别为1mg/L、20mg/L和5mg/L。加入SDS后,由于沉积速率过大,使得镀层颗粒变大。加入CTAB和吐温-80可以细化镀层的颗粒且更加致密。添加不同的表面活性剂后,镀层的晶粒尺寸没有太大改变,含铜量均为100%且镀层的晶粒呈现面心立方晶体结构。表面活性剂主要通过影响甲醛的氧化反应影响化学镀铜过程。     

Ti3SiC2陶瓷颗粒表面超声波化学镀铜

钛碳化硅（Ti3SiC2）陶瓷导电材料有许多优异的性能,其摩擦系数甚至比石墨更低,完全可以取代石墨用来制备性能更加优良的铜基电接触复合材料,但是由于其与铜基体之间的浸润性不是很好,研究了利用超声波化学镀覆技术在Ti3SiC2颗粒表面均匀镀上一层连续的铜镀层。通过扫描电子显微镜对铜镀层表面形貌的观察表明：通过严格的镀前预处理工艺的优化设计以增加活化点,对传统镀液配方的调整以降低镀速,能够成功的在Ti3SiC2颗粒表面均匀镀覆一层铜微粒,改善了Ti3SiC2和铜基体间的润湿性,从而增强二者之间的界面结合力。     

化学镀法制备Cu/Al2O3复合粉体及其烧结行为

为了解决颗粒增强铜基复合材料中颗粒与铜基体相容性的问题,采用化学镀法使得颗粒表面金属化,通过XRD、SEM、EDS等技术研究了Al2O3纳米粉化学镀铜的工艺,并对Cu/Al2O3复合粉体的烧结行为做了初步探讨.结果表明:Al2O3粉前处理工艺、镀液的各种成分都对粉体表面铜的含量有影响,通过改变装载量可有效控制粉体表面Cu含量.实验中确定了最佳的镀覆工艺,并得到了颗粒较为弥散的Cu/Al2O3复合粉体烧结体.     

离子注入陶瓷化学镀Cu工艺的优化

离子注入可作为前处理工艺辅助Al2O3陶瓷表面化学镀铜,优化了离子注入后以甲醛为还原剂、酒石酸钾钠为络合剂的碱性化学镀铜的基本配方.探讨了主盐浓度、甲醛、pH值、温度等对沉铜速度和镀层表面粗糙度的影响.研究了注入不同金属对沉铜速度的影响,结果表明注入铜比注入镍的化学镀铜速度快.     

化学镀法制备铜包覆SiC颗粒的研究

采用化学镀法制备了镀铜SiC粉体,研究了预处理、镀液成分、pH值和装载量对SiC化学镀铜的影响,并比较了主盐含量和装载量对复合粉体中铜含量变化的影响。利用XRD,SEM和EDS对粉体的物相、形貌、成分进行了分析,得到了最佳施镀工艺。结果表明:用于预处理的活化敏化液要放置一段时间后使用,才能成功地实施化学镀铜;随着pH值和主盐含量的升高,镀速呈上升趋势,但粉体的包覆完整性和均一性下降;通过改变装载量来控制复合粉体中的铜含量可行。     

Al2O3陶瓷表面化学镀铜工艺及其低温连接

进行了Al2O3陶瓷表面的化学镀铜处理,制定了前处理流程.研究了硫酸铜浓度、甲醛浓度、施镀温度、施镀时间等对镀层沉积速率的影响,对镀层进行了金相分析,在此基础上得到化学镀铜的优化工艺.进行了镀铜后Al2O3陶瓷低温钎焊工艺试验,研究了不同化学镀工艺条件对接头组织及力学的影响.结果表明,在试验条件下,随着焊接温度升高,接头致密度变差;焊接时间增加,焊缝宽度也增加;硫酸铜,甲醛浓度增加,镀层厚度增加,相对影响了钎焊焊缝宽度和质量.     

Effect of triethanolamine on deposition rate of electroless copper plating

Abstract

The addition of bis(3-sulphopropyl) disulphide in Cu electroless plating results in Cu superfilling. However, the deposition rate of superfilling copper plating is decreased, which hinders its application for filling Cu into via holes of ultralarge scale integrations. In the present study, the effect of triethanolamine (TEA) on the deposition rate of electroless copper plating was investigated. The deposition rates of electroless plated copper both in traditional and superfilling copper plating were accelerated with an addition of TEA, which was attributed to a decrease in reaction activation energy of a dominant reduction reaction. X-ray diffractometry and atomic force microscopy measurements indicated that with an addition of TEA, the peak intensity ratio /(111)//(200) of electroless plated Cu film was increased and the average surface roughness was decreased.     

石墨颗粒表面化学镀铜研究

为了充分利用Cu的导电性能，碳石墨的润滑性能，改善Cu/C的润湿性，用化学镀铜的方法成功地对石墨颗粒表面进行镀覆，详细地研究了镀铜液组分及工艺与石墨颗粒表面镀铜层厚度、沉积速率的关系，并得出较好的组分工艺方案，采用优化工艺可以得到平均厚度约7．1μm的镀铜层。同时应用X射线、金相显微镜、扫描电镜及电子探针对镀铜层的厚度、表面形貌、镀铜层与基体的界面进行了全面观察。分析表明，Cu/C界面存在过渡层，界面成锯齿状，机械冶金结合的特征十分明显，改善了铜碳界面的相溶性。     

温度对碳化硅粉体表面镀镍的影响

为改善碳化硅陶瓷粉体与金属的润湿性,在碱性条件下,以水合肼为还原剂,采用化学镀方法在 碳化硅粉体表面沉积镍层,结合镀层的表面形貌、组织结构和实验现象,研究了镀液温度对镀镍的影响,此外还研究了水合肼用量对镀速的影响.结果表明:反应温度为70,75,80℃时,所得包覆粉体的表面镀层由颗粒状、胞状的Ni组成,基体完全被镀层...     

A method for polyaniline coatings on solid polystyrene surfaces and electroless copper deposition

A new efficient method is presented for electroless copper deposition on solid polystyrene surfaces via polyaniline (PANI) coatings. It was demonstrated that, partial polymerization of aniline by catalytic air oxidation in the presence of dissolved polystyrene (PS) (M_n: 87.000 K) gives viscous solution of PANI-PS mixture in aniline. Direct application of the polymerization mixture with copper catalyst onto polystyrene sheets (5 × 15 cm) resulted in extension of the polymerization by air oxygen to give a smooth PANI-PS composite layer on the host surface. Treatment of the surface with a similar PANI solution without PS gave Emeraldine base film with homogenously dispersed copper. Reduction of the surface copper by diluted hydrazine (5%) yielded zero-valent copper serving as seed points for accumulation of more copper from an electroless plating solution in the following process. Experiments showed that, the method presented offers a simple pathway to produce excellent copper deposits on PS substrate. This method is superior to traditional electroless plating process, since tedious surface etching and expensive palladium activation steps are being avoided. The surface characteristics were examined by X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), adhesion tests and contact angle measurements. The results showed that, the electroless plating process gives a homogeneous and highly robust copper layer with 34.2 μm of thickness within 48 h. Adhesion of the copper layer to the underlining surface was satisfactory as inferred from pull-off measurements (1.6 N/mm²).     

镀铜石墨粉的制备研究

表面镀铜的非金属材料是当前功能材料开发的一个热点.利用化学镀的方法在石墨粉的表面进行化学镀铜,通过对化学镀铜沉积速度和镀层表面形貌进行分析,探讨了如何获得表面包覆良好的镀层.石墨粉表面化学镀铜工艺可以分为表面预处理、化学镀和性能测试三大步骤.研究重点放在化学镀施镀步骤上,对化学镀铜的影响因素进行了研究,得出最佳的镀铜工艺配方,并将此配方应用于实际,得到了色泽光亮、分散性好的石墨镀铜粉.     

氧化铝陶瓷基板化学镀铜工艺优化

目的化学镀铜是氧化铝陶瓷基板金属化的一种重要手段,为了进一步优化氧化铝陶瓷基板化学镀铜工艺,研究了化学镀铜液配比(尤其是镀液中铜离子和甲醛含量)对氧化铝陶瓷覆铜板微结构和导电性的影响。方法在对氧化铝陶瓷基板经过前期处理后,采用化学镀铜法在基板上镀铜。采用X射线衍射仪、光学显微镜对氧化铝基板上的化学镀铜层物相和形貌进行观察。采用覆层测厚仪、四探针测试仪对化学铜镀层的膜厚和方阻进行测量。结果 XRD结果表明,不同配比镀液得到的化学镀铜层均具有较好的晶化程度,镀液中甲醛和铜含量较低的镀液可制备出晶粒更为细小的化学镀铜层。甲醛和铜离子含量均较高时,沉积速度过快,使镀铜层的均匀性和致密性不佳。但当甲醛含量较高、铜离子含量较低时,沉积速度适中,从而获得了均匀性和致密性较好的镀铜层,同时这种镀层具有良好的导电性。结论采用表面活性化学镀铜工艺,当镀液中甲醛浓度为0.25 mol/L和硫酸铜质量浓度为1.2 g/L时,无需高温热处理,即获得了均匀性和致密性俱佳的铜镀层,可满足覆铜板的使用要求。     

PRIMARY STUDY FOR THE TECHNOLOGY OF ELECTROLESS PLATING Fe Al P ALLOYS

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