Metallization of Kevlar fibers with gold

Electrochemical gold plating processes were examined for the metallization of Kevlar yarn. Conventional Sn(2+)/Pd(2+) surface activation coupled with electroless Ni deposition rendered the fibers conductive enough to serve as cathodes for electrochemical plating. The resulting coatings were quantified gravimetrically and characterized via adhesion tests together with XRD, SEM, TEM; the coatings effect on fiber strength was also probed. XRD data showed that metallic Pd formed during surface activation whereas amorphous phases and trace amounts of pure Ni metal were plated via the electroless process. Electrodeposition in a thiosulfate bath was the most efficient Au coating process as compared with the analogous electroless procedure, and with electroplating using a commercial cyanide method. Strongly adhering coatings resulted upon metallization with three consecutive electrodepositions, which produced conductive fibers able to sustain power outputs in the range of 1 W. On the other hand, metallization affected the tensile strength of the fiber and defects present in the metal deposits make questionable the effectiveness of the coatings as protective barriers.     

铜铁界面含氧层对镀层结合强度的影响

镀层与基体界面间含氧层的存在,影响电镀层与基体之间金属键的形成,进而影响镀层的结合强度.用氰化物和焦磷酸盐两种工艺在铁片上镀铜,对镀层进行恒电流极化,并以氩离子深度刻蚀和X射线光电子能谱相结合的方法进行检测.电沉积初始电位-时间曲线显示,两种镀铜工艺,结合强度好的出现了基体表面的还原活化电位平阶,结合强度差的焦酸盐镀铜未出现活化就发生了金属的电沉积,而且铜镀层与基体界面含氧量有增高的现象.铜镀层与铁基底界面间含氧层的存在是影响镀层结合强度的主要原因.通过控制金属电沉积初始电位可提高镀层的结合强度.     

Investigation of solar selective and microstructural properties of molybdenum black immersion coatings on cobalt substrates

Molybdenum black solar selective coatings have been produced on cobalt by immersion in a solution of ammonium paramolybdate and nickel sulphate. The cobalt was electroplated on nickel-plated copper prior to immersion in the paramolybdate solution. The maximum solar absorptance of the resulting molybdenum black coating was about 0.91. The minimum emittance was about 0.1 for coatings on cobalt deposited with an addition agent and about 0.23 for coatings on cobalt deposited without addition agent in the 60 °C plating solution. These differences have been related to the coating morphology determined by scanning electron microscopy. The emittance of coatings on cobalt deposited without addition agent decreases (or remains unchanged) during short-term heat treatment while that of coatings deposited on cobalt plated with addition agent increases somewhat. Reduction of the cobalt plating bath temperature to 45 °C can also lead to good initial coating properties but without the requirement for an addition agent in the cobalt plating bath. XPS studies show that the oxidation state of molybdenum in the coatings is approximately + 5 corresponding to Mo₄O₁₁. This reduces to + 4 after argon ion bombardment. Some cobalt may be present in the coatings in the form of CoO.     

氧化铝陶瓷局部活化及选择性化学镀铜的研究

为解决陶瓷表面局部化学镀存在的问题,研制了一种针对氧化铝陶瓷局部化学镀铜前处理用的活化胶,其由具有活化能力的银盐(或钯盐)和粘稠的复合物有机载体组成.将活化胶印于氧化铝陶瓷表面,经500℃高温烧结形成局部活化层后,可直接置于化学镀液中进行镀铜处理,得到与印刷图形一致的局部镀铜层.利用电化学工作站测定样品在化学镀铜溶液中电位随时间的变化情况,考察不同活化条件对Cu2+还原的催化活性,利用SEM/EDS进行表面形貌及成分分析,确定了活化胶中银盐和钯盐的适宜浓度.结果表明,该两种活化胶应用于氧化铝陶瓷表面化学镀铜的活化工艺,可实现敏化活化的一步化,使陶瓷表面局部化学镀工艺流程简化,成本降低,具有较高的实用价值.     

纳米螺旋碳纤维表面化学镀Ni-Co-B涂层研究

利用铁片试样研究以二甲基胺硼烷为还原剂的化学镀Ni-Co-B合金涂层的工艺,考察了还原剂、金属盐浓度之比、pH值对化学镀反应沉积速率的影响.利用优化的工艺配方在经过敏化、活化处理后的纳米螺旋碳纤维表面沉积Ni-Co-B合金涂层.采用等离子发射光谱仪(ICP)分析涂层成分,利用扫描电子显微镜(SEM)观察涂层形貌,利用振动样品磁强计测试涂层磁学性能(VSM).结果表明:在纳米螺旋碳纤维表面获得了连续、均匀的Ni-Co-B合金涂层,材料磁性明显改善.     

Preparation and Research of Electroless Copper on Carbon Fibers

In this paper, Cu coated carbon fibers were prepared using the electroless plating method. Effects of pretreatment, dispersing capability, formaldehyde, temperature, and pH on electroless plating process were studied. The connection between the Cu²⁺ concentration in the electroless plating solution and the plating time at different temperatures was studied. The process of the electroless Cu plating was analyzed and calculated, which derived the activation energy of the electroless copper plating on carbon fibers: Ea = 32.68 kJ/mol. The effect of the mass of carbon fibers and Cu coated carbon fibers which were dispersed in 80 mL distilled water on the conductivity of the solution was also studied. And as a result, the conductivity of the solution increased with the amount increasing. However, when the amount of the fibers was more than 0.08 g, the fibers would be incompletely dispersed. Thus, it could be concluded that the best accession amount of carbon fibers in 80 mL distilled water was 0.08 g. The corresponding conductivity values of carbon fibers and copper-coated fibers were 12.5 and 20.5 µs/cm, respectively.     

碳纤维表面电镀铜工艺的研究

首先对碳纤维进行氧化处理,然后尝试采用三种电镀工艺对碳纤维进行电镀铜处理,并对处理结果进行SEM观察与分析.氧化结果表明:单一氧化处理结果并不理想,采用气相-液相联合氧化法效果良好.电镀铜处理结果表明:采用普通酸性镀铜工艺,镀层组织粗大且易脱落,碳纤维易出现"结块"现象;采用焦磷酸盐电镀工艺易出现"黑心"现象;采用柠檬酸盐电镀工艺效果最佳,镀层均匀致密且界面结合力强,有效避免了电镀过程中的"结块"和"黑心"现象,实现成束碳纤维的均匀镀.     

Fabrication of conductive copper-coated glass fibers through electroless plating process

A simple electroless copper plating process was employed to prepare copper-coated glass fibers with excellent conductivity. The glass fibers were pretreated by etching, sensitizing, and activating procedures. Disodium ethylenediamine tetra acetate (EDTA-2Na) and hydrazine hydrate (N₂H₄·H₂O) were employed as complex reagent and reductant, respectively. It was found that the copper deposition was greatly influenced by dosage of EDTA-2Na, concentration of sodium hydroxide (NaOH), temperature, and volume of N₂H₄·H₂O. The optimal temperature for electroless copper plating ranged from 40 to 60 °C. The composites were characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy techniques. The result showed that the minimum volume resistivity of 0.0010 Ω cm was obtained for the sample with perfect copper coatings on the surface of glass fibers. This method is simple, low-cost, and large production, and can be extended to fabricate other metal-coated glass fibers with distinct conductivity.     

Facile electroless copper plating on diamond particles without conventional sensitization and activation

Conventional electroless plating of copper on diamond particles needs SnCl₂ sensitization and PdCl₂ activation pretreatments, which needs noble metal and consumes a large amount of reducing agent. In this paper, metallic tungsten coatings were first plated onto diamond particles by microwave-heating salt-bath plating (MHSBP) method, and then copper layer was directly plated onto the out surface of the tungsten layer by an electroless plating method with no need of SnCl₂ sensitization and PdCl₂ activation pretreatments. Composition and morphology of the coatings was analyzed by XRD, SEM, and EDS. The results show that the copper coating on the diamond surfaces can be adjusted by control the concentration of CuSO₄·5H₂O and plating temperature, and a full copper coating is achieved with content of CuSO₄·5H₂O of 19.6 g/L in the plating solution at 60 °C. The bending strength of the coated diamond/Cu composites is as high as 630 MPa, which increases 93.3% than the uncoated composites. This work presents an electroless plating of copper can directly on the surfaces of diamond particles with no need of conventional sensitization and activation, and a strong interface combination between coated diamond and copper.     

Effect of the incorporation of interfacial elements on the thermophysical properties of Cu/VGCNFs composites

Vapour grown carbon nanofibres exhibit high mechanical properties and thermal conductivities. Therefore they are potential reinforcements in composites materials for high strength and high thermal conductivity applications. A problem not yet solved is the promotion of an improved copper/carbon interface. Several strategies have been envisaged for the incorporation of alloying elements (Ni, Co, B and Ti) at the interface. These techniques are based on duplex electroless plating coatings (combination of Cu and Ni or Cu and Co), electroless plating of alloys (Cu-B) and addition of metal nanoparticles (Ti) to Cu matrix deposited by electroless plating. The effect of the incorporation of these metallic elements on the microstructure and thermophysical properties is discussed. B and Ti lead to higher interaction at the Cu/C interface over Ni and Co. This allows the reduction of the coefficient of thermal expansion but regarding the thermal conductivity it was not possible to obtain a value higher than that of copper.     

碳纤维涂层技术进展

本文对金属基复合材料用增强碳纤维的涂层技术研究作了综述。讨论了用电镀、化学镀、化学气相沉积、溶胶-凝胶、热扩散和热浸等技术获得金属、氧化物、碳化物、氮化物及硼化物纤维涂层的状况并指出了存在的问题及可能的解决途径。     

Effect of process parameters on coating composition of cathodic-plasma-electrolysis-treated copper

Cathodic plasma electrolysis is a novel technique to form nanostructured layers on metallic surfaces by application of high voltage in a suitable aqueous electrolyte. In the present study, copper is treated by plasma electrolysis in 50 vol% ethanol electrolyte and coatings comprising carbon nanostructure and copper oxide are formed on the copper. The effect of some process parameters such as electrical conductivity, volume and temperature of electrolyte and ratio of anode to cathode surface area on current–voltage behaviour and subsequently coating compositions are investigated at 150 V deposition voltage. The composition and morphology of these coatings are characterized by X-ray diffraction, Raman spectroscopy and scanning electron microscopy. Different current–voltage behaviours, temperatures of substrate and the contents and energies of radicals and ions around the substrate by changes in the mentioned parameters cause different compositions from 100 vol% copper oxide to different ratios of copper oxide to carbon, the structure changing from amorphous to graphitic structure in carbon and amorphous to cubic morphology in copper oxide on the substrate. Therefore, the understanding of cathodic plasma electrolysis can be developed.     

碳纤维表面化学镀镍工艺及机理研究

研究了碱性条件下碳纤维表面化学镀镍工艺及机理。结果表明随着施镀温度的升高,pH值的增大,络合剂含量的减少,金属镍的沉积速率越大,但是镀液稳定性越差;碳纤维表面化学镀镍过程有明显的诱导期、加速期、减速期和稳定期4个阶段,并且当沉积时间过长、温度过高、pH值越大时,镀层出现胞状沉积结构。实验条件下,反应速率方程V=K[OH-]a[Na6H5O7]b[Ni 2＋]c[H2PO2-]dexp（-Ea/RT）中的[OH-]反应级数a=0.26565,[Na6H5O7]的反应级数b=-0.23287,表面活化能Ea=61.034kJ/mol。     

化学镀镍碳纤维/环氧树脂复合材料电磁屏蔽性能

采用化学镀方法对碳纤维进行表面镀镍, 采用SEM、 EDX、 XRD分析了镀镍碳纤维的微观形貌、 镀层成分和镀层结构, 通过电阻测试研究了镀镍碳纤维的导电性。将体积分数为2.5%、 5%、 7.5%、 10%的镀镍碳纤维作为导电填料制备镀镍碳纤维/环氧树脂复合材料, 并用屏蔽室法测试了不同频段复合材料的屏蔽效能。结果表明: 碳纤维化学镀镍后, 表面形成了一层均匀的复合镀层, 镀层中镍的质量分数高达94%, 镀镍碳纤维的电阻值仅为碳纤维原丝的1/54。镀镍碳纤维/环氧树脂复合材料的电磁屏蔽能力较碳纤维原丝有所提高。复合材料的屏蔽效能随镀镍碳纤维添加量的增加而升高。在低频频段(kHz频段), 复合材料的屏蔽能力主要决定于材料的本征参数, 不同镀镍碳纤维含量的镀镍碳纤维/环氧树脂复合材料的屏蔽能力相差不大; 在中高频频段(MHz、 GHz频段), 镀镍碳纤维/环氧树脂复合材料屏蔽效能主要决定于材料的电阻率。     

碳纤维表面化学镀铜工艺研究

传统的化学镀铜以甲醛作还原剂,污染环境.以环保型还原剂次亚磷酸钠代替甲醛,加入各种不同的稳定剂在碳纤维表面进行化学镀铜,获得了具有一定厚度、均匀、光亮的铜镀层.研究了镀液pH值、温度及还原剂、配位剂、稳定剂用量对化学镀铜溶液稳定性和碳纤维增重率的影响,确定了新的镀铜配方.用扫描电子显微镜(SEM)、X射线衍射仪(XRD)、能谱、冷热循环处理等手段,分析了化学镀铜层的微观形貌、结构及成分.结果表明,通过此新型的环保镀液配方和工艺条件,可获得光亮、致密、均匀及含铜量较高的镀层.     

焦磷酸盐镀铜生产工艺(Ⅲ)

13常见故障及其排除方法[1,4,12] 13.1镀层粗糙、毛刺和结瘤 基体金属或预镀层粗糙;镀液中有"铜粉"或其他固体悬浮粒子;镀液中有机杂质过多,铅等异金属杂质过多或被CN-沾污;镀液pH值太高;温度偏高;电流密度过大;阳极溶解不正常;铜含量过高或焦磷酸钾含量过低等都会引起镀层粗糙、毛刺和结瘤.     

焦磷酸盐镀铜生产工艺(Ⅰ)

对焦磷酸盐镀铜的前处理、预镀、焦磷酸盐镀铜的工艺配方、操作条件及原理、镀液的配制、镀液成分及其作用、操作条件对镀层的影响、镀液的维护、杂质的影响及其排除方法、镀液成分失调的影响与纠正、磷酸根对镀液和镀层的影响、铜粉的产生及其排除、常见故障及其排除方法等都作了详细阐述.此外,对镀铜液中磷酸根和焦磷酸根的分析方法以及不合格铜层的退除也作了一定的介绍.     

焦磷酸盐镀铜生产工艺(Ⅱ)

7 操作条件对镀层的影响 7.1 pH值 pH值是焦磷酸盐镀铜很重要的工艺参数,不同pH值时会有不同形式的配合物出现,为保证得到所需要的浓度最高配位数的配合物形式,就需要严格控制pH值在规范之内.     

铜镀层复合材料的吸波性能

以2种织物材料为基材,采用化学镀铜的方法,进行铜镀层和吸波涂层复合材料的试验研究。分析了铜镀层的成分结构、织物种类、叠层顺序等因素对复合材料在9. 35 GHz下反射率的影响规律,并探讨了铜镀层对吸波特性的影响机制。研究表明,对于织物基材先涂敷吸波涂层再化学镀铜的复合结构,与未氧化的铜镀层相比,空气中氧化8天的铜镀层使无纺布吸波复合材料的反射率峰值由 - 11 dB降低至 - 13. 2 dB。对于织物基材先化学镀铜再涂敷吸波涂层的复合结构,40℃ 镀铜与常温镀铜相比,在反射率曲线峰值接近的情况下,吸波材料总厚度下降了约 1. 4 mm,说明铜镀层可用于改进吸波材料的微波吸收效果。      

促进剂及其优化对化学镀Ni-Sn-P层性能的影响

为了提高Ni-Sn-P化学镀层的沉积速率与镀液的稳定性,采用化学镀Ni-P合金复合稳定剂,研究了促进剂丙酸、甘氨酸、丁二酸对化学镀Ni-Sn-P镀层性能的影响,通过正交试验对3因素进行了优化,对镀速、孔隙率及显微硬度进行了测定.结果表明:甘氨酸、丙酸和丁二酸对镀层加速越快,镀层孔隙率越低、硬度越高;甘氨酸、丙酸对化学镀Ni-Sn-P加速显著;甘氨酸和丁二酸对镀层硬度都有所提高,而丙酸对Ni-Sn-P镀层硬度影响较小;甘氨酸、丙酸和丁二酸使化学镀Ni-Sn-P镀层的孔隙率都有不同程度降低,其中甘氨酸和丙酸作用显著;当甘氨酸为25 mg/L、丙酸为4 mL/L、丁二酸为2.5 g/L时,镀速提高至14～15 μm/h,硬度为480～550 HV0.5 N,孔隙率几乎为0.