NaOH和NiSO_4添加剂浓度对短碳纤维化学镀银结构和导电率的影响
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摘要
目的制备镀层均匀、结合力好的短碳纤维镀银层。方法以葡萄糖为还原剂,在短碳纤维表面进行化学镀银,研究了NaOH浓度、NiSO_4添加剂浓度对短碳纤维化学镀银层结构和性能的影响。采用X射线衍射仪、扫描电子显微镜对镀银碳纤维的结构、形貌和成分进行分析,测试了镀银后纤维的密度、导电率。采用冷热循环法评估镀层与碳纤维的结合强度。结果增大NaOH浓度可提高银氨络合物离子浓度,加快了反应速率。合适的NaOH浓度有助于获得高质量的镀银层,低浓度和高浓度NaOH条件下均会产生漏镀和镀层不均匀现象,导致镀银碳纤维性能的降低。NiSO_4添加剂加入到溶液中后,Ni~(2+)将优先吸附在碳纤维表面,这不仅增大了碳纤维表面银单质的形核率,同时也降低了反应速率。合适的NiSO_4浓度有助于改善银镀层的质量,低浓度和高浓度NiSO_4条件下得到的镀层性能均不足。结论 NaOH质量浓度为7g/L时获得的镀银层分布均匀,结晶度良好,密度较大,导电率也较好。NiSO_4浓度为5×10~(-5) mol/L时能获得光滑、均匀、平整的镀层,密度最大,导电率最优。
The work aims to prepare the short carbon fiber silver layer with good uniformity and binding force. The silver-coated short carbon fibers were prepared by plating methods with glucose as reducing agent. The effects of NaOH and NiSO_4 concentrations on the microstructure and properties of the silver-plated layers were studied. X-ray diffraction method and scanning electron microscopy were used to analyze the microstructure, morphology and composition of the electroless plated silver layers. The density and conductivity of silver-plated fibers were tested. The hot and cold cycling test method was employed to evaluate the bonding strength between the silver-plated layers and the short carbon fibers. Increasing NaOH concentrations led to the increase of the silver-ammonium complex ions, and thus accelerated the reaction rate. Proper NaOH concentration was beneficial to obtaining high-quality silver-plated layer. However, the leakage plating phenomena and coating unevenness occurred under both low and high concentrations of NaOH, which reduced the performance of silver-plated carbon fiber. The Ni~(2+) ions in NiSO_4 additives could be adsorbed on the surface of the carbon fibers prior to other particles. This could improve the nucleation rates during silver depositions. However, the high concentrations of NiSO_4 additives depressed the reaction rate of silver depositions. When NaOH concentration is 7 g/L, uniform silver-plated layer with good crystallinity, large density and better conductivity can be obtained. When 5×10~(-5) mol/L NiSO_4 is selected, the smooth, uniform and flat silver-plated layer with the highest density and the best conductivity can be produced.
The work aims to prepare the short carbon fiber silver layer with good uniformity and binding force. The silver-coated short carbon fibers were prepared by plating methods with glucose as reducing agent. The effects of NaOH and NiSO_4 concentrations on the microstructure and properties of the silver-plated layers were studied. X-ray diffraction method and scanning electron microscopy were used to analyze the microstructure, morphology and composition of the electroless plated silver layers. The density and conductivity of silver-plated fibers were tested. The hot and cold cycling test method was employed to evaluate the bonding strength between the silver-plated layers and the short carbon fibers. Increasing NaOH concentrations led to the increase of the silver-ammonium complex ions, and thus accelerated the reaction rate. Proper NaOH concentration was beneficial to obtaining high-quality silver-plated layer. However, the leakage plating phenomena and coating unevenness occurred under both low and high concentrations of NaOH, which reduced the performance of silver-plated carbon fiber. The Ni~(2+) ions in NiSO_4 additives could be adsorbed on the surface of the carbon fibers prior to other particles. This could improve the nucleation rates during silver depositions. However, the high concentrations of NiSO_4 additives depressed the reaction rate of silver depositions. When NaOH concentration is 7 g/L, uniform silver-plated layer with good crystallinity, large density and better conductivity can be obtained. When 5×10~(-5) mol/L NiSO_4 is selected, the smooth, uniform and flat silver-plated layer with the highest density and the best conductivity can be produced.
引文
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[2]高嵩,姚广春.化学镀铜前碳纤维预处理的研究[J].材料保护,2005,38(7):43-45.GAO Song,YAO Guang-chun.Pretreatment of carbon fiber for electroless copper plating[J].Materials protection,2005,38(7):43-45.
[3]ZHANG Y H,WU G H.Interface and thermal expansion of carbon fiber reinforced aluminum matrix composites[J].Transactions of Nonferrous Metals Society of China,2010,20(11):2148-2151.
[4]易增博,冯利邦,郝相忠,等.表面处理对碳纤维及其复合材料性能的影响[J].材料研究学报,2015,29(1):67-74.YI Zeng-bo,FENG Li-bang,HAO Xiang-zhong,et al.Effect of surface treatment on properties of carbon fiber and reinforced composites[J].Chinese journal of materials research,2015,29(1):67-74.
[5]CHEN H,LIU G,XU C,et al.Copper@carbon fiber composites prepared by a simple electroless plating technique[J].Materials letters,2016,173:211-213.
[6]LIU L,TANG Y,ZHAO H,et al.Fabrication and properties of short carbon fibers reinforced copper matrix composites[J].Journal of materials science,2008,43(3):974-979.
[7]RAMS J,URE?A A,ESCALERA M D,et al.Electroless nickel coated short carbon fibres in aluminium matrix composites[J].Composites part A:Applied science&manufacturing,2007,38(2):566-575.
[8]WAN Y Z,WANG Y L,LUO H L,et al.Effect of metal diffusion barrier on thermal stability of metal-coated carbon fibers[J].Journal of materials science,2001,36(11):2809-2814.
[9]唐爱东,李传常,周涛.化学镀银在材料表面金属化中的应用[J].电镀与精饰,2007,26(10):20-24.TANG Ai-dong,LI Chuan-chang,ZHOU Tao.Application of electroless silver plating to metallization of material surface[J].Electroplating&finishing,2007,26(10):20-24.
[10]WANG W,LI W,GAO C,et al.A novel preparation of silver-plated polyacrylonitrile fibers functionalized with antibacterial and electromagnetic shielding properties[J].Applied surface science,2015,342:120-126.
[11]刘延坤,冯玉杰,高培源,等.碳纤维表面化学镀银工艺的研究[C]//全国功能材料学术年会专辑.兰州:[出版者不详],2006.LIU Yan-kun,FENG Yu-jie,GAO Pei-yuan,et al.Study on electroless silver plating on carbon fiber surface[C]//National Functional Materials Academic Annual Conference Album.Lanzhou:[s.n],2006.
[12]关华,潘功配,侯伟,等.碳纤维布化学镀银工艺的优化[J].电镀与涂饰,2008,27(1):20-23.GUAN Hua,PAN Gong-pei,HOU Wei,et al.Optimization of electroless silver plating process on carbon fiber fabric[J].Electroplating&finishing,2008,27(1):20-23.
[13]WANG C,ZHAO M,LI J,et al.Silver nanoparticles/graphene oxide decorated carbon fiber synergistic reinforcement in epoxy-based composites[J].Polymer,2017,131:263-271.
[14]HE J,HUANG Y,LI L,et al.Controlled interface between carbon fiber and epoxy by molecular self-assembly method[J].Materials chemistry&physics,2006,99(2):388-393.
[15]YU D,MU S,LIU L,et al.Preparation of electroless silver plating on aramid fiber with good conductivity and adhesion strength[J].Colloids and surfaces A:Physicochemical and engineering aspects,2015,483:53-59.
[16]CAI J,LAN M,ZHANG D,et al.Electrical resistivity and dielectric properties of helical microorganism cells coated with silver by electroless plating[J].Applied surface science,2012,258(22):8769-8774.
[17]黄少强,邱文革,李生华.非金属材料表面化学镀银[J].北京工业大学学报,2005,31(1):75-80.HUANG Shao-qiang,QIU Wen-ge,LI Sheng-hua.Electroless silver plating on the surface of nonmetallic materials[J].Journal of Beijing University of Technology,2005,31(1):75-80.
[18]张乾,谢发勤.碳纤维的表面改性研究进展[J].金属热处理,2001,26(8):1-4.ZHANG Qian,XIE Fa-qin.Review of carbon fiber’s surface modification progress[J].Heat treatment of metals,2001,26(8):1-4.
[19]曾大海,张鹏,李卫.石墨纤维表面镀铜工艺及性能研究[J].功能材料,2016,47(4):218-224.ZENG Da-hai,ZHANG Peng,LI Wei.Study on copper plating and properties on surface of graphite fiber[J].Journal of functional materials,2016,47(4):218-224.
[20]胡健.银/碳复合纳米纤维的制备及其导电性能的研究[D].哈尔滨:哈尔滨工业大学,2013.HU Jian.Research on preparation of silver/carbon composite nanofibers and their conductive properties[D].Harbin:Harbin Institute of Technology,2013.
[21]MERGA G,WILSON R,LYNN G,et al.Redox catalysis on“naked”silver nanoparticles[J].Physics chemistry,2007,111(33):12220-12226.
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