目的 在连续氧化铝纤维（Al2O3f）表面制备均匀、致密化的金属铜涂层;系统研究连续氧化铝纤维表面覆铜的影响因素,确定最佳的Al2O3f表面涂层施镀方案。方法 采用化学镀方法在连续Al2O3f表面成功制备了铜涂层。采用扫描电子显微镜（SEM）和能量色散X射线光谱（EDS）技术,深入分析涂层的微观形貌和元素组成。测试分析了化学镀后Al2O3f增重率、电阻值和涂层微观形貌;综合探讨研究了化学镀主盐、络合剂、还原剂的种类、浓度及KOH的浓度对连续Al2O3f表面铜涂层性能的影响。结果 主盐为CuSO4时,形成连续均匀的铜涂层。络合剂为NaKC4H4O6时,形成连续完整的铜涂层。还原剂为CH2O时,纤维表面形成连续致密的铜涂层。涂层纤维电阻值随KOH浓度的增大呈下降趋势,增重率随着KOH浓度的增大呈上升趋势,镀液中KOH的最佳浓度为9 g/L。施镀时间可以分为三个阶段,表面涂层成长期时纤维从绝缘状态逐渐转变为导电状态;成熟期时电阻值稳定下降,并保持一个较低的水平;衰退期时电阻值上下波动。结论 1）制备出的表面涂层具有明确的“芯-壳”结构,芯部为氧化铝纤维、表层为完整的铜涂层（Al2O3f@Cu）;2）实验条件下,当CuSO4为主盐、NaKC4H4O6为络合剂、CH2O为还原剂,KOH浓度9 g/L时,纤维表面铜涂层均匀、光滑、致密、完整。最佳施镀时间为10 min。
Abstract
Uniform and dense copper coatings are fabricated on the surface of continuous Al2O3 fibers (Al2O3f) by chemical plating. The influence factors of surface coating of copper on continuous alumina fibers are systematically studied, and the best coating deposition scheme of Al2O3f surface is determined. The prepared copper coating improves the wettability between the metal and alumina fibers, and expands the functional application of electrical, magnetic and so on. The microscopic morphology and elemental analysis of the coating are analyzed by SEM and EDS. The fiber weight gain rate after plating, fiber resistance, and surface coating morphology are tested and analyzed. The influences of the kinds and concentration of the main salt, complexing agent, reducing agent, and KOH concentration on the properties of the copper coating on Al2O3f surface prepared by chemical plating are comprehensively investigated and explored. When the main salt is CuSO4, the copper coating on the fiber surface is continuous, uniform and dense; when the main salt is CuCl2, there is only a granular coating on the fiber surface and it is not continuous; when the main salt is Cu(NO3)2, the surface does not form a continuous and complete coating. When no complexing agent is added, the coating is very easy to fall off; when NaKC4H4O6 is used as the complexing agent, Cu2+ can be uniformly and orderly deposited on the surface of the fiber to form a complete and continuous copper coating; when EDTA-2Na is used as the complexing agent, the coating on the fiber surface is thinner and there is a shedding; when double complexing agent is used, the coating on the fiber surface is thinner, and the deposited particles are different sizes and discontinuous. When there is no reducing agent in the plating solution, the fiber has no weight gain and is in an insulating state; when sucrose and glucose are used as reducing agents, there is almost no copper deposition on the fiber surface; when CH2O is used as the reducing agent, it can be observed that there is a uniform, dense and complete copper coating on the fiber surface. The resistance of the plated fibers shows an overall decreasing trend with the increase of KOH concentration, and the fiber weight gain rate shows an increasing trend with the increase of KOH concentration, and the optimal concentration of KOH in the plating solution is 9 g/L. The plating time can be divided into three stages, the surface coating growth period when the fibers are gradually transformed from an insulating state to a conductive state; the maturity period when the fiber surface resistance is in a stable state and decreases steadily with the increase of plating time; the decline period when the resistance is gradually changed from an insulating state to a conductive state. In the mature stage, the resistance of fiber surface is stable and decreases with the increase of plating time; in the decline stage, the resistance fluctuates up and down. The prepared surface coating has a clear "core-shell" structure, with an alumina core and a complete copper coating on the surface (Al2O3f@Cu); Under the experimental conditions, the copper coating is uniform, smooth, dense and complete on the surface of alumina fibers at KOH concentration of 9 g/L, with a resistance as low as 0.15 Ω/cm after plating, with CuSO4 as the main salt, NaKC4H4O6 as the complexing agent and CH2O as the reducing agent. At KOH concentration of 9 g/L, the copper coating on the surface of alumina fiber is uniform, smooth, dense and complete, and the weight gain rate of Al2O3f reaches 31% after plating, with the resistance as low as 0.15 Ω/cm. Meanwhile, the quality of the plating layer is qualitatively evaluated by the resistance, and the optimal plating application time is determined. The plating time of 10 min results in a uniform and complete coating with a low resistance of 0.15 Ω/cm.
关键词
氧化铝纤维 /
化学镀 /
铜涂层 /
Al2O3f@Cu /
电阻值 /
增重率
Key words
alumina fiber /
chemical plating /
copper coating /
Al2O3f@Cu /
resistance /
weight gain rate
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基金
国家自然科学基金（51201060）; 江苏省科技项目（BE2021056）; 姑苏创新创业领军人才计划（ZXL2021070）
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