目的 优化多通道大丝束镍复合碳纤维连续制备工艺,解决镀镍碳纤维镀层“黑心”缺陷、多通道纤维性能不均的问题,降低镀镍碳纤维制备成本。方法 对24K碳纤维进行四通道连续电镀镍,利用管式炉在空气气氛下高温氧化去除碳纤维表面上浆剂;研究电解液温度、电镀时间、电流密度对镀镍碳纤维表面形貌和性能的影响,分析四通道镀镍碳纤维性能的一致性。结果 碳纤维在空气中高温除胶,随着温度升高,其表面残留的上浆剂逐渐减少,但碳纤维拉伸强度同步下降。电解液温度过低,镍原子形核速率受抑制,镍晶粒分布不均,导致镍层连续差、导电性不佳。随着电镀时间延长,镍晶粒尺寸增大,镍层厚度逐渐增加。电流密度可精确调控镍离子还原量,直接影响镍层的厚度均匀性、致密程度及表面粗糙度。结论 碳纤维在空气气氛中高温除胶的最佳温度为400 ℃;当电解液温度50 ℃、镀镍时间8.0 min、电流密度0.3 A/dm2时,四通道制备的24K镀镍碳纤维性能一致性良好,镍含量稳定在50%~54%（质量分数）、线电阻0.42~ 0.58 Ω/m、镍层厚度0.32~0.37 μm、电导率为1.33~1.48×106 S/m。镍镀层均匀致密,与碳纤维间界面结合紧密,镀镍碳纤维既保持了碳纤维的柔韧性,又提高了抗氧化性。相较于单通道制备24K镀镍碳纤维,本制备技术效率提高3倍,制备成本降低50%以上。该技术适用于所有规格镀镍碳纤维的制备,为大丝束镀镍碳纤维的低成本、高质量、规模化生产提供了可行的技术方案。
Abstract
The work aims to optimize multi-channel continuous nickel electroplating process for large-tow carbon fibers (CFs) and address the "black corn" defect of nickel coatings and the poor performance consistency of nickel-coated carbon fibers (CF@Ni) prepared by different channels, so as to reduce the preparation cost of CF@Ni for its large-scale industrial application. 24K carbon fiber was used as substrate material for nickel electroplating in a four-channel continuous production line. The surface sizing agent of CFs was removed before electroplating, as residual sizing agent would cause coating peeling or uneven deposition which was eliminated by high-temperature oxidation in air atmosphere with a tube furnace. The effects of electrolyte temperature, electroplating time, and current density on the surface morphology and physical properties of CF@Ni were also studied. The performance consistency of CF@Ni prepared from the four channels together was investigated through nickel content, linear resistance, coating thickness, and electrical conductivity. When CF underwent high-temperature degumming in air atmosphere, the residual sizing agent on its surface decreased continuously as the temperature rose, but its tensile strength dropped accordingly. When the electrolyte temperature was only 30 ℃, it would inhibit the nucleation rate of nickel atoms and the distribution of crystal grains, leading to discontinuous nickel coating and poor electrical conductivity. When it increased to 50 ℃, ion diffusion and reaction kinetics were optimized, resulting in dense and uniform nucleation, forming a continuous nickel coating. As electroplating time prolonged, the nickel grains on the CF surface tended to enlarge and the thickness of nickel coating increased linearly. However, excessive electroplating time caused the coating too thick, reducing the flexibility of CF@Ni. Current density precisely regulated the reduction amount of nickel ions, directly affecting the thickness uniformity, compactness and surface roughness of the nickel coating. It slowed down the reduction rate of nickel ions below 0.1 A/dm², causing thin coatings and occurrence of "black core". When the current density increased to 0.3 A/dm2, it formed a compact coating with uniform thickness on CF. However, when current density exceeded 0.4 A/dm2, it increased surface roughness and affected the corrosion resistance of CF@Ni. In terms of multi-channel performance consistency, the CF@Ni prepared under the optimized conditions from the four channels showed excellent consistency. The optimal temperature for removing the sizing agent of CF at high temperature in an air atmosphere was 400 ℃. When electrolyte temperature was 50 ℃, electroplating time was 8.0 min/m, and current density was 0.3 A/dm2, the 24K CF@Ni prepared by four channels exhibited no "black corn" defects and good performance consistency, with a nickel content maintained at 50wt.%-54wt.%, a linear resistance around 0.42-0.58 Ω/m, a nickel layer thickness of 0.32-0.37 μm per filament, and an electrical conductivity reaching 1.33- 1.48×108 S/m. The nickel coating is uniform and dense, with a tight interfacial bonding to CF. The CF@Ni retains the flexibility of CF and shows significantly improved oxidation resistance. Compared with the preparation of 24K CF@Ni by a single channel, the four-channel continuous preparation technology adopted in this work significantly improves production efficiency by 3 times, and the unit preparation cost is reduced by more than 50%. This technology is applicable to produce large-tow CF@Ni and any other specifications with the low cost, high quality, and large scale.
关键词
大丝束碳纤维 /
多通道 /
除胶 /
电解液温度 /
电流密度 /
电镀时间
Key words
large-tow carbon fiber /
multi-channel /
degumming /
electrolyte temperature /
current density /
plating time
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