合金镀层对碳纤维催化石墨化研究
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摘要
碳纤维是一种新型的高性能增强材料,它具有低密度、高强度、高模量、耐高温、抗化学腐蚀、低电阻、高导热、低热膨胀、耐化学辐射和良好的生物相容性等特性。主要用作树脂、碳、金属、陶瓷、水泥基复合材料的增强体,在航空航天、汽车工业、土木建筑、文体器材、医疗器材等方面应用非常广泛。而碳纤维表面金属化可进一步拓展其应用范围。碳纤维石墨化后其性能得到极大增强,但较高的热处理温度一直是影响石墨纤维价格的主要因素。通过添加催化剂可以降低热处理温度使得碳纤维石墨化过程更加容易进行。而如何添加催化剂一直是研究的热点。碳纤维催化石墨化研究一般都集中在单元素催化,而对于多元催化研究甚少。本文针对以上问题,研究并开发了碳纤维表面电沉积合金工艺,并就碳纤维表面电沉积合金催化剂对其催化石墨化进行了深入的探讨。研究工作主要包括以下几个方面:
1.研究了碳纤维表面电沉积Ni-B合金工艺,结果表明碳纤维的预处理、镀液组分以及电解参数对沉积速度及镀层质量有明显的影响。通过扫描电子显微镜(SEM)、X射线衍射(XRD)、电感耦合等离子体发射光谱仪(ICP-AES)对镀层的微观形貌、结构及组分进行了分析,结果表明在确定的电镀条件下可获得镀层中B的质量分数为0.8%～4%的Ni-B微晶镀层,且镀层细致、均匀、致密、结合力好。
2.研究了碳纤维表面电沉积Ni-B合金对其催化石墨化的影响。将镀有含B质量分数为4%的Ni-B合金的碳纤维和碳纤维原丝在不同温度下热处理,通过XRD、激光拉曼(Raman)光谱、SEM对其结构进行分析,结果表明:有Ni-B催化剂的碳纤维在较低的热处理温度下能获得较高的石墨化度,而碳纤维原丝即使在很高的热处理温度下石墨化程度也很低,Ni-B合金对碳纤维有很好的催化石墨化效果。改变镀层中B含量,在相同温度下热处理,研究结果表明:随着镀层中B含量的增加,碳纤维石墨化程度相应增大,Ni和B有很好的协同催化效果。另外,还对Ni-B合金的催化石墨化机理进行了探讨。
3.研究了碳纤维表面电沉积Fe-P合金对其催化石墨化的影响。将镀有含P质量分数为7%的Fe-P合金的碳纤维在不同温度下热处理,通过XRD、Raman光谱、SEM对其结构进行分析,结果表明:碳纤维在较低的热处理温度下能获得很高的石墨化度,随着热处理温度的增加,碳纤维石墨化度相应增大,Fe-P合金对碳纤维有很好的低温催化石墨化效果。改变Fe-P合金中P的含量,在相同温度下热处理,研究结果表明:随着镀层中P含量的增加,碳纤维石墨化程度相应增大。改变Fe-P合金催化剂的沉积时间,在相同温度下热处理,研究结果表明:随着沉积时间的增加,碳纤维石墨化程度逐渐增大。而当催化剂达到一定的量后,其石墨化程度基本不变。另外,还对Fe-P合金的催化石墨化机理进行了探讨。
Carbon fibers are a new type of high-performance reinforced material which has characteristics of low density, high strength, high modulus, resistance to high-temperature, good chemical anti-corrosion, low resistance, high thermal conductivity, low thermal expansion, resistance to chemical radiation and good biocompatibility. Carbon fibers are used mostly as reinforced materials of resin, carbon, metal, ceramic and cement and have extensive applications in aerospace, automotive, civil engineering, cultural and sports equipment, medical devices and so on. Carbon fibers coated with metals can further expand their application scope. The properties of carbon fibers can be greatly enhanced after graphitization. However, high heat treatment temperature (HTT) to graphitization is the main factor leading to high price of graphite fibers. The graphitization temperature can be reduced and the graphitization process will be facile by adding catalysts. Studies on catalytic graphitization of carbon fibers have mainly concentrated on single elements. However, there is little research on multi-element catalytic graphitization. Electroplating alloy on the surface of carbon fibers and the catalytic graphitization mechanism of carbon fibers with electrodeposited alloy coating were studied in this paper. The main contents are presented as follows:
1. The process of electroplating Ni-B alloy on the surface of carbon fibers was investigated. The results show that the Ni-B deposits performance and deposition rate were evidently affected by pretreatment, bath composition and electrodeposition parameters. scanning electron microscope (SEM) , X-ray diffraction (XRD) and ICP-AES techniques were used to analyze the morphology, structure and composition of the Ni-B deposit. The results show that uniform, compact Ni-0.8～4 wt%B microcrystalline coatings with good adhension can be obtained under certain conditions.
2. Catalytic graphitization of carbon fibers with electrodeposited Ni-B alloy coating was studied. Carbon fibers with and without electrodeposited Ni-B coating were heat treated at different temperatures and the structural changes were characterized by XRD, Raman spectroscopy and SEM The results show that high graphitization can be achieved for carbon fibers at low heat treatment temperature (HTT) when the Ni-B coating is present. Moreover, the degree of graphitization increases with the increasing of B content in Ni-B coating for Ni-B coated carbon fibers at the same HTT. The mechanism of catalytic graphitization was discussed.
3. Catalytic graphitization of carbon fibers with electrodeposited Fe-P alloy coating was studied. Carbon fibers with electrodeposited Fe-P coating were heat treated at different temperatures and the structural changes were characterized by X-ray diffraction, Raman spectroscopy and scanning electron microscope. The results show that high graphitization can be achieved for carbon fibers at lower HTT when the Fe-P coating is present. Moreover, the degree of graphitization increases with the increasing of P content in Fe-P coating for Fe-P coated carbon fibers at the same HTT. And the degree of graphitization increases with the increasing of the electrodepositing time of Fe-P coating. But the degree of graphitization is unchanged when the catalyst reaches a certain quantity. The mechanism of catalytic graphitization was also discussed.
1.研究了碳纤维表面电沉积Ni-B合金工艺,结果表明碳纤维的预处理、镀液组分以及电解参数对沉积速度及镀层质量有明显的影响。通过扫描电子显微镜(SEM)、X射线衍射(XRD)、电感耦合等离子体发射光谱仪(ICP-AES)对镀层的微观形貌、结构及组分进行了分析,结果表明在确定的电镀条件下可获得镀层中B的质量分数为0.8%～4%的Ni-B微晶镀层,且镀层细致、均匀、致密、结合力好。
2.研究了碳纤维表面电沉积Ni-B合金对其催化石墨化的影响。将镀有含B质量分数为4%的Ni-B合金的碳纤维和碳纤维原丝在不同温度下热处理,通过XRD、激光拉曼(Raman)光谱、SEM对其结构进行分析,结果表明:有Ni-B催化剂的碳纤维在较低的热处理温度下能获得较高的石墨化度,而碳纤维原丝即使在很高的热处理温度下石墨化程度也很低,Ni-B合金对碳纤维有很好的催化石墨化效果。改变镀层中B含量,在相同温度下热处理,研究结果表明:随着镀层中B含量的增加,碳纤维石墨化程度相应增大,Ni和B有很好的协同催化效果。另外,还对Ni-B合金的催化石墨化机理进行了探讨。
3.研究了碳纤维表面电沉积Fe-P合金对其催化石墨化的影响。将镀有含P质量分数为7%的Fe-P合金的碳纤维在不同温度下热处理,通过XRD、Raman光谱、SEM对其结构进行分析,结果表明:碳纤维在较低的热处理温度下能获得很高的石墨化度,随着热处理温度的增加,碳纤维石墨化度相应增大,Fe-P合金对碳纤维有很好的低温催化石墨化效果。改变Fe-P合金中P的含量,在相同温度下热处理,研究结果表明:随着镀层中P含量的增加,碳纤维石墨化程度相应增大。改变Fe-P合金催化剂的沉积时间,在相同温度下热处理,研究结果表明:随着沉积时间的增加,碳纤维石墨化程度逐渐增大。而当催化剂达到一定的量后,其石墨化程度基本不变。另外,还对Fe-P合金的催化石墨化机理进行了探讨。
Carbon fibers are a new type of high-performance reinforced material which has characteristics of low density, high strength, high modulus, resistance to high-temperature, good chemical anti-corrosion, low resistance, high thermal conductivity, low thermal expansion, resistance to chemical radiation and good biocompatibility. Carbon fibers are used mostly as reinforced materials of resin, carbon, metal, ceramic and cement and have extensive applications in aerospace, automotive, civil engineering, cultural and sports equipment, medical devices and so on. Carbon fibers coated with metals can further expand their application scope. The properties of carbon fibers can be greatly enhanced after graphitization. However, high heat treatment temperature (HTT) to graphitization is the main factor leading to high price of graphite fibers. The graphitization temperature can be reduced and the graphitization process will be facile by adding catalysts. Studies on catalytic graphitization of carbon fibers have mainly concentrated on single elements. However, there is little research on multi-element catalytic graphitization. Electroplating alloy on the surface of carbon fibers and the catalytic graphitization mechanism of carbon fibers with electrodeposited alloy coating were studied in this paper. The main contents are presented as follows:
1. The process of electroplating Ni-B alloy on the surface of carbon fibers was investigated. The results show that the Ni-B deposits performance and deposition rate were evidently affected by pretreatment, bath composition and electrodeposition parameters. scanning electron microscope (SEM) , X-ray diffraction (XRD) and ICP-AES techniques were used to analyze the morphology, structure and composition of the Ni-B deposit. The results show that uniform, compact Ni-0.8～4 wt%B microcrystalline coatings with good adhension can be obtained under certain conditions.
2. Catalytic graphitization of carbon fibers with electrodeposited Ni-B alloy coating was studied. Carbon fibers with and without electrodeposited Ni-B coating were heat treated at different temperatures and the structural changes were characterized by XRD, Raman spectroscopy and SEM The results show that high graphitization can be achieved for carbon fibers at low heat treatment temperature (HTT) when the Ni-B coating is present. Moreover, the degree of graphitization increases with the increasing of B content in Ni-B coating for Ni-B coated carbon fibers at the same HTT. The mechanism of catalytic graphitization was discussed.
3. Catalytic graphitization of carbon fibers with electrodeposited Fe-P alloy coating was studied. Carbon fibers with electrodeposited Fe-P coating were heat treated at different temperatures and the structural changes were characterized by X-ray diffraction, Raman spectroscopy and scanning electron microscope. The results show that high graphitization can be achieved for carbon fibers at lower HTT when the Fe-P coating is present. Moreover, the degree of graphitization increases with the increasing of P content in Fe-P coating for Fe-P coated carbon fibers at the same HTT. And the degree of graphitization increases with the increasing of the electrodepositing time of Fe-P coating. But the degree of graphitization is unchanged when the catalyst reaches a certain quantity. The mechanism of catalytic graphitization was also discussed.
引文
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