碳纤维增强镍基复合材料的制备方法研究
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摘要
本文以1K聚丙烯腈纤维编制成的有纬平纹碳纤维织物作为增强体,利用化学镀的方法对纤维表面进行处理,通过等离子喷涂方法在增强体双侧表面喷涂厚度数十微米的Ni基合金,粉料为Al3%wt+Ni97%wt的微米级粒度混合粉,再经过热等静压、真空热压等致密化工艺制备出了纤维体积分数为25.7~32.8%的碳纤维增强镍基复合材料。
为增加镍金属与碳纤维的浸润性,阻止二者发生反应,采用了化学镀对碳纤维进行表面防护处理,对化学镀的前处理工艺和镀液配方进行了系统研究,得到了低含磷量的致密镀层。
采用扫描电镜(SEM)、X荧光光谱(XRF)、X射线光电子能谱(XPS)、X射线衍射(XRD)、差示扫描量热法(DSC)、能谱分析(EDS)等手段研究了碳纤维表面化学镀镍工艺和配方,并对制备出的碳纤维增强镍基复合材料的微观组织结构、相组成,高温拉伸性能进行了研究。并与未经表面镀镍的碳纤维增强镍基复合材料进行了对比分析。
结果表明,增强体经表面处理所制备的复合材料的界面强度明显高于未经表面处理的复合材料。分析发现此材料具有明显的三个特点:1.在X射线衍射分析和能谱分析都发现材料中出现氧化铝相,致使材料呈现很大的脆性;2.热压工艺过程对复合材料中纤维强度损伤很大;3.材料的高温拉伸性能不理想,原因主要是热压工艺中的高温对碳纤维的损伤,基体材料的微孔型缺陷较多也是导致抗拉强度较低的重要因素。
In this paper, latitudinal tabby carbon fiber cloth weaved by 1K acrylic fiber was used as reinforcement, whose surface was firstly modified by electroless nickel plating, then treated by plasma spray of Al3%wt+Ni97%wt micro powders on both sides with thickness of hundreds of microns. Subsequently, Hot Isostatic Pressing (HIP) and Vacuum Hot Pressing (VHP) were performed to densify the material and finally carbon fiber reinforced nickel base composite with 25.7～32.8vol.% fiber was prepared.
Electroless plating was used to increase the infiltration and prevent the reaction between Ni and carbon fiber. Both the treatment before the electroless plating and the composition of the plating agent were investigated. And eventually we successfully got compact plating layer with low phosphorus.
Scanning Electron Microscope (SEM), X-ray fluorescence analysis (XRF), X-ray Photoelectron Spectroscopy (XPS), X-ray diffraction, Differential Scanning Calorimetry(DSC), Energy Difusion Spectrum(EDS) and high-temperature stretcher were used to study morphology, microstructure, phase composition, and mechanical properties of carbon fiber reinforced Ni-base composites, so as to improve the technique and optimize the Composition of plating agent of electroless nickel plating on carbon fibers. We also prepared carbon fiber reinforced composite without plating layer for comparison.
It was found that interfacial strength of composite with modified carbon fiber is much better than that of composite reinforced by untreated carbon fiber. Three characteristics in terms of the treated composite were revealed: a. Al2O3 phase was detected by XRD and EDS analysis, which brought brittleness to this material; b. the process of HP may seriously damage the carbon fibers inside the composite; c. The tensile strength at high temperature was not good, mainly due to the damage of carbon fiber caused by HP at high temperature, and also because there were many flaws such as micropores inside the matrix.
为增加镍金属与碳纤维的浸润性,阻止二者发生反应,采用了化学镀对碳纤维进行表面防护处理,对化学镀的前处理工艺和镀液配方进行了系统研究,得到了低含磷量的致密镀层。
采用扫描电镜(SEM)、X荧光光谱(XRF)、X射线光电子能谱(XPS)、X射线衍射(XRD)、差示扫描量热法(DSC)、能谱分析(EDS)等手段研究了碳纤维表面化学镀镍工艺和配方,并对制备出的碳纤维增强镍基复合材料的微观组织结构、相组成,高温拉伸性能进行了研究。并与未经表面镀镍的碳纤维增强镍基复合材料进行了对比分析。
结果表明,增强体经表面处理所制备的复合材料的界面强度明显高于未经表面处理的复合材料。分析发现此材料具有明显的三个特点:1.在X射线衍射分析和能谱分析都发现材料中出现氧化铝相,致使材料呈现很大的脆性;2.热压工艺过程对复合材料中纤维强度损伤很大;3.材料的高温拉伸性能不理想,原因主要是热压工艺中的高温对碳纤维的损伤,基体材料的微孔型缺陷较多也是导致抗拉强度较低的重要因素。
In this paper, latitudinal tabby carbon fiber cloth weaved by 1K acrylic fiber was used as reinforcement, whose surface was firstly modified by electroless nickel plating, then treated by plasma spray of Al3%wt+Ni97%wt micro powders on both sides with thickness of hundreds of microns. Subsequently, Hot Isostatic Pressing (HIP) and Vacuum Hot Pressing (VHP) were performed to densify the material and finally carbon fiber reinforced nickel base composite with 25.7～32.8vol.% fiber was prepared.
Electroless plating was used to increase the infiltration and prevent the reaction between Ni and carbon fiber. Both the treatment before the electroless plating and the composition of the plating agent were investigated. And eventually we successfully got compact plating layer with low phosphorus.
Scanning Electron Microscope (SEM), X-ray fluorescence analysis (XRF), X-ray Photoelectron Spectroscopy (XPS), X-ray diffraction, Differential Scanning Calorimetry(DSC), Energy Difusion Spectrum(EDS) and high-temperature stretcher were used to study morphology, microstructure, phase composition, and mechanical properties of carbon fiber reinforced Ni-base composites, so as to improve the technique and optimize the Composition of plating agent of electroless nickel plating on carbon fibers. We also prepared carbon fiber reinforced composite without plating layer for comparison.
It was found that interfacial strength of composite with modified carbon fiber is much better than that of composite reinforced by untreated carbon fiber. Three characteristics in terms of the treated composite were revealed: a. Al2O3 phase was detected by XRD and EDS analysis, which brought brittleness to this material; b. the process of HP may seriously damage the carbon fibers inside the composite; c. The tensile strength at high temperature was not good, mainly due to the damage of carbon fiber caused by HP at high temperature, and also because there were many flaws such as micropores inside the matrix.
引文
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2 Zhenyi Liu, Guoding Zhang, Hong Li,etc. Al infiltrated C–C hybrid composites. Materials and Design. 2005, 26: 83~87
3 Sang-Kwan Lee, Joon-Hyung Byun, Soon Hyung Hong. Effect of fiber geometry on the elastic constants of the plain woven fabric reinforced aluminum matrix com- posites. Materials Science and Engineering. 2003, A347:346~358
4 J.T. Blucher, J. Dobranszky, U. Narusawa. Aluminium double composite structures reinforced with composite wires. Materials Science and Engineering. A2004, (387~389):867~872
5 Wang Yu-Qing, Zhou Ben-Liam. Effect of a fiber coating on the fabrication of fiber reinforced metal-matrix composites. Journal of Materials Processing Technology. 1998, (73) : 78~81
6付传起,王宙,于媛等.低磷化学镀镍合金工艺研究.表面技术. 2004, 3 (33):47~48
7穆柏春,刘秉余,孟力凯.化学镀碳纤维增强钛酸铝基复合材料的研究.材料与表面处理. 2004, 3:45~50
8国为民,张风戈,张莹等.镍基粉末高温合金的组织、性能与成型和热处理工艺关系的研究.材料导报. 2003, 17(3):11~16
9邹莉.等离子喷涂技术及其应用.昆明冶金高等转科学校学报. 2005, 5(21):52~55
10陈丽梅,李强.等离子喷涂技术现状及发展.热处理技术与装备. 2006, 1(27):1~5
11 Duan-Jen Wang, Shinn-Tyan Wul. The Wettability of Copper Containing Alum-inium M Elton Sapphire. A cta.Metall.Mater. 1995, 43( 8):2917~2920
12 K.Landry, C .Radoand Eustathopoulos. Influenceo fInterfacial Reaction Rateson- the Weting Driving Force Metal/Ceramic System. Metall.Trans. 1996, (27): 3181 ~3186
13殷永霞,沃西源.碳纤维表面改性研究进展.航天返回与遥感. 2004, 25(1):51~54
14 J.Narciso, A.Alonso, etc. Wettability of Binary and Ternary Alloys of the System Al-Si-Mg with SiCP articulates. Scripta.Metal.Mater. 1994, 31(11): 1495~1496
15于家康.金属基复合材料增强相涂层.稀有金属材料与工程. 1996, 25(6):14~20
16贺福,王润娥.碳纤维表面处理方法及其设备.高科技纤维及应用. 2002, 21(4):108~112
17顾里之.纤维增强复合材料.机械工业出版社. 1988:335~398
18 Wurm R, Denovseko, Greil P. Sol-Gel Derived SrTi03 and SrZr03 Coating on SiC and C Fibers. Mater.Sci.1999, 34 (16):4031~4037
19 Yu-Qing Wang, Ben-Liar Zhou. Behavior of Coatings on Reinforcements in Some Metal M atrix Composites. Composites. PartA, 1996, (27):1139~1145
20田军,薛群基,周兆福等.提高中强碳纤维表面活性的Y射线处理方法.复合材料学报. 1999, (2):3~8
21 Machino, Fumikazu, Fujita, etc. Manufacture of Woollike Pitch Carbonor Graphite Fibers by Simplified Process Using FarIR Radiation in Fussibilizing pitchpre cursorfibers. 1999, (5):112~113
22 J.T. Blucher, J. Dobranszky, U. Narusawa, Aluminium double composite structures reinforced with composite wires. Materials Science and Engineering. 2004, A 387~389:867~872
23曾庆冰.溶胶凝胶法TiO2涂层碳纤维增强铝基复合材料的研制.高分子材料科学与工程. 1999, 15(4):171~175
24韩变华,罗天骄,姚广春等.碳纤维镀镍.有色矿冶. 2006, 22(2):37~40
25何为,唐先忠,迟兰州.碳纤维表面化学镀镍工艺研究.电镀与涂饰. 2003, 1(22):8~11
26 Y. Tanaka, Y. Kagawa, Yu-Fu Liu, etc. Interface damage mechanism during high temperature fatigue test in SiC fiber-reinforced Ti alloy matrix composite. Materials Science and Engineering. 2001, A(314):110~117
27杨永岗,贺福,王茂章等.碳纤维表面处理及其评价.材料研究学报. 1996, 10(5):460~466
28刘杰,郭云霞,梁节英.碳纤维电化学氧化表面处理效果的动态力学热分析研究.复合材料学报. 2004, 21(4):40~44
29崔国峰.化学镀镍合金过程中磷的析出及其对镀层性能的影响.理学博士. 2006:9~10
30李宁,袁国伟,黎德育.化学镀镍基合金理论与技术.哈尔滨工业大学出版社, 2000:63
31罗建东.中温低磷化学镀镍工艺研究.电镀与环保. 2002, 22(2):11~12
32王福生,许芸芸,兵魁等.化学镀Ni-P合金工艺的研究.天津化工. 2004, 18(5):1~3
33 http://www.imaterials.org/archive/index.php/t24947.html
34冯玉.真空等离子表面处理技术的应用.涂料涂装与电镀. 2006:23~25
35崔景东,张永锋.低温碱性化学镀镍工艺的研究.电镀与污染控制. 2004, 2 (24):30~31
36徐启文,吴源清,黄岳山等.化学镀镍液中硫酸镍与次磷酸钠的快速测定.电镀与精饰. 2004, 1(26):31~33
37智建,陈芳,唐雪娇等.化学镀镍在高科技领域中的应用.天津化工. 2004, 4(18):1~3
38杨延清,朱艳,陈彦等.长纤维增强Ti基复合材料的制备.稀有金属材料与工程. 2002, 31(3):201~203
39武洪臣,姚振中,冯建基等.先进的涂层技术—EB-PVD.航空制造技术. 2005, 5:112~114
40 G.S.马林斯基.新型电子束物理气相沉积设备.航空工艺技术. 1998, 2:31~38
41赵浩峰,王玲,刘红梅等.碳纤维及其与金属的作用.铸造设备研究. 2001, 3:49~53
42 Soo-Jin Park, Yu-Sin Jang. X-ray diffraction and X-ray photoelectron spectroscopy studies of Ni-P deposited onto carbon fiber surfaces:impact properties of a carbon-fiber-reinforced matrix.Journal of Colloid and Interface Science. 2003, 263:170~176
43 Tiancun Xiao, HaitaoWang, Jianwen Da, etc. Study of the Preparation and Catalytic Performance of Molybdenum Carbide Catalysts Prepared with C2H2/H2 Carburizing Mixture. Journal of Catalysis. 2002, 211:183~191
44 Yuanxin Zhou, Wang Yang, Yuanmin Xia, etc. An experimental study on the tensile behavior of a unidirectional carbon fiber reinforced aluminum composite at different strain rates.Materials Science and Engineering. 2003, 362: 112~117
45 T. Taguchi, T. Nozawa, N. Igawa, etc. Fabrication of advanced SiC fiber/F-CVI SiC matrix composites with SiC/C multi-layer interphase. Journal of Nuclear Materials. 2004, 329~333,572~576
46 Jinhai Gu, Xiaonong Zhang, Mingyuan Gu, etc. The damping capacity of aluminum matrix composites reinforced with coated carbon fibers. Materials Letters. 2004, (58):3170~3174
47 H. Ismar, F. Schroèter, F. Streicher. Inelastic behavior of metal-matrix composites reinforced with ?bres of silicon carbide, alumina or carbon: a ?nite-element analysis. Composites Science and Technology. 2000, 60 :2129~2136
48殷永霞,沃西源.碳纤维表面改性研究进展.航天返回与遥感. 2004, 25(1): 51~54
2 Zhenyi Liu, Guoding Zhang, Hong Li,etc. Al infiltrated C–C hybrid composites. Materials and Design. 2005, 26: 83~87
3 Sang-Kwan Lee, Joon-Hyung Byun, Soon Hyung Hong. Effect of fiber geometry on the elastic constants of the plain woven fabric reinforced aluminum matrix com- posites. Materials Science and Engineering. 2003, A347:346~358
4 J.T. Blucher, J. Dobranszky, U. Narusawa. Aluminium double composite structures reinforced with composite wires. Materials Science and Engineering. A2004, (387~389):867~872
5 Wang Yu-Qing, Zhou Ben-Liam. Effect of a fiber coating on the fabrication of fiber reinforced metal-matrix composites. Journal of Materials Processing Technology. 1998, (73) : 78~81
6付传起,王宙,于媛等.低磷化学镀镍合金工艺研究.表面技术. 2004, 3 (33):47~48
7穆柏春,刘秉余,孟力凯.化学镀碳纤维增强钛酸铝基复合材料的研究.材料与表面处理. 2004, 3:45~50
8国为民,张风戈,张莹等.镍基粉末高温合金的组织、性能与成型和热处理工艺关系的研究.材料导报. 2003, 17(3):11~16
9邹莉.等离子喷涂技术及其应用.昆明冶金高等转科学校学报. 2005, 5(21):52~55
10陈丽梅,李强.等离子喷涂技术现状及发展.热处理技术与装备. 2006, 1(27):1~5
11 Duan-Jen Wang, Shinn-Tyan Wul. The Wettability of Copper Containing Alum-inium M Elton Sapphire. A cta.Metall.Mater. 1995, 43( 8):2917~2920
12 K.Landry, C .Radoand Eustathopoulos. Influenceo fInterfacial Reaction Rateson- the Weting Driving Force Metal/Ceramic System. Metall.Trans. 1996, (27): 3181 ~3186
13殷永霞,沃西源.碳纤维表面改性研究进展.航天返回与遥感. 2004, 25(1):51~54
14 J.Narciso, A.Alonso, etc. Wettability of Binary and Ternary Alloys of the System Al-Si-Mg with SiCP articulates. Scripta.Metal.Mater. 1994, 31(11): 1495~1496
15于家康.金属基复合材料增强相涂层.稀有金属材料与工程. 1996, 25(6):14~20
16贺福,王润娥.碳纤维表面处理方法及其设备.高科技纤维及应用. 2002, 21(4):108~112
17顾里之.纤维增强复合材料.机械工业出版社. 1988:335~398
18 Wurm R, Denovseko, Greil P. Sol-Gel Derived SrTi03 and SrZr03 Coating on SiC and C Fibers. Mater.Sci.1999, 34 (16):4031~4037
19 Yu-Qing Wang, Ben-Liar Zhou. Behavior of Coatings on Reinforcements in Some Metal M atrix Composites. Composites. PartA, 1996, (27):1139~1145
20田军,薛群基,周兆福等.提高中强碳纤维表面活性的Y射线处理方法.复合材料学报. 1999, (2):3~8
21 Machino, Fumikazu, Fujita, etc. Manufacture of Woollike Pitch Carbonor Graphite Fibers by Simplified Process Using FarIR Radiation in Fussibilizing pitchpre cursorfibers. 1999, (5):112~113
22 J.T. Blucher, J. Dobranszky, U. Narusawa, Aluminium double composite structures reinforced with composite wires. Materials Science and Engineering. 2004, A 387~389:867~872
23曾庆冰.溶胶凝胶法TiO2涂层碳纤维增强铝基复合材料的研制.高分子材料科学与工程. 1999, 15(4):171~175
24韩变华,罗天骄,姚广春等.碳纤维镀镍.有色矿冶. 2006, 22(2):37~40
25何为,唐先忠,迟兰州.碳纤维表面化学镀镍工艺研究.电镀与涂饰. 2003, 1(22):8~11
26 Y. Tanaka, Y. Kagawa, Yu-Fu Liu, etc. Interface damage mechanism during high temperature fatigue test in SiC fiber-reinforced Ti alloy matrix composite. Materials Science and Engineering. 2001, A(314):110~117
27杨永岗,贺福,王茂章等.碳纤维表面处理及其评价.材料研究学报. 1996, 10(5):460~466
28刘杰,郭云霞,梁节英.碳纤维电化学氧化表面处理效果的动态力学热分析研究.复合材料学报. 2004, 21(4):40~44
29崔国峰.化学镀镍合金过程中磷的析出及其对镀层性能的影响.理学博士. 2006:9~10
30李宁,袁国伟,黎德育.化学镀镍基合金理论与技术.哈尔滨工业大学出版社, 2000:63
31罗建东.中温低磷化学镀镍工艺研究.电镀与环保. 2002, 22(2):11~12
32王福生,许芸芸,兵魁等.化学镀Ni-P合金工艺的研究.天津化工. 2004, 18(5):1~3
33 http://www.imaterials.org/archive/index.php/t24947.html
34冯玉.真空等离子表面处理技术的应用.涂料涂装与电镀. 2006:23~25
35崔景东,张永锋.低温碱性化学镀镍工艺的研究.电镀与污染控制. 2004, 2 (24):30~31
36徐启文,吴源清,黄岳山等.化学镀镍液中硫酸镍与次磷酸钠的快速测定.电镀与精饰. 2004, 1(26):31~33
37智建,陈芳,唐雪娇等.化学镀镍在高科技领域中的应用.天津化工. 2004, 4(18):1~3
38杨延清,朱艳,陈彦等.长纤维增强Ti基复合材料的制备.稀有金属材料与工程. 2002, 31(3):201~203
39武洪臣,姚振中,冯建基等.先进的涂层技术—EB-PVD.航空制造技术. 2005, 5:112~114
40 G.S.马林斯基.新型电子束物理气相沉积设备.航空工艺技术. 1998, 2:31~38
41赵浩峰,王玲,刘红梅等.碳纤维及其与金属的作用.铸造设备研究. 2001, 3:49~53
42 Soo-Jin Park, Yu-Sin Jang. X-ray diffraction and X-ray photoelectron spectroscopy studies of Ni-P deposited onto carbon fiber surfaces:impact properties of a carbon-fiber-reinforced matrix.Journal of Colloid and Interface Science. 2003, 263:170~176
43 Tiancun Xiao, HaitaoWang, Jianwen Da, etc. Study of the Preparation and Catalytic Performance of Molybdenum Carbide Catalysts Prepared with C2H2/H2 Carburizing Mixture. Journal of Catalysis. 2002, 211:183~191
44 Yuanxin Zhou, Wang Yang, Yuanmin Xia, etc. An experimental study on the tensile behavior of a unidirectional carbon fiber reinforced aluminum composite at different strain rates.Materials Science and Engineering. 2003, 362: 112~117
45 T. Taguchi, T. Nozawa, N. Igawa, etc. Fabrication of advanced SiC fiber/F-CVI SiC matrix composites with SiC/C multi-layer interphase. Journal of Nuclear Materials. 2004, 329~333,572~576
46 Jinhai Gu, Xiaonong Zhang, Mingyuan Gu, etc. The damping capacity of aluminum matrix composites reinforced with coated carbon fibers. Materials Letters. 2004, (58):3170~3174
47 H. Ismar, F. Schroèter, F. Streicher. Inelastic behavior of metal-matrix composites reinforced with ?bres of silicon carbide, alumina or carbon: a ?nite-element analysis. Composites Science and Technology. 2000, 60 :2129~2136
48殷永霞,沃西源.碳纤维表面改性研究进展.航天返回与遥感. 2004, 25(1): 51~54