短碳纤维增强镁基复合材料的制备及其性能的研究
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摘要
金属镁由于具有低密度和良好的阻尼减震性、导热性以及电磁屏蔽性等特点,在航空航天、交通运输和电子工业等领域有着广阔的应用前景,但由于纯镁的力学性能及耐腐蚀性能较差,因此在工业上一般不直接使用纯镁作为结构材料。金属镁的工业应用多采取以下两种途径来实现:一是添加合金元素形成镁合金;二是加入增强体制备成镁基复合材料;在镁合金中引入不同功能增强体可显著地改善镁基复合材料的力学性能、耐磨性能、阻尼性能及耐高温性能。
碳纤维由于具有高的比强度、比模量、耐高温、耐疲劳、低膨胀和自润滑等优异的综合性能,使其成为一种非常理想的制备镁基复合材料的增强体材料。但是,碳纤维与金属镁之间的润湿性较差,为此往往需要对碳纤维进行表面处理,化学镀镍一方面由于其与金属镁之间良好的润湿性使得碳纤维增强镁基复合材料的力学性能大幅度提高;另一方面其在界面层中引入金属镍还可以显著地改善镁基复合材料的阻尼性能。
本文采用粉末冶金和热挤压的工艺技术制备了短碳纤维增强镁基复合材料,对其制备技术、组织结构、力学性能及阻尼性能等进行了研究。采用化学镀镍的方法对碳纤维进行了表面处理,并对金属镍的沉积机理及其对镁复合材料力学性能及阻尼性能的影响进行了研究,最后采用有限元法对复合材料的热挤压过程进行了计算机模拟,研究了挤压过程中各参数对复合材料微观结构的影响。论文取取得了以下主要成果:
1、在预备试验的基础上,设计了碳纤维化学镀镍处理的L16(4~5)正交试验,得到了最佳的施镀工艺条件:T=65℃,t=3min,pH=8.0,络合剂含量25g/L。采用此工艺条件,在碳纤维表面得到了结构均匀0.5um厚的金属镍涂层。
2、通过化学镀镍沉积过程研究发现,整个化学镀过程可分为诱导期-加速期-减速期-稳定期四个阶段。[OH-]的反应级数为0.265,[C_6H_5O_7~-]的反应级数为-0.233,化学镀的活化能为62.82KJ/mol。随着热处理温度的升高,金属镍涂层向碳纤维内部扩散而使其发生了石墨化、镀层内部晶粒明显长大、结晶度提高近1倍,其物相组成由初始的沿(111)晶面择优取向的金属Ni和少量的P转变为无序取向的Ni和Ni3P。
3、以纯镁为基体金属,采用粉末冶金挤压法成功制备了短碳纤维分布均匀且定向排列的镁基复合材料。压坯制备过程中不规则镁颗粒对短碳纤维有剪切作用,复合材料内部的纤维会变短,其平均长度约为30μm;TEM测试结果表明,复合材料界面层厚度约500nm,界面结合良好,界面生成的Mg_2Ni对碳纤维有一定的催化石墨化作用。
4、综合理论计算和试验结果发现,涂层碳纤维增强镁基复合材料的增强机理主要是“载荷传递效应”;随着增强体体积分数的增加,在高于临界振幅的范围内复合材料的阻尼性能更加优良,常温下复合材料阻尼除位错阻尼机制外还有其他的阻尼机制存在。纯Mg、5.5vol%uncoated cf/Mg和5.5vol%Ni-coated cf/Mg三种材料在整个测试温度范围内都只存在一个阻尼峰,且随着频率的增加其阻尼峰值温度升高,显示了热激活弛豫过程的特征,三种材料的热激活能H的大小分别为:1.287eV、1.129eV和1.725eV;前两种材料起作用的主要是位错阻尼机制,而5.5vol%Ni-coated cf/Mg复合材料由于碳纤维表面金属镍涂层的引入改善了界面润湿性,使界面附近的位错密度降低,在低温及相同外加应力的作用下通过位错运动耗散的能量最少,随着温度的升高通过界面和晶界的滑移所耗散的能量增加导致其在200~260℃范围内具有最大的阻尼值。
5、成功地制备了短碳纤维增强的AZ91D镁基复合材料,复合材料中短碳纤维的长度为30~40μm。TEM观察发现,复合材料界面结合良好,5.0vol%Ni-coated cf/AZ91D复合材料的力学性能与纯AZ91D及5.0vol%uncoated cf/AZ91D相比最优。5.0vol%Ni-coated cf/AZ91D复合材料随着频率的增大阻尼峰值温度移向高温,同样表现出热激活弛豫过程的特征,其热激活能H为3.448eV;在温度高于220℃的条件下,随着热挤压温度的升高和挤压比的减小5.0vol%Ni-coated cf/AZ91D复合材料的阻尼值减小,这与复合材料内部的晶粒大小有关。
6、DEFORM-3D有限元软件对热挤压过程的模拟结果表明,复合材料中碳纤维长度减小的主要原因是压制过程中金属颗粒对纤维的剪切作用;在热挤压过程中复合材料内部的应力场、应变场和温度场都对称分布,且在定径带处出现明显的应力和应变集中;通过对此区域复合材料的金相组织观察发现,在挤压开始阶段复合材料内部基体金属颗粒由于受到挤压力的影响而被逐渐拉长,且发生了明显的动态再结晶,晶粒尺寸在此过程中出现明显的细化现象,当材料流出定径带后由于材料内部应力和应变的释放而使晶粒尺寸变大。
Magnesium metal has broad application prospects in aerospace, transportation and electronics industries because it has low density, good damping capacity, good thermal conductivity and electromagnetic shielding characteristics. However, it is not been directly used as structural materials due to its poor mechanical properties and corrosion resistance. The application of magnesium metal is usually take the following two ways: one is alloying and another is magnesium matrix composites. The introduction of different reinforcements into the magnesium alloys can significantly improve the mechanics performance, wear-resisting performance, damping performance and high temperature resistant performance of magnesium matrix composite.
Carbon fiber is a very ideal reinforcement to make the magnesium based composite on account of its excellent performance such as high specific strength and modulus, thermostability, fatigue resistance, low inflation and self-lubricating etc. But it is well known that the wettability between it and magnesium is poor. So it is often required to carbon fiber’s surface treatment. Electroless nickel plating is one of surface treatment measures. On the one hand the good wettability between nickel and magnesium could improve the mechanical properties of carbon fiber reinforced magnesium based composite; On the other hand the introduced metal nickel in the interface can significantly improve the damping capacity of magnesium matrix composite.
In this thesis the short carbon fibers reinforced magnesium matrix composites were fabricated by powder metallurgy and hot extrusion technology. Then its preparation technology, organization structure, mechanical properties and damping properties were studied. The deposition mechanism of nickel,and its influence on the mechanical properties and damping performance of the magnesium-based composite was studied. Finally the hot extrusion process of composite was simulated by finite element method. The influences of extrusion process parameters to the composite material’s microscopic structure were studied. The following main achievements were obtained in this paper:
1、The L16 (4~5) orthogonal experiments were designed based on the preliminary experiments and it was got the best plating technology conditions: T = 65℃, t = 3min, pH = 8.0, complexity agent content 25g/L. Using this technology conditions, the uniform nickel coating about 0.5μm thickness was obtained.
2、It was found the whole electroless plating process could be divided into four obvious stages: induction period - accelerating period - slow period - stabilization period. The orders of reaction of [OH -] and [C_6H_5O_7~-] were 0.265 and -0.233 respectively. The activation energy of electroless plating was 62.82 KJ/mol. Along with the heat treatment temperature elevation, the following results were appeared. The graphitization appeared because the interior diffusion of nickel coating from the surface carbon fibers. The grains were obvious grown up in the coating and its crystallization improved nearly doubled. Its phase composition changed from the initial preferred orientation along (111) faces of metal Ni and a small amount of P to the disorder. Ni3P and Ni.
3、Using the magnesium as matrix, the magnesium-based composites which the short carbon fiber distribution was distributed uniformly and directionally aligned were fabricated by powder metallurgical and hot extrusion. The average length of short carbon fibers was about 30μm which was shorter than its initial because the shearing action of irregular magnesium granules to the short carbon fiber during the pressure billets process. TEM test results showed that the thickness of good interface layer was 500nm and the interfacial product of Mg_2Ni had a certain catalytic graphitization role.
4、Comprehensive theoretical calculation and test results,it was found that the enhancement mechanism of magnesium matrix composite reinforced by coated short carbon fibers was mainly "load transfer effect"; At ambient temperature, the composites possess the more excellent damping performance above the critical amplitude with the increase of volume fraction and there existed other damping mechanisms in addition to dislocation damping mechanism in it. Whether it be Pure Mg, 5.5 vol % uncoated cf/Mg or 5.5 vol % Ni - coated cf/Mg, only one damping peak on the damping-temperature curves and the peak temperature shift to high temperature with the increased frequency which shows the characteristics of heat activating relaxation process. The thermal activation energies of above three different materials were 1.287eV, 1.129eV and 1.725eV, respectively. There existed mainly the dislocation damping mechanism in the first two kinds of materials. However, the dislocation density near the interface reduced due to the introduction of nickel coating which improved interfacial wettability in the 5.5vol%Ni-coated cf/Mg composite. The dissipated energy by dislocation motion was decreased at low temperature and the same applied stress. The maximum damping values appeared in 200 ~ 260℃due to the increased dissipated energy through the interface and grain boundary sliding with the rise of temperature.
5、The AZ91D magnesium-based composites reinforced by short carbon fibers were successfully prepared and the length of carbon fibers was 30 ~ 40μm in them. The results of TEM observation shown that the bonding of the interface between metal substrate and carbon fibers is good. The mechanical properties of 5.0vol%Ni-coated cf/AZ91D composite was optimal compared with pure AZ91D and 5.0vol%uncoated cf/AZ91D composite. The damping peak temperature shifted to higher temperature with the increase the frequency and also displayed the characteristics of heat activating relaxation process. Its thermal activation energy was 3.448 vetches damping capacity of 5.0vol%Ni-coated cf/AZ91D composite decreased with the rising hot extrusion temperature and increased extrusion ratio at the temperatures higher than 220℃.This was responsible for the grain size internal the composite.
6、The simulation results of hot extrusion process carried out by DEFORM -3D finite element software shown that the decrease of carbon fiber’s length was due to the magnesium particle’s shearing action during the pressing process. In hot extrusion process the stress field, strain field and temperature field were distributed symmetrically and the obvious stress and strain concentration was appeared in the sizing area. The metallographic structure near this regional in the composite shown that the metal particles were gradually been stretched and the obvious dynamic recrystallization was appeared .But the grain size become bigger due to the release of the internal stress and strain when the composite outflow the sizing region.
碳纤维由于具有高的比强度、比模量、耐高温、耐疲劳、低膨胀和自润滑等优异的综合性能,使其成为一种非常理想的制备镁基复合材料的增强体材料。但是,碳纤维与金属镁之间的润湿性较差,为此往往需要对碳纤维进行表面处理,化学镀镍一方面由于其与金属镁之间良好的润湿性使得碳纤维增强镁基复合材料的力学性能大幅度提高;另一方面其在界面层中引入金属镍还可以显著地改善镁基复合材料的阻尼性能。
本文采用粉末冶金和热挤压的工艺技术制备了短碳纤维增强镁基复合材料,对其制备技术、组织结构、力学性能及阻尼性能等进行了研究。采用化学镀镍的方法对碳纤维进行了表面处理,并对金属镍的沉积机理及其对镁复合材料力学性能及阻尼性能的影响进行了研究,最后采用有限元法对复合材料的热挤压过程进行了计算机模拟,研究了挤压过程中各参数对复合材料微观结构的影响。论文取取得了以下主要成果:
1、在预备试验的基础上,设计了碳纤维化学镀镍处理的L16(4~5)正交试验,得到了最佳的施镀工艺条件:T=65℃,t=3min,pH=8.0,络合剂含量25g/L。采用此工艺条件,在碳纤维表面得到了结构均匀0.5um厚的金属镍涂层。
2、通过化学镀镍沉积过程研究发现,整个化学镀过程可分为诱导期-加速期-减速期-稳定期四个阶段。[OH-]的反应级数为0.265,[C_6H_5O_7~-]的反应级数为-0.233,化学镀的活化能为62.82KJ/mol。随着热处理温度的升高,金属镍涂层向碳纤维内部扩散而使其发生了石墨化、镀层内部晶粒明显长大、结晶度提高近1倍,其物相组成由初始的沿(111)晶面择优取向的金属Ni和少量的P转变为无序取向的Ni和Ni3P。
3、以纯镁为基体金属,采用粉末冶金挤压法成功制备了短碳纤维分布均匀且定向排列的镁基复合材料。压坯制备过程中不规则镁颗粒对短碳纤维有剪切作用,复合材料内部的纤维会变短,其平均长度约为30μm;TEM测试结果表明,复合材料界面层厚度约500nm,界面结合良好,界面生成的Mg_2Ni对碳纤维有一定的催化石墨化作用。
4、综合理论计算和试验结果发现,涂层碳纤维增强镁基复合材料的增强机理主要是“载荷传递效应”;随着增强体体积分数的增加,在高于临界振幅的范围内复合材料的阻尼性能更加优良,常温下复合材料阻尼除位错阻尼机制外还有其他的阻尼机制存在。纯Mg、5.5vol%uncoated cf/Mg和5.5vol%Ni-coated cf/Mg三种材料在整个测试温度范围内都只存在一个阻尼峰,且随着频率的增加其阻尼峰值温度升高,显示了热激活弛豫过程的特征,三种材料的热激活能H的大小分别为:1.287eV、1.129eV和1.725eV;前两种材料起作用的主要是位错阻尼机制,而5.5vol%Ni-coated cf/Mg复合材料由于碳纤维表面金属镍涂层的引入改善了界面润湿性,使界面附近的位错密度降低,在低温及相同外加应力的作用下通过位错运动耗散的能量最少,随着温度的升高通过界面和晶界的滑移所耗散的能量增加导致其在200~260℃范围内具有最大的阻尼值。
5、成功地制备了短碳纤维增强的AZ91D镁基复合材料,复合材料中短碳纤维的长度为30~40μm。TEM观察发现,复合材料界面结合良好,5.0vol%Ni-coated cf/AZ91D复合材料的力学性能与纯AZ91D及5.0vol%uncoated cf/AZ91D相比最优。5.0vol%Ni-coated cf/AZ91D复合材料随着频率的增大阻尼峰值温度移向高温,同样表现出热激活弛豫过程的特征,其热激活能H为3.448eV;在温度高于220℃的条件下,随着热挤压温度的升高和挤压比的减小5.0vol%Ni-coated cf/AZ91D复合材料的阻尼值减小,这与复合材料内部的晶粒大小有关。
6、DEFORM-3D有限元软件对热挤压过程的模拟结果表明,复合材料中碳纤维长度减小的主要原因是压制过程中金属颗粒对纤维的剪切作用;在热挤压过程中复合材料内部的应力场、应变场和温度场都对称分布,且在定径带处出现明显的应力和应变集中;通过对此区域复合材料的金相组织观察发现,在挤压开始阶段复合材料内部基体金属颗粒由于受到挤压力的影响而被逐渐拉长,且发生了明显的动态再结晶,晶粒尺寸在此过程中出现明显的细化现象,当材料流出定径带后由于材料内部应力和应变的释放而使晶粒尺寸变大。
Magnesium metal has broad application prospects in aerospace, transportation and electronics industries because it has low density, good damping capacity, good thermal conductivity and electromagnetic shielding characteristics. However, it is not been directly used as structural materials due to its poor mechanical properties and corrosion resistance. The application of magnesium metal is usually take the following two ways: one is alloying and another is magnesium matrix composites. The introduction of different reinforcements into the magnesium alloys can significantly improve the mechanics performance, wear-resisting performance, damping performance and high temperature resistant performance of magnesium matrix composite.
Carbon fiber is a very ideal reinforcement to make the magnesium based composite on account of its excellent performance such as high specific strength and modulus, thermostability, fatigue resistance, low inflation and self-lubricating etc. But it is well known that the wettability between it and magnesium is poor. So it is often required to carbon fiber’s surface treatment. Electroless nickel plating is one of surface treatment measures. On the one hand the good wettability between nickel and magnesium could improve the mechanical properties of carbon fiber reinforced magnesium based composite; On the other hand the introduced metal nickel in the interface can significantly improve the damping capacity of magnesium matrix composite.
In this thesis the short carbon fibers reinforced magnesium matrix composites were fabricated by powder metallurgy and hot extrusion technology. Then its preparation technology, organization structure, mechanical properties and damping properties were studied. The deposition mechanism of nickel,and its influence on the mechanical properties and damping performance of the magnesium-based composite was studied. Finally the hot extrusion process of composite was simulated by finite element method. The influences of extrusion process parameters to the composite material’s microscopic structure were studied. The following main achievements were obtained in this paper:
1、The L16 (4~5) orthogonal experiments were designed based on the preliminary experiments and it was got the best plating technology conditions: T = 65℃, t = 3min, pH = 8.0, complexity agent content 25g/L. Using this technology conditions, the uniform nickel coating about 0.5μm thickness was obtained.
2、It was found the whole electroless plating process could be divided into four obvious stages: induction period - accelerating period - slow period - stabilization period. The orders of reaction of [OH -] and [C_6H_5O_7~-] were 0.265 and -0.233 respectively. The activation energy of electroless plating was 62.82 KJ/mol. Along with the heat treatment temperature elevation, the following results were appeared. The graphitization appeared because the interior diffusion of nickel coating from the surface carbon fibers. The grains were obvious grown up in the coating and its crystallization improved nearly doubled. Its phase composition changed from the initial preferred orientation along (111) faces of metal Ni and a small amount of P to the disorder. Ni3P and Ni.
3、Using the magnesium as matrix, the magnesium-based composites which the short carbon fiber distribution was distributed uniformly and directionally aligned were fabricated by powder metallurgical and hot extrusion. The average length of short carbon fibers was about 30μm which was shorter than its initial because the shearing action of irregular magnesium granules to the short carbon fiber during the pressure billets process. TEM test results showed that the thickness of good interface layer was 500nm and the interfacial product of Mg_2Ni had a certain catalytic graphitization role.
4、Comprehensive theoretical calculation and test results,it was found that the enhancement mechanism of magnesium matrix composite reinforced by coated short carbon fibers was mainly "load transfer effect"; At ambient temperature, the composites possess the more excellent damping performance above the critical amplitude with the increase of volume fraction and there existed other damping mechanisms in addition to dislocation damping mechanism in it. Whether it be Pure Mg, 5.5 vol % uncoated cf/Mg or 5.5 vol % Ni - coated cf/Mg, only one damping peak on the damping-temperature curves and the peak temperature shift to high temperature with the increased frequency which shows the characteristics of heat activating relaxation process. The thermal activation energies of above three different materials were 1.287eV, 1.129eV and 1.725eV, respectively. There existed mainly the dislocation damping mechanism in the first two kinds of materials. However, the dislocation density near the interface reduced due to the introduction of nickel coating which improved interfacial wettability in the 5.5vol%Ni-coated cf/Mg composite. The dissipated energy by dislocation motion was decreased at low temperature and the same applied stress. The maximum damping values appeared in 200 ~ 260℃due to the increased dissipated energy through the interface and grain boundary sliding with the rise of temperature.
5、The AZ91D magnesium-based composites reinforced by short carbon fibers were successfully prepared and the length of carbon fibers was 30 ~ 40μm in them. The results of TEM observation shown that the bonding of the interface between metal substrate and carbon fibers is good. The mechanical properties of 5.0vol%Ni-coated cf/AZ91D composite was optimal compared with pure AZ91D and 5.0vol%uncoated cf/AZ91D composite. The damping peak temperature shifted to higher temperature with the increase the frequency and also displayed the characteristics of heat activating relaxation process. Its thermal activation energy was 3.448 vetches damping capacity of 5.0vol%Ni-coated cf/AZ91D composite decreased with the rising hot extrusion temperature and increased extrusion ratio at the temperatures higher than 220℃.This was responsible for the grain size internal the composite.
6、The simulation results of hot extrusion process carried out by DEFORM -3D finite element software shown that the decrease of carbon fiber’s length was due to the magnesium particle’s shearing action during the pressing process. In hot extrusion process the stress field, strain field and temperature field were distributed symmetrically and the obvious stress and strain concentration was appeared in the sizing area. The metallographic structure near this regional in the composite shown that the metal particles were gradually been stretched and the obvious dynamic recrystallization was appeared .But the grain size become bigger due to the release of the internal stress and strain when the composite outflow the sizing region.
引文
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