仪表级SiC/Gr/Al复合材料制备与性能研究
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摘要
本文以惯性仪表为应用背景,在SiC/Al复合材料的基础上以易加工、高比刚度、低膨胀、高阻尼及高尺寸稳定性等性能为目标进行了材料设计,通过添加3%~7%,1μm~70μm的鳞片状石墨的手段获得上述性能。采用透射电子显微镜(TEM)、扫描电子显微镜(SEM)、体式显微镜、摩擦磨损试验机、原子力显微镜(AFM)、切削力测试仪、热膨胀仪、电子拉伸机、硬度计、X射线衍射仪(XRD)和内耗仪等手段研究了石墨的加入对SiC/Gr/Al复合材料微观组织、力学性能、加工性能和尺寸稳定性的影响,并深入探讨了其影响机理。
根据化学稳定性和润滑性能要求,选择具有固体润滑性质的石墨作为添加颗粒,并采用固体润滑的相关理论分析了减磨机制。通过H-S模型和混合定律确定了石墨润滑剂的上限值7.2%。定性分析了影响复合材料尺寸稳定性的的各种因素。综合考虑石墨对加工性能、力学性能和尺寸稳定性的影响,提出了SiC/Gr/Al复合材料的设计原则。
TEM观察表明,SiC-Al和Gr-Al界面都未观察到界面反应物,这与制备工艺相关,同时Gr-Al界面未生成界面反应物与高的石墨化率相关。石墨与基体为弱界面结合,且片层间容易滑移,在材料制备和热处理过程中石墨可以释放微观应力,这使得SiC/Gr/Al复合材料中位错密度较低或形成亚晶界;同时,依赖位错形核的析出相密度也相应降低。
SiC/Gr/Al复合材料的热膨胀系数介于11.5~13×10-6/℃之间,可以与轴承钢的热膨胀系数(12~13×10-6/℃)较好的匹配,阻尼性能达到铝合金的2~6倍左右,满足仪表级复合材料对热膨胀匹配及高阻尼性能的需求。
石墨体积分数增加,颗粒间距减小,基体连续性破坏,SiC/Gr/Al复合材料的拉伸强度显著降低。SiC/Gr/Al复合材料的断裂方式以石墨片层间或石墨/基体界面的脆性断裂为主,但SiC+Al基体中具有一定的塑性变形特征;根据断口分析将SiC+Al看成基体,石墨作为增强体,采用H-S模型SiC/Gr/Al复合材料的弹性模量进行预测,准确度可达到实际值的93.5%。
通过摩擦磨损试验对刀具/复合材料摩擦副切削过程中的摩擦状况进行分析,揭示了SiC/Gr/Al复合材料表面磨擦过程中固体润滑膜的生成是其摩擦系数和磨损率降低的主要原因。进一步通过润滑理论对减磨机理进行分析,认为在摩擦副之间既使润滑膜不完整或极薄也能起到减磨作用.
石墨添加通过降低复合材料的强度和硬度,有利于切屑形成及石墨的固体润滑性质三种机制改善SiC/Gr/Al复合材料的加工性能。刀具磨损与石墨加入的体积分数相关,与粒径关系不大,但切削力的大小受石墨粒径影响较大。石墨的加入没有改变SiC/Al复合材料切削过程背向力大于主切削力的特点。
尺寸稳定性的研究表明:石墨的加入有利于材料的尺寸稳定提高,主要原因粒径为6μm,体积分数为5%石墨颗粒的加入使SiC/Al复合材料的宏观应力降低30%,微观应力降低20%,满足应力的稳定性,同时石墨的加入促进了位错结构的稳定化。无负载下的尺寸稳定性和微屈服强度综合考虑,确定A+TCC(0)为提高SiC/Gr/Al复合材料尺寸稳定性的最佳热处理工艺。
本文基于仪表级复合材料的性能要求设计了SiC/Gr/Al复合材料,并找到了合适的热处理工艺。在添加高纯石墨颗粒(粒径: 6μm,体积分数:5%)的SiC/Gr/Al复合材料,刀具寿命提高40%,弹性模量保持在150GPa,σ0.0001达到333MPa,变温的尺寸性稳定性低于0.61×10-6,满足惯性仪表材料的性能需求。
In the present paper, material design on the background of inertial instrument application is carried out with the aim of acquiring good machinability,high special elastic modulus, high damping properties and good dimension stability, which is on the basis of SiC/Gr/Al composites. For this purpose, flaky graphite (volume fraction of 3%~7%, and particle size of 1μm~70μm) were additioned. Effects of graphite particles on microstructure, mechanical properties, machinability and dimension stability were studied by using scanning electron microscope (SEM), transmission electron microscope(TEM), optical microscope , friction-wear tester, atomic forces microscope (AFM), cutting force tester, thermal conductivity tester, tensile testing machine, Brinell hardness, X-ray diffraction and internal friction apparatus. And their influencing factors were also discussed.
Graphite with solid lubrication is selected according to chemical stability and lubrication, and wear-resistence is explained by solid lubrication theory. The appropriate upper limit of the addition of graphite particles should be 7.2% on the based of analysis H-S model and the mixing rule. Effect of graphite particles on thermal expansion was analysised according to theory model, and influencing factors to dimension stability was analysised. Those factors was summarized, the design principle of SiC/Gr/Al was established.
TEM observations indicate SiC-Al and Gr-Al interfaces are clean and free from interfacial reaction products, which are attributed to fabrication process. Meanwhile, there is no interface reactivity in Gr-Al interfaces, which is due to high degree of graphization. The bonding strength between graphite and matrix alloy is weak, and the lamellar is sliding easily. Micro-stress is relaxed in the process of fabrication and heat treatment, The addition of graphite particles decreases the dislocation density in the composite. Moreover, the dislocation in the casting microstructure generates the sub-boundary, and the density of precipitate phase dependent on the dislocation nucleation also reduces
The coefficient of thermal expansion (CTE) and daming properties are tested, and the results show that CTE is between 11.5~13×10-6/℃and Q-1 for SiC/Gr/Al composite is 2~6 times higher than that of the aluminum matrix. These meet the requirements of thermal expansion matching the corresponding materials and high damping in precision instrument.
The increment of graphite volume fraction, the decrement of particle spacing, destroyed continuity of matrix, result in the reducing of tensile strength of SiC/Gr/Al composites。The increment of interfacial area and reduction of partilcle spacing result in the increasing amount of crack source and destroy the continuity of aluminum matrix, which is the main reason for decrease of mechanical properties.
Tribological conditions of tool/ composite in the process of cutting are analsized by wear test. Results show that the tribo-layer formed during wear cause the decreasing of friction coefficient and wear loss. Further analysis to the mechanism of the increase in wear resistance, the worn surface of SiC/Gr/Al composite covered by a continuous or thin tribo-layer can also improve wear resistance.
Graphite particles improve that machinability from tool wear, cutting force and surface roughness. It is due to the decreasing of hardness and strength of composites, which has decreased the coefficient of chip distortion and promoting crack propagation of chip, and solid lubrication to tool. With increasing Vf of graphite particles, tool wear increase. Particle size of graphite has little effect on the tool wear, but has very remarble effect on cutting force. The characteristic of thrust force (Ft) higher than cutting force (Fc) is not change by the addition of graphite particles. The SiC+Al matrix failed in ductile manner while graphite particle fail in a brittle manner. The elastic modulus was estimated by H-S models and the estimated value is 93.5% of the tested values.
The investigation of dimension stability show that: the addition of graphite is beneficial to improving dimensional stability Sufficient aging precipitation, stable dislocation structure and lower macro residual stress ensure dimension stability by appropriate thermal cycling procedure (A+TCC(0)and A+TCC(-70)) when compared with aging procedure. Besides thermal cycling procedure, relaxation of micro stress by graphite particles further improved dimension stability of SiC/Gr/Al. From analysis both micro-deformation resistance and dimension stability under no load, A+TCC (0) is the optimum procedure for improving the dimension stability.
In the paper, we design SiC/Gr/Al composites according to the requirement of instrument materials, and find proper heat treatment process. For the 40%SiC/5%Gr(6μm)/Al composites, the tool life maching the composite was prolonged by 40%, the elastic modulus are maintained 150GPa, variable dimentional stability is lower than 0.61×10-6, which meet the requirements of instrument properties.
根据化学稳定性和润滑性能要求,选择具有固体润滑性质的石墨作为添加颗粒,并采用固体润滑的相关理论分析了减磨机制。通过H-S模型和混合定律确定了石墨润滑剂的上限值7.2%。定性分析了影响复合材料尺寸稳定性的的各种因素。综合考虑石墨对加工性能、力学性能和尺寸稳定性的影响,提出了SiC/Gr/Al复合材料的设计原则。
TEM观察表明,SiC-Al和Gr-Al界面都未观察到界面反应物,这与制备工艺相关,同时Gr-Al界面未生成界面反应物与高的石墨化率相关。石墨与基体为弱界面结合,且片层间容易滑移,在材料制备和热处理过程中石墨可以释放微观应力,这使得SiC/Gr/Al复合材料中位错密度较低或形成亚晶界;同时,依赖位错形核的析出相密度也相应降低。
SiC/Gr/Al复合材料的热膨胀系数介于11.5~13×10-6/℃之间,可以与轴承钢的热膨胀系数(12~13×10-6/℃)较好的匹配,阻尼性能达到铝合金的2~6倍左右,满足仪表级复合材料对热膨胀匹配及高阻尼性能的需求。
石墨体积分数增加,颗粒间距减小,基体连续性破坏,SiC/Gr/Al复合材料的拉伸强度显著降低。SiC/Gr/Al复合材料的断裂方式以石墨片层间或石墨/基体界面的脆性断裂为主,但SiC+Al基体中具有一定的塑性变形特征;根据断口分析将SiC+Al看成基体,石墨作为增强体,采用H-S模型SiC/Gr/Al复合材料的弹性模量进行预测,准确度可达到实际值的93.5%。
通过摩擦磨损试验对刀具/复合材料摩擦副切削过程中的摩擦状况进行分析,揭示了SiC/Gr/Al复合材料表面磨擦过程中固体润滑膜的生成是其摩擦系数和磨损率降低的主要原因。进一步通过润滑理论对减磨机理进行分析,认为在摩擦副之间既使润滑膜不完整或极薄也能起到减磨作用.
石墨添加通过降低复合材料的强度和硬度,有利于切屑形成及石墨的固体润滑性质三种机制改善SiC/Gr/Al复合材料的加工性能。刀具磨损与石墨加入的体积分数相关,与粒径关系不大,但切削力的大小受石墨粒径影响较大。石墨的加入没有改变SiC/Al复合材料切削过程背向力大于主切削力的特点。
尺寸稳定性的研究表明:石墨的加入有利于材料的尺寸稳定提高,主要原因粒径为6μm,体积分数为5%石墨颗粒的加入使SiC/Al复合材料的宏观应力降低30%,微观应力降低20%,满足应力的稳定性,同时石墨的加入促进了位错结构的稳定化。无负载下的尺寸稳定性和微屈服强度综合考虑,确定A+TCC(0)为提高SiC/Gr/Al复合材料尺寸稳定性的最佳热处理工艺。
本文基于仪表级复合材料的性能要求设计了SiC/Gr/Al复合材料,并找到了合适的热处理工艺。在添加高纯石墨颗粒(粒径: 6μm,体积分数:5%)的SiC/Gr/Al复合材料,刀具寿命提高40%,弹性模量保持在150GPa,σ0.0001达到333MPa,变温的尺寸性稳定性低于0.61×10-6,满足惯性仪表材料的性能需求。
In the present paper, material design on the background of inertial instrument application is carried out with the aim of acquiring good machinability,high special elastic modulus, high damping properties and good dimension stability, which is on the basis of SiC/Gr/Al composites. For this purpose, flaky graphite (volume fraction of 3%~7%, and particle size of 1μm~70μm) were additioned. Effects of graphite particles on microstructure, mechanical properties, machinability and dimension stability were studied by using scanning electron microscope (SEM), transmission electron microscope(TEM), optical microscope , friction-wear tester, atomic forces microscope (AFM), cutting force tester, thermal conductivity tester, tensile testing machine, Brinell hardness, X-ray diffraction and internal friction apparatus. And their influencing factors were also discussed.
Graphite with solid lubrication is selected according to chemical stability and lubrication, and wear-resistence is explained by solid lubrication theory. The appropriate upper limit of the addition of graphite particles should be 7.2% on the based of analysis H-S model and the mixing rule. Effect of graphite particles on thermal expansion was analysised according to theory model, and influencing factors to dimension stability was analysised. Those factors was summarized, the design principle of SiC/Gr/Al was established.
TEM observations indicate SiC-Al and Gr-Al interfaces are clean and free from interfacial reaction products, which are attributed to fabrication process. Meanwhile, there is no interface reactivity in Gr-Al interfaces, which is due to high degree of graphization. The bonding strength between graphite and matrix alloy is weak, and the lamellar is sliding easily. Micro-stress is relaxed in the process of fabrication and heat treatment, The addition of graphite particles decreases the dislocation density in the composite. Moreover, the dislocation in the casting microstructure generates the sub-boundary, and the density of precipitate phase dependent on the dislocation nucleation also reduces
The coefficient of thermal expansion (CTE) and daming properties are tested, and the results show that CTE is between 11.5~13×10-6/℃and Q-1 for SiC/Gr/Al composite is 2~6 times higher than that of the aluminum matrix. These meet the requirements of thermal expansion matching the corresponding materials and high damping in precision instrument.
The increment of graphite volume fraction, the decrement of particle spacing, destroyed continuity of matrix, result in the reducing of tensile strength of SiC/Gr/Al composites。The increment of interfacial area and reduction of partilcle spacing result in the increasing amount of crack source and destroy the continuity of aluminum matrix, which is the main reason for decrease of mechanical properties.
Tribological conditions of tool/ composite in the process of cutting are analsized by wear test. Results show that the tribo-layer formed during wear cause the decreasing of friction coefficient and wear loss. Further analysis to the mechanism of the increase in wear resistance, the worn surface of SiC/Gr/Al composite covered by a continuous or thin tribo-layer can also improve wear resistance.
Graphite particles improve that machinability from tool wear, cutting force and surface roughness. It is due to the decreasing of hardness and strength of composites, which has decreased the coefficient of chip distortion and promoting crack propagation of chip, and solid lubrication to tool. With increasing Vf of graphite particles, tool wear increase. Particle size of graphite has little effect on the tool wear, but has very remarble effect on cutting force. The characteristic of thrust force (Ft) higher than cutting force (Fc) is not change by the addition of graphite particles. The SiC+Al matrix failed in ductile manner while graphite particle fail in a brittle manner. The elastic modulus was estimated by H-S models and the estimated value is 93.5% of the tested values.
The investigation of dimension stability show that: the addition of graphite is beneficial to improving dimensional stability Sufficient aging precipitation, stable dislocation structure and lower macro residual stress ensure dimension stability by appropriate thermal cycling procedure (A+TCC(0)and A+TCC(-70)) when compared with aging procedure. Besides thermal cycling procedure, relaxation of micro stress by graphite particles further improved dimension stability of SiC/Gr/Al. From analysis both micro-deformation resistance and dimension stability under no load, A+TCC (0) is the optimum procedure for improving the dimension stability.
In the paper, we design SiC/Gr/Al composites according to the requirement of instrument materials, and find proper heat treatment process. For the 40%SiC/5%Gr(6μm)/Al composites, the tool life maching the composite was prolonged by 40%, the elastic modulus are maintained 150GPa, variable dimentional stability is lower than 0.61×10-6, which meet the requirements of instrument properties.
引文
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