AZ91D镁合金—漂珠复合材料的制备及性能
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摘要
镁基复合材料具有高的比强度和比刚度，可以改善镁合金的耐热和耐磨损性能，是汽车、电子工业及航空航天领域中最有希望采用的一种复合材料。镁基复合材料的成本主要取决于增强相和制备工艺，针对不同工作条件的要求，研发高性能、低成本、易规模化生产的镁基复合材料仍是当前研究的主要任务。研究表明，采用廉价的增强相是降低镁基复合材料成本的最有效途径，因此，寻找成本更低的增强相制备颗粒增强镁基复合材料，使之满足不同工况的使用需求，具有重要的实用价值。本文采用搅熔铸造法，以资源丰富、成本低廉的粉煤灰漂珠为添加物，开发了一种新型的AZ91D镁合金-粉煤灰漂珠复合材料，并对其开展了室温准静态、动态和高温压缩变形行为以及摩擦磨损性能的研究。采用光学显微镜、扫描电镜(SEM)和透射电镜(TEM)等方法，研究了铸态复合材料的显微组织和界面结构；同时，以漂珠为反应物，通过调控制备工艺，原位制备出内生Mg2Si/AZ91D复合材料。
在研究过程中，设计了用于镁合金熔体浇注的底注式低碳钢模具，有效地节省了镁合金原料，避免了在试样浇注过程中因熔体保护不好而出现氧化的情况，使试样制备简便易行。
本文主要研究内容和研究结果如下：
(1)计算了AZ91D镁合金-漂珠体系中各组元之间可能发生的反应的吉布斯自由能，建立了该体系反应的动力学模型，导出了漂珠在基体中沉降的速度方程。通过调控制备工艺参数，成功制得了漂珠/AZ91D复合材料，得到了有关参数对体系反应动力学的影响规律。
(2)系统地研究了在半固态温度区间内，搅拌温度、时间和速度对漂珠/AZ91D复合材料组织的影响，获得了制备该复合材料的最佳工艺；研究了该复合材料的密度和热膨胀系数等物理性能以及硬度和拉伸强度等力学性能。结果表明：随着漂珠质量分数的增加，漂珠/AZ91D复合材料的密度增大、热膨胀系数降低；漂珠粒径越小，复合材料的热膨胀系数越小。随着漂珠质量分数的增加，漂珠/AZ91D复合材料的布氏硬度增加，当漂珠质量分数超过12wt.%时，复合材料布氏硬度开始下降。漂珠/AZ91D复合材料的拉伸断裂强度因漂珠的加入而降低，它的屈服强度随漂珠的粒径减小和质量分数的增加而提高，但其延伸率表现出与屈服强度相反的趋势。复合材料的弹性模量因漂珠质量分数的增加而提高。
(3)利用MTS810-22M试验机和分离式Hopkinson压杆系统研究了漂珠/AZ91D复合材料在准静态和动态条件下的压缩性能，获得了复合材料在准静态条件下和高应变率下的压缩力学性能的变化规律。在本试验条件下，漂珠/AZ91D复合材料的室温准静态压缩断裂强度高于基体，增加漂珠的质量分数或减小漂珠的粒径或降低应变率均能提高复合材料的室温准静态压缩强度。室温动态压缩试验表明，漂珠/AZ91D复合材料具有显著的应变率效应和小尺寸效应，即复合材料的动态压缩强度随应变率的增加及漂珠粒径的减小而增大。复合材料室温准静态压缩和动态压缩断口均为脆性断口。
(4)利用Instron-5500热模拟试验机研究了漂珠/AZ91D复合材料的高温压缩变形行为。采用幂指数方程计算得到其变形激活能的最小值为199.33kJ/mol、最大值为292.45kJ/mol。显微组织观察表明，低应变率较高温度下，复合材料发生了较充分的再结晶转变，而且再结晶晶粒的尺寸也随应变率增加而变大。高应变率下，在漂珠周围与基体中产生大量的条带状组织和孪晶，条带状组织由许多再结晶晶粒组成。透射电镜（TEM）证实了复合材料经高温压缩变形后发生动态再结晶和形成较高的位错密度。
(5)研究了漂珠/AZ91D复合材料在干摩擦磨损条件下的磨损行为，获得了载荷、时间等外部试验参数以及漂珠含量等内部因素对复合材料摩擦磨损行为的影响规律。结果表明：漂珠/AZ91D复合材料的摩擦磨损表面存在大量的平行沟槽，表现为犁沟特征。在低载荷时复合材料的磨损方式以磨粒磨损为主；而在高载荷时，复合材料的磨损机制转变为以粘着、氧化磨损为主。
(6)在较高温度下对AZ91D-漂珠熔体进行长时间等温，并采用分离浇注的方法，原位制备出Mg2Si/AZ91D复合材料。探索了AZ91D-漂珠熔体等温温度、等温时间、熔体搅拌时间及固溶处理等因素对Mg2Si形貌的影响。Mg2Si/AZ91D复合材料经固溶处理后，抗拉强度显著提高，最高达到184MPa。挤压态Mg2Si/AZ91D复合材料的抗拉强度为302MPa，比铸态(123MPa)提高了2.45倍。铸态Mg2Si/AZ91D复合材料具有较高的高温拉伸强度，在200oC下，抗拉强度为132MPa，比基体提高了约24%。铸态、固溶处理以及高温拉伸条件下，Mg2Si/AZ91D复合材料的拉伸断口均表现为脆性断裂方式，挤压态Mg2Si/AZ91D复合材料拉伸断口表现为韧性断裂方式。
Magnesium matrix composites (MMCS) can improve the heat resistant and wearresistance properties of Mg alloy and are promising materials in the automotive andaerospace industries and electron products because of the combination properties ofhigh specific strength and specific stiffness. The cost of MMCs depends mainly onreinforcements and preparation process. It is still primary jobs at present to researchand develop MMCs with the low cost, high performance and easy to scale productionaccording to the requirement of the different working conditions. The researchindicated that the use of cheap reinforcement was the most effectual way to reduce thecost of MMCs. So, it was of important practical value to seek the lowest costreinforcements and prepare the particle reinforced MMCS in order to meet thedemand in different application conditions. A new type of AZ91D Mg alloy-flyashcenosphere (FAC/AZ91D) composites was developed by adding the flyashcenospheres (FAC) which were rich in natural resources and low cost, by means ofcompo-casting technology, and the room quasi-static compression, dynamiccompression and hot compression behaviour and friction and wear properties of thecomposites were studied. Optical microscopy, scanning electronic microscopy (SEM)and transmission electronic microscopy (TEM) were employed to study themicrostructure and interface structure of the as-cast composites; in the mean time,FAC were used as reactants, in situ Mg2Si/AZ91D composites were prepared bycontrolling the fabrication prarameters.
In the course of the study, a low carbon steel mold with bottom pouring systemwas designed and used for pouring the molten Mg alloy, which saved efficiently theraw material of magnesium alloy and avoided the oxidation of the Mg alloy in thecourse of pouring and made the preparation of specimens simple and available.
The main results were as follows:
(1) The Gibbs free energy of the possible reactions was thermodynamicallycalculated between the various components in FAC/AZ91D Mg alloy systems. The kinetic model of the reaction of this system was established，and the sedimentationvelocity equation of the cenospheres was deduced. The FAC/AZ91D Mg alloycomposites were successfully prepared by controlling the process parameters, and theeffects of the related parameters on the reaction kinetics were obtained.
(2) The effects of the stirring temperature, time and rate on the microstructures ofthe FAC/AZ91D Mg alloy composites were systematically studied in the semi-solidtemperature range, and the best techniques was obtained about this composite; thephysical properties (the density and thermal expansion coefficient) and themechanical properties (the hardness and tensile strength) were investigated. Theresults showed the densities of FAC/AZ91D Mg alloy composites increased andthermal expansion coefficient reduced with increasing cenospheres mass fraction; thelarger the size of cenospheres, the smaller the thermal expansion coefficient. TheBrinell hardness of the FAC/AZ91D Mg alloy composites increased with increasingthe mass fraction of the cenospheres, and the Brinell hardness began to reduce whenthe mass fraction of the cenospheres exceeds12wt.%. The ultimate tensile strength ofthe FAC/AZ91D Mg alloy composites reduced owing to adding the cenospheres, itsyield strength was enhanced with decreasing size of the cenospheres and increasingcenospheres mass fraction, however, its the elongation appeared the contrary trends toits yield strength. The elastic modulus increased due to the increase in the massfraction of the cenospheres.
(3) The properties of quasi-static compression and dynasmic compression of theFAC/AZ91D Mg alloy composites were systematically studied by MTS810-22Mtesting machine and Split Hopkinson Press Bar (SHPB) system, the variation rules ofthe compressive properties under the conditions of the quasi-static compression anddynasmic compression were obtained. Under the conditions of this experiment, theroom quasi-static compression fracture strength of the FAC/AZ91D Mg alloycomposites was higher than that of the matrix Mg alloy and increased with increasingmass fraction of cenospheres or decreasing size of cenospheres or decreasing strainrate. The dynasmic compression test results showed that FAC/AZ91D Mg alloycomposites had obviously strain rate effect and small size effect, namely, thedynasmic compressive strength of the composites increased with increasing strain rateor decreasing size of cenospheres. The room quasi-static or dynasmic compressivefracture was brittle one.
(4) The hot compression deformation behaviors of the FAC/AZ91D composites were studied by means of Instron-5500type thermal simulation machine. Theminimal value of the true activation energy of the hot compression deformation of thecomposites was199.33kJ/mol and the maximum value was292.45kJ/mol bycalculation according to the power law equation. The microstructures investigationshave demonstrated that the full dynamic recrystallization (DRX) was found in thiscomposite, and size of DRX increased with increasing strain rate at lower strain rateand high temperature. Lots of brand structures and twins were observed in matrix andaround cenospheres, and the brand structures consist of the lots of DRX grains. DRXand high dislocation density were comfirmed by TEM in hot compressive deformationcomposites.
(5) The wear behavior of FAC/AZ91D composites was studied under theconditions of dry friction and wear. The effect of the load, wearing time and the massfraction of cenospheres on the wear behavior of FAC/AZ91D composites wereobtained. The results showed that there existed a large number of grooves on the wornsurface of the composites, which were of the furrow features. The wear mechanism ofthe composites was mainly abrasive wear under the low load, and the wearmechanism transformed into adhere abrasion and oxidation wear under high load.
(6) The in situ Mg2Si/AZ91D composites were prepared by the means ofseparation pouring process after the AZ91D-cenosphers melt was isothermally keptfor a long time at high temperature. The effects of such as isothermal temperature,time and stirring time of the AZ91D-cenosphers melt and the solution treatment onthe mophorlogy of Mg2Si were investigated. The tensile strength of the compositeswas improved after solution treatment, and up to184MPa. The tensile srength of theextruded Mg2Si/AZ91D composites was302MPa,2.45times more than that of the ascast composites (123MPa). The as cast composites had better tensile strength at hightemperature, which was132MPa at200oC, and about increased24%than that thematrix. The tensile fracture of Mg2Si/AZ91D composites showed brittle one, and thatof the extruded composites was ductile fracture.
在研究过程中，设计了用于镁合金熔体浇注的底注式低碳钢模具，有效地节省了镁合金原料，避免了在试样浇注过程中因熔体保护不好而出现氧化的情况，使试样制备简便易行。
本文主要研究内容和研究结果如下：
(1)计算了AZ91D镁合金-漂珠体系中各组元之间可能发生的反应的吉布斯自由能，建立了该体系反应的动力学模型，导出了漂珠在基体中沉降的速度方程。通过调控制备工艺参数，成功制得了漂珠/AZ91D复合材料，得到了有关参数对体系反应动力学的影响规律。
(2)系统地研究了在半固态温度区间内，搅拌温度、时间和速度对漂珠/AZ91D复合材料组织的影响，获得了制备该复合材料的最佳工艺；研究了该复合材料的密度和热膨胀系数等物理性能以及硬度和拉伸强度等力学性能。结果表明：随着漂珠质量分数的增加，漂珠/AZ91D复合材料的密度增大、热膨胀系数降低；漂珠粒径越小，复合材料的热膨胀系数越小。随着漂珠质量分数的增加，漂珠/AZ91D复合材料的布氏硬度增加，当漂珠质量分数超过12wt.%时，复合材料布氏硬度开始下降。漂珠/AZ91D复合材料的拉伸断裂强度因漂珠的加入而降低，它的屈服强度随漂珠的粒径减小和质量分数的增加而提高，但其延伸率表现出与屈服强度相反的趋势。复合材料的弹性模量因漂珠质量分数的增加而提高。
(3)利用MTS810-22M试验机和分离式Hopkinson压杆系统研究了漂珠/AZ91D复合材料在准静态和动态条件下的压缩性能，获得了复合材料在准静态条件下和高应变率下的压缩力学性能的变化规律。在本试验条件下，漂珠/AZ91D复合材料的室温准静态压缩断裂强度高于基体，增加漂珠的质量分数或减小漂珠的粒径或降低应变率均能提高复合材料的室温准静态压缩强度。室温动态压缩试验表明，漂珠/AZ91D复合材料具有显著的应变率效应和小尺寸效应，即复合材料的动态压缩强度随应变率的增加及漂珠粒径的减小而增大。复合材料室温准静态压缩和动态压缩断口均为脆性断口。
(4)利用Instron-5500热模拟试验机研究了漂珠/AZ91D复合材料的高温压缩变形行为。采用幂指数方程计算得到其变形激活能的最小值为199.33kJ/mol、最大值为292.45kJ/mol。显微组织观察表明，低应变率较高温度下，复合材料发生了较充分的再结晶转变，而且再结晶晶粒的尺寸也随应变率增加而变大。高应变率下，在漂珠周围与基体中产生大量的条带状组织和孪晶，条带状组织由许多再结晶晶粒组成。透射电镜（TEM）证实了复合材料经高温压缩变形后发生动态再结晶和形成较高的位错密度。
(5)研究了漂珠/AZ91D复合材料在干摩擦磨损条件下的磨损行为，获得了载荷、时间等外部试验参数以及漂珠含量等内部因素对复合材料摩擦磨损行为的影响规律。结果表明：漂珠/AZ91D复合材料的摩擦磨损表面存在大量的平行沟槽，表现为犁沟特征。在低载荷时复合材料的磨损方式以磨粒磨损为主；而在高载荷时，复合材料的磨损机制转变为以粘着、氧化磨损为主。
(6)在较高温度下对AZ91D-漂珠熔体进行长时间等温，并采用分离浇注的方法，原位制备出Mg2Si/AZ91D复合材料。探索了AZ91D-漂珠熔体等温温度、等温时间、熔体搅拌时间及固溶处理等因素对Mg2Si形貌的影响。Mg2Si/AZ91D复合材料经固溶处理后，抗拉强度显著提高，最高达到184MPa。挤压态Mg2Si/AZ91D复合材料的抗拉强度为302MPa，比铸态(123MPa)提高了2.45倍。铸态Mg2Si/AZ91D复合材料具有较高的高温拉伸强度，在200oC下，抗拉强度为132MPa，比基体提高了约24%。铸态、固溶处理以及高温拉伸条件下，Mg2Si/AZ91D复合材料的拉伸断口均表现为脆性断裂方式，挤压态Mg2Si/AZ91D复合材料拉伸断口表现为韧性断裂方式。
Magnesium matrix composites (MMCS) can improve the heat resistant and wearresistance properties of Mg alloy and are promising materials in the automotive andaerospace industries and electron products because of the combination properties ofhigh specific strength and specific stiffness. The cost of MMCs depends mainly onreinforcements and preparation process. It is still primary jobs at present to researchand develop MMCs with the low cost, high performance and easy to scale productionaccording to the requirement of the different working conditions. The researchindicated that the use of cheap reinforcement was the most effectual way to reduce thecost of MMCs. So, it was of important practical value to seek the lowest costreinforcements and prepare the particle reinforced MMCS in order to meet thedemand in different application conditions. A new type of AZ91D Mg alloy-flyashcenosphere (FAC/AZ91D) composites was developed by adding the flyashcenospheres (FAC) which were rich in natural resources and low cost, by means ofcompo-casting technology, and the room quasi-static compression, dynamiccompression and hot compression behaviour and friction and wear properties of thecomposites were studied. Optical microscopy, scanning electronic microscopy (SEM)and transmission electronic microscopy (TEM) were employed to study themicrostructure and interface structure of the as-cast composites; in the mean time,FAC were used as reactants, in situ Mg2Si/AZ91D composites were prepared bycontrolling the fabrication prarameters.
In the course of the study, a low carbon steel mold with bottom pouring systemwas designed and used for pouring the molten Mg alloy, which saved efficiently theraw material of magnesium alloy and avoided the oxidation of the Mg alloy in thecourse of pouring and made the preparation of specimens simple and available.
The main results were as follows:
(1) The Gibbs free energy of the possible reactions was thermodynamicallycalculated between the various components in FAC/AZ91D Mg alloy systems. The kinetic model of the reaction of this system was established，and the sedimentationvelocity equation of the cenospheres was deduced. The FAC/AZ91D Mg alloycomposites were successfully prepared by controlling the process parameters, and theeffects of the related parameters on the reaction kinetics were obtained.
(2) The effects of the stirring temperature, time and rate on the microstructures ofthe FAC/AZ91D Mg alloy composites were systematically studied in the semi-solidtemperature range, and the best techniques was obtained about this composite; thephysical properties (the density and thermal expansion coefficient) and themechanical properties (the hardness and tensile strength) were investigated. Theresults showed the densities of FAC/AZ91D Mg alloy composites increased andthermal expansion coefficient reduced with increasing cenospheres mass fraction; thelarger the size of cenospheres, the smaller the thermal expansion coefficient. TheBrinell hardness of the FAC/AZ91D Mg alloy composites increased with increasingthe mass fraction of the cenospheres, and the Brinell hardness began to reduce whenthe mass fraction of the cenospheres exceeds12wt.%. The ultimate tensile strength ofthe FAC/AZ91D Mg alloy composites reduced owing to adding the cenospheres, itsyield strength was enhanced with decreasing size of the cenospheres and increasingcenospheres mass fraction, however, its the elongation appeared the contrary trends toits yield strength. The elastic modulus increased due to the increase in the massfraction of the cenospheres.
(3) The properties of quasi-static compression and dynasmic compression of theFAC/AZ91D Mg alloy composites were systematically studied by MTS810-22Mtesting machine and Split Hopkinson Press Bar (SHPB) system, the variation rules ofthe compressive properties under the conditions of the quasi-static compression anddynasmic compression were obtained. Under the conditions of this experiment, theroom quasi-static compression fracture strength of the FAC/AZ91D Mg alloycomposites was higher than that of the matrix Mg alloy and increased with increasingmass fraction of cenospheres or decreasing size of cenospheres or decreasing strainrate. The dynasmic compression test results showed that FAC/AZ91D Mg alloycomposites had obviously strain rate effect and small size effect, namely, thedynasmic compressive strength of the composites increased with increasing strain rateor decreasing size of cenospheres. The room quasi-static or dynasmic compressivefracture was brittle one.
(4) The hot compression deformation behaviors of the FAC/AZ91D composites were studied by means of Instron-5500type thermal simulation machine. Theminimal value of the true activation energy of the hot compression deformation of thecomposites was199.33kJ/mol and the maximum value was292.45kJ/mol bycalculation according to the power law equation. The microstructures investigationshave demonstrated that the full dynamic recrystallization (DRX) was found in thiscomposite, and size of DRX increased with increasing strain rate at lower strain rateand high temperature. Lots of brand structures and twins were observed in matrix andaround cenospheres, and the brand structures consist of the lots of DRX grains. DRXand high dislocation density were comfirmed by TEM in hot compressive deformationcomposites.
(5) The wear behavior of FAC/AZ91D composites was studied under theconditions of dry friction and wear. The effect of the load, wearing time and the massfraction of cenospheres on the wear behavior of FAC/AZ91D composites wereobtained. The results showed that there existed a large number of grooves on the wornsurface of the composites, which were of the furrow features. The wear mechanism ofthe composites was mainly abrasive wear under the low load, and the wearmechanism transformed into adhere abrasion and oxidation wear under high load.
(6) The in situ Mg2Si/AZ91D composites were prepared by the means ofseparation pouring process after the AZ91D-cenosphers melt was isothermally keptfor a long time at high temperature. The effects of such as isothermal temperature,time and stirring time of the AZ91D-cenosphers melt and the solution treatment onthe mophorlogy of Mg2Si were investigated. The tensile strength of the compositeswas improved after solution treatment, and up to184MPa. The tensile srength of theextruded Mg2Si/AZ91D composites was302MPa,2.45times more than that of the ascast composites (123MPa). The as cast composites had better tensile strength at hightemperature, which was132MPa at200oC, and about increased24%than that thematrix. The tensile fracture of Mg2Si/AZ91D composites showed brittle one, and thatof the extruded composites was ductile fracture.
引文
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