轻质高强高阻尼Ni-Ti形状记忆合金与复合材料的制备及其性能研究
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摘要
NiTi形状记忆合金因其独特的形状记忆效应、超弹性和优良的力学性能而广泛应用于航空航天、机械工程、生物医学工程和仪器仪表等领域；但在面向造价和运行成本均相对昂贵的航天航空结构和部件及高速回转机械等领域的应用时，面临着苛刻的材料性能和部件轻量化要求。近年来利用不同方法制备的多孔NiTi形状记忆合金因具有小于致密合金的密度但比强度高，有望实现结构轻量化和节省材料以期获得商业化应用。然而，目前制备的多孔NiTi形状记忆合金由于强度相对较低、存储模量低和阻尼能力不高，在航天航空和土木工程等领域的应用仍受到限制；因此，从材料设计和制备方面改善多孔NiTi合金的力学性能和阻尼能力已成为工程应用中的迫切需要。
本研究以纳米尺度SiC颗粒为增强相并结合NH_4HCO_3低温分解造孔技术，运用粉末冶金梯级烧结法成功制备出轻质高强SiC颗粒增强NiTi合金基形状记忆复合材料（SiC/NiTi），有效地解决了多孔NiTi合金压缩强度低和存储模量小的问题。研究结果表明，制备的多孔SiC/NiTi复合材料孔隙率在25.4～49.7%之间，主要相组成为B19′马氏体相、B2奥氏体相以及NiTi_2、Ni_2Ti和Ni_4Ti_3等微量析出相，采用NH_4HCO_3颗粒造孔剂对多孔SiC/NiTi复合材料的物相组成没有影响，而纳米SiC颗粒对合金相组成有一定影响；多孔SiC/NiTi复合材料在经过若干次压缩训练后可获得稳定的线性超弹性，其形状回复率随SiC颗粒体积分数的增加而减小；纳米SiC颗粒的引入使NiTi合金基复合材料具有较高的压缩强度和等效压缩强度，且强度随SiC体积分数的增加而提高。研究结果还表明，多孔SiC/NiTi复合材料仍具有NiTi合金的马氏体转变特征，并保持多孔NiTi合金的高阻尼特性及较高的存储模量；多孔SiC/NiTi复合材料的内耗值（阻尼能力）随SiC颗粒体积分数的增加的而降低，当SiC颗粒体积分数较小时（3wt.%），多孔SiC/NiTi复合材料仍能具有较高的内耗值或等效内耗值及较高的存储模量。
采用粉末冶金梯级烧结法成功制备出具有高阻尼能力的多孔TiNiCu形状记忆合金，有效地解决了多孔NiTi二元合金阻尼能力不高的问题。研究结果表明：多孔TiNiCu合金孔隙率在35～40%之间，其孔隙率和孔隙尺寸均随Cu含量的增加而增大，但表观密度则呈降低趋势，其中多孔Ti50Ni30Cu20合金的密度比同类致密Ti50Ni30Cu20合金低38%；多孔TiNiCu合金的压缩强度随Cu含量的增加而下降，在经过若干次循环压缩后多孔TiNiCu合金具有稳定的超弹性。加入Cu元素后TiNi合金的物相组成发生了改变，但Cu含量变化及时效时间的改变对合金的物相组成性质没有影响；在降温和加热过程中，Ti_(50)Ni_(40)Cu_(10)合金中由于出现B2-B19′和B2-B19-B19′两种类型相变的滞后，使合金的相变温度区间较宽，形状回复率下降；而多孔Ti_(50)Ni_(30)Cu_(20)合金仅发生B2-B19相变，使得合金具有较高的形状回复率。研究结果还表明，多孔TiNiCu合金的内耗值（阻尼能力）随Cu含量的增加而增大；多孔Ti_(50)Ni_(30)Cu_(20)合金具有较高的内耗值和等效内耗值，其最大内耗值是多孔Ti_(50)Ni_(50)合金的五倍，而等效内耗值比同类致密TiNiCu合金高37%。随时效时间的延长，多孔TiNiCu合金的压缩强度、形状恢复率和阻尼性能均呈现先增加后下降的趋势。
采用真空熔炼和水冷吸铸铜模的快速凝固工艺制备出近等原子比NiTi形状记忆合金，并对其显微组织、相变行为、力学性能和阻尼性能进行了研究。研究结果表明：与常规铸态NiTi合金相比较，快速凝固（吸铸）NiTi合金具有小的晶粒尺寸，均匀分布的组织，尤其是具有均匀分布的各种细小析出相；在差热分析（DSC）时降温和加热过程中，快速凝固NiTi合金呈现出较强的相变峰和较窄的相变温度区间；快速凝固NiTi合金的最大内耗值比常规铸态NiTi合金高20%，其在8%应变水平下的形状回复率明显高于常规铸态NiTi合金，而压缩强度则比常规铸态NiTi合金高4%。
NiTi shape memory alloys (SMAs) have attracted significant interests in applications dueto their unique shape memory effect, superelasticity and excellent mechanical performance.These outstanding properties allow commercial applications of NiTi SMAs in the fields ofaerospace, mechanical engineering, biomedical engineering and instrumentation engineeringetc. However, for the materials used to make aerospace/aeronautical structures andcomponents as well as high-speed rotating machines, in which both manufacturing andoperating costs are very high, there is a rigorous requirement for them to be of lightweightand high-performance. In recent decades, porous NiTi SMAs have been extensivelydeveloped through several methods, and they have advantages of low density (or lightweight)and high specific strength, thus show great potential for commercial applications. Thus far,the strength, storage modulus and damping capacity of porous NiTi SMAs fabricated byconventional methods are not satisfactory, and their applications in aerospace/aeronautical andcivil engineering fields have been limited. Therefore, aiming at the above engineeingapplications, there is a great demand in development of porous NiTi shape memory alloyswith enhanced mechanical properties and damping capacity.
In this thesis study, the pore pre-forming technique by using low-temperature-decomposable NH_4HCO_3powder and the nano-sized SiC reinforcement particle were used tofabricate the porous SiC/NiTi composites by means of the step powder-sintering method. Thefabricated porous SiC/NiTi composites show unique characteristics of lightweight and highstrength, yet still exhibiting the shape memory effect and a steady superelasticity, this hasmade a big step forward in solving the problem of low compressive strength and storagemodulus of porous NiTi alloys. The results show that the porous SiC/NiTi composites exhibitthe porosity ratio in the range of25.4～49.7%and consist of B19′and B2as the main phasestogether with some minor phases such as NiTi_2, Ni_2Ti and Ni_4Ti_3. Use of NH_4HCO_3powderas the space-holder has no effect on phase constituents of porous SiC/NiTi composites, but theaddition of nano-sized SiC particles has some influence on phase constituents of thecomposites. The porous SiC/NiTi composites show steady linear superelasticity after several pre-strain training compression cycles, the shape recovery rate of the composites decreaseswith increasing the fraction of SiC particles. The porous SiC/NiTi composites show highcompressive strength and equivalent compression strength, which increase with increasing thefraction of SiC particles. Moreover, it has been shown that the porous SiC/NiTi compositesstill have martensitic transformation characteristics, yet exhibiting high damping capacity andstorage modulus on a par with that of porous NiTi alloys. The internal friction (or dampingcapacity) of the porous SiC/NiTi composites decreases with increasing the fraction of SiCparticles; in particular the composite with SiC fraction of3wt.%still shows high values ofinternal friction and equivalent internal friction as well storage modulus.
Furthermore, porous TiNiCu shape memory alloys were successfully fabricated bymeans of the step powder-sintering method, which exhibit much higher damping capcity overthe porous NiTi binary alloys. The results clearly manifest that the porous TiNiCu alloys showthe porosity ratio in the range of35%to40%, and both the porosity and pore-size of thealloys increase while the alloys’ apparent density decreases with increasing Cu content; inparticular, the apparent density of porous Ti_(50)Ni_(30)Cu_(20)alloy is38%lower than that of thedense Ti_(50)Ni_(30)Cu_(20)alloy. The compressiver strength of porous TiNiCu alloys decreases withincreasing Cu content, the alloys’ residual deformation increases with increasing Cu content,the alloys show steady linear superelasticity after several pre-strain training compressioncycles. After adding Cu element into NiTi alloy, the phase constituents of TiNi alloy changedsignificantly, but the addition amount of Cu element in TiNi alloys and the aging time have noinfluence on phase constituents of the alloys. Both on cooling and heating, the porousTi_(50)Ni_(40)Cu_(10)alloy has a wide temperature range of martensitic transformation raised from thehysteresis of both B2-B19′and B2-B19-B19′phase transformations, leading to a decrease inthe shape recovery rate, while the porous Ti_(50)Ni_(30)Cu_(20)alloy shows high shape recovery ratecorresponding to a narrow temperature range of martensitic transformation which is B2-B19one-step transformation. It has also been shown that the internal friction of porous TiNiCualloys increases with increasing Cu content. The porous Ti_(50)Ni_(30)Cu_(20)alloy shows highinternal friction and equivalent internal friction, with the maximum internal friction valuebeing five times higher than that of porous Ti_(50)Ni_(50)alloy and the maximum equivalentinternal friction value being37%higher than that of the dense TiNiCu alloy. Moreover, it has been shown that with increasing thermal aging time, the compressive strength, shape recoveryrate and internal friction value of porous TiNiCu alloys increase initially and then decreasegradually.
In addition, the near-equiatomic NiTi shape memory alloy was fabricated by rapidsolidification process through vacuum arc melting followed by vacuum suction casting inwater cooled thick copper-mould. The alloy’s microstructure, martensitic transformationbehavior, mechanical properties and damping performance were characterized systematically.The results show that the rapidly solidified (or suction cast) NiTi alloy shows much finergrains and homogeneous microstructure, in particular a uniform distribution of various fineprecipitates, compared to the conventional cast one. In the differential scanning calorimetry(DSC) curves both on cooling and heating, the rapidly solidified NiTi alloy exhibits muchstronger and narrower endothermic and exothermic peaks during the martensitic transformation.Moreover, under a strain level of8%the suction cast NiTi alloy shows a significantimprovement over the conventional cast one, in terms of possessing higher deformationrecovery rates and displaying the increased compressive strength and damping capacity by4%and20%respectively.
本研究以纳米尺度SiC颗粒为增强相并结合NH_4HCO_3低温分解造孔技术，运用粉末冶金梯级烧结法成功制备出轻质高强SiC颗粒增强NiTi合金基形状记忆复合材料（SiC/NiTi），有效地解决了多孔NiTi合金压缩强度低和存储模量小的问题。研究结果表明，制备的多孔SiC/NiTi复合材料孔隙率在25.4～49.7%之间，主要相组成为B19′马氏体相、B2奥氏体相以及NiTi_2、Ni_2Ti和Ni_4Ti_3等微量析出相，采用NH_4HCO_3颗粒造孔剂对多孔SiC/NiTi复合材料的物相组成没有影响，而纳米SiC颗粒对合金相组成有一定影响；多孔SiC/NiTi复合材料在经过若干次压缩训练后可获得稳定的线性超弹性，其形状回复率随SiC颗粒体积分数的增加而减小；纳米SiC颗粒的引入使NiTi合金基复合材料具有较高的压缩强度和等效压缩强度，且强度随SiC体积分数的增加而提高。研究结果还表明，多孔SiC/NiTi复合材料仍具有NiTi合金的马氏体转变特征，并保持多孔NiTi合金的高阻尼特性及较高的存储模量；多孔SiC/NiTi复合材料的内耗值（阻尼能力）随SiC颗粒体积分数的增加的而降低，当SiC颗粒体积分数较小时（3wt.%），多孔SiC/NiTi复合材料仍能具有较高的内耗值或等效内耗值及较高的存储模量。
采用粉末冶金梯级烧结法成功制备出具有高阻尼能力的多孔TiNiCu形状记忆合金，有效地解决了多孔NiTi二元合金阻尼能力不高的问题。研究结果表明：多孔TiNiCu合金孔隙率在35～40%之间，其孔隙率和孔隙尺寸均随Cu含量的增加而增大，但表观密度则呈降低趋势，其中多孔Ti50Ni30Cu20合金的密度比同类致密Ti50Ni30Cu20合金低38%；多孔TiNiCu合金的压缩强度随Cu含量的增加而下降，在经过若干次循环压缩后多孔TiNiCu合金具有稳定的超弹性。加入Cu元素后TiNi合金的物相组成发生了改变，但Cu含量变化及时效时间的改变对合金的物相组成性质没有影响；在降温和加热过程中，Ti_(50)Ni_(40)Cu_(10)合金中由于出现B2-B19′和B2-B19-B19′两种类型相变的滞后，使合金的相变温度区间较宽，形状回复率下降；而多孔Ti_(50)Ni_(30)Cu_(20)合金仅发生B2-B19相变，使得合金具有较高的形状回复率。研究结果还表明，多孔TiNiCu合金的内耗值（阻尼能力）随Cu含量的增加而增大；多孔Ti_(50)Ni_(30)Cu_(20)合金具有较高的内耗值和等效内耗值，其最大内耗值是多孔Ti_(50)Ni_(50)合金的五倍，而等效内耗值比同类致密TiNiCu合金高37%。随时效时间的延长，多孔TiNiCu合金的压缩强度、形状恢复率和阻尼性能均呈现先增加后下降的趋势。
采用真空熔炼和水冷吸铸铜模的快速凝固工艺制备出近等原子比NiTi形状记忆合金，并对其显微组织、相变行为、力学性能和阻尼性能进行了研究。研究结果表明：与常规铸态NiTi合金相比较，快速凝固（吸铸）NiTi合金具有小的晶粒尺寸，均匀分布的组织，尤其是具有均匀分布的各种细小析出相；在差热分析（DSC）时降温和加热过程中，快速凝固NiTi合金呈现出较强的相变峰和较窄的相变温度区间；快速凝固NiTi合金的最大内耗值比常规铸态NiTi合金高20%，其在8%应变水平下的形状回复率明显高于常规铸态NiTi合金，而压缩强度则比常规铸态NiTi合金高4%。
NiTi shape memory alloys (SMAs) have attracted significant interests in applications dueto their unique shape memory effect, superelasticity and excellent mechanical performance.These outstanding properties allow commercial applications of NiTi SMAs in the fields ofaerospace, mechanical engineering, biomedical engineering and instrumentation engineeringetc. However, for the materials used to make aerospace/aeronautical structures andcomponents as well as high-speed rotating machines, in which both manufacturing andoperating costs are very high, there is a rigorous requirement for them to be of lightweightand high-performance. In recent decades, porous NiTi SMAs have been extensivelydeveloped through several methods, and they have advantages of low density (or lightweight)and high specific strength, thus show great potential for commercial applications. Thus far,the strength, storage modulus and damping capacity of porous NiTi SMAs fabricated byconventional methods are not satisfactory, and their applications in aerospace/aeronautical andcivil engineering fields have been limited. Therefore, aiming at the above engineeingapplications, there is a great demand in development of porous NiTi shape memory alloyswith enhanced mechanical properties and damping capacity.
In this thesis study, the pore pre-forming technique by using low-temperature-decomposable NH_4HCO_3powder and the nano-sized SiC reinforcement particle were used tofabricate the porous SiC/NiTi composites by means of the step powder-sintering method. Thefabricated porous SiC/NiTi composites show unique characteristics of lightweight and highstrength, yet still exhibiting the shape memory effect and a steady superelasticity, this hasmade a big step forward in solving the problem of low compressive strength and storagemodulus of porous NiTi alloys. The results show that the porous SiC/NiTi composites exhibitthe porosity ratio in the range of25.4～49.7%and consist of B19′and B2as the main phasestogether with some minor phases such as NiTi_2, Ni_2Ti and Ni_4Ti_3. Use of NH_4HCO_3powderas the space-holder has no effect on phase constituents of porous SiC/NiTi composites, but theaddition of nano-sized SiC particles has some influence on phase constituents of thecomposites. The porous SiC/NiTi composites show steady linear superelasticity after several pre-strain training compression cycles, the shape recovery rate of the composites decreaseswith increasing the fraction of SiC particles. The porous SiC/NiTi composites show highcompressive strength and equivalent compression strength, which increase with increasing thefraction of SiC particles. Moreover, it has been shown that the porous SiC/NiTi compositesstill have martensitic transformation characteristics, yet exhibiting high damping capacity andstorage modulus on a par with that of porous NiTi alloys. The internal friction (or dampingcapacity) of the porous SiC/NiTi composites decreases with increasing the fraction of SiCparticles; in particular the composite with SiC fraction of3wt.%still shows high values ofinternal friction and equivalent internal friction as well storage modulus.
Furthermore, porous TiNiCu shape memory alloys were successfully fabricated bymeans of the step powder-sintering method, which exhibit much higher damping capcity overthe porous NiTi binary alloys. The results clearly manifest that the porous TiNiCu alloys showthe porosity ratio in the range of35%to40%, and both the porosity and pore-size of thealloys increase while the alloys’ apparent density decreases with increasing Cu content; inparticular, the apparent density of porous Ti_(50)Ni_(30)Cu_(20)alloy is38%lower than that of thedense Ti_(50)Ni_(30)Cu_(20)alloy. The compressiver strength of porous TiNiCu alloys decreases withincreasing Cu content, the alloys’ residual deformation increases with increasing Cu content,the alloys show steady linear superelasticity after several pre-strain training compressioncycles. After adding Cu element into NiTi alloy, the phase constituents of TiNi alloy changedsignificantly, but the addition amount of Cu element in TiNi alloys and the aging time have noinfluence on phase constituents of the alloys. Both on cooling and heating, the porousTi_(50)Ni_(40)Cu_(10)alloy has a wide temperature range of martensitic transformation raised from thehysteresis of both B2-B19′and B2-B19-B19′phase transformations, leading to a decrease inthe shape recovery rate, while the porous Ti_(50)Ni_(30)Cu_(20)alloy shows high shape recovery ratecorresponding to a narrow temperature range of martensitic transformation which is B2-B19one-step transformation. It has also been shown that the internal friction of porous TiNiCualloys increases with increasing Cu content. The porous Ti_(50)Ni_(30)Cu_(20)alloy shows highinternal friction and equivalent internal friction, with the maximum internal friction valuebeing five times higher than that of porous Ti_(50)Ni_(50)alloy and the maximum equivalentinternal friction value being37%higher than that of the dense TiNiCu alloy. Moreover, it has been shown that with increasing thermal aging time, the compressive strength, shape recoveryrate and internal friction value of porous TiNiCu alloys increase initially and then decreasegradually.
In addition, the near-equiatomic NiTi shape memory alloy was fabricated by rapidsolidification process through vacuum arc melting followed by vacuum suction casting inwater cooled thick copper-mould. The alloy’s microstructure, martensitic transformationbehavior, mechanical properties and damping performance were characterized systematically.The results show that the rapidly solidified (or suction cast) NiTi alloy shows much finergrains and homogeneous microstructure, in particular a uniform distribution of various fineprecipitates, compared to the conventional cast one. In the differential scanning calorimetry(DSC) curves both on cooling and heating, the rapidly solidified NiTi alloy exhibits muchstronger and narrower endothermic and exothermic peaks during the martensitic transformation.Moreover, under a strain level of8%the suction cast NiTi alloy shows a significantimprovement over the conventional cast one, in terms of possessing higher deformationrecovery rates and displaying the increased compressive strength and damping capacity by4%and20%respectively.
引文
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