原位自生TiB晶须增强Al_2O_3/TC4钎焊接头组织结构及性能研究
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摘要
具有高熔点、耐高温、耐腐蚀、耐磨损等特殊性能及抗辐射、耐高频高压绝缘等电气性能的陶瓷材料与具有良好塑韧性金属材的高质量连接一直是工程材料应用研究的重点。钎焊对连接性能差异较大的材料和熔化敏感的材料具有独特优点，因此广泛用于陶瓷与金属的连接，但如何避免因陶瓷与金属间冶金不相容和物性不匹配而产生的钎焊接头残余热应力是目前亟待解决的问题。本课题以降低陶瓷/金属接头残余热应力，提高接头的室温强度和高温强度为目标，将原位自生技术与钎焊相结合，提出一种利用原位自生的TiB晶须增强陶瓷/金属钎焊接头的方法，采用机械混合方法制备的AgCuTi+B、CuTi+TiB_2和Cu+TiB_2复合钎料钎焊Al_2O_3和TC4，研究了原位自生的TiB晶须对接头界面组织及力学性能的影响，并揭示了TiB在钎焊过程中的生成机制。
通过对钎焊接头界面组织所进行的SEM、EDS、XRD和TEM分析，采用AgCuTi+B复合钎料钎焊Al_2O_3与TC4时，接头界面组织结构为：Al_2O_3/Ti_3(Cu,Al)_3O/Ti_2Cu+Ti_2(Cu,Al)/Ag(s.s)+TiCu+Ti(Cu,Al)+Ti_2Cu+TiB/(αTi)+Ti_2Cu/TC4。当B添加过量或Ti添加量不足时，接头中出现TiB_2颗粒。随B粉添加量增大，Ti_3(Cu,Al)_3O层不变，TiB晶须生成量增加。随Ti粉添加量增大，Ti_3(Cu,Al)_3O层增厚，Ti_2Cu和Ti_2(Cu,Al)混合区先增厚后减薄，TC4向钎料中的溶解量减小。随钎焊温度升高或保温时间延长，Ti_3(Cu,Al)_3O可与Al_2O_3进一步反应生成TiO，TC4向钎料中的溶解量增大，钎缝中Ti_2Cu和Ti_2(Cu,Al)生成量增大，Ti_2Cu和Ti_2(Cu,Al)混合区增厚。
采用CuTi+TiB_2或Cu+TiB_2复合钎料钎焊Al_2O_3与TC4时，接头界面组织结构均为Al_2O_3/Ti_3(Cu,Al)_3O+Ti_4(Cu,Al)2O/Ti_2Cu+Ti_2(Cu,Al)+Ti_3Al/Ti_2(Cu,Al)/Ti_2Cu+AlCu2Ti+TiB/(αTi)+Ti_2Cu/TC4。随TiB_2添加量增大，TiB晶须生成量增加，钎缝中先出现Ti_2(Cu,Al)组成区，继而该区变得连续并逐渐向Al_2O_3侧移动。随Ti添加量增大，Ti_2Cu晶界处出现(αTi)+Ti_2Cu组织，钎缝中由Ti_2(Cu,Al)组成的区域变连续并逐渐增厚，AlCu2Ti逐渐减少并消失。随钎焊温度升高和保温时间延长，Ti_3(Cu,Al)_3O和Ti_4(Cu,Al)2O组成区增厚；TC4向钎料中溶解量增大，Ti_2Cu生成量增多，而Ti_2(Cu,Al)先增加后减小，且其组成区远离Al_2O_3；Ti_2Cu晶界处的Ti_3Al增加，Ti_2(Cu,Al)和AlCu2Ti消失。
TiB晶须由钎料中的B或TiB_2与Ti在钎焊过程发生的原位反应而生成，并随B原子在TiB中的扩散而生长。原位自生的TiB尺寸和形貌受B源类型及其添加量、钎焊温度和保温时间的影响。添加B粉时生成的TiB比添加TiB_2时生成的TiB细小。接头中TiB的生成量增多时，TiB逐渐由单独分布变为簇状分布，且其尺寸先增加后减小。随钎焊温度升高和保温时间延长TiB尺寸和生成量逐渐减小。而熔化钎料在Al_2O_3表面的润湿铺展性能则随钎料中添加B或TiB_2量的增加而下降。
通过有限元模拟Al_2O_3/TC4钎焊接头的残余应力，最大残余拉应力产生在Al_2O_3拐角处，最大残余剪应力产生在靠近Al_2O_3/钎缝界面的Al_2O_3与钎缝中。随接头中TiB生成量增加，Al_2O_3中的最大残余拉应力减小，但靠近Al_2O_3/钎缝界面的Al_2O_3与钎缝处最大残余剪应力增大，而且Al_2O_3中的等效残余应力减小，钎缝中的等效残余应力增大。当接头断裂时，TiB晶须使裂纹扩展时发生偏转，由于TiB的弹性模量高于钎缝的弹性模量，使接头内模量载荷发生转移，将应力从裂纹尖端转移至远离裂纹尖端区域，从而降低裂纹尖端应力集中，提高接头抗剪强度。测试环境为室温时，Al_2O_3/CuTi+TiB_2/TC4钎焊接头的最大抗剪强度为143MPa，比Al_2O_3/CuTi/TC4钎焊接头的抗剪强度提高了239%；Al_2O_3/Cu+TiB_2/TC4钎焊接头的最大抗剪强度为97MPa，比Al_2O_3/Cu/TC4钎焊接头的抗剪强度提高了269%；Al_2O_3/AgCuTi+B/TC4钎焊接头的最大抗剪强度为78MPa，比Al_2O_3/AgCuTi/TC4钎焊接头的抗剪强度提高了81%。TiB晶须高熔点及大长径比的特性，使其作为陶瓷骨架存在于钎缝中，有效提高钎焊接头高温性能，Al_2O_3/Cu+TiB_2/TC4钎焊接头在高温下的抗剪强度比Al_2O_3/Cu/TC4的钎焊接头提高40~125%。
In view of the excellent performance of ceramics, such as the high meltingpoint, high temperture resistance, corrosion resistance, radiation resistance, highfrequency and high voltage resistance, as well as insulation perfomances, it issignificant to join ceramics and metals characterized good ductility. Brazing isapplied widely to join ceramics and metals, because it has unique advantages forjoining great property difference materials and melting sensitively materials.However, it is necessary to avoid the residual stresses of joint caused by metallurgyincompatibility and physical properties mismatch. Combining with in situ synthesistechnology and brazing method, the method of in situ synthesizing TiB whiskers tostrengthen ceramic/metal brazed joints is proposed. The method can reduce theceramic/metal joints residual stresses, and improve the joints room-temperature andhigh-temperature shear strength. AgCuTi+B, CuTi+TiB_2and Cu+TiB_2fillersprepared with mechanical mixing are used to braze Al_2O_3to TC4respectively.Effect of TiB on joint microstructure and mechanical properties is investigated. Theformation mechanism of TiB during brazing is revealed.
According to SEM, EDS, XRD and TEM, the microstructure of Al_2O_3/TC4joint with AgCuTi+B composite fillers is Al_2O_3/Ti_3(Cu,Al)_3O/Ti_2Cu+Ti_2(Cu,Al)/Ag(s.s)+TiCu+Ti(Cu,Al)+Ti_2Cu+TiB/(αTi)+Ti_2Cu/TC4. Excessive Bpowders or deficient Ti powders results in the presence of TiB_2in joint. As the Bincrease, TiB whiskers increase, while Ti_3(Cu,Al)_3O area remains nearly constant.As the Ti powders increase, Ti_3(Cu,Al)_3O area thickens. The area consist of Ti_2Cuand Ti_2(Cu,Al) thickens and then thins. The dissolution of TC4dissolved into liquidbrazing fillers decreases. As brazing temperature rises and holding time extends,Ti_3(Cu,Al)_3O reacts with Al_2O_3to form TiO. The dissolution of TC4dissolved intoliquid brazing fillers increases. Both Ti_2Cu and Ti_2(Cu,Al) increase, and then thearea consist of Ti_2Cu and Ti_2(Cu,Al) thickens.
The microstructure of Al_2O_3/TC4joint using CuTi+TiB_2or CuTi+TiB_2composite fillers is Al_2O_3/Ti_3(Cu,Al)_3O+Ti_4(Cu,Al)2O/Ti_2Cu+Ti_2(Cu,Al)+Ti_3Al/Ti_2(Cu,Al)/Ti_2Cu+AlCu2Ti+TiB/(αTi)+Ti_2Cu/TC4. When TiB_2increases, TiBwhiskers increase. The area consist of Ti_2(Cu,Al) appears and becomes continuous,then moves to Al_2O_3. When Ti increases,(αTi)+Ti_2Cu appears in Ti_2Cu grainboundaries. The area consist Ti_2(Cu,Al) becomes continuous and thickens. AlCu2Tidecreases gradually, enen disappears. When brazing temperature rises and holdingtime extends, the area consist of Ti_3(Cu,Al)_3O and Ti_4(Cu,Al)2O thickens. The dissolution of TC4dissolved into liquid brazing fillers increases. Ti_2Cu increases,yet Ti_2(Cu,Al) increases at first and then decreases. The area consist of Ti_2(Cu,Al)gradually moves away from Al_2O_3. Ti_3Al increases in the grain boundaries of Ti_2Cu,while Ti_2(Cu,Al) and AlCu2Ti decrease.
During brazing, B or TiB_2reacts with Ti to form TiB. TiB grows by B atomsdiffusing into TiB. TiB sizes and shapes are responsive to the kind and additiveamount of B source, brazing temperature and holding time. The size of TiBgenerated from B is smaller than that from TiB_2. When it increases, TiB changesfrom single to clusters, and its size increases at first and then decreases. In addition,the size and formation amount of TiB decrease when brazing temperature andholding time increase. When B or TiB_2content increases, the wetting and spreadingof brazing fillers on Al_2O_3decrease.
According to Al_2O_3/TC4joints residual stresses caculated by finite elementsimulations, the highest residual tensil stress appears on the corner of Al_2O_3, and thehighest residual shear stress appears at Al_2O_3and brazing seam near Al_2O_3/brazingseam interface. With the increasing of TiB content, the highest residual tensil stressin Al_2O_3decreases, the highest residual shear stress in Al_2O_3and brazing seam nearAl_2O_3/brazing seam interface increases, and the equivalent residual stressesdistributed in Al_2O_3decrease, but that in brazing seam decrease. When joint fractureoccurs, TiB whiskers can make cracks deflect during propagation. For the elasticmodulus of TiB is higher than the brazing seam, TiB can transfer the modulus loadin joint, and move stresses at a crack tip to regions remote from the crack tip.Finally, the stress intensity at the crack tip decreases, and the joint shear strength isimproved. At room temperture, the maximum shear strength ofAl_2O_3/CuTi+TiB_2/TC4joints is143MPa, which is239%higher than that of theAl_2O_3/CuTi/TC4joints; the maximum shear strength of Al_2O_3/Cu+TiB_2/TC4jointsis97MPa, which is269%higher than that of the Al_2O_3/Cu/TC4joints; themaximum shear strength of Al_2O_3/AgCuTi+B/TC4joints is78MPa, which is81%higher than that of the Al_2O_3/AgCuTi/TC4joints. At high temperture, the maximumshear strength of Al_2O_3/Cu+TiB_2/TC4joints is40~125%higher than that of theAl_2O_3/Cu/TC4joints. It can be attributed that TiB whiskers exist in joints, acted asceramic skeleton, owing to its high melting point and large aspect ratio.
通过对钎焊接头界面组织所进行的SEM、EDS、XRD和TEM分析，采用AgCuTi+B复合钎料钎焊Al_2O_3与TC4时，接头界面组织结构为：Al_2O_3/Ti_3(Cu,Al)_3O/Ti_2Cu+Ti_2(Cu,Al)/Ag(s.s)+TiCu+Ti(Cu,Al)+Ti_2Cu+TiB/(αTi)+Ti_2Cu/TC4。当B添加过量或Ti添加量不足时，接头中出现TiB_2颗粒。随B粉添加量增大，Ti_3(Cu,Al)_3O层不变，TiB晶须生成量增加。随Ti粉添加量增大，Ti_3(Cu,Al)_3O层增厚，Ti_2Cu和Ti_2(Cu,Al)混合区先增厚后减薄，TC4向钎料中的溶解量减小。随钎焊温度升高或保温时间延长，Ti_3(Cu,Al)_3O可与Al_2O_3进一步反应生成TiO，TC4向钎料中的溶解量增大，钎缝中Ti_2Cu和Ti_2(Cu,Al)生成量增大，Ti_2Cu和Ti_2(Cu,Al)混合区增厚。
采用CuTi+TiB_2或Cu+TiB_2复合钎料钎焊Al_2O_3与TC4时，接头界面组织结构均为Al_2O_3/Ti_3(Cu,Al)_3O+Ti_4(Cu,Al)2O/Ti_2Cu+Ti_2(Cu,Al)+Ti_3Al/Ti_2(Cu,Al)/Ti_2Cu+AlCu2Ti+TiB/(αTi)+Ti_2Cu/TC4。随TiB_2添加量增大，TiB晶须生成量增加，钎缝中先出现Ti_2(Cu,Al)组成区，继而该区变得连续并逐渐向Al_2O_3侧移动。随Ti添加量增大，Ti_2Cu晶界处出现(αTi)+Ti_2Cu组织，钎缝中由Ti_2(Cu,Al)组成的区域变连续并逐渐增厚，AlCu2Ti逐渐减少并消失。随钎焊温度升高和保温时间延长，Ti_3(Cu,Al)_3O和Ti_4(Cu,Al)2O组成区增厚；TC4向钎料中溶解量增大，Ti_2Cu生成量增多，而Ti_2(Cu,Al)先增加后减小，且其组成区远离Al_2O_3；Ti_2Cu晶界处的Ti_3Al增加，Ti_2(Cu,Al)和AlCu2Ti消失。
TiB晶须由钎料中的B或TiB_2与Ti在钎焊过程发生的原位反应而生成，并随B原子在TiB中的扩散而生长。原位自生的TiB尺寸和形貌受B源类型及其添加量、钎焊温度和保温时间的影响。添加B粉时生成的TiB比添加TiB_2时生成的TiB细小。接头中TiB的生成量增多时，TiB逐渐由单独分布变为簇状分布，且其尺寸先增加后减小。随钎焊温度升高和保温时间延长TiB尺寸和生成量逐渐减小。而熔化钎料在Al_2O_3表面的润湿铺展性能则随钎料中添加B或TiB_2量的增加而下降。
通过有限元模拟Al_2O_3/TC4钎焊接头的残余应力，最大残余拉应力产生在Al_2O_3拐角处，最大残余剪应力产生在靠近Al_2O_3/钎缝界面的Al_2O_3与钎缝中。随接头中TiB生成量增加，Al_2O_3中的最大残余拉应力减小，但靠近Al_2O_3/钎缝界面的Al_2O_3与钎缝处最大残余剪应力增大，而且Al_2O_3中的等效残余应力减小，钎缝中的等效残余应力增大。当接头断裂时，TiB晶须使裂纹扩展时发生偏转，由于TiB的弹性模量高于钎缝的弹性模量，使接头内模量载荷发生转移，将应力从裂纹尖端转移至远离裂纹尖端区域，从而降低裂纹尖端应力集中，提高接头抗剪强度。测试环境为室温时，Al_2O_3/CuTi+TiB_2/TC4钎焊接头的最大抗剪强度为143MPa，比Al_2O_3/CuTi/TC4钎焊接头的抗剪强度提高了239%；Al_2O_3/Cu+TiB_2/TC4钎焊接头的最大抗剪强度为97MPa，比Al_2O_3/Cu/TC4钎焊接头的抗剪强度提高了269%；Al_2O_3/AgCuTi+B/TC4钎焊接头的最大抗剪强度为78MPa，比Al_2O_3/AgCuTi/TC4钎焊接头的抗剪强度提高了81%。TiB晶须高熔点及大长径比的特性，使其作为陶瓷骨架存在于钎缝中，有效提高钎焊接头高温性能，Al_2O_3/Cu+TiB_2/TC4钎焊接头在高温下的抗剪强度比Al_2O_3/Cu/TC4的钎焊接头提高40~125%。
In view of the excellent performance of ceramics, such as the high meltingpoint, high temperture resistance, corrosion resistance, radiation resistance, highfrequency and high voltage resistance, as well as insulation perfomances, it issignificant to join ceramics and metals characterized good ductility. Brazing isapplied widely to join ceramics and metals, because it has unique advantages forjoining great property difference materials and melting sensitively materials.However, it is necessary to avoid the residual stresses of joint caused by metallurgyincompatibility and physical properties mismatch. Combining with in situ synthesistechnology and brazing method, the method of in situ synthesizing TiB whiskers tostrengthen ceramic/metal brazed joints is proposed. The method can reduce theceramic/metal joints residual stresses, and improve the joints room-temperature andhigh-temperature shear strength. AgCuTi+B, CuTi+TiB_2and Cu+TiB_2fillersprepared with mechanical mixing are used to braze Al_2O_3to TC4respectively.Effect of TiB on joint microstructure and mechanical properties is investigated. Theformation mechanism of TiB during brazing is revealed.
According to SEM, EDS, XRD and TEM, the microstructure of Al_2O_3/TC4joint with AgCuTi+B composite fillers is Al_2O_3/Ti_3(Cu,Al)_3O/Ti_2Cu+Ti_2(Cu,Al)/Ag(s.s)+TiCu+Ti(Cu,Al)+Ti_2Cu+TiB/(αTi)+Ti_2Cu/TC4. Excessive Bpowders or deficient Ti powders results in the presence of TiB_2in joint. As the Bincrease, TiB whiskers increase, while Ti_3(Cu,Al)_3O area remains nearly constant.As the Ti powders increase, Ti_3(Cu,Al)_3O area thickens. The area consist of Ti_2Cuand Ti_2(Cu,Al) thickens and then thins. The dissolution of TC4dissolved into liquidbrazing fillers decreases. As brazing temperature rises and holding time extends,Ti_3(Cu,Al)_3O reacts with Al_2O_3to form TiO. The dissolution of TC4dissolved intoliquid brazing fillers increases. Both Ti_2Cu and Ti_2(Cu,Al) increase, and then thearea consist of Ti_2Cu and Ti_2(Cu,Al) thickens.
The microstructure of Al_2O_3/TC4joint using CuTi+TiB_2or CuTi+TiB_2composite fillers is Al_2O_3/Ti_3(Cu,Al)_3O+Ti_4(Cu,Al)2O/Ti_2Cu+Ti_2(Cu,Al)+Ti_3Al/Ti_2(Cu,Al)/Ti_2Cu+AlCu2Ti+TiB/(αTi)+Ti_2Cu/TC4. When TiB_2increases, TiBwhiskers increase. The area consist of Ti_2(Cu,Al) appears and becomes continuous,then moves to Al_2O_3. When Ti increases,(αTi)+Ti_2Cu appears in Ti_2Cu grainboundaries. The area consist Ti_2(Cu,Al) becomes continuous and thickens. AlCu2Tidecreases gradually, enen disappears. When brazing temperature rises and holdingtime extends, the area consist of Ti_3(Cu,Al)_3O and Ti_4(Cu,Al)2O thickens. The dissolution of TC4dissolved into liquid brazing fillers increases. Ti_2Cu increases,yet Ti_2(Cu,Al) increases at first and then decreases. The area consist of Ti_2(Cu,Al)gradually moves away from Al_2O_3. Ti_3Al increases in the grain boundaries of Ti_2Cu,while Ti_2(Cu,Al) and AlCu2Ti decrease.
During brazing, B or TiB_2reacts with Ti to form TiB. TiB grows by B atomsdiffusing into TiB. TiB sizes and shapes are responsive to the kind and additiveamount of B source, brazing temperature and holding time. The size of TiBgenerated from B is smaller than that from TiB_2. When it increases, TiB changesfrom single to clusters, and its size increases at first and then decreases. In addition,the size and formation amount of TiB decrease when brazing temperature andholding time increase. When B or TiB_2content increases, the wetting and spreadingof brazing fillers on Al_2O_3decrease.
According to Al_2O_3/TC4joints residual stresses caculated by finite elementsimulations, the highest residual tensil stress appears on the corner of Al_2O_3, and thehighest residual shear stress appears at Al_2O_3and brazing seam near Al_2O_3/brazingseam interface. With the increasing of TiB content, the highest residual tensil stressin Al_2O_3decreases, the highest residual shear stress in Al_2O_3and brazing seam nearAl_2O_3/brazing seam interface increases, and the equivalent residual stressesdistributed in Al_2O_3decrease, but that in brazing seam decrease. When joint fractureoccurs, TiB whiskers can make cracks deflect during propagation. For the elasticmodulus of TiB is higher than the brazing seam, TiB can transfer the modulus loadin joint, and move stresses at a crack tip to regions remote from the crack tip.Finally, the stress intensity at the crack tip decreases, and the joint shear strength isimproved. At room temperture, the maximum shear strength ofAl_2O_3/CuTi+TiB_2/TC4joints is143MPa, which is239%higher than that of theAl_2O_3/CuTi/TC4joints; the maximum shear strength of Al_2O_3/Cu+TiB_2/TC4jointsis97MPa, which is269%higher than that of the Al_2O_3/Cu/TC4joints; themaximum shear strength of Al_2O_3/AgCuTi+B/TC4joints is78MPa, which is81%higher than that of the Al_2O_3/AgCuTi/TC4joints. At high temperture, the maximumshear strength of Al_2O_3/Cu+TiB_2/TC4joints is40~125%higher than that of theAl_2O_3/Cu/TC4joints. It can be attributed that TiB whiskers exist in joints, acted asceramic skeleton, owing to its high melting point and large aspect ratio.
引文
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