晶态和非晶钎料连接ZrO_2与Ti6Al4V的组织与强度
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摘要
氧化锆具有高硬度、高耐磨性及耐高温氧化腐蚀等特点，但是其加工性能差，易碎、且不能被加工成复杂零部件。Ti–6Al–4V合金具有轻质高强度、较高的拉伸性能和韧性、高抗腐蚀性等特点。将氧化锆与Ti–6Al–4V合金相结合，使二者优势互补，广泛应用于航空航天等领域中。将二者进行钎焊连接采用的钎料大部分是加入2–5wt.%Ti的近共晶成分的银系合金Ag–28wt.%Cu。但是该钎料中含有60–70wt.%的贵金属银，大幅提高了其成本。近年来，非晶合金被广泛作为钎料应用于连接金属和陶瓷。非晶钎料具有不同于晶态钎料的独特延展性和成形加工性能，而且加入活性元素Ti和Zr不但有利于提高其非晶形成能力还有利于提高其与陶瓷的润湿性。非晶钎料有望取代传统的贵金属Ag–Cu–Ti钎料。
因此，本文对比研究了Ag–Cu–Ti和Ti、Zr、Cu基三种非晶钎料连接ZrO_2陶瓷和Ti–6Al–4V合金。利用X–射线衍射(XRD)、扫描电镜(SEM)、场发射扫描电镜（FESEM）、能谱仪(EDS)以及MTS材料性能测试机等分析检测手段表征了不同钎焊工艺参数对连接处界面微观结构及其演变行为、界面反应机理及界面结合的影响规律及机制。对各种钎料及其钎焊工艺参数影响的界面微观结构与剪切强度的影响规律及两者的内在联系进行了认真的研究和讨论。进而演绎出控制或决定性能的界面结构特征，以及决定界面结构的钎焊工艺参数。建立钎料成分、钎焊工艺及界面结构和界面结合的相互关系。为开发新型非晶钎料及促进其应用奠定了必要的理论基础。本文的主要研究结果如下：
(1)揭示了晶态Ag–Cu–Ti合金熔体在ZrO_2陶瓷基板上的润湿机制为反应性润湿。润湿过程中发生界面反应产物有TiO、Cu–Ti–O相和Cu–Ti金属间化合物。研究了合金钎料中Ti元素的含量(4–10at%)以及温度对该反应体系的润湿行为以及润湿性变化规律：Ag–Cu–Ti钎料合金在ZrO_2陶瓷基板上的润湿性随Ti含量的增加逐渐改善；Ag_(54)Cu_(43)Ti_4合金熔体在ZrO_2陶瓷基板上的润湿性对温度有明显的反常依赖性。
(2)研究了ZrO_2/Ag_(53)Cu_(41)Ti6/Ti–6Al–4V体系中钎焊工艺参数对接头界面结构以及接头性能的影响规律。典型界面组织结构为ZrO_2/TiO+Ti_2O+Cu_2Ti_4O反应层/Ag/CuTi+CuTi_2金属间化合物/针状魏氏体组织/Ti–6Al–4V。得出钎焊温度和保温时间及冷却速度不宜过高或者过快，钎焊温度过高保温时间过长，合金钎料中活性元素Ti与母材反应程度加剧，容易导致TiO+Ti_2O+Cu_2Ti_4O反应层和魏氏体组织层厚增加；冷却速度过快，易产生裂纹和孔洞等微观缺陷，均对界面强度造成不利的影响。当钎焊温度为1123K，保温时间为10min，冷却速度为5K/min时接头结合较好，为最佳工艺参数，其钎焊接头剪切强度可以达到178MPa。
(3)揭示了Cu_(50)Ti_(33)Zr17、Ti_47Zr28Cu14Ni11和Zr_(55)Cu_(30)Al_(10)Ni_5三种非晶熔体在ZrO_2陶瓷基板上的润湿行为及润湿类型均为反应性润湿，对温度有明显的依赖性，高温有助于润湿。反应产物主要有TiO、Cu–Ti–O相和金属间化合物。由于钎料中的活性组元Ti, Zr在界面的富集并参与界面反应，极大地改善了体系的润湿性。但是较高的Zr浓度会抑制元素Ti与ZrO_2反应生成TiO+Ti_2O化合物，从而减弱Ti对反应润湿的促进作用。同时Ti和Zr的含量不宜过高，在较高温度下，产生过多的脆性金属间化合物会导致合金液滴与陶瓷基板的界面处出现微裂纹甚至剥离。Cu和Ni元素可以无限固溶，有利于提高非晶熔体熔化后的流动性。润湿性能由大到小的顺序是：Cu_(50)Ti_(33)Zr17/ZrO_2>Ti_47Zr28Cu14Ni11/ZrO_2> Zr_(55)Cu_(30)Al_(10)Ni_5/ZrO_2。
(4)建立了三种非晶钎料钎焊体系中工艺参数、界面微观结构与接头剪切强度三者之间的内在联系。总体上，钎焊温度、保温时间及冷却速度决定了反应界面反应层的厚度，金属间化合物和魏氏体组织的数量及分布，进而最终决定了接头的剪切强度。在具体工艺上，钎焊温度对界面反应层的厚度影响较大，界面反应层厚度又是剪切强度的关键。保温时间对金属间化合物和魏氏体组织的分布和数量具有关键的作用；缓慢的冷却速度可以降低残余应力，减少微观缺陷的发生。剪切强度的高低主要取决于界面反应层的厚度、较少的金属间化合物和魏氏体组织以及缓慢的冷却速度。
(5)总结出了三个体系连接的最佳工艺参数。①ZrO_2/Cu_(50)Ti_(33)Zr17/Ti–6Al–4V体系，当钎焊温度为1173K，保温时间为10min，冷却速度为5K/min为最佳工艺参数，其钎焊接头剪切强度可以达到162MPa。②ZrO_2/Ti_47Zr28Cu14Ni11/Ti–6Al–4V体系，当钎焊温度为1123K，保温时间为45min，冷却速度为5K/min为最佳工艺参数，其钎焊接头剪切强度可以达到85MPa。③ZrO_2/Zr_(55)Cu_(30)Al_(10)Ni_5/Ti–6Al–4V体系，当钎焊温度为1173K，保温时间为10min，冷却速度为5K/min为最佳工艺参数，其钎焊接头剪切强度可以达到95MPa。
Zirconia is a beneficial ceramic material in many structures and devices due to its highstrength, fracture toughness and hardness. However, its brittleness and lack of flexibilitymake the fabrication of complex shaped and/or large-sized components difficult. Manystructural applications of zirconia demonstrate its reliable and durable joining to metals.Among these metals, Ti–6Al–4V alloy is most often introduced to bonding with zirconia.The combination of high specific strength, good tensile strength at moderate temperatureand excellent corrosion resistance make them widely be applied in the aerospace industries.
One of the mostly widely used filler metal is based on the Ag–Cu–Ti system, namely onthe Ag–28wt.%Cu eutectic composition, with about2–5wt.%of titanium additions.Nevertheless, consumption of a large amount (60-70wt.%) of the noble metal, Ag, in thebrazing filler is the main disadvantage of these alloys. Recently, amorphous alloys have beenused as brazing fillers. The amorphous fillers have significant advantages such as unique offoil form combined with outstanding ductility and flexibility, wide range of width andthickness available. In particular, the amorphous fillers containing active Ti and Zr elementswith good glass forming ability may replace the traditional Ag–Cu–Ti filler alloys in somecases.
In this paper, the interface reaction mechanism was studied, and the effect of brazingprocess parameters on microstructure and shear strength was investigated when the ZrO_2ceramic and Ti–6Al–4V alloy were brazed with Ag–Cu–Ti and Ti, Zr and Cu–based threekinds of amorphous fillers using by XRD, SEM, FESEM, EDS and the MTS material testingmachine and so on detection means. And then deduce the interface structure of control ordecision properties characteristics, and defines interface microstructure of the brazingprocess parameters. Establish the relationship of filler composition, brazing processparameters and interface microstructure. It provides a necessary theoretical basis andapplications for the development of novel amorphous fillers in the ZrO_2/Ti–6Al–4V joints.The major results of the present study are as follows:
(1) Reveals the wetting of molten Ag–Cu–Ti metallic glass alloy on the ZrO_2substratebelongs to the reactive wetting. The reaction products are mainly TiO, Cu–Ti–O phases andCu–Ti intermetallic compounds. Study the Ti element content in the alloy filler (4–10at%) and temperature on the reaction system of wetting behavior, and wettability change rule.With the increase in the content of Ti, the wettability of Ag–Cu–Ti/ZrO_2systems areimproved significantly. It is the anomalous dependence of wettability of Ag_(54)Cu43Ti_4/ZrO_2system on the temperatures.
(2) The ZrO_2/Ag_(53)Cu_(41)Ti6/Ti–6Al–4V system in the brazing process parameters affectthe performance of joint interface microstructure and joint are studied. The interfacestructure was ZrO_2/TiO+Ti_2O+Cu_2Ti_4O/Ag/CuTi+CuTi_2/Widmanst ten/Ti–6Al–4V withAg_(53)Cu_(41)Ti6filler. Brazing temperature, holding time and cooling rate is unfavorable higheror too fast, higher brazing temperature and holding time is too long, active element Ti in thealloy filler with parent metal reaction degree aggravate, easily lead to TiO+Ti_2O+Cu_2Ti_4Oreaction and Widmanst ten layer thickness increases. Cooling rate too fast, easy to producethe micro defects such as cracks and holes, have adverse effects on the interface strength.When the brazing temperature was1123K for10min, the cooling rate of5K/min for theoptimal parameters, the joint is better; the reaction layer thickness is moderate. The shearstrength was178MPa.
(3) Reveals the wetting of molten Cu_(50)Ti_(33)Zr17, Ti_47Zr28Cu14Ni11and Zr_(55)Cu_(30)Al_(10)Ni_5three amorphous alloys on the ZrO_2substrate belongs to the reactive wetting. The wettabilityof the amorphous fillers on the ZrO_2substrates obvious dependence on temperature, hightemperature helps the wetting. The reaction products are mainly TiO, Cu–Ti–O phases andintermetallic compounds. Due to the active elements of Ti, Zr in the fillers, enrichment andparticipate in the interface and reaction, greatly improve the wettability of the system. Buthigher element Zr concentration would inhibit Ti and ZrO_2reaction generated TiO+Ti_2Ocompounds, thereby weakening Ti wetting role in the reaction. But in the high temperature,high content of Ti and Zr will also generate a large number of brittle phases, resulting in thealloy droplets and ceramic substrate at the interface of micro–crack or even peel. Cu and Nielement can be infinite solid solution, amorphous fillers after the melt flow rate is enhanced.Wettability order: Cu_(50)Ti_(33)Zr17/ZrO_2>Ti_47Zr28Cu14Ni11/ZrO_2> Zr_(55)Cu_(30)Al_(10)Ni_5/ZrO_2.
(4) Set up three kinds of amorphous fillers brazing system of process parameters, theinterface microstructure and the inner link between and among joint shear strength. Overall,the brazing temperature, holding time and cooling rate determines the thickness of theinterfacial reaction layer, intermetallic compounds and Widmanst ten stucture and thenumber of distribution, and finally decided to the shear strength of joint. On the specificprocess, brazing temperature had a greater influence on the thickness of the interfacialreaction layer, is critical in shear strength. Holding time has a key role of intermetalliccompounds and Widmanst ten stucture distribution and the number. Slow cooling rate canreduce the residual stress, reducing the occurrence of the micro defects. Shear strengthmainly depends on the thickness of the interfacial reaction layer, the less of intermetalliccompound and Widmanst ten stucture and the slow cooling rate.
(5) Summed up the brazing optimal parameters of the three systems:① ZrO_2/Cu_(50)Ti_(33)Zr17/Ti–6Al–4V system, when the brazing temperature was1173K for10min,the cooling rate of5K/min for the optimal parameters, the shear strength was162MPa.②ZrO_2/Ti_47Zr28Cu14Ni11/Ti–6Al–4V system, when the brazing temperature was1173K for10min, the cooling rate of5K/min for the optimal parameters，the shear strength was85MPa.③ZrO_2/Zr_(55)Cu_(30)Al_(10)Ni_5/Ti–6Al–4V system, when the brazing temperature was1173K for10min, the cooling rate of5K/min for the optimal parameters, the shear strength was95MPa.
因此，本文对比研究了Ag–Cu–Ti和Ti、Zr、Cu基三种非晶钎料连接ZrO_2陶瓷和Ti–6Al–4V合金。利用X–射线衍射(XRD)、扫描电镜(SEM)、场发射扫描电镜（FESEM）、能谱仪(EDS)以及MTS材料性能测试机等分析检测手段表征了不同钎焊工艺参数对连接处界面微观结构及其演变行为、界面反应机理及界面结合的影响规律及机制。对各种钎料及其钎焊工艺参数影响的界面微观结构与剪切强度的影响规律及两者的内在联系进行了认真的研究和讨论。进而演绎出控制或决定性能的界面结构特征，以及决定界面结构的钎焊工艺参数。建立钎料成分、钎焊工艺及界面结构和界面结合的相互关系。为开发新型非晶钎料及促进其应用奠定了必要的理论基础。本文的主要研究结果如下：
(1)揭示了晶态Ag–Cu–Ti合金熔体在ZrO_2陶瓷基板上的润湿机制为反应性润湿。润湿过程中发生界面反应产物有TiO、Cu–Ti–O相和Cu–Ti金属间化合物。研究了合金钎料中Ti元素的含量(4–10at%)以及温度对该反应体系的润湿行为以及润湿性变化规律：Ag–Cu–Ti钎料合金在ZrO_2陶瓷基板上的润湿性随Ti含量的增加逐渐改善；Ag_(54)Cu_(43)Ti_4合金熔体在ZrO_2陶瓷基板上的润湿性对温度有明显的反常依赖性。
(2)研究了ZrO_2/Ag_(53)Cu_(41)Ti6/Ti–6Al–4V体系中钎焊工艺参数对接头界面结构以及接头性能的影响规律。典型界面组织结构为ZrO_2/TiO+Ti_2O+Cu_2Ti_4O反应层/Ag/CuTi+CuTi_2金属间化合物/针状魏氏体组织/Ti–6Al–4V。得出钎焊温度和保温时间及冷却速度不宜过高或者过快，钎焊温度过高保温时间过长，合金钎料中活性元素Ti与母材反应程度加剧，容易导致TiO+Ti_2O+Cu_2Ti_4O反应层和魏氏体组织层厚增加；冷却速度过快，易产生裂纹和孔洞等微观缺陷，均对界面强度造成不利的影响。当钎焊温度为1123K，保温时间为10min，冷却速度为5K/min时接头结合较好，为最佳工艺参数，其钎焊接头剪切强度可以达到178MPa。
(3)揭示了Cu_(50)Ti_(33)Zr17、Ti_47Zr28Cu14Ni11和Zr_(55)Cu_(30)Al_(10)Ni_5三种非晶熔体在ZrO_2陶瓷基板上的润湿行为及润湿类型均为反应性润湿，对温度有明显的依赖性，高温有助于润湿。反应产物主要有TiO、Cu–Ti–O相和金属间化合物。由于钎料中的活性组元Ti, Zr在界面的富集并参与界面反应，极大地改善了体系的润湿性。但是较高的Zr浓度会抑制元素Ti与ZrO_2反应生成TiO+Ti_2O化合物，从而减弱Ti对反应润湿的促进作用。同时Ti和Zr的含量不宜过高，在较高温度下，产生过多的脆性金属间化合物会导致合金液滴与陶瓷基板的界面处出现微裂纹甚至剥离。Cu和Ni元素可以无限固溶，有利于提高非晶熔体熔化后的流动性。润湿性能由大到小的顺序是：Cu_(50)Ti_(33)Zr17/ZrO_2>Ti_47Zr28Cu14Ni11/ZrO_2> Zr_(55)Cu_(30)Al_(10)Ni_5/ZrO_2。
(4)建立了三种非晶钎料钎焊体系中工艺参数、界面微观结构与接头剪切强度三者之间的内在联系。总体上，钎焊温度、保温时间及冷却速度决定了反应界面反应层的厚度，金属间化合物和魏氏体组织的数量及分布，进而最终决定了接头的剪切强度。在具体工艺上，钎焊温度对界面反应层的厚度影响较大，界面反应层厚度又是剪切强度的关键。保温时间对金属间化合物和魏氏体组织的分布和数量具有关键的作用；缓慢的冷却速度可以降低残余应力，减少微观缺陷的发生。剪切强度的高低主要取决于界面反应层的厚度、较少的金属间化合物和魏氏体组织以及缓慢的冷却速度。
(5)总结出了三个体系连接的最佳工艺参数。①ZrO_2/Cu_(50)Ti_(33)Zr17/Ti–6Al–4V体系，当钎焊温度为1173K，保温时间为10min，冷却速度为5K/min为最佳工艺参数，其钎焊接头剪切强度可以达到162MPa。②ZrO_2/Ti_47Zr28Cu14Ni11/Ti–6Al–4V体系，当钎焊温度为1123K，保温时间为45min，冷却速度为5K/min为最佳工艺参数，其钎焊接头剪切强度可以达到85MPa。③ZrO_2/Zr_(55)Cu_(30)Al_(10)Ni_5/Ti–6Al–4V体系，当钎焊温度为1173K，保温时间为10min，冷却速度为5K/min为最佳工艺参数，其钎焊接头剪切强度可以达到95MPa。
Zirconia is a beneficial ceramic material in many structures and devices due to its highstrength, fracture toughness and hardness. However, its brittleness and lack of flexibilitymake the fabrication of complex shaped and/or large-sized components difficult. Manystructural applications of zirconia demonstrate its reliable and durable joining to metals.Among these metals, Ti–6Al–4V alloy is most often introduced to bonding with zirconia.The combination of high specific strength, good tensile strength at moderate temperatureand excellent corrosion resistance make them widely be applied in the aerospace industries.
One of the mostly widely used filler metal is based on the Ag–Cu–Ti system, namely onthe Ag–28wt.%Cu eutectic composition, with about2–5wt.%of titanium additions.Nevertheless, consumption of a large amount (60-70wt.%) of the noble metal, Ag, in thebrazing filler is the main disadvantage of these alloys. Recently, amorphous alloys have beenused as brazing fillers. The amorphous fillers have significant advantages such as unique offoil form combined with outstanding ductility and flexibility, wide range of width andthickness available. In particular, the amorphous fillers containing active Ti and Zr elementswith good glass forming ability may replace the traditional Ag–Cu–Ti filler alloys in somecases.
In this paper, the interface reaction mechanism was studied, and the effect of brazingprocess parameters on microstructure and shear strength was investigated when the ZrO_2ceramic and Ti–6Al–4V alloy were brazed with Ag–Cu–Ti and Ti, Zr and Cu–based threekinds of amorphous fillers using by XRD, SEM, FESEM, EDS and the MTS material testingmachine and so on detection means. And then deduce the interface structure of control ordecision properties characteristics, and defines interface microstructure of the brazingprocess parameters. Establish the relationship of filler composition, brazing processparameters and interface microstructure. It provides a necessary theoretical basis andapplications for the development of novel amorphous fillers in the ZrO_2/Ti–6Al–4V joints.The major results of the present study are as follows:
(1) Reveals the wetting of molten Ag–Cu–Ti metallic glass alloy on the ZrO_2substratebelongs to the reactive wetting. The reaction products are mainly TiO, Cu–Ti–O phases andCu–Ti intermetallic compounds. Study the Ti element content in the alloy filler (4–10at%) and temperature on the reaction system of wetting behavior, and wettability change rule.With the increase in the content of Ti, the wettability of Ag–Cu–Ti/ZrO_2systems areimproved significantly. It is the anomalous dependence of wettability of Ag_(54)Cu43Ti_4/ZrO_2system on the temperatures.
(2) The ZrO_2/Ag_(53)Cu_(41)Ti6/Ti–6Al–4V system in the brazing process parameters affectthe performance of joint interface microstructure and joint are studied. The interfacestructure was ZrO_2/TiO+Ti_2O+Cu_2Ti_4O/Ag/CuTi+CuTi_2/Widmanst ten/Ti–6Al–4V withAg_(53)Cu_(41)Ti6filler. Brazing temperature, holding time and cooling rate is unfavorable higheror too fast, higher brazing temperature and holding time is too long, active element Ti in thealloy filler with parent metal reaction degree aggravate, easily lead to TiO+Ti_2O+Cu_2Ti_4Oreaction and Widmanst ten layer thickness increases. Cooling rate too fast, easy to producethe micro defects such as cracks and holes, have adverse effects on the interface strength.When the brazing temperature was1123K for10min, the cooling rate of5K/min for theoptimal parameters, the joint is better; the reaction layer thickness is moderate. The shearstrength was178MPa.
(3) Reveals the wetting of molten Cu_(50)Ti_(33)Zr17, Ti_47Zr28Cu14Ni11and Zr_(55)Cu_(30)Al_(10)Ni_5three amorphous alloys on the ZrO_2substrate belongs to the reactive wetting. The wettabilityof the amorphous fillers on the ZrO_2substrates obvious dependence on temperature, hightemperature helps the wetting. The reaction products are mainly TiO, Cu–Ti–O phases andintermetallic compounds. Due to the active elements of Ti, Zr in the fillers, enrichment andparticipate in the interface and reaction, greatly improve the wettability of the system. Buthigher element Zr concentration would inhibit Ti and ZrO_2reaction generated TiO+Ti_2Ocompounds, thereby weakening Ti wetting role in the reaction. But in the high temperature,high content of Ti and Zr will also generate a large number of brittle phases, resulting in thealloy droplets and ceramic substrate at the interface of micro–crack or even peel. Cu and Nielement can be infinite solid solution, amorphous fillers after the melt flow rate is enhanced.Wettability order: Cu_(50)Ti_(33)Zr17/ZrO_2>Ti_47Zr28Cu14Ni11/ZrO_2> Zr_(55)Cu_(30)Al_(10)Ni_5/ZrO_2.
(4) Set up three kinds of amorphous fillers brazing system of process parameters, theinterface microstructure and the inner link between and among joint shear strength. Overall,the brazing temperature, holding time and cooling rate determines the thickness of theinterfacial reaction layer, intermetallic compounds and Widmanst ten stucture and thenumber of distribution, and finally decided to the shear strength of joint. On the specificprocess, brazing temperature had a greater influence on the thickness of the interfacialreaction layer, is critical in shear strength. Holding time has a key role of intermetalliccompounds and Widmanst ten stucture distribution and the number. Slow cooling rate canreduce the residual stress, reducing the occurrence of the micro defects. Shear strengthmainly depends on the thickness of the interfacial reaction layer, the less of intermetalliccompound and Widmanst ten stucture and the slow cooling rate.
(5) Summed up the brazing optimal parameters of the three systems:① ZrO_2/Cu_(50)Ti_(33)Zr17/Ti–6Al–4V system, when the brazing temperature was1173K for10min,the cooling rate of5K/min for the optimal parameters, the shear strength was162MPa.②ZrO_2/Ti_47Zr28Cu14Ni11/Ti–6Al–4V system, when the brazing temperature was1173K for10min, the cooling rate of5K/min for the optimal parameters，the shear strength was85MPa.③ZrO_2/Zr_(55)Cu_(30)Al_(10)Ni_5/Ti–6Al–4V system, when the brazing temperature was1173K for10min, the cooling rate of5K/min for the optimal parameters, the shear strength was95MPa.
引文
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