Cu-Ni-Sn-Ti活性钎料的研究及其与c-BN的连接
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摘要
立方氮化硼(Cubic Boron Nitride,简称c-BN)的硬度高,抗氧化性强,具有优越的物理、化学和热稳定性能,尤其是避免了金刚石制品加工铁基合金材料发生化学反应的局限性,被国际材料界作为金刚石的替代材料。c-BN制品非常适合加工黑色铁基合金材料、钛合金和高硅铝合金等硬度高韧性大的金属材料,广泛地应用在精密加工、石材加工、汽车制造、机械加工、建材、航空航天及新材料加工等领域。c-BN的延性与冲击韧度低,机械加工性能差,限制其二次开发应用。本文针对c-BN与金属基体连接困难,结合强度低,常在高温条件下工作等问题,开展了以Cu作为活性钎料的基础成分,添加Ni、Sn和Ti等元素的多元铜基活性钎料及其与c-BN连接技术的研究。采用二次回归混料试验设计方法,优化钎料成分;通过SEM、EDS和XRD等方法研究CuNi_5Sn_(5.1)Ti_(11.1)活性钎料钎焊c-BN的界面微观结构和组织,揭示了钎料与c-BN界面冶金结合形成机制;探讨了界面残余应力的分布。
依据键参数理论计算及试验结果,选择Ti元素作为钎焊c-BN多元铜基活性钎料的活性元素。通过对In、Sn、Al、Ag、Pb、Bi和Ga等元素的筛选,并研究In和Sn元素对多元铜基活性钎料组织、性能及钎焊c-BN焊接性的影响,从而选择Sn元素作为多元铜基活性钎料的合金元素。试验研究确定多元铜基活性钎料的组元为Cu、Ni、Sn和Ti。活性元素Ti的含量对Cu-Ni-Sn-Ti系钎料与其钎焊c-BN的微观结构和性能有直接影响。Ti含量增加,钎料对c-BN的润湿性提高,钎料与c-BN间的相互作用加剧,相互作用产生的脆性化合物增多会降低钎料与c-BN界面结合强度,因此Ti含量需要进行优化设计。
采用兼有上下界约束的极端顶点设计方法,对Cu-Ni-Sn-Ti活性钎料成分进行优化分析,建立二阶规范多项式回归模型,计算得到用于钎焊c-BN的Cu-Ni-Sn-Ti活性钎料的最佳成分,(wt%) Ti:11.1%;Sn:5.1%;Ni:5%,余量为Cu。采用DSC差热分析仪测得CuNi_5Sn_(5.1)Ti_(11.1)活性钎料的熔化温度区间为834.6-1000℃。粉状CuNi_5Sn_(5.1)Ti_(11.1)活性钎料对c-BN聚晶复合片的润湿角为28~(-3)0°,对c-BN颗粒的润湿性也很好。CuNi_5Sn_(5.1)Ti_(11.1)活性钎料钎焊c-BN颗粒,界面处Ti元素呈梯度分布,Ti与c-BN颗粒在界面处发生相互作用,实现化学冶金结合。
研究工艺参数对CuNi_5Sn_(5.1)Ti_(11.1)活性钎料钎焊c-BN界面微观结构与性能的变化规律。结果表明,随着钎焊温度提高和保温时间延长,界面处钎料中的活性元素Ti与c-BN间的相互作用加剧,相互作用产生的新相增多,界面形成的反应层变宽,对CuNi_5Sn_(5.1)Ti_(11.1)钎料/c-BN界面结合强度有直接影响。当真空度高于9.0×10~(-3)Pa,钎焊温度T=1100℃,保温时间t=10min时,钎料/c-BN界面的结合强度较高。
热力学和动力学分析表明,在钎焊过程中,钎料中的活性元素Ti与c-BN发生化学反应,生成具有一定金属性和陶瓷性的Ti-N和Ti-B化合物,对钎料与c-BN间的物理化学性质起到过渡作用,界面实现化学冶金结合,形成钎料/TiN/TiB/TiB2/c-BN的结构形式,有利于提高钎料与c-BN界面的结合强度,从而揭示了CuNi_5Sn_(5.1)Ti_(11.1)活性钎料钎焊c-BN界面的形成机制。
采用有限元分析方法研究了CuNi_5Sn_(5.1)Ti_(11.1)活性钎料钎焊c-BN界面连接的大小和分布,残余应力较大值出现在钎料与c-BN接触的最高点处。c-BN的包埋深度会影响界面残余应力的大小和分布。在c-BN包埋35%-75%范围内,随着包埋深度的增加,界面残余应力增大。考虑减小钎焊c-BN所产生的残余应力,满足c-BN颗粒的强度要求,c-BN颗粒的最佳包埋深度为30%-40%。
The cubic boron nitride (c-BN) has some distinguished properties, such as extremely high hardness, good oxidation resistance ability and excellent physical, chemical properties and superior thermal stability. Especially the c-BN does not react with black iron-based alloys while the diamond will do. The c-BN is considered the alternative material of diamond by international materials community. c-BN products are very suitable for machining materials with high hardenss and great tenacity, such as iron-based alloys, titanium alloys and high-silicon aluminum alloys, and so on. c-BN is comprehensively applied to produce various tools or superabrasive against abrasion in the field of precision processing, stone materials processing, auto manufacture, mechanical processing, constructional materials, aviation, new materials processing, and so on. The range and field of application for c-BN is restricted due to the poor processing property of c-BN superhard material. In this paper, aimed at the difficult joining between c-BN and metal substrate, poor joining strength, working at high temperature and other issues, a new type of multi-component Cu-based active filler metal adding Ni, Sn and Ti elements is developed and the brazing mechanism of c-BN brazed with new Cu-based active filler metal is analyzed. The quadratic regression mixture experiment design method is adopted to optimize the composition of Cu-Ni-Sn-Ti active filler metal. The microstructure of the interface between c-BN and CuNi_5Sn_(5.1)Ti_(11.1) active filler metal is researched by means of SEM, EDS and XRD, which reveal the interfacial formation mechanism. The distribution of interfacial residual stress is studied.
According to the theoretical calculation of bond parameters and the experimental results, Ti elements are chosen as active elements of the Cu-based active filler metal for brazing c-BN. By the screen analysis of In, Sn, Al, Ag, Pb, Bi and Ga and other elements and the research on effects of In and Sn elements on the microstructures and properties of multi-component Cu-based active filler metal and the weldability of brazing c-BN, Sn elements are identified as alloy elements of the multi-component Cu-based active filler metal for brazing c-BN. Experimental results show that elements of new Cu-based active filler metal are Cu, Ni, Sn and Ti. Ti contents have effect on microstructures and properties of the Cu-Ni-Sn-Ti active filler metal and brazing c-BN. As Ti contents increase, the wettability of Cu-Ni-Sn-Ti active filler metal on c-BN is improved and the interaction between the filler metal and c-BN is intensified. The brittle compounds resulting from the interaction have an increase, which reduce the interfacial strength between the filler metal and c-BN. Therefore, the Ti contents in the filler metal need to optimize the design.
By the method of extreme vertices design constrained by both upper and lower bounds, the composition of Cu-Ni-Sn-Ti active filler metal is optimized and the regression model of second order polynomial is established. The optimal composition of the Cu-Ni-Sn-Ti active filler metal is Ti:11.1wt.%, Sn:5.1wt.%, Ni:5wt.%, and margin is Cu. The melting temperature range of CuNi_5Sn_(5.1)Ti_(11.1) active filler metal is 834.6-1000℃measured by differential thermal analyzer. The wetting angle of c-BN polycrystalline wet powder CuNi_5Sn_(5.1)Ti_(11.1) active filler metal is 28-30°and the CuNi_5Sn_(5.1)Ti_(11.1) active filler metal exhibits a good wettability on c-BN grains. During the process of brazing, Ti elements in the active filler metals interact with c-BN grains to achieve chemical metallurgical joining at the interface.
The microstructures and mechanical properties of CuNi_5Sn_(5.1)Ti_(11.1) active filler metal/ c-BN interface have been studied through changing processing parameters. The results show that, with the increase of the brazing temperature and the extension of the holding time, the interaction between Ti elements and c-BN enhances and new generating phases at interface increase, which have an important effect on the joining strength of CuNi_5Sn_(5.1)Ti_(11.1) filler metal/c-BN interface. When vacuum degree is above 9.0×10-3Pa, brazing temperature is T=1100℃and holding time is t=10min, the interfacial joining strength is higher.
The formation mechanism of the interface between CuNi_5Sn_(5.1)Ti_(11.1) active filler metal and c-BN is discovered after the thermodynamics and kinetics analysis. During the brazing process, the chemical reaction occurs between active element Ti and c-BN. The compounds with certain metal and ceramic characteristics of Ti-N and Ti-B are pruduced, which play good transitional roles in the chemical and physical performance between CuNi_5Sn_(5.1)Ti_(11.1) active filler metal and c-BN. The filler metal/c-BN interface realizes the chemical metallurgical combination. The structure of filler metal /TiN/TiB/TiB2/c-BN is formed at interface, helping to improve the interfacial joining strength.
Residual stress and its distribution on CuNi_5Sn_(5.1)Ti_(11.1) filler metal/c-BN interface are studied with finite element analysis method. The results show that the larger residual stress value appears at the highest contact point between filler metal and c-BN. The embedding depth of c-BN will affect the value and distribution of interfacial residual stress. In c-BN embedded in 35%-75% range, the interfacial residual stress increases with the increase of the embedding depth. In order to reduce the residual stresses generated brazing c-BN, ensure the c-BN strength requirements, the embedding depth of c-BN in the filler metal is feasible to be controlled at 30%-40% of the whole c-BN grain.
依据键参数理论计算及试验结果,选择Ti元素作为钎焊c-BN多元铜基活性钎料的活性元素。通过对In、Sn、Al、Ag、Pb、Bi和Ga等元素的筛选,并研究In和Sn元素对多元铜基活性钎料组织、性能及钎焊c-BN焊接性的影响,从而选择Sn元素作为多元铜基活性钎料的合金元素。试验研究确定多元铜基活性钎料的组元为Cu、Ni、Sn和Ti。活性元素Ti的含量对Cu-Ni-Sn-Ti系钎料与其钎焊c-BN的微观结构和性能有直接影响。Ti含量增加,钎料对c-BN的润湿性提高,钎料与c-BN间的相互作用加剧,相互作用产生的脆性化合物增多会降低钎料与c-BN界面结合强度,因此Ti含量需要进行优化设计。
采用兼有上下界约束的极端顶点设计方法,对Cu-Ni-Sn-Ti活性钎料成分进行优化分析,建立二阶规范多项式回归模型,计算得到用于钎焊c-BN的Cu-Ni-Sn-Ti活性钎料的最佳成分,(wt%) Ti:11.1%;Sn:5.1%;Ni:5%,余量为Cu。采用DSC差热分析仪测得CuNi_5Sn_(5.1)Ti_(11.1)活性钎料的熔化温度区间为834.6-1000℃。粉状CuNi_5Sn_(5.1)Ti_(11.1)活性钎料对c-BN聚晶复合片的润湿角为28~(-3)0°,对c-BN颗粒的润湿性也很好。CuNi_5Sn_(5.1)Ti_(11.1)活性钎料钎焊c-BN颗粒,界面处Ti元素呈梯度分布,Ti与c-BN颗粒在界面处发生相互作用,实现化学冶金结合。
研究工艺参数对CuNi_5Sn_(5.1)Ti_(11.1)活性钎料钎焊c-BN界面微观结构与性能的变化规律。结果表明,随着钎焊温度提高和保温时间延长,界面处钎料中的活性元素Ti与c-BN间的相互作用加剧,相互作用产生的新相增多,界面形成的反应层变宽,对CuNi_5Sn_(5.1)Ti_(11.1)钎料/c-BN界面结合强度有直接影响。当真空度高于9.0×10~(-3)Pa,钎焊温度T=1100℃,保温时间t=10min时,钎料/c-BN界面的结合强度较高。
热力学和动力学分析表明,在钎焊过程中,钎料中的活性元素Ti与c-BN发生化学反应,生成具有一定金属性和陶瓷性的Ti-N和Ti-B化合物,对钎料与c-BN间的物理化学性质起到过渡作用,界面实现化学冶金结合,形成钎料/TiN/TiB/TiB2/c-BN的结构形式,有利于提高钎料与c-BN界面的结合强度,从而揭示了CuNi_5Sn_(5.1)Ti_(11.1)活性钎料钎焊c-BN界面的形成机制。
采用有限元分析方法研究了CuNi_5Sn_(5.1)Ti_(11.1)活性钎料钎焊c-BN界面连接的大小和分布,残余应力较大值出现在钎料与c-BN接触的最高点处。c-BN的包埋深度会影响界面残余应力的大小和分布。在c-BN包埋35%-75%范围内,随着包埋深度的增加,界面残余应力增大。考虑减小钎焊c-BN所产生的残余应力,满足c-BN颗粒的强度要求,c-BN颗粒的最佳包埋深度为30%-40%。
The cubic boron nitride (c-BN) has some distinguished properties, such as extremely high hardness, good oxidation resistance ability and excellent physical, chemical properties and superior thermal stability. Especially the c-BN does not react with black iron-based alloys while the diamond will do. The c-BN is considered the alternative material of diamond by international materials community. c-BN products are very suitable for machining materials with high hardenss and great tenacity, such as iron-based alloys, titanium alloys and high-silicon aluminum alloys, and so on. c-BN is comprehensively applied to produce various tools or superabrasive against abrasion in the field of precision processing, stone materials processing, auto manufacture, mechanical processing, constructional materials, aviation, new materials processing, and so on. The range and field of application for c-BN is restricted due to the poor processing property of c-BN superhard material. In this paper, aimed at the difficult joining between c-BN and metal substrate, poor joining strength, working at high temperature and other issues, a new type of multi-component Cu-based active filler metal adding Ni, Sn and Ti elements is developed and the brazing mechanism of c-BN brazed with new Cu-based active filler metal is analyzed. The quadratic regression mixture experiment design method is adopted to optimize the composition of Cu-Ni-Sn-Ti active filler metal. The microstructure of the interface between c-BN and CuNi_5Sn_(5.1)Ti_(11.1) active filler metal is researched by means of SEM, EDS and XRD, which reveal the interfacial formation mechanism. The distribution of interfacial residual stress is studied.
According to the theoretical calculation of bond parameters and the experimental results, Ti elements are chosen as active elements of the Cu-based active filler metal for brazing c-BN. By the screen analysis of In, Sn, Al, Ag, Pb, Bi and Ga and other elements and the research on effects of In and Sn elements on the microstructures and properties of multi-component Cu-based active filler metal and the weldability of brazing c-BN, Sn elements are identified as alloy elements of the multi-component Cu-based active filler metal for brazing c-BN. Experimental results show that elements of new Cu-based active filler metal are Cu, Ni, Sn and Ti. Ti contents have effect on microstructures and properties of the Cu-Ni-Sn-Ti active filler metal and brazing c-BN. As Ti contents increase, the wettability of Cu-Ni-Sn-Ti active filler metal on c-BN is improved and the interaction between the filler metal and c-BN is intensified. The brittle compounds resulting from the interaction have an increase, which reduce the interfacial strength between the filler metal and c-BN. Therefore, the Ti contents in the filler metal need to optimize the design.
By the method of extreme vertices design constrained by both upper and lower bounds, the composition of Cu-Ni-Sn-Ti active filler metal is optimized and the regression model of second order polynomial is established. The optimal composition of the Cu-Ni-Sn-Ti active filler metal is Ti:11.1wt.%, Sn:5.1wt.%, Ni:5wt.%, and margin is Cu. The melting temperature range of CuNi_5Sn_(5.1)Ti_(11.1) active filler metal is 834.6-1000℃measured by differential thermal analyzer. The wetting angle of c-BN polycrystalline wet powder CuNi_5Sn_(5.1)Ti_(11.1) active filler metal is 28-30°and the CuNi_5Sn_(5.1)Ti_(11.1) active filler metal exhibits a good wettability on c-BN grains. During the process of brazing, Ti elements in the active filler metals interact with c-BN grains to achieve chemical metallurgical joining at the interface.
The microstructures and mechanical properties of CuNi_5Sn_(5.1)Ti_(11.1) active filler metal/ c-BN interface have been studied through changing processing parameters. The results show that, with the increase of the brazing temperature and the extension of the holding time, the interaction between Ti elements and c-BN enhances and new generating phases at interface increase, which have an important effect on the joining strength of CuNi_5Sn_(5.1)Ti_(11.1) filler metal/c-BN interface. When vacuum degree is above 9.0×10-3Pa, brazing temperature is T=1100℃and holding time is t=10min, the interfacial joining strength is higher.
The formation mechanism of the interface between CuNi_5Sn_(5.1)Ti_(11.1) active filler metal and c-BN is discovered after the thermodynamics and kinetics analysis. During the brazing process, the chemical reaction occurs between active element Ti and c-BN. The compounds with certain metal and ceramic characteristics of Ti-N and Ti-B are pruduced, which play good transitional roles in the chemical and physical performance between CuNi_5Sn_(5.1)Ti_(11.1) active filler metal and c-BN. The filler metal/c-BN interface realizes the chemical metallurgical combination. The structure of filler metal /TiN/TiB/TiB2/c-BN is formed at interface, helping to improve the interfacial joining strength.
Residual stress and its distribution on CuNi_5Sn_(5.1)Ti_(11.1) filler metal/c-BN interface are studied with finite element analysis method. The results show that the larger residual stress value appears at the highest contact point between filler metal and c-BN. The embedding depth of c-BN will affect the value and distribution of interfacial residual stress. In c-BN embedded in 35%-75% range, the interfacial residual stress increases with the increase of the embedding depth. In order to reduce the residual stresses generated brazing c-BN, ensure the c-BN strength requirements, the embedding depth of c-BN in the filler metal is feasible to be controlled at 30%-40% of the whole c-BN grain.
引文
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