氢在TC4钛合金扩散连接中的作用机理研究
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摘要
钛合金置氢加工工艺是将氢作为一种临时合金元素,通过改变钛合金的相组成和微观结构,进而达到改善钛合金加工性能的目的。自从该技术被提出以来,国内外学者主要对置氢与除氢基础理论,氢改善塑性加工性能及热氢处理细化晶粒等方面进行了大量的研究,然而对氢改善扩散连接性方面的研究较少。本文针对置氢TC4钛合金,分别开展了直接和间接扩散连接试验,研究了置氢合金母材相组成和微观组织演化演化规律,确定了扩散连接接头的界面结构以及连接工艺参数对界面结构的影响规律,并对TiH_2粉末和高氢含量置氢合金的脱氢分解动力学进行了系统分析,在此基础上探讨了氢致低温扩散连接机理。
研究了置氢TC4钛合金的相组成以及微观组织演化规律。板状原始合金由一定轧制方向的(α+β)组成,随着氢含量的增加β_H相和氢化物δ相依次出现,微观组织中轧制方向逐渐消失,当氢含量增加到0.4wt.%以上时α′马氏体大量形成。棒状原始合金由等轴状(α+β)组成,置氢0.15wt.%时,初生α相在原始β晶界面处形核并长大,随后β相中聚集的氢导致了片层状(β_H+α)的形成,而置氢0.3wt.%时,较高的氢含量导致了共析产物(α+δ)和α′马氏体的形成。
直接扩散连接了置氢TC4钛合金,分析了其界面结构以及工艺参数对界面结构的影响。接头界面处只有扩散孔隙的存在,且随着连接温度、连接时间、连接压力、合金中氢含量以及加热速率的升高,界面处的扩散孔隙数量逐渐减少且尺寸逐渐变小;高含氢量的置氢合金在快速升温下扩散连接温度降低了大约150℃左右。在缓慢加热条件下,合金中含氢不稳定相逐渐发生分解,在氢的作用下合金元素发生了充分的扩散。在快速加热条件下,含氢不稳定相几乎同时发生分解,合金元素扩散不充分且在快速的冷却速度下导致大量α′马氏体形成。
采用Ni、Al、Nb和Ti中间层间接扩散连接了置氢TC4钛合金,分析了各类扩散偶中接头的界面结构。采用Ni中间层时接头界面处分别生成了β相变区、Ti2Ni、TiNi和TiNi3,采用Al中间层时界面处只生成TiAl3,采用Nb中间层时界面处只生成固溶体层。在相同的连接工艺参数下随着氢含量的增加,接头界面处扩散层的厚度逐渐增加。采用Ti中间层时,接头界面只由扩散孔隙组成,且在相同连接工艺参数下随着氢含量的增加,扩散孔隙数量及尺寸逐渐减小。
置氢TC4钛合金在600℃～950℃之间脱氢,而高氢含量置氢合金中氢主要以δ氢化物的形式存在。详细研究了TiH_2粉末的脱氢分解动力学,其分解过程包括以下几个步骤: TiH_2→TiH_(1.5)+H_2↑;δ→β_H+H_2↑;β_H→β_H+H_2↑和β_H→α_H ;β_H→α_H+H_2↑。在此基础上确定了置氢0.5wt.%合金的脱氢分解动力学,具体脱氢分解过程如下:TiH_(1.5～2)→TiH_(1.5)+H_2↑;δ→β_H+H_2↑;β_H→β_H+H_2↑和β_H→α_H+H_2↑。借助动力学模型探讨了置氢TC4钛合金低温扩散连接机理,氢的加入导致了在孔隙闭合过程中扩散系数的增大,也导致了变形和蠕变的改善,因而其扩散连接性得到了改善。且较快速度下升温能保证在扩散连接前,氢几乎不逸出,从而保证了活性氢含量,这有利于进一步增强扩散连接性。而在有反应层生成的间接扩散连接过程中,氢的加入导致了互扩散系数的升高。
The so-called thermohydrogen processing (THP) is a technique in which hydrogen is used as a temporary alloying element in titanium alloys by controlling the microstructure and phase structure to improve the mechanical working properties. Since the appearance of THP, it has gained considerable interests. A large number of researches have been done including the basic theory of hydrogenation and dehydrogenation, the enhancement of plastic working properties and different THP methods used to modify the microstructure. However, little work has been reported about diffusion bonding of hydrogenated titanium alloys. The investigation about diffusion bonding with or without interlayer of hydrogenated TC4 titanium alloys was carried out. The phase structure and microstructure evolution of the substrates were researched, the interface structure of diffusion bonding with or without interlayer was determined, the effect of processing parameter on interface structure was analyzed, the nonisothermal dehydrogenation kinetics of the TiH_2 powders and the TC4 alloy with high hydrogen content was established, and the positive effect of hydrogen on diffusion bonding was investigated.
The phase structure and microstructure evolution of the substrates were researched. The platelike substrate before hydrogenation had a (α+β) dual phase structure with rolling direction. With the increase of the hydrogen theβ_H andδphases gradually formed, and the rolling direction gradually disappeared with the hydrogen content increasing. The needleα′martensite appeared when the hydrogen content was up to 0.4wt.%. The rodlike substrate before hydrogenation had an equiaxed (α+β) dual phase structure. When the hydrogen content was 0.15wt.%, the primaryαphase started to nucleate and grow up in the boundary ofβphase and the hydrogen inβphase led to the formation of lamellar (β_H+α). The high hydrogen content resulted in the formation of (α+δ) andα′phase when the hydrogen content was 0.3wt.%.
The diffusion bonding without interlayer was carried out, and the interface structure and the effect of processing parameter were analyzed. The voids were only observed in the interface, and the quantity of the voids gradually decreased with the increase of bonding temperature, holding time, bonding pressure and heating rate. Moreover, the bonding temperature decreased by 150℃under high hydrogen content at the fast heating rate. The phases with hydrogen sequential decomposed at low heating rate, and the elements in alloy sufficiently diffused. However, the phases with hydrogen decomposed at the same time at fast heating rate, and the elements in alloy insufficiently diffused and the fast cooling rate led to the formation ofα′phase.
The diffusion bonding with different interlayers was carried out, and the interface structure was analyzed. The reaction layers in the interface structure with Ni interlayer was theβ(Ni) phase and the Ti2Ni/TiNi/TiNi3 intermetallics, the reaction layers in the interface structure with Al interlayer was the TiAl3 intermetallics, and the diffusion layer in the interface structure with Nb interlayer was the solid solution.
The thickness of layers gradually increased with the hydrogen content increasing when bonded at the same processing parameter. But the interface structure with Ti interlayer was only composed of the voids, and the quantity of the voids gradually decreased with the increase of hydrogen content at the same processing parameter. The nonisothermal dehydrogenation of hydrogenated TC4 alloys happened between 600℃and 950℃, and the hydrogen in the TC4 alloy with high hydrogen content mainly located inδtitanium hydride. The nonisothermal dehydrogenation kinetics of the TiH_2 powders was established. The results show the nonisothermal dehydrogenation occurred in a four-step process: TiH_2→TiH_(1.5)+H_2↑;δ→β_H+H_2↑;β_H→β_H+H_2↑andβ_H→α_H,β_H→α_H+H_2↑. Also the dehydrogenation kinetics of the TC4 alloy with 0.5wt.% hydrogen was established. It consisted of TiH_(1.5～2)→TiH_(1.5)+H_2↑,δ→β_H+H_2↑,β_H→β_H+H_2↑andβ_H→α_H+H_2↑. Moreover, the positive effect of hydrogen on diffusion bonding was investigated. The enhancement of diffusion bonding quality was attributed to the increase of diffusion coefficient and the improvement of creep deformation and distortion. The fast heating prevented the most hydrogen escaping during rise in temperature, which helped to improve the diffusion bonding quality. In addition, the hydrogen in titanium alloys arouses the interdiffusion enhancenment for the diffusion bonding joints with reaction layer.
研究了置氢TC4钛合金的相组成以及微观组织演化规律。板状原始合金由一定轧制方向的(α+β)组成,随着氢含量的增加β_H相和氢化物δ相依次出现,微观组织中轧制方向逐渐消失,当氢含量增加到0.4wt.%以上时α′马氏体大量形成。棒状原始合金由等轴状(α+β)组成,置氢0.15wt.%时,初生α相在原始β晶界面处形核并长大,随后β相中聚集的氢导致了片层状(β_H+α)的形成,而置氢0.3wt.%时,较高的氢含量导致了共析产物(α+δ)和α′马氏体的形成。
直接扩散连接了置氢TC4钛合金,分析了其界面结构以及工艺参数对界面结构的影响。接头界面处只有扩散孔隙的存在,且随着连接温度、连接时间、连接压力、合金中氢含量以及加热速率的升高,界面处的扩散孔隙数量逐渐减少且尺寸逐渐变小;高含氢量的置氢合金在快速升温下扩散连接温度降低了大约150℃左右。在缓慢加热条件下,合金中含氢不稳定相逐渐发生分解,在氢的作用下合金元素发生了充分的扩散。在快速加热条件下,含氢不稳定相几乎同时发生分解,合金元素扩散不充分且在快速的冷却速度下导致大量α′马氏体形成。
采用Ni、Al、Nb和Ti中间层间接扩散连接了置氢TC4钛合金,分析了各类扩散偶中接头的界面结构。采用Ni中间层时接头界面处分别生成了β相变区、Ti2Ni、TiNi和TiNi3,采用Al中间层时界面处只生成TiAl3,采用Nb中间层时界面处只生成固溶体层。在相同的连接工艺参数下随着氢含量的增加,接头界面处扩散层的厚度逐渐增加。采用Ti中间层时,接头界面只由扩散孔隙组成,且在相同连接工艺参数下随着氢含量的增加,扩散孔隙数量及尺寸逐渐减小。
置氢TC4钛合金在600℃～950℃之间脱氢,而高氢含量置氢合金中氢主要以δ氢化物的形式存在。详细研究了TiH_2粉末的脱氢分解动力学,其分解过程包括以下几个步骤: TiH_2→TiH_(1.5)+H_2↑;δ→β_H+H_2↑;β_H→β_H+H_2↑和β_H→α_H ;β_H→α_H+H_2↑。在此基础上确定了置氢0.5wt.%合金的脱氢分解动力学,具体脱氢分解过程如下:TiH_(1.5～2)→TiH_(1.5)+H_2↑;δ→β_H+H_2↑;β_H→β_H+H_2↑和β_H→α_H+H_2↑。借助动力学模型探讨了置氢TC4钛合金低温扩散连接机理,氢的加入导致了在孔隙闭合过程中扩散系数的增大,也导致了变形和蠕变的改善,因而其扩散连接性得到了改善。且较快速度下升温能保证在扩散连接前,氢几乎不逸出,从而保证了活性氢含量,这有利于进一步增强扩散连接性。而在有反应层生成的间接扩散连接过程中,氢的加入导致了互扩散系数的升高。
The so-called thermohydrogen processing (THP) is a technique in which hydrogen is used as a temporary alloying element in titanium alloys by controlling the microstructure and phase structure to improve the mechanical working properties. Since the appearance of THP, it has gained considerable interests. A large number of researches have been done including the basic theory of hydrogenation and dehydrogenation, the enhancement of plastic working properties and different THP methods used to modify the microstructure. However, little work has been reported about diffusion bonding of hydrogenated titanium alloys. The investigation about diffusion bonding with or without interlayer of hydrogenated TC4 titanium alloys was carried out. The phase structure and microstructure evolution of the substrates were researched, the interface structure of diffusion bonding with or without interlayer was determined, the effect of processing parameter on interface structure was analyzed, the nonisothermal dehydrogenation kinetics of the TiH_2 powders and the TC4 alloy with high hydrogen content was established, and the positive effect of hydrogen on diffusion bonding was investigated.
The phase structure and microstructure evolution of the substrates were researched. The platelike substrate before hydrogenation had a (α+β) dual phase structure with rolling direction. With the increase of the hydrogen theβ_H andδphases gradually formed, and the rolling direction gradually disappeared with the hydrogen content increasing. The needleα′martensite appeared when the hydrogen content was up to 0.4wt.%. The rodlike substrate before hydrogenation had an equiaxed (α+β) dual phase structure. When the hydrogen content was 0.15wt.%, the primaryαphase started to nucleate and grow up in the boundary ofβphase and the hydrogen inβphase led to the formation of lamellar (β_H+α). The high hydrogen content resulted in the formation of (α+δ) andα′phase when the hydrogen content was 0.3wt.%.
The diffusion bonding without interlayer was carried out, and the interface structure and the effect of processing parameter were analyzed. The voids were only observed in the interface, and the quantity of the voids gradually decreased with the increase of bonding temperature, holding time, bonding pressure and heating rate. Moreover, the bonding temperature decreased by 150℃under high hydrogen content at the fast heating rate. The phases with hydrogen sequential decomposed at low heating rate, and the elements in alloy sufficiently diffused. However, the phases with hydrogen decomposed at the same time at fast heating rate, and the elements in alloy insufficiently diffused and the fast cooling rate led to the formation ofα′phase.
The diffusion bonding with different interlayers was carried out, and the interface structure was analyzed. The reaction layers in the interface structure with Ni interlayer was theβ(Ni) phase and the Ti2Ni/TiNi/TiNi3 intermetallics, the reaction layers in the interface structure with Al interlayer was the TiAl3 intermetallics, and the diffusion layer in the interface structure with Nb interlayer was the solid solution.
The thickness of layers gradually increased with the hydrogen content increasing when bonded at the same processing parameter. But the interface structure with Ti interlayer was only composed of the voids, and the quantity of the voids gradually decreased with the increase of hydrogen content at the same processing parameter. The nonisothermal dehydrogenation of hydrogenated TC4 alloys happened between 600℃and 950℃, and the hydrogen in the TC4 alloy with high hydrogen content mainly located inδtitanium hydride. The nonisothermal dehydrogenation kinetics of the TiH_2 powders was established. The results show the nonisothermal dehydrogenation occurred in a four-step process: TiH_2→TiH_(1.5)+H_2↑;δ→β_H+H_2↑;β_H→β_H+H_2↑andβ_H→α_H,β_H→α_H+H_2↑. Also the dehydrogenation kinetics of the TC4 alloy with 0.5wt.% hydrogen was established. It consisted of TiH_(1.5～2)→TiH_(1.5)+H_2↑,δ→β_H+H_2↑,β_H→β_H+H_2↑andβ_H→α_H+H_2↑. Moreover, the positive effect of hydrogen on diffusion bonding was investigated. The enhancement of diffusion bonding quality was attributed to the increase of diffusion coefficient and the improvement of creep deformation and distortion. The fast heating prevented the most hydrogen escaping during rise in temperature, which helped to improve the diffusion bonding quality. In addition, the hydrogen in titanium alloys arouses the interdiffusion enhancenment for the diffusion bonding joints with reaction layer.
引文
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