激光熔覆INCONEL 718合金涂层的成分偏聚与强化机理研究
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摘要
激光熔覆技术以其高的能量密度和加工精度、宽泛的材料选择及良好的冶金结合界面等特点成为再制造工程的关键技术之一。再制造工程是以延长具有高附加价值零件使用寿命为出发点，同时以提升废旧零件表面性能为目的，契合构建循环经济的国家战略需求。激光熔覆层晶粒生长取向良好，优于铸锻合金力学性能，在发动机和发电机涡轮叶片等零件的修复再制造等方面具有广阔应用前景。
本文面向再制造工程，以激光熔覆镍基高温合金涂层为研究对象，主要研究内容有：激光熔覆涂层的制备及组织分析，冷却速度对熔覆层组织形态和成分偏聚的影响规律；多层堆积过程中的组织定向生长行为及多层堆积熔覆层中裂纹形态及裂纹敏感性因素分析；热处理对熔覆层组织、成分偏聚和力学性能的影响，揭示成分偏聚行为与熔覆层强韧化机制的关系。主要的研究结果有：
采用优化工艺参数可制备成形良好、稀释率低、无缺陷且与基体冶金结合良好的激光熔覆INCONEL718合金涂层。在熔覆过程中，最大温度梯度方向从熔覆层底部的垂直于基材表面转变为熔覆层顶部的趋近平行于激光行走方向。熔覆层横截面从底部到顶部依次形成平面晶、胞状晶、树枝晶和等轴晶形态组织。熔覆涂层的析出相Laves相内偏聚大量Nb和Mo，碳化物和氮化物中偏聚大量Nb和Ti。
通过提高冷却速度，可减小熔池中成分过冷Cs和增大温度梯度Gm，使熔覆层中树枝晶间Laves相细化且含量减少，可抑制Nb偏聚程度并提高熔覆层中Nb的固溶强化作用。液氮强制冷却涂层中Laves相含量约为3.5vol.%，Laves相中Nb含量约为8.5~14mass.%，均显著低于空冷涂层，而奥氏体中Nb含量约为3.5~7.5mass.%，明显高于空冷涂层，显著改善了熔覆层中Nb的偏聚程度。
激光重熔涂层中有尺寸约0.2~0.9μm的颗粒状Nb(Al, Ti)复合相在Laves相处于999℃析出。颗粒相析出是由于过饱和的Laves相在凝固冷却过程中连续自发地分解后粗化长大形成，Laves相中的Al和Ti上坡扩散到颗粒相中，使Al和Ti偏聚于颗粒相中。熔覆层中颗粒状碳化物(Nb0.12Ti0.88)C1.5和四方状氮化物(Nb0.88Ti0.12)N1.5的形成是由于极大过冷度和温度梯度使过饱和合金元素在碳化物/氮化物和Laves相中相互扩散和再分布，使富集Ti和Nb的碳化物和氮化物在Laves相处析出。碳化物和氮化物的平均硬度和弹性模量均远高于奥氏体，因切割机制引起的第二相强化作用为134.34MPa。
通过EBSD分析发现堆积熔覆层底部横截面树枝晶组织具有沿堆积方向较强的织构取向，堆积过程中树枝晶粗化且枝晶间距增大；在底部水平截面，晶粒受循环热作用形成了较弱织构特征的组织，大部分晶粒的生长方向受最大温度梯度影响而趋近于<100>方向。熔覆层横截面中间区域组织主要为受最大温度梯度方向控制，且沿堆积方向定向生长的柱状晶，熔覆层晶粒沿<001>方向形成晶界取向差约2°的强织构组织。熔覆层组织在顶部横截面沿<001>方向生长且具有小角度晶界取向和大晶粒尺寸特征；在熔覆层顶部水平截面，晶粒受最大温度梯度影响形成强织构组织。
堆积熔覆层中的裂纹为结晶裂纹和液化裂纹。横向拉应力可使尖端处存在应力集中的熔覆缺陷和小液化裂纹，在粗大Laves相和碳化物共晶处，沿堆积方向和激光熔覆方向扩展，液态金属来不及填充开裂的枝晶间隙，裂纹末端在熔覆层顶部和熔覆结束点愈合，而形成液化裂纹。熔覆层中低熔点粗大连续Laves相或碳化物共晶均可为液化裂纹提供扩展通道；熔覆层中随堆积层数增加而增大的横向残余应力可诱发小裂纹扩展而增加裂纹敏感性。
熔覆层中只有少部分Nb以γ″-Ni3Nb析出，由于冷却速度不够快，熔覆层中起固溶强化作用的大部分Nb严重偏聚而形成大量Laves相。高温固溶可使Laves相中的Nb重溶到奥氏体γ中，在时效过程中以尺寸为15~25nm的γ″-Ni3Nb在晶内弥散析出，其与γ之间存在高错配度，提高熔覆层的力学性能。热处理前后熔覆层中Laves相含量及Laves相中Nb含量沿堆积方向增加，熔覆的循环热和热处理作用使部分Laves相分解，Laves相与γ间的浓度梯度、熔覆晶格缺陷和残余应力均可在高温条件下促进元素扩散和Laves相的溶解。
标准热处理熔覆层的室温拉伸强度达1334MPa，高于熔覆态涂层的918MPa，亦高于锻造和铸造合金；熔覆层断裂方式为穿晶断裂。标准热处理熔覆层的650℃高温拉伸性能高于980STA态熔覆层和直接时效态熔覆层。织构组织的形成引起熔覆层力学性能各向异性。标准热处理态堆积熔覆层沿堆积方向在650℃拉伸强度为938MPa，与锻造合金高温拉伸性能相当，高于激光行走方向的903MPa和搭接方向的780MPa。熔覆层在激光行走方向和搭接方向高温拉伸时均为韧性断裂和脆性断裂相结合，沿堆积方向的断口完全由韧窝组成，断裂方式为韧性断裂。
Laser cladding technology is one of pivotal technologies for remanufacturing engineering dueto the superior technical characteristics such as high energy density, high processing accuracy,wide materials selection and excellent metallurgical bonding between coating and substrate.Remanufacturing engineering takes the prolonging service life of component with added value asinstruction, and takes the improvement surface properties of the waster components as the goal,which meet the demand of national strategic development for constructing cyclic economy. Thelaser cladding technology has wide application in remanufacturing field of turbine blade for powergeneration because the laser cladded coating has the advantage of favorable grain growthorientation and superior mechanical properties than wrought and as-cast alloys.
In the paper, the remanufacturing engineering is taken as the research background, and thelaser cladded Ni-based superalloy coating is taken as the research object. The laser claddedNi-based superalloy was fabricated using high power diode laser cladding system. The researchcontent mainly includes the optimize process parameters for laser cladding and the microstructureof the coating, effect of cooling rate on the microstructure and segregation, the oriented growthbehavior and the crack morphology and crack sensitivity factors, effect of heat treatment on themicrostructure, segregation and mechanical properties. The studies provide scientific andtheoretical bases for the remanufacturing engineering of laser cladding on Ni-based superalloy.Some of main experimental results and conclusions are listed as follows.
The microstructure of the epitaxial deposited coating was studied. The cladded coating withgood shape, low dilution rate, without defect and good metallurgical bonding with the substratewas fabricated with optimized process parameters. The direction of maximum temperaturegradient in the cross section of the coating varied from perpendicular to substrate surface in thedown region of the coating to paralleling to the direction of laser beam. The planar crystal, cellularcrystal, columnar dendrite and equiaxied crystal were formed from down region and up region ofthe coating. The precipitation phases in the cladded coating were dendritic (Nb, Mo)-rich Lavesphase and a small amount (Nb, Ti)-rich carbide and nitride.
The effect of cooling rate on the microstructure and segregation in the cladded coating wasinvestigated. The constitutional supercooling Csand the temperature gradient Gmwere improvedby increasing cooling speed, and then the Laves was refined, and the concentration of dendriticLaves a was decreased, indicating that Nb segregation in the coating was restrained, and more Nbatom played the solution strengthening on the matrix. The Laves concentration in the liquid nitridecooled coating was reduced to3.5vol.%, and Nb concentration in Laves was reduced to8.5~14mass.%, which were both lower than the air-cooled coating. The Nb concentration in the austenitewas increased to3.5~7.5mass.%that was higher than the air cooled coating. The Nb segregationwas alleviated by the rapid cooling rate provided by liquid nitride.
The granule complex phase Nb(Al, Ti) with0.2~0.9μm was precipitated at about999℃during the laser remelted coating. Al and Ti atoms were redistributed between Laves and thegranule complex phase via the uphill diffusion, and the intermetallic was precipitated from thesupersaturated Laves phase when the temperature was decreased to the spontaneous decompositiontemperature. Carbide (Nb0.12Ti0.88)C1.5and nitride (Nb0.88Ti0.12)N1.5were formed due to alloyingelements interdiffuse and redistribute between MC/MN and supersaturated Laves under the largerthe degree of supercooling and temperature gradient. The carbide and nitride were segregated withNb and Ti and were precipitated along the Laves. The average hardness and the average elasticitymodulus of (Nb0.12Ti0.88)C1.5and (Nb0.88Ti0.12)N1.5were much higher than the austenite, and thestrengthening effects of second-phase particles carbide and nitride are134.34MPa.
The grain growth behavior of the epitaxial deposited coating was studied. EBSD analysisresults showed that strong texture with various growth directions was formed in the down regionof the cross section of the coating. Most grains was formed as texture with grain misorientationangle about2°and growth direction towards to <100> in the horizontal cross-section, while thegrain was coarsened due to the thermal cycle. In the middle region of the deposition coating, thedirectional dendrite was formed as the strong texture along <001> with misorientation angle about2°under the controlling of direction of maximum temperature gradient. In the top region of thecoating, the texture in the cross section was formed with large grain size, and strong texture in thehorizontal cross section with small misorientation angle about2°.
The tips of small solidification crack with stress concentration was activated by the transversetensile stress, and the crack was propagated with the coarsening Laves and carbide along thedirection of deposition and laser beam. The liquation crack was form before the liquid alloy fillingthe dendrite clearance, and was healed at the topmost the deposition coating and the ending of thelaser beam. The propagation path of the crack was provided by the coarsening Laves and carbide eutectic with the effect of transverse residual stress that was increased with increasing the numberof deposition layers.
The effect of heat treatment on the microstructure and composition segregation in the coatingwas studied, and the mechanical properties of the coating were test. Only a small portion of Nb inIN718alloy coating was precipitated as the constituent of the strengthening phase. The rest of Nbplayed the role of solution strengthening and segregated in the form of Laves in the laser-claddingprocess due to the slow cooling rate. Laves phase in the coating was dissolved during the elevatedtemperature solid solution, and the Nb was redissoluted in the austenite and precipitateddispersedly as strengthening phase γ″-Ni3Nb with dimension of15~25nm during the double agingtreatment. The mechanical properties of the coating were improved by γ″-Ni3Nb due to the largemismatch between γ″-Ni3Nb and austenite γ. Laves concentration in the coating and Nbconcentration in Laves increase along the deposited direction. Laves concentration and Nbconcentration in Laves were increased along the deposition direction. Part of Laves was dissolvedby the thermal cycle during the successive laser deposition, concentration gradient between Lavesand austenite, lattice imperfection of the coating and residual stress.
The tensile strength of the standard heat treated coating at ambient temperature was1334MPa that was higher than the as-deposited coating918MPa as well as the wrought alloy and castalloy. The coating was destroyed as transgranular fracture. The tensile strength of the standard heattreated coating at650℃was higher than that of980STA coating and DA coating. Theanisotropic tensile property of the coating was generated by the texture formed during the epitaxialdeposition. The tensile strength of the standard heat treated coating along the deposition directionat650℃was938MPa that was about the same to the wrought alloy and was higher than903MPa along the direction of laser scanning and780MPa along the direction of overlapping. Thefracture mode of the coating along the direction of laser scanning and the direction of overlappingwere mixed-mode of ductile fracture and brittle fracture, and was changed to ductile fracture alongthe deposition direction.
本文面向再制造工程，以激光熔覆镍基高温合金涂层为研究对象，主要研究内容有：激光熔覆涂层的制备及组织分析，冷却速度对熔覆层组织形态和成分偏聚的影响规律；多层堆积过程中的组织定向生长行为及多层堆积熔覆层中裂纹形态及裂纹敏感性因素分析；热处理对熔覆层组织、成分偏聚和力学性能的影响，揭示成分偏聚行为与熔覆层强韧化机制的关系。主要的研究结果有：
采用优化工艺参数可制备成形良好、稀释率低、无缺陷且与基体冶金结合良好的激光熔覆INCONEL718合金涂层。在熔覆过程中，最大温度梯度方向从熔覆层底部的垂直于基材表面转变为熔覆层顶部的趋近平行于激光行走方向。熔覆层横截面从底部到顶部依次形成平面晶、胞状晶、树枝晶和等轴晶形态组织。熔覆涂层的析出相Laves相内偏聚大量Nb和Mo，碳化物和氮化物中偏聚大量Nb和Ti。
通过提高冷却速度，可减小熔池中成分过冷Cs和增大温度梯度Gm，使熔覆层中树枝晶间Laves相细化且含量减少，可抑制Nb偏聚程度并提高熔覆层中Nb的固溶强化作用。液氮强制冷却涂层中Laves相含量约为3.5vol.%，Laves相中Nb含量约为8.5~14mass.%，均显著低于空冷涂层，而奥氏体中Nb含量约为3.5~7.5mass.%，明显高于空冷涂层，显著改善了熔覆层中Nb的偏聚程度。
激光重熔涂层中有尺寸约0.2~0.9μm的颗粒状Nb(Al, Ti)复合相在Laves相处于999℃析出。颗粒相析出是由于过饱和的Laves相在凝固冷却过程中连续自发地分解后粗化长大形成，Laves相中的Al和Ti上坡扩散到颗粒相中，使Al和Ti偏聚于颗粒相中。熔覆层中颗粒状碳化物(Nb0.12Ti0.88)C1.5和四方状氮化物(Nb0.88Ti0.12)N1.5的形成是由于极大过冷度和温度梯度使过饱和合金元素在碳化物/氮化物和Laves相中相互扩散和再分布，使富集Ti和Nb的碳化物和氮化物在Laves相处析出。碳化物和氮化物的平均硬度和弹性模量均远高于奥氏体，因切割机制引起的第二相强化作用为134.34MPa。
通过EBSD分析发现堆积熔覆层底部横截面树枝晶组织具有沿堆积方向较强的织构取向，堆积过程中树枝晶粗化且枝晶间距增大；在底部水平截面，晶粒受循环热作用形成了较弱织构特征的组织，大部分晶粒的生长方向受最大温度梯度影响而趋近于<100>方向。熔覆层横截面中间区域组织主要为受最大温度梯度方向控制，且沿堆积方向定向生长的柱状晶，熔覆层晶粒沿<001>方向形成晶界取向差约2°的强织构组织。熔覆层组织在顶部横截面沿<001>方向生长且具有小角度晶界取向和大晶粒尺寸特征；在熔覆层顶部水平截面，晶粒受最大温度梯度影响形成强织构组织。
堆积熔覆层中的裂纹为结晶裂纹和液化裂纹。横向拉应力可使尖端处存在应力集中的熔覆缺陷和小液化裂纹，在粗大Laves相和碳化物共晶处，沿堆积方向和激光熔覆方向扩展，液态金属来不及填充开裂的枝晶间隙，裂纹末端在熔覆层顶部和熔覆结束点愈合，而形成液化裂纹。熔覆层中低熔点粗大连续Laves相或碳化物共晶均可为液化裂纹提供扩展通道；熔覆层中随堆积层数增加而增大的横向残余应力可诱发小裂纹扩展而增加裂纹敏感性。
熔覆层中只有少部分Nb以γ″-Ni3Nb析出，由于冷却速度不够快，熔覆层中起固溶强化作用的大部分Nb严重偏聚而形成大量Laves相。高温固溶可使Laves相中的Nb重溶到奥氏体γ中，在时效过程中以尺寸为15~25nm的γ″-Ni3Nb在晶内弥散析出，其与γ之间存在高错配度，提高熔覆层的力学性能。热处理前后熔覆层中Laves相含量及Laves相中Nb含量沿堆积方向增加，熔覆的循环热和热处理作用使部分Laves相分解，Laves相与γ间的浓度梯度、熔覆晶格缺陷和残余应力均可在高温条件下促进元素扩散和Laves相的溶解。
标准热处理熔覆层的室温拉伸强度达1334MPa，高于熔覆态涂层的918MPa，亦高于锻造和铸造合金；熔覆层断裂方式为穿晶断裂。标准热处理熔覆层的650℃高温拉伸性能高于980STA态熔覆层和直接时效态熔覆层。织构组织的形成引起熔覆层力学性能各向异性。标准热处理态堆积熔覆层沿堆积方向在650℃拉伸强度为938MPa，与锻造合金高温拉伸性能相当，高于激光行走方向的903MPa和搭接方向的780MPa。熔覆层在激光行走方向和搭接方向高温拉伸时均为韧性断裂和脆性断裂相结合，沿堆积方向的断口完全由韧窝组成，断裂方式为韧性断裂。
Laser cladding technology is one of pivotal technologies for remanufacturing engineering dueto the superior technical characteristics such as high energy density, high processing accuracy,wide materials selection and excellent metallurgical bonding between coating and substrate.Remanufacturing engineering takes the prolonging service life of component with added value asinstruction, and takes the improvement surface properties of the waster components as the goal,which meet the demand of national strategic development for constructing cyclic economy. Thelaser cladding technology has wide application in remanufacturing field of turbine blade for powergeneration because the laser cladded coating has the advantage of favorable grain growthorientation and superior mechanical properties than wrought and as-cast alloys.
In the paper, the remanufacturing engineering is taken as the research background, and thelaser cladded Ni-based superalloy coating is taken as the research object. The laser claddedNi-based superalloy was fabricated using high power diode laser cladding system. The researchcontent mainly includes the optimize process parameters for laser cladding and the microstructureof the coating, effect of cooling rate on the microstructure and segregation, the oriented growthbehavior and the crack morphology and crack sensitivity factors, effect of heat treatment on themicrostructure, segregation and mechanical properties. The studies provide scientific andtheoretical bases for the remanufacturing engineering of laser cladding on Ni-based superalloy.Some of main experimental results and conclusions are listed as follows.
The microstructure of the epitaxial deposited coating was studied. The cladded coating withgood shape, low dilution rate, without defect and good metallurgical bonding with the substratewas fabricated with optimized process parameters. The direction of maximum temperaturegradient in the cross section of the coating varied from perpendicular to substrate surface in thedown region of the coating to paralleling to the direction of laser beam. The planar crystal, cellularcrystal, columnar dendrite and equiaxied crystal were formed from down region and up region ofthe coating. The precipitation phases in the cladded coating were dendritic (Nb, Mo)-rich Lavesphase and a small amount (Nb, Ti)-rich carbide and nitride.
The effect of cooling rate on the microstructure and segregation in the cladded coating wasinvestigated. The constitutional supercooling Csand the temperature gradient Gmwere improvedby increasing cooling speed, and then the Laves was refined, and the concentration of dendriticLaves a was decreased, indicating that Nb segregation in the coating was restrained, and more Nbatom played the solution strengthening on the matrix. The Laves concentration in the liquid nitridecooled coating was reduced to3.5vol.%, and Nb concentration in Laves was reduced to8.5~14mass.%, which were both lower than the air-cooled coating. The Nb concentration in the austenitewas increased to3.5~7.5mass.%that was higher than the air cooled coating. The Nb segregationwas alleviated by the rapid cooling rate provided by liquid nitride.
The granule complex phase Nb(Al, Ti) with0.2~0.9μm was precipitated at about999℃during the laser remelted coating. Al and Ti atoms were redistributed between Laves and thegranule complex phase via the uphill diffusion, and the intermetallic was precipitated from thesupersaturated Laves phase when the temperature was decreased to the spontaneous decompositiontemperature. Carbide (Nb0.12Ti0.88)C1.5and nitride (Nb0.88Ti0.12)N1.5were formed due to alloyingelements interdiffuse and redistribute between MC/MN and supersaturated Laves under the largerthe degree of supercooling and temperature gradient. The carbide and nitride were segregated withNb and Ti and were precipitated along the Laves. The average hardness and the average elasticitymodulus of (Nb0.12Ti0.88)C1.5and (Nb0.88Ti0.12)N1.5were much higher than the austenite, and thestrengthening effects of second-phase particles carbide and nitride are134.34MPa.
The grain growth behavior of the epitaxial deposited coating was studied. EBSD analysisresults showed that strong texture with various growth directions was formed in the down regionof the cross section of the coating. Most grains was formed as texture with grain misorientationangle about2°and growth direction towards to <100> in the horizontal cross-section, while thegrain was coarsened due to the thermal cycle. In the middle region of the deposition coating, thedirectional dendrite was formed as the strong texture along <001> with misorientation angle about2°under the controlling of direction of maximum temperature gradient. In the top region of thecoating, the texture in the cross section was formed with large grain size, and strong texture in thehorizontal cross section with small misorientation angle about2°.
The tips of small solidification crack with stress concentration was activated by the transversetensile stress, and the crack was propagated with the coarsening Laves and carbide along thedirection of deposition and laser beam. The liquation crack was form before the liquid alloy fillingthe dendrite clearance, and was healed at the topmost the deposition coating and the ending of thelaser beam. The propagation path of the crack was provided by the coarsening Laves and carbide eutectic with the effect of transverse residual stress that was increased with increasing the numberof deposition layers.
The effect of heat treatment on the microstructure and composition segregation in the coatingwas studied, and the mechanical properties of the coating were test. Only a small portion of Nb inIN718alloy coating was precipitated as the constituent of the strengthening phase. The rest of Nbplayed the role of solution strengthening and segregated in the form of Laves in the laser-claddingprocess due to the slow cooling rate. Laves phase in the coating was dissolved during the elevatedtemperature solid solution, and the Nb was redissoluted in the austenite and precipitateddispersedly as strengthening phase γ″-Ni3Nb with dimension of15~25nm during the double agingtreatment. The mechanical properties of the coating were improved by γ″-Ni3Nb due to the largemismatch between γ″-Ni3Nb and austenite γ. Laves concentration in the coating and Nbconcentration in Laves increase along the deposited direction. Laves concentration and Nbconcentration in Laves were increased along the deposition direction. Part of Laves was dissolvedby the thermal cycle during the successive laser deposition, concentration gradient between Lavesand austenite, lattice imperfection of the coating and residual stress.
The tensile strength of the standard heat treated coating at ambient temperature was1334MPa that was higher than the as-deposited coating918MPa as well as the wrought alloy and castalloy. The coating was destroyed as transgranular fracture. The tensile strength of the standard heattreated coating at650℃was higher than that of980STA coating and DA coating. Theanisotropic tensile property of the coating was generated by the texture formed during the epitaxialdeposition. The tensile strength of the standard heat treated coating along the deposition directionat650℃was938MPa that was about the same to the wrought alloy and was higher than903MPa along the direction of laser scanning and780MPa along the direction of overlapping. Thefracture mode of the coating along the direction of laser scanning and the direction of overlappingwere mixed-mode of ductile fracture and brittle fracture, and was changed to ductile fracture alongthe deposition direction.
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