镍基非晶复合涂层的半导体激光制备及表征
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摘要
激光熔覆技术是20世纪70年代随着大功率激光器的发展而兴起的一种新的表面工程技术。它是集激光加热熔化、熔池中物质交互作用及快速凝固成形等多学科交叉的一门新技术。而激光熔凝（激光重熔）处理是用较高功率密度的激光束，在金属或合金表面扫描，使表层金属熔化，随后快速冷却凝固。冷却速率通常为102～106K/s，有时甚至能达到1012K/s，从而得到细微的接近均匀的表层组织。因此利用激光熔覆获得稀释率极低的熔覆层，使得非晶合金体系的成分得到保证，再利用激光重熔产生的大凝固速度使得在传统晶体材料的表面制备非晶涂层成为可能。
本文在低碳钢表面通过半导体激光熔覆+重熔的工艺制备了镍基非晶纳米晶复合涂层，主要研究内容有：Ni-Fe-B-Si-Nb非晶合金体系的成分设计与制备，涂层的显微组织和相结构的演变规律和形成机制，以及涂层硬度分布和耐磨性能的表征。主要研究成果如下：
针对Ni-Fe-B-Si-Nb合金体系，基于判断非晶形成能力三条经验准则和共晶点准则进行了混合焓、归一化错配熵的计算和相图分析，在此基础上初步设计了合金成分范围。并结合合金元素含量对涂层非晶形成能力影响的试验研究，最终确定了适合采用激光熔覆+重熔制备非晶复合涂层的合金粉末成分为(Ni_(0.6)Fe_(0.4))_(68)B_(18)Si_(10)Nb_4（原子百分比），此时所得激光重熔涂层具有相对最大的非晶体积含量。
系统研究了激光熔覆和激光重熔参数变化对重熔涂层非晶体积含量的影响。发现激光功率密度会影响稀释率，随激光功率密度的增加，熔覆层的熔深增加，熔池搅拌作用增强，稀释率也会提高。稀释率较低时，熔覆层内的成分和名义成分接近，因此在重熔层内获得了较大体积含量的非晶组织，而当稀释率较大时，导致重熔层内非晶含量降低，甚至不能形成非晶。在保证熔覆层成分接近名义成分的基础上，随激光功率密度的增加，熔覆层的组织和成分更加均匀，在激光重熔后，重熔层的非晶体积含量也随之增加。重熔时激光扫描速度为4m/min和5m/min时，重熔层内基本无非晶相生成，速度为6m/min时重熔层内开始形成非晶，随重熔时激光扫描速度的进一步增加，重熔层非晶含量也随之升高，当激光重熔扫描速度为9m/min时，重熔层内的非晶体积含量为64%。
观察和分析了激光重熔层的组织分布，发现激光熔覆功率密度为12100W/cm~2，扫描速度为0.36m/min，激光重熔功率密度为53000W/cm~2，扫描速度大于6m/min（含）可在重熔层内获得非晶相，8m/min时，其重熔层组织主要为非晶相和NbC颗粒相，在其他参数条件下（非晶含量降低时），重熔层内还可能形成等轴晶、纳米晶相及枝晶相和非晶相的混合组织等。计算了(Ni_(0.6)Fe_(0.4))_(68)B_(18)Si_(10)Nb_4合金涂层在激光重熔时的热循环曲线，并结合热力学、动力学对激光熔覆+重熔条件下的非晶相形成特点及机制进行了探讨。结果表明，采用激光熔覆+重熔获得镍基非晶复合涂层的临界冷却速率约为10118.8K/s，高于相同成分的镍基合金在采用铜模吸铸制备大块非晶时的临界冷却速率。认为出现这一现象的主要原因是：热力学方面，在熔覆层/重熔层界面处会出现部分熔化区，以及在重熔层内部存在NbC颗粒相，都可以作为异质形核的基底，其形核自由能会降低，有利于形核，必须继续增加冷却速率才能防止晶体形核及晶粒长大行为的产生。动力学方面，由于采用激光重熔工艺，在激光重熔时会产生不可忽视的熔体流动和溶质迁移行为，加速了元素的长程扩散，因此也必须通过提高激光扫描速度（熔体冷却速率），降低熔体表面张力梯度和高温停留时间，来提高其非晶形成能力。
系统测试了(Ni_(0.6)Fe_(0.4))_(68)B_(18)Si_(10)Nb_4合金激光熔覆+重熔涂层的显微硬度分布及耐磨性能。显微硬度测试结果表明在涂层截面上由表及里显微硬度值逐渐降低，在重熔层内其显微硬度值最大，并且随重熔层内非晶含量的增加，显微硬度值不断提高。激光重熔涂层的平均硬度和弹性模量分别为1227.9HV和277.4GPa，高于相同合金体系的大块非晶合金，探讨了重熔涂层的强化机制。摩擦磨损试验结果表明随摩擦转速、载荷以及摩擦时间的增加，涂层的失重逐渐增加。摩擦系数随载荷的增加呈减小的趋势。针对(Ni_(0.6)Fe_(0.4))_(68)B_(18)Si_(10)Nb_4合金激光熔覆涂层、激光重熔涂层（非晶复合涂层）以及大块非晶，H~3/E~(*2)比值可以反映对其耐磨性影响的变化规律，随H~3/E~(*2)比值的增加，耐磨性得到提高。重熔涂层非晶含量增加时，涂层耐磨性能也得到提高。
Laser cladding technology is a novel technology developed in1970s dueto the development of high power laser equipment. It is a multidisciplinarytechnology with laser heating and melting, mass exchange in the melted pooland rapid solidification. Laser melting or laser remelting is a technique that ahigh power density laser beam scans on surface of metals or alloys, leads tothe melting of surface metals, and solidifies followed. The cooling rate isusually at102～106K/s, even to1012K/s, so fine and homogeneous structurescould be obtained at the surface. It is possible to form composite amorphouslayer in the surface crystalline materials when using laser cladding andremelting process. The laser cladding process can give low dilution claddedcoating to guarantee the composition; laser remelting process can lead to highsolidification rate.
In this paper, an amorphous composite coating was fabricated by usinghigh power diode laser cladding and remelting process on mild steel surface.Design and preparation of Ni-Fe-B-Si-Nb amorphous alloys systems wascarried out. The microstructure and phase were observed and analyzed. Themicrohardness and wear resistance properties of the coating were also tested.Some of main experimental results and conclusions are listed as follows.
For Ni-Fe-B-Si-Nb alloy systems, based on the three empirical rules anddeep eutectic rule for high glass-foming ability in metallic glasses, the mixingenthalpy and mismatch entropy were calculated, the alloys phase diagrams were analyzed. A preliminary composition of the alloy is obtained.Furthermore, considering the characteristics of laser processing andexperimental studies, the final composition of (Ni_(0.6)Fe_(0.4))_(68)B_(18)Si_(10)Nb_4(at.%)was determined. The biggest amorphous volume fraction could be obtained inthe laser cladding and remelted coating.
The influence of laser cladding and remelting processing parameters onamorphous volume fractions of the remelted coating was studiedsystematically. It can be seen that dilution ratio was affected by laser powerinput. With the increasing of laser power, the penetration and dilution willincrease. A high amorphous volume fraction could be obtained at low dilutioncoating where the nominal composition of the powder was kept. While forhigh dilution coating, the amorphous volume fraction was relatively low,even no amorphous phase was formed in the remelted coating. When thenominal composition was guaranteed, the structure and composition weremore homogeneous at higher laser power input. The amorphous volumefraction was also at higher standards in the remelted coating. The amorphousphase was not formed when the laser scanning speed is4m/min and5m/minduring the laser remelting process. For6m/min or more, the amorphous phasewas observed, and the amorphous volume fraction increased with theincreasing of laser scanning speed. The amorphous volume fraction was64%for6m/min.
Structure of amorphous phase matrix and NbC particles were observedin the remelted coating when the laser cladding power was800W, scanningspeed was0.36m/min, laser remlting power was3500W and remeltingscanning speed was8m/min. The fine equiaxed grains, nano-grains anddendrites/amorphous structures could also be obtained in the remeltedcoating for low amorphous volume fraction remelted coatings. The thermalcycle of the coating during laser remelting process was calculated using FEM method. Combined with the thermodynamics and kinetic aspects, theformation characteristics and mechanisms of amorphous phase for lasercladding and remlting process were studied. The results showed that thecritical cooling rate was10118.8K/s for (Ni_(0.6)Fe_(0.4))_(68)B_(18)Si_(10)Nb_4alloyfabricated by laser cladding and remelting process which is higher than thatof BMGs. In thermodynamics aspect, the semi-melted zone atremlted/cladded interface and NbC particles in remelted zone are both thesites of heterogeneous nucleation. The barrier energy needed forheterogeneous nucleation is reduced. So much more cooling speed is neededto suppressing crystallization within the supercooled liquid. In kinetics aspect,the liquid flow and solute transport behavior in remelted pool can not beneglected, which accelerated the element diffusion. Therefore, the Surfacetention gradient and holding time at high termperature should be decreasedby increasing the scanning speed (cooling rate) during the laser remeltingprocess.
The microhardness and wear resistance properties of the coating weretested systematically. The graded microhardness distribution was exhibited inthe coating, the microhardness increased from the interface of clad/substratesurface to the top of the remelted coating. The microhardness was higher forcoatings with bigger amorphous volume fraction. The mean microhardnessand elastic modulus are1227.9HV and277.4GPa, respectively which arehigher than that of the BMGs with same compositions. The strengtheningmechanism of this phenomenon was also studied. Wear tests results showedthat the wear losses increased with increasing of the wear rotation speed, loadand time. Friction coefficient decreased with the increase of load. The ratio ofH3/E*2can represent the changing rule of wear resistance properties of thecladded coating, remelted coating and BMGs. Wear resistance propertiesincreases with the increasing of H3/E*2ratio. In addition, the increase of amorphous volume fraction also leads to the increase of wear resistanceproperties of the remelted coating.
本文在低碳钢表面通过半导体激光熔覆+重熔的工艺制备了镍基非晶纳米晶复合涂层，主要研究内容有：Ni-Fe-B-Si-Nb非晶合金体系的成分设计与制备，涂层的显微组织和相结构的演变规律和形成机制，以及涂层硬度分布和耐磨性能的表征。主要研究成果如下：
针对Ni-Fe-B-Si-Nb合金体系，基于判断非晶形成能力三条经验准则和共晶点准则进行了混合焓、归一化错配熵的计算和相图分析，在此基础上初步设计了合金成分范围。并结合合金元素含量对涂层非晶形成能力影响的试验研究，最终确定了适合采用激光熔覆+重熔制备非晶复合涂层的合金粉末成分为(Ni_(0.6)Fe_(0.4))_(68)B_(18)Si_(10)Nb_4（原子百分比），此时所得激光重熔涂层具有相对最大的非晶体积含量。
系统研究了激光熔覆和激光重熔参数变化对重熔涂层非晶体积含量的影响。发现激光功率密度会影响稀释率，随激光功率密度的增加，熔覆层的熔深增加，熔池搅拌作用增强，稀释率也会提高。稀释率较低时，熔覆层内的成分和名义成分接近，因此在重熔层内获得了较大体积含量的非晶组织，而当稀释率较大时，导致重熔层内非晶含量降低，甚至不能形成非晶。在保证熔覆层成分接近名义成分的基础上，随激光功率密度的增加，熔覆层的组织和成分更加均匀，在激光重熔后，重熔层的非晶体积含量也随之增加。重熔时激光扫描速度为4m/min和5m/min时，重熔层内基本无非晶相生成，速度为6m/min时重熔层内开始形成非晶，随重熔时激光扫描速度的进一步增加，重熔层非晶含量也随之升高，当激光重熔扫描速度为9m/min时，重熔层内的非晶体积含量为64%。
观察和分析了激光重熔层的组织分布，发现激光熔覆功率密度为12100W/cm~2，扫描速度为0.36m/min，激光重熔功率密度为53000W/cm~2，扫描速度大于6m/min（含）可在重熔层内获得非晶相，8m/min时，其重熔层组织主要为非晶相和NbC颗粒相，在其他参数条件下（非晶含量降低时），重熔层内还可能形成等轴晶、纳米晶相及枝晶相和非晶相的混合组织等。计算了(Ni_(0.6)Fe_(0.4))_(68)B_(18)Si_(10)Nb_4合金涂层在激光重熔时的热循环曲线，并结合热力学、动力学对激光熔覆+重熔条件下的非晶相形成特点及机制进行了探讨。结果表明，采用激光熔覆+重熔获得镍基非晶复合涂层的临界冷却速率约为10118.8K/s，高于相同成分的镍基合金在采用铜模吸铸制备大块非晶时的临界冷却速率。认为出现这一现象的主要原因是：热力学方面，在熔覆层/重熔层界面处会出现部分熔化区，以及在重熔层内部存在NbC颗粒相，都可以作为异质形核的基底，其形核自由能会降低，有利于形核，必须继续增加冷却速率才能防止晶体形核及晶粒长大行为的产生。动力学方面，由于采用激光重熔工艺，在激光重熔时会产生不可忽视的熔体流动和溶质迁移行为，加速了元素的长程扩散，因此也必须通过提高激光扫描速度（熔体冷却速率），降低熔体表面张力梯度和高温停留时间，来提高其非晶形成能力。
系统测试了(Ni_(0.6)Fe_(0.4))_(68)B_(18)Si_(10)Nb_4合金激光熔覆+重熔涂层的显微硬度分布及耐磨性能。显微硬度测试结果表明在涂层截面上由表及里显微硬度值逐渐降低，在重熔层内其显微硬度值最大，并且随重熔层内非晶含量的增加，显微硬度值不断提高。激光重熔涂层的平均硬度和弹性模量分别为1227.9HV和277.4GPa，高于相同合金体系的大块非晶合金，探讨了重熔涂层的强化机制。摩擦磨损试验结果表明随摩擦转速、载荷以及摩擦时间的增加，涂层的失重逐渐增加。摩擦系数随载荷的增加呈减小的趋势。针对(Ni_(0.6)Fe_(0.4))_(68)B_(18)Si_(10)Nb_4合金激光熔覆涂层、激光重熔涂层（非晶复合涂层）以及大块非晶，H~3/E~(*2)比值可以反映对其耐磨性影响的变化规律，随H~3/E~(*2)比值的增加，耐磨性得到提高。重熔涂层非晶含量增加时，涂层耐磨性能也得到提高。
Laser cladding technology is a novel technology developed in1970s dueto the development of high power laser equipment. It is a multidisciplinarytechnology with laser heating and melting, mass exchange in the melted pooland rapid solidification. Laser melting or laser remelting is a technique that ahigh power density laser beam scans on surface of metals or alloys, leads tothe melting of surface metals, and solidifies followed. The cooling rate isusually at102～106K/s, even to1012K/s, so fine and homogeneous structurescould be obtained at the surface. It is possible to form composite amorphouslayer in the surface crystalline materials when using laser cladding andremelting process. The laser cladding process can give low dilution claddedcoating to guarantee the composition; laser remelting process can lead to highsolidification rate.
In this paper, an amorphous composite coating was fabricated by usinghigh power diode laser cladding and remelting process on mild steel surface.Design and preparation of Ni-Fe-B-Si-Nb amorphous alloys systems wascarried out. The microstructure and phase were observed and analyzed. Themicrohardness and wear resistance properties of the coating were also tested.Some of main experimental results and conclusions are listed as follows.
For Ni-Fe-B-Si-Nb alloy systems, based on the three empirical rules anddeep eutectic rule for high glass-foming ability in metallic glasses, the mixingenthalpy and mismatch entropy were calculated, the alloys phase diagrams were analyzed. A preliminary composition of the alloy is obtained.Furthermore, considering the characteristics of laser processing andexperimental studies, the final composition of (Ni_(0.6)Fe_(0.4))_(68)B_(18)Si_(10)Nb_4(at.%)was determined. The biggest amorphous volume fraction could be obtained inthe laser cladding and remelted coating.
The influence of laser cladding and remelting processing parameters onamorphous volume fractions of the remelted coating was studiedsystematically. It can be seen that dilution ratio was affected by laser powerinput. With the increasing of laser power, the penetration and dilution willincrease. A high amorphous volume fraction could be obtained at low dilutioncoating where the nominal composition of the powder was kept. While forhigh dilution coating, the amorphous volume fraction was relatively low,even no amorphous phase was formed in the remelted coating. When thenominal composition was guaranteed, the structure and composition weremore homogeneous at higher laser power input. The amorphous volumefraction was also at higher standards in the remelted coating. The amorphousphase was not formed when the laser scanning speed is4m/min and5m/minduring the laser remelting process. For6m/min or more, the amorphous phasewas observed, and the amorphous volume fraction increased with theincreasing of laser scanning speed. The amorphous volume fraction was64%for6m/min.
Structure of amorphous phase matrix and NbC particles were observedin the remelted coating when the laser cladding power was800W, scanningspeed was0.36m/min, laser remlting power was3500W and remeltingscanning speed was8m/min. The fine equiaxed grains, nano-grains anddendrites/amorphous structures could also be obtained in the remeltedcoating for low amorphous volume fraction remelted coatings. The thermalcycle of the coating during laser remelting process was calculated using FEM method. Combined with the thermodynamics and kinetic aspects, theformation characteristics and mechanisms of amorphous phase for lasercladding and remlting process were studied. The results showed that thecritical cooling rate was10118.8K/s for (Ni_(0.6)Fe_(0.4))_(68)B_(18)Si_(10)Nb_4alloyfabricated by laser cladding and remelting process which is higher than thatof BMGs. In thermodynamics aspect, the semi-melted zone atremlted/cladded interface and NbC particles in remelted zone are both thesites of heterogeneous nucleation. The barrier energy needed forheterogeneous nucleation is reduced. So much more cooling speed is neededto suppressing crystallization within the supercooled liquid. In kinetics aspect,the liquid flow and solute transport behavior in remelted pool can not beneglected, which accelerated the element diffusion. Therefore, the Surfacetention gradient and holding time at high termperature should be decreasedby increasing the scanning speed (cooling rate) during the laser remeltingprocess.
The microhardness and wear resistance properties of the coating weretested systematically. The graded microhardness distribution was exhibited inthe coating, the microhardness increased from the interface of clad/substratesurface to the top of the remelted coating. The microhardness was higher forcoatings with bigger amorphous volume fraction. The mean microhardnessand elastic modulus are1227.9HV and277.4GPa, respectively which arehigher than that of the BMGs with same compositions. The strengtheningmechanism of this phenomenon was also studied. Wear tests results showedthat the wear losses increased with increasing of the wear rotation speed, loadand time. Friction coefficient decreased with the increase of load. The ratio ofH3/E*2can represent the changing rule of wear resistance properties of thecladded coating, remelted coating and BMGs. Wear resistance propertiesincreases with the increasing of H3/E*2ratio. In addition, the increase of amorphous volume fraction also leads to the increase of wear resistanceproperties of the remelted coating.
引文
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