工业纯铁表面纳米合金化改性及原子扩散行为研究
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摘要
现有的金属表面合金化手段往往要在高温下、长时间处理，以实现原子的渗入，这不仅可能会对基体的组织性能产生不利影响，也造成了资源、能源的浪费。针对这一问题，本文将金属表面自纳米化技术与表面合金化技术相结合，对工业纯铁进行纳米合金化改性。其核心思想是利用纳米晶铁中的晶界、缺陷等为原子扩散提供大量扩散通道，从而能够在较低的温度下实现原子的快速扩散，降低表面合金化温度，缩短扩渗时间。表面纳米合金化改性主要涉及四个方面的内容，即自纳米化组织的获得、纳米晶中原子的扩散、扩散过程中的相变以及纳米合金化改性层的性能。
本文首先利用高能喷丸法对工业纯铁进行了表面自纳米化处理，运用OM、XRD、SEM、EBSD等手段对其自纳米化组织结构进行了系统表征与分析，得到了工业纯铁高能喷丸自纳米化工艺和机理。在此基础上，通过不同扩散源和应力加载方式的扩散处理，在工业纯铁表面获得了多种表面纳米合金化改性层；重点对镍原子在纳米晶铁中的扩散行为进行了研究；然后对纳米合金化改性过程中的相变进行了分析；最后对纳米合金化改性层的显微硬度、耐蚀性及耐磨性进行了表征与研究。
研究结果表明，在喷丸压力0.6MPa，喷丸弹丸直径1.0mm，喷嘴距喷丸表面距离50mm的工艺条件下，经6min喷丸处理，工业纯铁的表层晶粒被细化到了43.9nm，微观畸变为0.0652%；获得了本文扩散处理所需的工业纯铁自纳米化样品。表面纳米化组织的退火和热分析试验结果表明，自纳米化工业纯铁在600℃时晶粒已开始长大。
工业纯铁高能喷丸表面自纳米化过程中的晶粒细化主要有三个方面的机制：一方面是通过位错运动在大晶粒内部形成较大取向差的亚晶界，随着位错不断的湮灭、重排，亚晶界的取向差不断增大，最后演变成为晶界，大晶粒被细化成小晶粒。二是利用晶粒取向差不同而变形不同步的特点，逐渐将不同晶粒和晶粒内部不同部分分开从而实现晶粒细化。三是在喷丸过程中发生了一定程度的再结晶，不断形成新的小晶粒，从而细化晶粒。
在650～850℃之间对扩散偶施加10MPa恒定压力扩散实验表明，镍原子在纳米晶纯铁中的扩散系数比其在常规粗晶中提高了一个数量级；在850℃对扩散偶施加8~16MPa脉冲压力扩散时，镍在纳米晶铁中的扩散系数较恒定加压进一步提高。在用Arrhenius公式计算纳米晶中原子扩散系数时，应该考虑升温会导致纳米晶晶界数量减少从而降低扩散系数因素。
对自纳米化工业纯铁扩散处理过程中的相变研究表明，在不同纳米合金化改性层中除了α-Fe外，主要形成了FeNi_3、Fe2Ni_(0.25)、NiCr和NiCr_2等金属间化合物。经退火处理后，不同纳米合金化改性层的金属间化合物数量大大减少，物相主要是固溶体，而且都出现了一定数量的奥氏体。
晶粒细化、应力集中以及晶格畸变共同作用导致工业纯铁自纳米化处理后的硬度增加；合金化改性后，由于合金元素的渗入，形成了固溶强化效应，导致其硬度较原始试样提高。表面自纳米化导致纯铁的耐腐蚀性有所降低，合金化改性后耐蚀性有所提高；自纳米化纯铁以化学腐蚀为主，而合金化改性层的腐蚀主要是以电化学腐蚀为主。纯铁在磨损过程中表现为粘着磨损，摩擦系数较大，磨损严重；自纳米化处理后，纯铁表面的硬度提高导致其耐磨性提高，此外，表面形成的梯度结构导致疲劳源放出的位错将受到内、外晶界的阻碍，也在在一定程度上提高了纯铁的耐磨性；对于合金化改性层，由于形成了硬而脆的金属间化合物，磨损量有所降低。
The metallic materials are often treated at high temperature for a long time todiffuse the alloying elements into them during the existing surface alloying process ofmetallic materials. Which not only has an adverse effect on the microstructure andperformance of the metallic materials, but also causes resource and energy wasting. Tosolve this problem, the surface self-nanocrystallization (SSNC) technology and surfacealloying were combined to realize the surface modification of commercial iron in thispaper. There were many grain boundaries and defects in the self-nanocrystalline iron,which will provide a large number of diffusion channels. Therefore the atoms maydiffuse more rapidly in the self-nanocrystalline iron than in the coarse iron, which leadthe surface alloying of commercial iron at lower temperature in a short time. Thecombination of the surface self-nanocrystallization (SSNC) technology and surfacealloying was called surface nanocrystallinzation and alloying (SNA) in this paper.
Firstly self-nanocrystallinzed layers were prepared on the commercial pure ironsamples by means of high energy shot peening (HESP) method, and the microstructureof the self-nanocrystallinzed layers was characterized through optical microscopy (OM),scanning electron microscopy (SEM), X-ray diffraction (XRD) and electronbackscattered diffraction (EBSD). Then different elements were diffused into theSSNCed commercial iron and different SNAed layers were obtained. The diffusion ofatoms in nanocrystallined iron, phase transformation during SNA and the performanceof the SNAed layers were investigated detailedly.
Results showed that under0.6MPa press,50mm distance from shotting gun to thesurface of samples, a nanocrystalline surface layer without oxidation, porosity andcontamination was obtained by means of HESP to a commercial iron cylinder with a1mm diameter cast iron ball after6min shot. The SSNCed commercial iron containedan average grain size of43.9nm and a microstrain of0.0652%, and the grain begun togrow when annealing at600℃.
The mechanism of SSNC process of commercial iron involved three aspects. Themotion of the dislocations was the main reason, which lead the formation of bigorientation subgrain boundaries in coarse iron grain. After continued annihilation andrearrangement of the dislocations, the subgrain boundaries evolved into grainboundaries and the coarse grains were refined. Secondly big orientation lead the nonsynchronous deformation appear among different grains and the different parts ofthe coarse grains, which would separate grains and the different parts of coarse grains.Thirdly recrystallization produced fine grains on the deformed grain boundaries duringHESP.
The diffusion test showed that the diffusion coefficient of nickel in SSNCedcommercial iron improved by one order of magnitude than that in coarse iron under a10MPa constant pressure on the diffusion couple. The diffusion coefficient of nickel inSSNCed commercial iron would be further improved if imposing a8-16MPa pulsepressure on the diffusion couple. When using Arrhenius formula to calculate thediffusion coefficient of atoms in nanocrystallines, the effect of temperature on the grainsof nanocrystallines must be considered.
During SNA of commercial iron, intermetallic compounds such as FeNi_3, Fe_2Ni_(0.25),NiCr and NiCr_2formed in the SNAed layers. But after annealing at900℃, theintermetallic compounds reduced and transformed into solid solution, and a certainamount of austenite appeared in the SNAed layers.
The hardness of the SSNCed commercial iron enhanced because of grainrefinement, stress concentration and lattice distortion, while solid solution strengtheningeffect was the reason of the enhancement of hardness of the SNAed layers. Thecorrosion resistance of the commercial iron decreased after SSNC treating, but SNAtreatment can enhance the corrosion resistance of the commercial iron. Chemicalcorrosion and electrochemical corrosion were the corrosion principles of the SSNCedcommercial iron and the SNAed layers respectively. The wear resistance of commercialiron got a different level of improvement after SSNC and SNA treatment. The motion ofthe dislocations emitted from the fatigue source would be subjected to block of innercoarse and outer fine grain boundaries in the gradient structure of the SSNCedcommercial iron, which lead the enhancement of the wear resistance of SSNCed layers.As for the SNAed layers, the formation of hard and brittle intermetallic compounds wasthe main reason why the wear resistance improved.
本文首先利用高能喷丸法对工业纯铁进行了表面自纳米化处理，运用OM、XRD、SEM、EBSD等手段对其自纳米化组织结构进行了系统表征与分析，得到了工业纯铁高能喷丸自纳米化工艺和机理。在此基础上，通过不同扩散源和应力加载方式的扩散处理，在工业纯铁表面获得了多种表面纳米合金化改性层；重点对镍原子在纳米晶铁中的扩散行为进行了研究；然后对纳米合金化改性过程中的相变进行了分析；最后对纳米合金化改性层的显微硬度、耐蚀性及耐磨性进行了表征与研究。
研究结果表明，在喷丸压力0.6MPa，喷丸弹丸直径1.0mm，喷嘴距喷丸表面距离50mm的工艺条件下，经6min喷丸处理，工业纯铁的表层晶粒被细化到了43.9nm，微观畸变为0.0652%；获得了本文扩散处理所需的工业纯铁自纳米化样品。表面纳米化组织的退火和热分析试验结果表明，自纳米化工业纯铁在600℃时晶粒已开始长大。
工业纯铁高能喷丸表面自纳米化过程中的晶粒细化主要有三个方面的机制：一方面是通过位错运动在大晶粒内部形成较大取向差的亚晶界，随着位错不断的湮灭、重排，亚晶界的取向差不断增大，最后演变成为晶界，大晶粒被细化成小晶粒。二是利用晶粒取向差不同而变形不同步的特点，逐渐将不同晶粒和晶粒内部不同部分分开从而实现晶粒细化。三是在喷丸过程中发生了一定程度的再结晶，不断形成新的小晶粒，从而细化晶粒。
在650～850℃之间对扩散偶施加10MPa恒定压力扩散实验表明，镍原子在纳米晶纯铁中的扩散系数比其在常规粗晶中提高了一个数量级；在850℃对扩散偶施加8~16MPa脉冲压力扩散时，镍在纳米晶铁中的扩散系数较恒定加压进一步提高。在用Arrhenius公式计算纳米晶中原子扩散系数时，应该考虑升温会导致纳米晶晶界数量减少从而降低扩散系数因素。
对自纳米化工业纯铁扩散处理过程中的相变研究表明，在不同纳米合金化改性层中除了α-Fe外，主要形成了FeNi_3、Fe2Ni_(0.25)、NiCr和NiCr_2等金属间化合物。经退火处理后，不同纳米合金化改性层的金属间化合物数量大大减少，物相主要是固溶体，而且都出现了一定数量的奥氏体。
晶粒细化、应力集中以及晶格畸变共同作用导致工业纯铁自纳米化处理后的硬度增加；合金化改性后，由于合金元素的渗入，形成了固溶强化效应，导致其硬度较原始试样提高。表面自纳米化导致纯铁的耐腐蚀性有所降低，合金化改性后耐蚀性有所提高；自纳米化纯铁以化学腐蚀为主，而合金化改性层的腐蚀主要是以电化学腐蚀为主。纯铁在磨损过程中表现为粘着磨损，摩擦系数较大，磨损严重；自纳米化处理后，纯铁表面的硬度提高导致其耐磨性提高，此外，表面形成的梯度结构导致疲劳源放出的位错将受到内、外晶界的阻碍，也在在一定程度上提高了纯铁的耐磨性；对于合金化改性层，由于形成了硬而脆的金属间化合物，磨损量有所降低。
The metallic materials are often treated at high temperature for a long time todiffuse the alloying elements into them during the existing surface alloying process ofmetallic materials. Which not only has an adverse effect on the microstructure andperformance of the metallic materials, but also causes resource and energy wasting. Tosolve this problem, the surface self-nanocrystallization (SSNC) technology and surfacealloying were combined to realize the surface modification of commercial iron in thispaper. There were many grain boundaries and defects in the self-nanocrystalline iron,which will provide a large number of diffusion channels. Therefore the atoms maydiffuse more rapidly in the self-nanocrystalline iron than in the coarse iron, which leadthe surface alloying of commercial iron at lower temperature in a short time. Thecombination of the surface self-nanocrystallization (SSNC) technology and surfacealloying was called surface nanocrystallinzation and alloying (SNA) in this paper.
Firstly self-nanocrystallinzed layers were prepared on the commercial pure ironsamples by means of high energy shot peening (HESP) method, and the microstructureof the self-nanocrystallinzed layers was characterized through optical microscopy (OM),scanning electron microscopy (SEM), X-ray diffraction (XRD) and electronbackscattered diffraction (EBSD). Then different elements were diffused into theSSNCed commercial iron and different SNAed layers were obtained. The diffusion ofatoms in nanocrystallined iron, phase transformation during SNA and the performanceof the SNAed layers were investigated detailedly.
Results showed that under0.6MPa press,50mm distance from shotting gun to thesurface of samples, a nanocrystalline surface layer without oxidation, porosity andcontamination was obtained by means of HESP to a commercial iron cylinder with a1mm diameter cast iron ball after6min shot. The SSNCed commercial iron containedan average grain size of43.9nm and a microstrain of0.0652%, and the grain begun togrow when annealing at600℃.
The mechanism of SSNC process of commercial iron involved three aspects. Themotion of the dislocations was the main reason, which lead the formation of bigorientation subgrain boundaries in coarse iron grain. After continued annihilation andrearrangement of the dislocations, the subgrain boundaries evolved into grainboundaries and the coarse grains were refined. Secondly big orientation lead the nonsynchronous deformation appear among different grains and the different parts ofthe coarse grains, which would separate grains and the different parts of coarse grains.Thirdly recrystallization produced fine grains on the deformed grain boundaries duringHESP.
The diffusion test showed that the diffusion coefficient of nickel in SSNCedcommercial iron improved by one order of magnitude than that in coarse iron under a10MPa constant pressure on the diffusion couple. The diffusion coefficient of nickel inSSNCed commercial iron would be further improved if imposing a8-16MPa pulsepressure on the diffusion couple. When using Arrhenius formula to calculate thediffusion coefficient of atoms in nanocrystallines, the effect of temperature on the grainsof nanocrystallines must be considered.
During SNA of commercial iron, intermetallic compounds such as FeNi_3, Fe_2Ni_(0.25),NiCr and NiCr_2formed in the SNAed layers. But after annealing at900℃, theintermetallic compounds reduced and transformed into solid solution, and a certainamount of austenite appeared in the SNAed layers.
The hardness of the SSNCed commercial iron enhanced because of grainrefinement, stress concentration and lattice distortion, while solid solution strengtheningeffect was the reason of the enhancement of hardness of the SNAed layers. Thecorrosion resistance of the commercial iron decreased after SSNC treating, but SNAtreatment can enhance the corrosion resistance of the commercial iron. Chemicalcorrosion and electrochemical corrosion were the corrosion principles of the SSNCedcommercial iron and the SNAed layers respectively. The wear resistance of commercialiron got a different level of improvement after SSNC and SNA treatment. The motion ofthe dislocations emitted from the fatigue source would be subjected to block of innercoarse and outer fine grain boundaries in the gradient structure of the SSNCedcommercial iron, which lead the enhancement of the wear resistance of SSNCed layers.As for the SNAed layers, the formation of hard and brittle intermetallic compounds wasthe main reason why the wear resistance improved.
引文
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