钢的激光辅助渗硅过程与组织性能
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摘要
硅钢是一种含碳量很低的Fe-Si软磁合金,是发展电力和电讯工业的基础材料。随着硅钢中Si含量的增加,其电阻率和最大磁导率增大、矫顽力和铁损降低,软磁性能提高。然而随着Si含量的增加,其加工性能也变差。高硅钢优异的软磁性能吸引着人们进行大量的研究和开发工作,一些新的高硅钢制备工艺如特殊轧制法、快速凝固法、喷射成型法、化学气相沉积法等相继展开,它们有其优点,同时也存在着方法本身带来的技术和成本方面的局限性。利用激光熔覆技术制备的涂层具有与基体呈冶金结合、外观形貌平整、微观组织致密、化学组成均匀、工艺参数容易控制、制备效率高、无污染、低能耗、成品率高等优点,显示出良好的应用前景。本文以提高硅钢表面硅含量为目的,提出激光辅助渗硅新技术,在低硅钢表面首先利用激光熔覆技术制备出质量良好的高Si涂层,再经过随后的退火处理,通过控制退火温度和保温时间制备Si成分均匀的高硅钢或Si成分呈梯度分布的高硅浓度梯度硅钢,为高硅钢片的开发研制提供一条新的技术路线,对于发展高硅钢制造技术和激光应用技术都具有十分重要的意义。
本文从熔覆材料体系设计、熔覆工艺探索和最优化等方面,进行了系统的实验研究；利用光学显微镜(OM)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线衍射仪(XRD)、能谱仪(EDS)和穆斯堡尔谱仪(MS)等对优化条件下制备的高Si涂层的形貌、微观组织、相组成、成分和显微硬度分布进行系统的表征；运用Miedema和Toop热力学模型结合熔覆过程中温度场的分布对熔池内Fe-Si-C熔体进行热力学计算,为控制熔覆工艺参数提供重要的理论依据；探索随后的扩散退火工艺,对高温扩散退火后试样组织、相组成、硬度和成分的分布进行观察和分析,并利用振动样品磁强计(VSM)对退火后试样的室温磁性能进行了检测和分析。
在低硅钢基体表面预置不同厚度的Fe和Si的混合粉末,利用Nd:YAG脉冲激光进行单道和多道搭接熔覆。在探索和调整工艺参数的过程中发现,激光功率和扫描速度是影响熔覆层质量的重要因素。激光功率过低,涂层与基体之间形成非冶金结合,裂纹等缺陷多；激光功率过高,熔覆涂层表面易发生氧化现象,且涂层被基体稀释严重。增大激光扫描速度有助于熔覆层组织的细化和均匀性的提高,同时,熔覆层厚度减小,稀释率减小。对于不同厚度的预置涂层来说,制备表面质量良好、无裂纹和气孔等缺陷的熔覆涂层存在所需的最小激光比能量值。比能量过高,熔覆材料烧损过多,不能形成平整的熔覆层,且涂层稀释现象严重；比能量过低,不能满足冶金反应所需的能量,熔覆层与基体之间不能形成冶金结合。
对优化参数下制备的单道和多道搭接熔覆涂层的表面形貌和微观组织的分析表明,熔覆涂层表面质量良好,无裂纹和气孔等缺陷,组织致密,与基体呈良好的冶金结合。自熔覆试样表面起,单道和多道搭接熔覆层的显微组织可分为熔覆区、界面结合区和热影响区。凝固组织受熔池内液相成分和凝固过程控制参数的影响,在熔覆层与基体的结合界面(即熔池底部)处,凝固组织以平面晶形式外延生长；随着距离结合界面距离的增加,显微组织由受热流方向控制而垂直于结合界面的柱状晶过渡到树枝晶,组织细化；熔覆层顶部为细小的枝晶组织,生长方向紊乱。在熔覆层中,垂直于结合界面方向存在一定程度的组织不均匀性,而同一高度不同部位的枝晶形貌无明显变化,组织是均匀的。热影响区是细小的淬火马氏体组织,基体仍保持原始铁素体组织。由于多道搭接熔覆过程中存在激光的二次扫描现象,故搭接区的枝晶尺寸较大且生长方向较紊乱。
测定优化参数下制备的两种熔覆涂层的室温Mossbauer谱,涂层超精细结构的分析结果表明,一种含Si量最高可达9.1wt.%左右的Fe-Si涂层中,存在相对含量分别为69.6%、13.0%和17.4%的α-Fe固溶体、Fe-Si化合物和y-Fe固溶体等三种类型的相,其中含Si主要相以A2型(体心立方)的a-Fe(Si)无序固溶体形式存在；另一种含Si量最高可达15.20wt.%左右的Fe-Si涂层中,存在相对含量分别为93.9%、5.8%和0.3%的Fe3Si、Fe-Si化合物和γ-Fe固溶体等三种类型的相,其中含Si主要相以D03型(面心立方超结构)的Fe3Si有序固溶体形式存在。
熔覆涂层的Si含量远远高于低硅钢基体的Si含量,且Si含量在熔覆区内变化不大,结合区和热影响区的Si含量呈下降趋势；熔覆层显微硬度分布曲线与Si含量分布曲线具有相同的变化趋势,涂层的硬度远远高于基体的硬度,其硬度提高的主要原因是Si原子的固溶强化作用和激光处理后组织的细晶强化作用。
在激光熔覆过程中,整个涂层处于高温熔化状态,形成Fe-Si-C合金熔池。垂直激光束扫描方向的熔池内Si活度以激光束入射方向为轴对称分布,而熔池内沿激光束扫描方向的前方Si的等活度线密集,后部Si的等活度线密度相对较低；熔池底面与表面激光束作用中心位置相比,Si活度低,这是熔覆层底部形成多种硅化物以及形成良好冶金结合的重要原因。
将Si含量约为15.20wt.%的高Si熔覆涂层试样在1100℃进行不同时间的退火处理。高温扩散退火处理后,制备出由单一α-Fe(Si)固溶体相组成的、横截面上显微硬度与Si含量呈梯度分布的高硅浓度梯度硅钢。搭接熔覆和退火处理后的样品均具有室温铁磁性,其中,1100℃退火处理6小时的试样表面Si含量为5.94wt.%,心部Si含量为3.68wt.%,与Fe-1Si基体比较,其具有更高的比饱和磁化强度(235.06emu/g)和更低的矫顽力(1.5395G),直流磁性能优于原始Fe-1Si低硅钢板。
Silicon steel is the Fe-Si soft magnetic alloy containing low Si content and is the base material of electric power and telecommunication. It is well known that increasing the Si content improves the soft magnetic properties of silicon steel. However, as the Si content is increased, the material becomes extremely brittle and it is difficult to produce thin sheets by conventional rolling. Several methods have been developed to obtain high silicon steels including special thermomechanical rolling, rapid solidification, spay forming and chemical vapor deposition, etc. But each method has its limitations. Laser cladding technique aims at obtaining high performance alloy coatings on steel substrates, in which adhesion is obtained by surface melting of the substrate. In this process, a thin surface layer of the substrate is melted by the laser beam together with the additive or preplaced material to form the coating. The process has received a lot of attention over the years and is now applied commercially in a range of industries such as the automotive, mining and aerospace. The main advantages of laser cladding compared with the processes mentioned above are that the source of the energy can be localized and the size of laser beam can be controlled precisely. Moreover, the higher solidification rates induce a fine microstructure consisting of crystalline or amorphous phases and with an extended solid solubility of key alloying elements. The aim of the present work is to improve the Si content of the surface of silicon steel. The new method of laser assisted siliconizing is to laser clad a well-qualified high Si coating on the low silicon steel surface and then to prepare a high silicon steel or high si gradient silicon steel through the subsequent diffusion annealing treatment. It is a new potential technique to produce high silicon steel.
The investigations of design of cladding material, exploration of the processing parameters and optimization of the parameters were carried out in the present work. Characterizations of surface morphology, microstructure, phase constituents, chemical composition and microhardness were carried out by using the optical microscope (OM), scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD), energy dispersive spectroscopy (EDS) and Mossbauer spectroscopy (MS). Based on the Miedema's formation heat model for binary alloys and the Toop's asymmetric model for ternary alloys, the formation heat, excess entropy and activity coefficients of Si from 1 900K to 4 100K in the Fe-Si-C melt formed during the laser cladding high Si coatings process were calculated. The exploration of the subsequent diffusion annealing treatment was carried and the magnetic properties of the laser cladding specimens after annealing were measured by vibrating sample magnetometer (VSM).
During the single-track and multi-track laser cladding mixed powders of Fe and Si on low silicon steel surface, the laser energy and the laser scanning speed are found to the the key factors affecting the cladding process. When the laser energy is lower, the non-metallurigical bonding formed between the cladding coating and the low silicon steel substrate and there are a lot of cracks in the coatings. When the laser energy is higher, the surface oxidation of laser cladding coating is easy to occur and the dilution is high. The increase of laser scanning speed is helpful for the refinement and uniformity of cladding microstructure. At the same time, the thickness of laser cladding coating decreased and the dilution rate is also decreased. As for the preplaced powder bed with different thickness, the specific laser energy exists to produce a pore and crack-free coating with dense microstructure and high Si content. The higher specific laser energy causes a severe burning loss and is not helpful for obtaining the smooth cladding coating. The dilution at higher specific laser energy is also high. When the specific laser energy is lower, the energy for forming the metallurgical bonding between the coating and the substrate is not satisfied.
By means of optimized single-track and multi-track laser cladding, a crack-and pore-free coating through excellent metallurgical bonding with the substrate was successfully prepared on the low silicon steel. After cladding, the surface of silicon steel could be divided into the cladding zone, the interface zone and the heat-affected zone (HAZ). The interface zone between the cladding zone and the substrate is a planar front solidified layer, epitaxially grown from the substrate. The cladding zone forms after rapid solidification of the molten cladding materials. In the cladding zone, the microstructures along the interface-to-top surface of the coating exhibit vertically aligned columnar and dendritic microstructures, which indicate that a vertical temperature gradient as heat is conducted away from the melt pool towards the substrate. And there are disoriented and finer dendrites near the top surface. In the cladding coating, the microstructure along the interface-to-top surface of the coating is not uniform and that of same highness has no obvious change and the microstructure is uniform. The HAZ near the substrate is characterized by a fine acicular martensite and the substrate still keeps ferrite microstructure. The secondary scanning occurs obviously during the multi-track laser cladding process and the microstructure of the overlapping zone is coarser and disoriented.
The results of Mossbauer spectroscopy show that there are two hyperfine structures in the cladding coatings prepared under the optimized process parameters. One is the Fe-Si coating containing Si as high as 9.1wt.%. In this coating, the relative content of the a-Fe solution, the Fe-Si compounds and the y-Fe solution are 69.6%,13.0% and 17.4%, respectively. The main phase containing Si element of this coating is existing in A2 type (body-centered cubic structured) disorder solid solution ofα-Fe. The other is the Fe-Si coating containing Si as high as 15.20wt.% in which the relative content of the Fe3Si, the Fe-Si compounds and the y-Fe solution are 93.9%,5.8%and 0.3%, respectively. The main phase containing Si element of this coating is DO3 type (face-centered cubic structured superlattice) order solid solution of Fe3Si.
The Si content of laser cladding zone is much higher than that of silicon steel substrate and the change of Si content is not obvious. And the Si content is decreasing in the interface zone and the HAZ. The change of microhardness is the same as that of Si content. The microhardness of the cladding zone is much higher that of the substrate as a result of the effect of solid solution hardened of Si atom and the refinement of the microstructure.
During the laser cladding process, the Fe-Si-C melt formed. The iso-activity lines of Si distribute axisymmetrically to the incident laser beam in the melt pool vertically to the laser scanning direction. And the iso-activity lines of Si in the front of the melt pool along the laser scanning direction are more intensive than those in the back of the melt pool. The activity of Si on the bottom of the melt pool is lower than that in the effecting center of laser beam on the top surface of the melt pool and it may be the important reason of the formation of the silicides and excellent metallurgical bonding between the laser cladding coating and the substrate.
The laser cladding specimens of Si content of 15.20wt.% were diffusion annealed at 1100℃for different times. The high Si gradient silicon steel with single phase ofα-Fe(Si) solution solid was obtained and the microhardness and Si content are distributed gradiently at the cross-sections of the specimens. The specimens as clad and as annealed are ferromagnetic at room temperature. The Si content of the surface of specimen as clad and annealed at 1100℃for 6 hours is 5.94wt.% and the Si content of the core of it is 3.68wt.%. And the DC magnetic property of specimens as clad and annealed at 1100℃for 6 hours is better with the specific saturation magnetization of 235.06emu/g and the coercivity of 1.5395G than the original low silicon steel.
本文从熔覆材料体系设计、熔覆工艺探索和最优化等方面,进行了系统的实验研究；利用光学显微镜(OM)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线衍射仪(XRD)、能谱仪(EDS)和穆斯堡尔谱仪(MS)等对优化条件下制备的高Si涂层的形貌、微观组织、相组成、成分和显微硬度分布进行系统的表征；运用Miedema和Toop热力学模型结合熔覆过程中温度场的分布对熔池内Fe-Si-C熔体进行热力学计算,为控制熔覆工艺参数提供重要的理论依据；探索随后的扩散退火工艺,对高温扩散退火后试样组织、相组成、硬度和成分的分布进行观察和分析,并利用振动样品磁强计(VSM)对退火后试样的室温磁性能进行了检测和分析。
在低硅钢基体表面预置不同厚度的Fe和Si的混合粉末,利用Nd:YAG脉冲激光进行单道和多道搭接熔覆。在探索和调整工艺参数的过程中发现,激光功率和扫描速度是影响熔覆层质量的重要因素。激光功率过低,涂层与基体之间形成非冶金结合,裂纹等缺陷多；激光功率过高,熔覆涂层表面易发生氧化现象,且涂层被基体稀释严重。增大激光扫描速度有助于熔覆层组织的细化和均匀性的提高,同时,熔覆层厚度减小,稀释率减小。对于不同厚度的预置涂层来说,制备表面质量良好、无裂纹和气孔等缺陷的熔覆涂层存在所需的最小激光比能量值。比能量过高,熔覆材料烧损过多,不能形成平整的熔覆层,且涂层稀释现象严重；比能量过低,不能满足冶金反应所需的能量,熔覆层与基体之间不能形成冶金结合。
对优化参数下制备的单道和多道搭接熔覆涂层的表面形貌和微观组织的分析表明,熔覆涂层表面质量良好,无裂纹和气孔等缺陷,组织致密,与基体呈良好的冶金结合。自熔覆试样表面起,单道和多道搭接熔覆层的显微组织可分为熔覆区、界面结合区和热影响区。凝固组织受熔池内液相成分和凝固过程控制参数的影响,在熔覆层与基体的结合界面(即熔池底部)处,凝固组织以平面晶形式外延生长；随着距离结合界面距离的增加,显微组织由受热流方向控制而垂直于结合界面的柱状晶过渡到树枝晶,组织细化；熔覆层顶部为细小的枝晶组织,生长方向紊乱。在熔覆层中,垂直于结合界面方向存在一定程度的组织不均匀性,而同一高度不同部位的枝晶形貌无明显变化,组织是均匀的。热影响区是细小的淬火马氏体组织,基体仍保持原始铁素体组织。由于多道搭接熔覆过程中存在激光的二次扫描现象,故搭接区的枝晶尺寸较大且生长方向较紊乱。
测定优化参数下制备的两种熔覆涂层的室温Mossbauer谱,涂层超精细结构的分析结果表明,一种含Si量最高可达9.1wt.%左右的Fe-Si涂层中,存在相对含量分别为69.6%、13.0%和17.4%的α-Fe固溶体、Fe-Si化合物和y-Fe固溶体等三种类型的相,其中含Si主要相以A2型(体心立方)的a-Fe(Si)无序固溶体形式存在；另一种含Si量最高可达15.20wt.%左右的Fe-Si涂层中,存在相对含量分别为93.9%、5.8%和0.3%的Fe3Si、Fe-Si化合物和γ-Fe固溶体等三种类型的相,其中含Si主要相以D03型(面心立方超结构)的Fe3Si有序固溶体形式存在。
熔覆涂层的Si含量远远高于低硅钢基体的Si含量,且Si含量在熔覆区内变化不大,结合区和热影响区的Si含量呈下降趋势；熔覆层显微硬度分布曲线与Si含量分布曲线具有相同的变化趋势,涂层的硬度远远高于基体的硬度,其硬度提高的主要原因是Si原子的固溶强化作用和激光处理后组织的细晶强化作用。
在激光熔覆过程中,整个涂层处于高温熔化状态,形成Fe-Si-C合金熔池。垂直激光束扫描方向的熔池内Si活度以激光束入射方向为轴对称分布,而熔池内沿激光束扫描方向的前方Si的等活度线密集,后部Si的等活度线密度相对较低；熔池底面与表面激光束作用中心位置相比,Si活度低,这是熔覆层底部形成多种硅化物以及形成良好冶金结合的重要原因。
将Si含量约为15.20wt.%的高Si熔覆涂层试样在1100℃进行不同时间的退火处理。高温扩散退火处理后,制备出由单一α-Fe(Si)固溶体相组成的、横截面上显微硬度与Si含量呈梯度分布的高硅浓度梯度硅钢。搭接熔覆和退火处理后的样品均具有室温铁磁性,其中,1100℃退火处理6小时的试样表面Si含量为5.94wt.%,心部Si含量为3.68wt.%,与Fe-1Si基体比较,其具有更高的比饱和磁化强度(235.06emu/g)和更低的矫顽力(1.5395G),直流磁性能优于原始Fe-1Si低硅钢板。
Silicon steel is the Fe-Si soft magnetic alloy containing low Si content and is the base material of electric power and telecommunication. It is well known that increasing the Si content improves the soft magnetic properties of silicon steel. However, as the Si content is increased, the material becomes extremely brittle and it is difficult to produce thin sheets by conventional rolling. Several methods have been developed to obtain high silicon steels including special thermomechanical rolling, rapid solidification, spay forming and chemical vapor deposition, etc. But each method has its limitations. Laser cladding technique aims at obtaining high performance alloy coatings on steel substrates, in which adhesion is obtained by surface melting of the substrate. In this process, a thin surface layer of the substrate is melted by the laser beam together with the additive or preplaced material to form the coating. The process has received a lot of attention over the years and is now applied commercially in a range of industries such as the automotive, mining and aerospace. The main advantages of laser cladding compared with the processes mentioned above are that the source of the energy can be localized and the size of laser beam can be controlled precisely. Moreover, the higher solidification rates induce a fine microstructure consisting of crystalline or amorphous phases and with an extended solid solubility of key alloying elements. The aim of the present work is to improve the Si content of the surface of silicon steel. The new method of laser assisted siliconizing is to laser clad a well-qualified high Si coating on the low silicon steel surface and then to prepare a high silicon steel or high si gradient silicon steel through the subsequent diffusion annealing treatment. It is a new potential technique to produce high silicon steel.
The investigations of design of cladding material, exploration of the processing parameters and optimization of the parameters were carried out in the present work. Characterizations of surface morphology, microstructure, phase constituents, chemical composition and microhardness were carried out by using the optical microscope (OM), scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD), energy dispersive spectroscopy (EDS) and Mossbauer spectroscopy (MS). Based on the Miedema's formation heat model for binary alloys and the Toop's asymmetric model for ternary alloys, the formation heat, excess entropy and activity coefficients of Si from 1 900K to 4 100K in the Fe-Si-C melt formed during the laser cladding high Si coatings process were calculated. The exploration of the subsequent diffusion annealing treatment was carried and the magnetic properties of the laser cladding specimens after annealing were measured by vibrating sample magnetometer (VSM).
During the single-track and multi-track laser cladding mixed powders of Fe and Si on low silicon steel surface, the laser energy and the laser scanning speed are found to the the key factors affecting the cladding process. When the laser energy is lower, the non-metallurigical bonding formed between the cladding coating and the low silicon steel substrate and there are a lot of cracks in the coatings. When the laser energy is higher, the surface oxidation of laser cladding coating is easy to occur and the dilution is high. The increase of laser scanning speed is helpful for the refinement and uniformity of cladding microstructure. At the same time, the thickness of laser cladding coating decreased and the dilution rate is also decreased. As for the preplaced powder bed with different thickness, the specific laser energy exists to produce a pore and crack-free coating with dense microstructure and high Si content. The higher specific laser energy causes a severe burning loss and is not helpful for obtaining the smooth cladding coating. The dilution at higher specific laser energy is also high. When the specific laser energy is lower, the energy for forming the metallurgical bonding between the coating and the substrate is not satisfied.
By means of optimized single-track and multi-track laser cladding, a crack-and pore-free coating through excellent metallurgical bonding with the substrate was successfully prepared on the low silicon steel. After cladding, the surface of silicon steel could be divided into the cladding zone, the interface zone and the heat-affected zone (HAZ). The interface zone between the cladding zone and the substrate is a planar front solidified layer, epitaxially grown from the substrate. The cladding zone forms after rapid solidification of the molten cladding materials. In the cladding zone, the microstructures along the interface-to-top surface of the coating exhibit vertically aligned columnar and dendritic microstructures, which indicate that a vertical temperature gradient as heat is conducted away from the melt pool towards the substrate. And there are disoriented and finer dendrites near the top surface. In the cladding coating, the microstructure along the interface-to-top surface of the coating is not uniform and that of same highness has no obvious change and the microstructure is uniform. The HAZ near the substrate is characterized by a fine acicular martensite and the substrate still keeps ferrite microstructure. The secondary scanning occurs obviously during the multi-track laser cladding process and the microstructure of the overlapping zone is coarser and disoriented.
The results of Mossbauer spectroscopy show that there are two hyperfine structures in the cladding coatings prepared under the optimized process parameters. One is the Fe-Si coating containing Si as high as 9.1wt.%. In this coating, the relative content of the a-Fe solution, the Fe-Si compounds and the y-Fe solution are 69.6%,13.0% and 17.4%, respectively. The main phase containing Si element of this coating is existing in A2 type (body-centered cubic structured) disorder solid solution ofα-Fe. The other is the Fe-Si coating containing Si as high as 15.20wt.% in which the relative content of the Fe3Si, the Fe-Si compounds and the y-Fe solution are 93.9%,5.8%and 0.3%, respectively. The main phase containing Si element of this coating is DO3 type (face-centered cubic structured superlattice) order solid solution of Fe3Si.
The Si content of laser cladding zone is much higher than that of silicon steel substrate and the change of Si content is not obvious. And the Si content is decreasing in the interface zone and the HAZ. The change of microhardness is the same as that of Si content. The microhardness of the cladding zone is much higher that of the substrate as a result of the effect of solid solution hardened of Si atom and the refinement of the microstructure.
During the laser cladding process, the Fe-Si-C melt formed. The iso-activity lines of Si distribute axisymmetrically to the incident laser beam in the melt pool vertically to the laser scanning direction. And the iso-activity lines of Si in the front of the melt pool along the laser scanning direction are more intensive than those in the back of the melt pool. The activity of Si on the bottom of the melt pool is lower than that in the effecting center of laser beam on the top surface of the melt pool and it may be the important reason of the formation of the silicides and excellent metallurgical bonding between the laser cladding coating and the substrate.
The laser cladding specimens of Si content of 15.20wt.% were diffusion annealed at 1100℃for different times. The high Si gradient silicon steel with single phase ofα-Fe(Si) solution solid was obtained and the microhardness and Si content are distributed gradiently at the cross-sections of the specimens. The specimens as clad and as annealed are ferromagnetic at room temperature. The Si content of the surface of specimen as clad and annealed at 1100℃for 6 hours is 5.94wt.% and the Si content of the core of it is 3.68wt.%. And the DC magnetic property of specimens as clad and annealed at 1100℃for 6 hours is better with the specific saturation magnetization of 235.06emu/g and the coercivity of 1.5395G than the original low silicon steel.
引文
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