激光冲击不锈钢抗腐蚀性能及微观强化机理研究
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摘要
激光冲击强化是一种新型的材料表面强化技术,具有高压、高能、超快和超高应变率等特点,具有常规加工方法无可比拟的优点,具有显著的技术优势。尽管激光冲击强化金属构件能够显著提高机械性能疲劳寿命,然而目前对于低层错能金属表层激光冲击细化晶粒的微观结构演变、性能结构关系以及抗应力腐蚀作用机理尚缺乏系统的研究,仍然缺乏统一的认识和深入的理解。
本文以ANSI304不锈钢为研究对象,对激光冲击强化不锈钢表面完整性、微观结构演变和晶粒细化机制、抗应力腐蚀性能以及激光复合处理工艺进行了若干基础研究和探索,获得了以下主要结论和创新性成果：
(1)系统研究了多次激光冲击诱导ANSI304不锈钢塑性变形层不同区域的微观组织结构,获得了深度方向激光冲击诱导的微观结构演变规律,首次深入系统地揭示了以多方向机械孪晶细化表层原始粗晶为主的激光冲击强化低层错能金属晶粒细化机制和微观强化机理：
单次激光冲击ANSI304不锈钢在表面形成厚度约为900μm的塑性变形层,并且随着离冲击表面距离越远,晶粒大小逐渐增大,细化原始晶粒是以片状机械孪晶为主要形式；多次激光冲击使奥氏体不锈钢塑性变形层的晶粒明显细化,在激光冲击ANSI304不锈钢的上表面,晶粒尺寸约为100-200nm。在观测试验结果的基础上,多次激光冲击ANSI304不锈钢微观结构演变规律和晶粒细化机制为：(ⅰ)高密度的机械挛晶将原始粗晶细分为层片状挛晶/基体片；(ⅱ)多次冲击能够形成不同方向的机械挛晶将粗晶细化为斜方形、三角形形状的结构,最小可以观察到亚微米量级；(ⅲ)具有取向差结构经过再结晶演变成细化的晶粒。研究成果发表在国际知名期刊Acta Materialia (2010,58(16):5354-5362)上,评审专家认为：‘'Combined with prior reporting of the work on high-stacking fault energy FCC aluminum, the work on low stacking fault energy stainless steel makes this an important collection that will be widely used(……形成一个完整的面心立方金属激光冲击晶粒细化的微观强化机理)”,该部分研究成果在国际上产生良好的影响。
(2)设计了不同晶粒尺寸和残余应力状态的三种不同U型弯曲试样,测试和表征了143±1℃42%MgCl2溶液条件下腐蚀裂纹萌生时间、裂纹形貌、残余应力以及微观结构,获得了残余压应力和晶粒细化共同作用的激光冲击不锈钢抗应力腐蚀的作用机制：
三种不同U型弯曲试样在143±1℃42%MgCl2溶液内应力腐蚀裂纹萌生时间、裂纹形貌、残余应力以及微观结构的试验结果表明：大面积搭接激光冲击能够诱导高幅残余压应力并且细化ANSI304不锈钢表层晶粒,未处理U型试样的开裂时间约为16小时,先冲后弯U型试样的开裂时间约为110小时,而先弯后冲试样300小时浸泡都未出现腐蚀裂纹,晶粒细化和残余应力是提高ANSI304奥氏体抗腐蚀能力的两大主要因素,其中残余压应力占主导作用,晶粒细化也是抑制应力裂纹萌生和扩展的主要因素。研究成果发表在国际知名期刊Corrosion Science (2012,60:145-152)上,评审专家认为"The effect of laser shock peening on mitigation of SCC by inducing compressive stress and refined grains is very interesting. This submission is well written and of high quality.(激光冲击导致的应力腐蚀裂纹延缓和减轻是非常有趣的,论文具有高质量…)”。
(3)实验研究了激光冲击对ANSI304不锈钢表面微观形貌、纳米硬度、弹性模量、残余应力和摩擦磨损性能的影响,研究结果表明激光冲击不锈钢不能明显诱导马氏体相变,获得了单次激光冲击ANSI304不锈钢表面残余应力变化和深度方向的分布规律以及激光冲击ANSI304不锈钢的复合结构特征,并揭示了复合结构的形成机理：
多次激光冲击ANSI304不锈钢不能诱导马氏体相变,其主要原因是因为激光冲击强化不锈钢过程不涉及热效应过程；激光冲击并没有提高ANSI304不锈钢的磨损性能和降低摩擦系数,相反在某些条件下激光冲击ANSI304不锈钢反而降低了不锈钢表面的磨损性能和增加了摩擦系数的不稳定性。系统研究了多次激光冲击对ANSI304不锈钢表面微观几何特征的影响,激光冲击明显增大表面波纹度,并造成波纹度尺度的双向加工纹理,纹理方向为顺搭接方向,在继承前一工艺的小微观尺度结构特征的基础上,叠加并形成新的大微观尺度结构的复合结构特征,并揭示了激光冲击ANSI304不锈钢表面复合结构的形成机理。研究成果发表在国际知名期刊Materials Science and Engineering:A (2011,528(13-14):4783-4788)上
(4)研究和分析了激光热力复合处理ANSI304不锈钢的宏观性能和断口形貌,探索激光热力复合处理工艺规律,揭示了多次激光冲击不锈钢焊接件的韧窝形成过程,这将开辟结构金属的激光热力复合再制造理论和技术的研究：
多次激光冲击强化将ANSI304不锈钢焊接接头的屈服强度提高21.79%,延伸率增长5.48%,其主要原因可能是激光冲击导致焊接接头的断裂面更明亮、无分层,韧窝分布更均匀；多次激光冲击不锈钢焊接件的韧窝形成过程为：(ⅰ)微空洞成核；(ⅱ)受外力作用微空洞生长；(ⅲ)微空洞连接；(ⅳ)在外在强载荷作用下的韧性断裂形成韧窝。采用激光雕刻和激光冲击复合处理制备了ANSI304不锈钢非光滑表面,其微观硬度、残余应力和表面粗糙度都有大幅度的提高或改善,这对提高非光滑表面的磨损性能是非常有益的。研究成果发表在国际知名期刊Materials Science and Engineering:A (2011,528(13-14):4652-4657)和Chinese Journal of Mechanical Engineering (2012,25(2):285-292)上,并获得两件授权发明专利
Laser shock processing (LSP) is a new and promising surface treatment technique, which has four notable feature:high-pressure, high-energy, ultra-fast and ultra-high strain-rate, so it has uncomparable advantages compared with conventional techniques. Although LSP can improve mechanical properties and fatigue lives of metallic components, a clear scenery between micro-structure and macro-properties of the refined layer, especially micro-structural evolution and improvement mechanism of stress corrosion resistance of low SFE metals, is still pending.
In this thesis, ANSI304stainless steel is regarded as the study subject. Four different topics were involved, i.e. the surface integrity (including residual stress, nano-hardness, elastic modulus, surface topography) of ANSI304stainless steel before and after LSP, the micro-structural evolution and grain refinement mechanism induced by LSP, stress corrosion resistance of ANSI304stainless steel induced by LSP, and laser hybrid processing of ANSI304stainless steel. Some important conclusions and innovative achievements of this work were listed as follows:
Firstly, we investigated micro-structures of ANSI304stainless steel during multiple LSP impacts were systematically, and presented micro-structural evolution along depth direction. The thesis proposed and entirely revealed grain refinement mechanism induced by plastic deformation during multiple LSP impacts on low SFE metal (such as ANSI304stainless steel) by the fact that multi-direction mechanical twins dividing the coarse grain based on the microstructure observations for the first time. Micro-structural evolution and grain refinement in ANSI304stainless steel subjected to multiple laser shock processing (LSP) impacts were investigated by means of cross-sectional optical microscopy and transmission electron microscopy observations. The plastic strain-induced grain refinement mechanism of the face-centered cubic (FCC) materials with very low stacking fault energy was identified. The micro-structure was obviously refined due to the ultra-high plastic strain induced by multiple LSP impacts. The minimum grain size in the top surface was about50-200nm. Multidirectional mechanical twin matrix (MT)-MT intersections led to grain subdivision at the top surface during multiple LSP impacts. Furthermore, a novel structure with submicron triangular blocks was found at the top surface subjected to three LSP impacts. The grain refinement process along the depth direction after multiple LSP impacts can be described as follows:(ⅰ) formation of planar dislocation arrays (PDAs) and stacking faults along multiple directions due to the pile up of dislocation lines;(ⅱ) formation of submicron triangular blocks (or irregularly shaped blocks) by the intersection of MT-MT (or MT-PDA or PDA-PDA) along multiple directions;(iii) transformation of MTs into subgrain boundaries;(iv) evolution by continuous dynamic recrystallization of subgrain boundaries to refined grain boundaries. The experimental results and analyses indicate that a high strain with an ultra-high strain rate play a crucial role in the grain refinement process of fcc materials subjected to multiple LSP impacts. The achievements have been published in the international well-known journal Acta Materialia (2010,58(16):5354-5362). The reviews thought that combined with prior reporting of the work on high-stacking fault energy FCC aluminum, the work on low stacking fault energy stainless steel made this an important collection that will be widely used. These researches has a good influence in the field of laser processing.
Secondly, we designed three types of the U-bend samples with diferent grain size and residual stress state, measured and characterized crack initiation time, crack appearance, residual stress and micro-structure for three types of U-bend samples. Based on these results, we gained the influence mechanism in combination with high-level compressive residual stress and grain refinement of LSP on stress corrosion resistance of ANSI304stainless steel. After immersion in the boiling42%MgCl2solution at143±1℃, the first type of sample cracks after an average value of16.06h, while the second type of sample cracks after an average value of110.43h. However, the third type of sample is tested for a total of300h without visible cracks in the LSPed surface, which is attributed to the combined effects of both high-level compressive residual stress and grain refinement induced by massive LP impacts. The improvement of the SCC resistance is caused by compressive residual stress and grain refinement during LP process. The compressive residual stress has a dominated beneficial effect on the SCC resistance, while tensile residual stresses has a negative effect on the SCC resistance. In addition, the refined grain can also effectively retard the SCC initiation. The above-mentioned results have been published in the international well-known journal Corrosion Science (2012,60:145-152). The reviews thought that "The effect of laser shock peening on mitigation of SCC by inducing compressive stress and refined grains is very interesting. This submission is well written and of high quality"
Thirdly, we experimentally studied the effects of LSP on surface appearance, nano-hardness, residual stress and wear performance of ANSI304stainless steel. Results showed that LSP cannot induce martensite phase transformation of ANSI304stainless steel. We obtained residual stress distribution in the sample surface and along depth direction after a single LSP impact, and revealed the formation mechanism of hybrid structure induced by LSP. Multiple LSP impacts cannot obviously induce martensite phase transformation of ANSI304stainless steel, which is due to the fact that the process of multiple LSP impacts isnot involved in laser thermal effect. Multiple LSP impacts cannot effectively improve wear performance and decrease friction coefficient of sample surface. We investigated the effects of LSP on surface geometric features of ANSI304 stainless steel. Results showed that LSP can obviously increase surface waviness, and induce dual-direction process texture. Hence, LSP can generate hybrid surface structure on the surface of ANSI304stainless steel. The above-mentioned results have been published in the international well-known journal Materials Science and Engineering:A (2011,528(13-14):4783-4788).
Finally, we studied and analyzed macro-peoperties and fracture morphologies of the treated stainless steel welded joint by LSP, and explored laser hybrid processing, and revealed the formation process of dimple in the surface of welded joint treated by multiple LSP impacts. Yield strength of welded joint treated by multiple LSP impacts was increased by21.79%, and elongation was improved by5.48%, which was attribute to more uniformly dimples and brighter without delamination splitting in the fracture surface of the welded joint induced by multiple LSP impacts. Based on the micro-structure features observed at the fracture surface, the following procedures are involved in the dimple formation process:(1) the nucleation of the microvoids;(2) the growth of these microvoids due to the effects of external force;(3) the coalescence of the microvoids;(4) the ductile fracture of the laser welded ANSI304stainless steel by multiple LSP impacts. In addition, we fabricated non-smooth surface of ANSI304stainless steel by laser engraving and LSP, and the non-smooth surface has excellent surface performances, such as micro-hardness, residual stress and surface roughness. The above-mentioned results have been published in the international well-known journal Materials Science and Engineering:A (2011,528(13-14):4652-4657) and Chinese Journal of Mechanical Engineering (2012,25(2):285-292). Three invention patents have been issued in China.
In summary, important innovative research results had been acquired in many aspects of this thesis, including the technological principles of LSP on ANSI304stainless steel, the micro-structure evolution, the micro-structural strengthening mechanism of LSP on ANSI304stainless steel by refining the coarse grain, the stress corrosion resistance, and the laser thermal-mechanical hybrid processing, etc.
本文以ANSI304不锈钢为研究对象,对激光冲击强化不锈钢表面完整性、微观结构演变和晶粒细化机制、抗应力腐蚀性能以及激光复合处理工艺进行了若干基础研究和探索,获得了以下主要结论和创新性成果：
(1)系统研究了多次激光冲击诱导ANSI304不锈钢塑性变形层不同区域的微观组织结构,获得了深度方向激光冲击诱导的微观结构演变规律,首次深入系统地揭示了以多方向机械孪晶细化表层原始粗晶为主的激光冲击强化低层错能金属晶粒细化机制和微观强化机理：
单次激光冲击ANSI304不锈钢在表面形成厚度约为900μm的塑性变形层,并且随着离冲击表面距离越远,晶粒大小逐渐增大,细化原始晶粒是以片状机械孪晶为主要形式；多次激光冲击使奥氏体不锈钢塑性变形层的晶粒明显细化,在激光冲击ANSI304不锈钢的上表面,晶粒尺寸约为100-200nm。在观测试验结果的基础上,多次激光冲击ANSI304不锈钢微观结构演变规律和晶粒细化机制为：(ⅰ)高密度的机械挛晶将原始粗晶细分为层片状挛晶/基体片；(ⅱ)多次冲击能够形成不同方向的机械挛晶将粗晶细化为斜方形、三角形形状的结构,最小可以观察到亚微米量级；(ⅲ)具有取向差结构经过再结晶演变成细化的晶粒。研究成果发表在国际知名期刊Acta Materialia (2010,58(16):5354-5362)上,评审专家认为：‘'Combined with prior reporting of the work on high-stacking fault energy FCC aluminum, the work on low stacking fault energy stainless steel makes this an important collection that will be widely used(……形成一个完整的面心立方金属激光冲击晶粒细化的微观强化机理)”,该部分研究成果在国际上产生良好的影响。
(2)设计了不同晶粒尺寸和残余应力状态的三种不同U型弯曲试样,测试和表征了143±1℃42%MgCl2溶液条件下腐蚀裂纹萌生时间、裂纹形貌、残余应力以及微观结构,获得了残余压应力和晶粒细化共同作用的激光冲击不锈钢抗应力腐蚀的作用机制：
三种不同U型弯曲试样在143±1℃42%MgCl2溶液内应力腐蚀裂纹萌生时间、裂纹形貌、残余应力以及微观结构的试验结果表明：大面积搭接激光冲击能够诱导高幅残余压应力并且细化ANSI304不锈钢表层晶粒,未处理U型试样的开裂时间约为16小时,先冲后弯U型试样的开裂时间约为110小时,而先弯后冲试样300小时浸泡都未出现腐蚀裂纹,晶粒细化和残余应力是提高ANSI304奥氏体抗腐蚀能力的两大主要因素,其中残余压应力占主导作用,晶粒细化也是抑制应力裂纹萌生和扩展的主要因素。研究成果发表在国际知名期刊Corrosion Science (2012,60:145-152)上,评审专家认为"The effect of laser shock peening on mitigation of SCC by inducing compressive stress and refined grains is very interesting. This submission is well written and of high quality.(激光冲击导致的应力腐蚀裂纹延缓和减轻是非常有趣的,论文具有高质量…)”。
(3)实验研究了激光冲击对ANSI304不锈钢表面微观形貌、纳米硬度、弹性模量、残余应力和摩擦磨损性能的影响,研究结果表明激光冲击不锈钢不能明显诱导马氏体相变,获得了单次激光冲击ANSI304不锈钢表面残余应力变化和深度方向的分布规律以及激光冲击ANSI304不锈钢的复合结构特征,并揭示了复合结构的形成机理：
多次激光冲击ANSI304不锈钢不能诱导马氏体相变,其主要原因是因为激光冲击强化不锈钢过程不涉及热效应过程；激光冲击并没有提高ANSI304不锈钢的磨损性能和降低摩擦系数,相反在某些条件下激光冲击ANSI304不锈钢反而降低了不锈钢表面的磨损性能和增加了摩擦系数的不稳定性。系统研究了多次激光冲击对ANSI304不锈钢表面微观几何特征的影响,激光冲击明显增大表面波纹度,并造成波纹度尺度的双向加工纹理,纹理方向为顺搭接方向,在继承前一工艺的小微观尺度结构特征的基础上,叠加并形成新的大微观尺度结构的复合结构特征,并揭示了激光冲击ANSI304不锈钢表面复合结构的形成机理。研究成果发表在国际知名期刊Materials Science and Engineering:A (2011,528(13-14):4783-4788)上
(4)研究和分析了激光热力复合处理ANSI304不锈钢的宏观性能和断口形貌,探索激光热力复合处理工艺规律,揭示了多次激光冲击不锈钢焊接件的韧窝形成过程,这将开辟结构金属的激光热力复合再制造理论和技术的研究：
多次激光冲击强化将ANSI304不锈钢焊接接头的屈服强度提高21.79%,延伸率增长5.48%,其主要原因可能是激光冲击导致焊接接头的断裂面更明亮、无分层,韧窝分布更均匀；多次激光冲击不锈钢焊接件的韧窝形成过程为：(ⅰ)微空洞成核；(ⅱ)受外力作用微空洞生长；(ⅲ)微空洞连接；(ⅳ)在外在强载荷作用下的韧性断裂形成韧窝。采用激光雕刻和激光冲击复合处理制备了ANSI304不锈钢非光滑表面,其微观硬度、残余应力和表面粗糙度都有大幅度的提高或改善,这对提高非光滑表面的磨损性能是非常有益的。研究成果发表在国际知名期刊Materials Science and Engineering:A (2011,528(13-14):4652-4657)和Chinese Journal of Mechanical Engineering (2012,25(2):285-292)上,并获得两件授权发明专利
Laser shock processing (LSP) is a new and promising surface treatment technique, which has four notable feature:high-pressure, high-energy, ultra-fast and ultra-high strain-rate, so it has uncomparable advantages compared with conventional techniques. Although LSP can improve mechanical properties and fatigue lives of metallic components, a clear scenery between micro-structure and macro-properties of the refined layer, especially micro-structural evolution and improvement mechanism of stress corrosion resistance of low SFE metals, is still pending.
In this thesis, ANSI304stainless steel is regarded as the study subject. Four different topics were involved, i.e. the surface integrity (including residual stress, nano-hardness, elastic modulus, surface topography) of ANSI304stainless steel before and after LSP, the micro-structural evolution and grain refinement mechanism induced by LSP, stress corrosion resistance of ANSI304stainless steel induced by LSP, and laser hybrid processing of ANSI304stainless steel. Some important conclusions and innovative achievements of this work were listed as follows:
Firstly, we investigated micro-structures of ANSI304stainless steel during multiple LSP impacts were systematically, and presented micro-structural evolution along depth direction. The thesis proposed and entirely revealed grain refinement mechanism induced by plastic deformation during multiple LSP impacts on low SFE metal (such as ANSI304stainless steel) by the fact that multi-direction mechanical twins dividing the coarse grain based on the microstructure observations for the first time. Micro-structural evolution and grain refinement in ANSI304stainless steel subjected to multiple laser shock processing (LSP) impacts were investigated by means of cross-sectional optical microscopy and transmission electron microscopy observations. The plastic strain-induced grain refinement mechanism of the face-centered cubic (FCC) materials with very low stacking fault energy was identified. The micro-structure was obviously refined due to the ultra-high plastic strain induced by multiple LSP impacts. The minimum grain size in the top surface was about50-200nm. Multidirectional mechanical twin matrix (MT)-MT intersections led to grain subdivision at the top surface during multiple LSP impacts. Furthermore, a novel structure with submicron triangular blocks was found at the top surface subjected to three LSP impacts. The grain refinement process along the depth direction after multiple LSP impacts can be described as follows:(ⅰ) formation of planar dislocation arrays (PDAs) and stacking faults along multiple directions due to the pile up of dislocation lines;(ⅱ) formation of submicron triangular blocks (or irregularly shaped blocks) by the intersection of MT-MT (or MT-PDA or PDA-PDA) along multiple directions;(iii) transformation of MTs into subgrain boundaries;(iv) evolution by continuous dynamic recrystallization of subgrain boundaries to refined grain boundaries. The experimental results and analyses indicate that a high strain with an ultra-high strain rate play a crucial role in the grain refinement process of fcc materials subjected to multiple LSP impacts. The achievements have been published in the international well-known journal Acta Materialia (2010,58(16):5354-5362). The reviews thought that combined with prior reporting of the work on high-stacking fault energy FCC aluminum, the work on low stacking fault energy stainless steel made this an important collection that will be widely used. These researches has a good influence in the field of laser processing.
Secondly, we designed three types of the U-bend samples with diferent grain size and residual stress state, measured and characterized crack initiation time, crack appearance, residual stress and micro-structure for three types of U-bend samples. Based on these results, we gained the influence mechanism in combination with high-level compressive residual stress and grain refinement of LSP on stress corrosion resistance of ANSI304stainless steel. After immersion in the boiling42%MgCl2solution at143±1℃, the first type of sample cracks after an average value of16.06h, while the second type of sample cracks after an average value of110.43h. However, the third type of sample is tested for a total of300h without visible cracks in the LSPed surface, which is attributed to the combined effects of both high-level compressive residual stress and grain refinement induced by massive LP impacts. The improvement of the SCC resistance is caused by compressive residual stress and grain refinement during LP process. The compressive residual stress has a dominated beneficial effect on the SCC resistance, while tensile residual stresses has a negative effect on the SCC resistance. In addition, the refined grain can also effectively retard the SCC initiation. The above-mentioned results have been published in the international well-known journal Corrosion Science (2012,60:145-152). The reviews thought that "The effect of laser shock peening on mitigation of SCC by inducing compressive stress and refined grains is very interesting. This submission is well written and of high quality"
Thirdly, we experimentally studied the effects of LSP on surface appearance, nano-hardness, residual stress and wear performance of ANSI304stainless steel. Results showed that LSP cannot induce martensite phase transformation of ANSI304stainless steel. We obtained residual stress distribution in the sample surface and along depth direction after a single LSP impact, and revealed the formation mechanism of hybrid structure induced by LSP. Multiple LSP impacts cannot obviously induce martensite phase transformation of ANSI304stainless steel, which is due to the fact that the process of multiple LSP impacts isnot involved in laser thermal effect. Multiple LSP impacts cannot effectively improve wear performance and decrease friction coefficient of sample surface. We investigated the effects of LSP on surface geometric features of ANSI304 stainless steel. Results showed that LSP can obviously increase surface waviness, and induce dual-direction process texture. Hence, LSP can generate hybrid surface structure on the surface of ANSI304stainless steel. The above-mentioned results have been published in the international well-known journal Materials Science and Engineering:A (2011,528(13-14):4783-4788).
Finally, we studied and analyzed macro-peoperties and fracture morphologies of the treated stainless steel welded joint by LSP, and explored laser hybrid processing, and revealed the formation process of dimple in the surface of welded joint treated by multiple LSP impacts. Yield strength of welded joint treated by multiple LSP impacts was increased by21.79%, and elongation was improved by5.48%, which was attribute to more uniformly dimples and brighter without delamination splitting in the fracture surface of the welded joint induced by multiple LSP impacts. Based on the micro-structure features observed at the fracture surface, the following procedures are involved in the dimple formation process:(1) the nucleation of the microvoids;(2) the growth of these microvoids due to the effects of external force;(3) the coalescence of the microvoids;(4) the ductile fracture of the laser welded ANSI304stainless steel by multiple LSP impacts. In addition, we fabricated non-smooth surface of ANSI304stainless steel by laser engraving and LSP, and the non-smooth surface has excellent surface performances, such as micro-hardness, residual stress and surface roughness. The above-mentioned results have been published in the international well-known journal Materials Science and Engineering:A (2011,528(13-14):4652-4657) and Chinese Journal of Mechanical Engineering (2012,25(2):285-292). Three invention patents have been issued in China.
In summary, important innovative research results had been acquired in many aspects of this thesis, including the technological principles of LSP on ANSI304stainless steel, the micro-structure evolution, the micro-structural strengthening mechanism of LSP on ANSI304stainless steel by refining the coarse grain, the stress corrosion resistance, and the laser thermal-mechanical hybrid processing, etc.
引文
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