不锈钢粉末选择性激光烧结/等静压复合成形技术研究
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摘要
选择性激光烧结(Selective Laser Sintering, SLS)技术是快速成形(Rapid Prototyping,RP)领域发展较成熟与应用较广泛的技术之一,一直受到国内外重视。但是通过SLS技术制造金属零件,存在致密度低与力学性能差等缺陷,严重限制了其发展与应用。尽管近年来国内外研究通过熔渗金属等方法提高SLS零件的致密度,但是其力学性能依然难以满足使用要求。针对上述问题,为了制造高致密高性能复杂不锈钢零件,本论文将等静压(Isostatic Pressure, IP)技术引入SLS领域,形成SLS/IP复合成形技术。采用SLS/IP技术制造AISI304与AISI316L不锈钢零件,通过TG热分析、X射线衍射(XRD)、SEM以及力学性能检测等手段研究AISI304与AISI316L SLS/IP零件致密化机理、金相组织与力学性能;在脱脂后续处理阶段零件各向收缩相同条件下,建立各环节尺寸精度数学物理模型,为进一步研究其尺寸精度奠定理论基础。主要研究内容与结论如下:
(1)研究了AISI304与AISI316L不锈钢粉末SLS成形与热脱脂机理及其工艺。针对本论文非晶态高聚物环氧树脂E12与晶态高聚物尼龙PA12两种粘结剂,采取混合法与覆膜法制取了上述两种SLS不锈钢复合材料,确定了相应最佳SLS成形工艺参数(预热温度、激光功率、扫描速度、扫描间距与单层层厚)分别为50-55℃、19-20W、1900-2000mm/s、0.1-0.12mm/s、0.1-0.12mm与150-165℃、15-17W、1800-2000mm/s、0.1-0.15mm、0.1-0.15mm;根据热脱脂机理以及E12和PA12的TG曲线,制定了合理的热脱脂工艺。
(2)研究了SLS/冷等静压(Cold Isostatic Pressure, CIP)包套材料(天然橡胶胶乳与硅橡胶),提出将天然橡胶胶乳运用到SLS/CIP工艺。相对于硅橡胶,天然橡胶胶乳成膜性较好,并且能够随形密封复杂SLS零件,适用于SLS/CIP包套制作。
(3)研究了AISI304与AISI316L SLS零件的热脱脂后续处理机理与工艺,以及相应工艺参数对其致密度与性能的影响规律,并提出其SLS/CIP致密化机理与最小SLS/CIP阀值思想。其中,根据CIP理论与SLS脱脂多孔材料特性,上述不锈钢SLS/CIP致密化机理为烧结颈破碎、金属颗粒重排与塑性变形综合作用;针对AISI304不锈钢脱脂试样,最小SLS/CIP阀值为400MPa;在经过650MPa CIP、1350℃高温烧结与1200℃/120MPa热等静压(Hold Isostatic Pressure, HIP)处理后,其致密度分别
达到86%、95%与98%;并且,其SLS/HIP试样的弹性模量、屈服强度、拉伸强度与延伸率分别达到93.15GPa、306MPa、577.5MPa与32.05%,力学性能与固溶处理AISI304致密材料相当;针对AISI316L不锈钢脱脂试样,最小SLS/CIP阀值为300MPa;在1320℃高温烧结与1250℃/120MPa HIP处理后,其致密度超过95%;同时,其弹性模量、屈服强度、拉伸强度与延伸率分别达到142.5GPa、277MPa、649.49MPa与45.7%。
(4)在高温烧结与HIP环节,研究了微量Cu与FeB对AISI304试样致密度、弹性模量、屈服强度、拉伸强度与延伸率的影响规律,以及微量Si与FeMn对AISI316L试样致密度、弹性模量、屈服强度、拉伸强度与延伸率的影响规律。根据液相烧结理论与XRD检测方法,微量Cu与FeB均能提高AISI304 SLS/IP试样致密度,并且,当Cu含量从1%增加到3%时,在奥氏体基体上析出NixCuy固溶体,致使其力学性能逐渐改善,当FeB含量从0.5%增加到5%,Fe-B与Ni-B低熔共晶物沿晶界析出,致使其力学性能逐渐降低;微量Si与FeMn可提高AISI316L SLS/IP试样致密度,但在SLS/CIP后续处理中,Si容易导致碳化铬沿晶界析出,致使其力学性能降低,但是微量FeMn可改善其力学性能。
(5)研究了SLS/IP制件在各环节上尺寸精度变化规律与控制措施以及脱脂后续处理尺寸精度数学物理模型。主要提出了SLS/CIP环节尺寸精度数学物理模型高温烧结环节尺寸精度数学物理模型HIP环节尺寸精度数学物理模型
综上所述,通过SLS/IP技术解决了SLS零件致密度低与力学性能差等缺陷,完善了SLS技术,拓宽了其应用领域,为制造高致密高性能高精度复杂金属零件奠定了技术基础。
At present, Selective Laser Sintering (SLS) is a more developed and widely applied technology of Rapid Prototyping (RP), so it has been paid attention to by researchers all along in the world. But relative density of SLS parts is often lower and their mechanical performance is worse so as to hinder its development and application strongly. Although relative density of SLS parts was improved by infiltrating lower melting point metal in the past, their mechanical didn’t still meet requirements. In order to manufacture high relative density, better mechanical performance and complicated parts, Isostatic pressure (IP) technology is introduced into SLS which is named as SLS/IP technology. Complicated AISI304 and AISI316L metal parts are manufactured by SLS/IP, then densification mechanism, metallurgical structure and mechanical performances of AISI304 and AISI316L SLS/IP metal parts are analyzed by TG, XRD, SEM and tension test etc. Their mathematic physics models of dimensional precision are derived under SLS parts evenly shrinking in degreasing process, CIP, high sintering and HIP, so the theory is established for analyzing the dimensional precisions of SLS samples further. Main research contents and conclusions are below.
(1) Mechanisms of SLS forming and thermal degreasing about AISI304 and AISI316L powders are investigated with their technology parameters. Mixed and coated composites of SLS are manufactured by resin E12 and nylon PA12, and optimized SLS technology parameters are determined, which include preheat temperature, laser power, scan speed, can interval and layer thickness. They are respectively 50-55℃,19-20W, 1900-2000mm/s, 0.1-0.12mm,0.1-0.12mm and 150-165℃, 15-17W, 1800-2000mm/s, 0.1-0.15mm, 0.1-0.15mm/s.According to thermal degreasing mechanism and TG curves of E12 and PA12, their thermal degreasing technologies of SLS prototype are set up.
(2) Canning materials used in SLS/Cold Isostatic Pressing (CIP) are investigated, which include natural rubber latex and silicon rubber, and natural rubber latex is firstly introduced into SLS/CIP. Compared with silicon rubber, complicated SLS parts could be sealed by natural rubber latex, which films more easily and is suitable for SLS/CIP canning material.
(3) Mechanisms and technologies of AISI304 and AISI316L parts after thermal degreasing are investigated with effects of their technology parameters on them, and their densification mechanics of SLS/CIP and minimal SLS/CIP threshold are brought forward. Thereinto, according to CIP theory and property of SLS degreasing part, densification mechanics of above stainless steel SLS/CIP parts is sintering neck crushing, metal rearranging and its plastic deformation. The threshold of SLS/CIP pressure is 400MPa when AISI304 degreasing part is CIPped. After CIP of 650MPa, high sintering of 1350℃and HIP of 1200℃/120MPa, relative density of AISI304 part is 86%, 95% and 98% respectively, and its mechanical performance is Young’s modulus of 93.15GPa, yield strength of 306MPa, tension strength of 577.5MPa and elongation percentage of 32.05%, which are close to solution treatment AISI304 dense material. The threshold of SLS/CIP pressure is 300MPa when AISI316L degreasing part is CIPped. After subsequent high sintering of 1320℃and HIP of 1250℃/120MPa, its relative density Its relative density is over 95%, and its mechanical performance is Young’s modulus of 142.5GPa, yield strength of 277MPa, tension strength of 649.49MPa and elongation percentage of 45.7%.
(4) Effects of Cu and FeB on relative density, Young’s modulus, yield strength, tension strength and elongation percentage of AISI304 parts are investigated in high sintering and HIP with effects of Si and FeMn on relative density, Young’s modulus, yield strength, tension strength and elongation percentage of AISI316L parts. According to liquid sintering and XRD, relative density of SLS/IP AISI304 parts could be improved. NixCuy solid solution is precipitated in austenite with mechanical performances improving when content of of Cu increases from 1% to 3%, and eutectics of Fe-B and Ni-B are precipitated along grain boundary so that their mechanical performances worsen gradually when content of of FeB increases from 0.5% to 5%. In addition, relative density of AISI316L SLS/IP parts could be improved gradually with addition of Si and FeMn, but Cr23C6 is precipitated along grain boundary with addition of Si so as to worsen their mechanical performances, but their mechanical performances could be improved with addition of FeMn in high sintering and HIP.
(5) Dimensional precision of SLS part in each process in SLS/IP are investigated, corresponding solved methods being introduced, and mathematic physics models of dimensional precision are brought forward after degreasing. Mathematic physics models of dimensional precision in SLS/CIP, high sintering and HIP are maily brought forward, which are respectively and
hi eonelusion，lower relative density and worse meehanieal Performanee of SLS Partshave been avoided by SLS/I P，whleh imProves SLS，俪dens aPPlieation domain of SLSand establishes foundation for manufaeturing dense，high Performanee，high definition andeomPlieated metal Parts.
(1)研究了AISI304与AISI316L不锈钢粉末SLS成形与热脱脂机理及其工艺。针对本论文非晶态高聚物环氧树脂E12与晶态高聚物尼龙PA12两种粘结剂,采取混合法与覆膜法制取了上述两种SLS不锈钢复合材料,确定了相应最佳SLS成形工艺参数(预热温度、激光功率、扫描速度、扫描间距与单层层厚)分别为50-55℃、19-20W、1900-2000mm/s、0.1-0.12mm/s、0.1-0.12mm与150-165℃、15-17W、1800-2000mm/s、0.1-0.15mm、0.1-0.15mm;根据热脱脂机理以及E12和PA12的TG曲线,制定了合理的热脱脂工艺。
(2)研究了SLS/冷等静压(Cold Isostatic Pressure, CIP)包套材料(天然橡胶胶乳与硅橡胶),提出将天然橡胶胶乳运用到SLS/CIP工艺。相对于硅橡胶,天然橡胶胶乳成膜性较好,并且能够随形密封复杂SLS零件,适用于SLS/CIP包套制作。
(3)研究了AISI304与AISI316L SLS零件的热脱脂后续处理机理与工艺,以及相应工艺参数对其致密度与性能的影响规律,并提出其SLS/CIP致密化机理与最小SLS/CIP阀值思想。其中,根据CIP理论与SLS脱脂多孔材料特性,上述不锈钢SLS/CIP致密化机理为烧结颈破碎、金属颗粒重排与塑性变形综合作用;针对AISI304不锈钢脱脂试样,最小SLS/CIP阀值为400MPa;在经过650MPa CIP、1350℃高温烧结与1200℃/120MPa热等静压(Hold Isostatic Pressure, HIP)处理后,其致密度分别
达到86%、95%与98%;并且,其SLS/HIP试样的弹性模量、屈服强度、拉伸强度与延伸率分别达到93.15GPa、306MPa、577.5MPa与32.05%,力学性能与固溶处理AISI304致密材料相当;针对AISI316L不锈钢脱脂试样,最小SLS/CIP阀值为300MPa;在1320℃高温烧结与1250℃/120MPa HIP处理后,其致密度超过95%;同时,其弹性模量、屈服强度、拉伸强度与延伸率分别达到142.5GPa、277MPa、649.49MPa与45.7%。
(4)在高温烧结与HIP环节,研究了微量Cu与FeB对AISI304试样致密度、弹性模量、屈服强度、拉伸强度与延伸率的影响规律,以及微量Si与FeMn对AISI316L试样致密度、弹性模量、屈服强度、拉伸强度与延伸率的影响规律。根据液相烧结理论与XRD检测方法,微量Cu与FeB均能提高AISI304 SLS/IP试样致密度,并且,当Cu含量从1%增加到3%时,在奥氏体基体上析出NixCuy固溶体,致使其力学性能逐渐改善,当FeB含量从0.5%增加到5%,Fe-B与Ni-B低熔共晶物沿晶界析出,致使其力学性能逐渐降低;微量Si与FeMn可提高AISI316L SLS/IP试样致密度,但在SLS/CIP后续处理中,Si容易导致碳化铬沿晶界析出,致使其力学性能降低,但是微量FeMn可改善其力学性能。
(5)研究了SLS/IP制件在各环节上尺寸精度变化规律与控制措施以及脱脂后续处理尺寸精度数学物理模型。主要提出了SLS/CIP环节尺寸精度数学物理模型高温烧结环节尺寸精度数学物理模型HIP环节尺寸精度数学物理模型
综上所述,通过SLS/IP技术解决了SLS零件致密度低与力学性能差等缺陷,完善了SLS技术,拓宽了其应用领域,为制造高致密高性能高精度复杂金属零件奠定了技术基础。
At present, Selective Laser Sintering (SLS) is a more developed and widely applied technology of Rapid Prototyping (RP), so it has been paid attention to by researchers all along in the world. But relative density of SLS parts is often lower and their mechanical performance is worse so as to hinder its development and application strongly. Although relative density of SLS parts was improved by infiltrating lower melting point metal in the past, their mechanical didn’t still meet requirements. In order to manufacture high relative density, better mechanical performance and complicated parts, Isostatic pressure (IP) technology is introduced into SLS which is named as SLS/IP technology. Complicated AISI304 and AISI316L metal parts are manufactured by SLS/IP, then densification mechanism, metallurgical structure and mechanical performances of AISI304 and AISI316L SLS/IP metal parts are analyzed by TG, XRD, SEM and tension test etc. Their mathematic physics models of dimensional precision are derived under SLS parts evenly shrinking in degreasing process, CIP, high sintering and HIP, so the theory is established for analyzing the dimensional precisions of SLS samples further. Main research contents and conclusions are below.
(1) Mechanisms of SLS forming and thermal degreasing about AISI304 and AISI316L powders are investigated with their technology parameters. Mixed and coated composites of SLS are manufactured by resin E12 and nylon PA12, and optimized SLS technology parameters are determined, which include preheat temperature, laser power, scan speed, can interval and layer thickness. They are respectively 50-55℃,19-20W, 1900-2000mm/s, 0.1-0.12mm,0.1-0.12mm and 150-165℃, 15-17W, 1800-2000mm/s, 0.1-0.15mm, 0.1-0.15mm/s.According to thermal degreasing mechanism and TG curves of E12 and PA12, their thermal degreasing technologies of SLS prototype are set up.
(2) Canning materials used in SLS/Cold Isostatic Pressing (CIP) are investigated, which include natural rubber latex and silicon rubber, and natural rubber latex is firstly introduced into SLS/CIP. Compared with silicon rubber, complicated SLS parts could be sealed by natural rubber latex, which films more easily and is suitable for SLS/CIP canning material.
(3) Mechanisms and technologies of AISI304 and AISI316L parts after thermal degreasing are investigated with effects of their technology parameters on them, and their densification mechanics of SLS/CIP and minimal SLS/CIP threshold are brought forward. Thereinto, according to CIP theory and property of SLS degreasing part, densification mechanics of above stainless steel SLS/CIP parts is sintering neck crushing, metal rearranging and its plastic deformation. The threshold of SLS/CIP pressure is 400MPa when AISI304 degreasing part is CIPped. After CIP of 650MPa, high sintering of 1350℃and HIP of 1200℃/120MPa, relative density of AISI304 part is 86%, 95% and 98% respectively, and its mechanical performance is Young’s modulus of 93.15GPa, yield strength of 306MPa, tension strength of 577.5MPa and elongation percentage of 32.05%, which are close to solution treatment AISI304 dense material. The threshold of SLS/CIP pressure is 300MPa when AISI316L degreasing part is CIPped. After subsequent high sintering of 1320℃and HIP of 1250℃/120MPa, its relative density Its relative density is over 95%, and its mechanical performance is Young’s modulus of 142.5GPa, yield strength of 277MPa, tension strength of 649.49MPa and elongation percentage of 45.7%.
(4) Effects of Cu and FeB on relative density, Young’s modulus, yield strength, tension strength and elongation percentage of AISI304 parts are investigated in high sintering and HIP with effects of Si and FeMn on relative density, Young’s modulus, yield strength, tension strength and elongation percentage of AISI316L parts. According to liquid sintering and XRD, relative density of SLS/IP AISI304 parts could be improved. NixCuy solid solution is precipitated in austenite with mechanical performances improving when content of of Cu increases from 1% to 3%, and eutectics of Fe-B and Ni-B are precipitated along grain boundary so that their mechanical performances worsen gradually when content of of FeB increases from 0.5% to 5%. In addition, relative density of AISI316L SLS/IP parts could be improved gradually with addition of Si and FeMn, but Cr23C6 is precipitated along grain boundary with addition of Si so as to worsen their mechanical performances, but their mechanical performances could be improved with addition of FeMn in high sintering and HIP.
(5) Dimensional precision of SLS part in each process in SLS/IP are investigated, corresponding solved methods being introduced, and mathematic physics models of dimensional precision are brought forward after degreasing. Mathematic physics models of dimensional precision in SLS/CIP, high sintering and HIP are maily brought forward, which are respectively and
hi eonelusion，lower relative density and worse meehanieal Performanee of SLS Partshave been avoided by SLS/I P，whleh imProves SLS，俪dens aPPlieation domain of SLSand establishes foundation for manufaeturing dense，high Performanee，high definition andeomPlieated metal Parts.
引文
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