采用HEBM-SPS制备430L纳米晶不锈钢材料的研究
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摘要
本文首先研究了高能球磨制备430L不锈钢纳米晶粉末,利用X射线衍射(XRD)、扫描电子显微镜(SEM)和马尔文激光粒度分析仪(MS2000)等手段分析了高能球磨中粉末的晶粒尺寸、颗粒形貌和粒度。采用相同的球磨时间(10h)不同球料比进行了430L不锈钢的球磨实验。研究结果发现:随球料比增大,粉末平均晶粒尺寸迅速减小,球料比从5:1增加到20:1,晶粒尺寸从32nm减小到23nm左右;球料比进一步增大,晶粒尺寸缓慢减小,球料比增大到30:1,晶粒尺寸约为19nm。采用相同球料比(20:1),经过不同球磨时间制备430L不锈钢粉末的实验研究结果表明:球磨初期(0～10h),粉末的晶粒尺寸迅速减小到23nm左右,其后晶粒尺寸缓慢减小,球磨时间达到50h,晶粒尺寸减小到15nm。SEM和MS2000分析结果表明,高能球磨中存在冷焊、断裂和加工硬化现象。粉末粒度的变化可分为四个阶段:即第一阶段,快速增大阶段(0～10h),平均粒度迅速增大到330μm左右,这期间以冷焊作用为主;第二阶段,快速减小阶段(10～20h),平均粒度约为100μm,这期间以断裂作用为主;第三阶段,粒度基本保持不变(20～30h),平均粒度约为98μm,这期间冷焊和断裂作用基本保持动态平衡;第四阶段,缓慢减小(30～50h),平均粒度约为55μm,这期间又以断裂作用为主。
本文还研究了纳米430L不锈钢粉末(球料比20:1,球磨时间30h)的SPS放电等离子快速烧结工艺。利用阿基米德排水法、维氏硬度计和MTS810材料试验机等手段分析了不同烧结工艺条件下烧结试样的相对密度、维氏硬度和抗拉强度,采用透射电子显微镜(TEM)观察了试样晶粒尺寸。将430L不锈钢粉末在800～1000℃温度范围内保温3～15min,分析结果显示,同800℃下试样相比较,烧结温度达到900℃时,试样的各项性能都有很大提高,在900℃下保温5min,试样的相对密度、维氏硬度和抗拉强度分别达到96.25%, 255HV和706MPa,而在800℃保温5min,试样的相对密度、维氏硬度和抗拉强度仅为93.83%、167HV和165MPa;温度达到1000℃时,维氏硬度和相对密度分别为501HV和98.72%,但抗拉强度却下降到522MPa;分析还发现,在900℃下保温5min和15min,试样的相对密度分别为96.25%和99.43%;保温时间对试样的抗拉强度影响显著,保温时间延长到10min时,抗拉强度达到最大值713MPa,而后减小。保温时间对试样的硬度影响较小,从3min延长到15min,维氏硬度值变化范围为238～255HV。TEM分析显示,经过SPS烧结后,试样的晶粒长大,平均晶粒尺寸约为144～345nm。
由上述研究结果得出:高能球磨制备430L纳米晶不锈钢粉末的合理球料比和球磨时间分别为20:1和20h;采用SPS放电等离子烧结,在900℃下保温5min试样具有较好的性能。
In this thesis, the preparation of 430L nanocrystalline stainless steel powders by high energy ball milling was investigated at first. The crystalline grain size was calculated according to the test results of XRD. The average particle size of milled 430L stainless steel powders were analyzed by Mastersizer 2000. The morphology and microstructure of samples was observed by SEM. The experiments for preparation of 430L nanocrystalline stainless steel powders with different weight ratio of balls to powders and the same ball milling time were performed. The research results indicated the crystalline grain size of the powders reduced rapidly with the increasing of weight ratio of balls to powders, the average crystalline grain size reduced from 32nm to 23nm as weight ratio of balls to powders increased from 5:1 to 20:1. As the weight ratio of balls to powders increased further, the crystalline grain size reduced slowly. It was 19nm as the weight ratio of balls to powders reached to 30:1. The experiments with various ball milling time and the same weight ratio of balls to powders were also performed. The research results showed that the crystalline grain size of the powders decreased drastically at the early stage (0-10h), which rapidly reduced to 23nm, then decreased slowly. After 50h ball milling, it reached to 15nm. The observation results of SEM and MS2000 indicate that cold welding, fragmentation and work harden occurred during high energy ball milling. The changes of particles size of 430L stainless steel powders could be divided into four stages: at the initial stage (0-10h), the particle size of the powders increased quickly because of cold welding, and the average particle size of the powders reached to 330μm; in the second stage(10-20h), the particle size of the powders decreased because of fragmentation, the average particle size reduced to 100μm.; in the third stage (20-30h), the particle size of the powders has less change, the average particle size was about 98μm, the dynamical equilibrium was held between cold welding and fragmentation; in the final stage(30-50h), the particle size of the powders decreased slowly, the average particle size reduced to 55μm, the dominative role was also fragmentation at this stage .
Nanocrystalline 430L stainless steel cermets produced using spark plasma sintering was also investigated. Bulk densities of the samples were determined by Archimedes method in distilled water, the hardness and the tensile strength were measured using Vickers hardness tester and MTS810 materials testing machine, the crystalline grain size was observed by TEM. Nanocrystalline 430L stainless steel powders prepared by high-energy ball milling(weight ratio of balls to powders 20:1 for ball milling time of 30h) were sintered by spark plasma sintering at 800-1000℃for holding time of 3 to 15min. Comparison with sample sintered at 800℃, the properties of samples sintered at 900℃has improved much. After having sintered at 900℃for
本文还研究了纳米430L不锈钢粉末(球料比20:1,球磨时间30h)的SPS放电等离子快速烧结工艺。利用阿基米德排水法、维氏硬度计和MTS810材料试验机等手段分析了不同烧结工艺条件下烧结试样的相对密度、维氏硬度和抗拉强度,采用透射电子显微镜(TEM)观察了试样晶粒尺寸。将430L不锈钢粉末在800～1000℃温度范围内保温3～15min,分析结果显示,同800℃下试样相比较,烧结温度达到900℃时,试样的各项性能都有很大提高,在900℃下保温5min,试样的相对密度、维氏硬度和抗拉强度分别达到96.25%, 255HV和706MPa,而在800℃保温5min,试样的相对密度、维氏硬度和抗拉强度仅为93.83%、167HV和165MPa;温度达到1000℃时,维氏硬度和相对密度分别为501HV和98.72%,但抗拉强度却下降到522MPa;分析还发现,在900℃下保温5min和15min,试样的相对密度分别为96.25%和99.43%;保温时间对试样的抗拉强度影响显著,保温时间延长到10min时,抗拉强度达到最大值713MPa,而后减小。保温时间对试样的硬度影响较小,从3min延长到15min,维氏硬度值变化范围为238～255HV。TEM分析显示,经过SPS烧结后,试样的晶粒长大,平均晶粒尺寸约为144～345nm。
由上述研究结果得出:高能球磨制备430L纳米晶不锈钢粉末的合理球料比和球磨时间分别为20:1和20h;采用SPS放电等离子烧结,在900℃下保温5min试样具有较好的性能。
In this thesis, the preparation of 430L nanocrystalline stainless steel powders by high energy ball milling was investigated at first. The crystalline grain size was calculated according to the test results of XRD. The average particle size of milled 430L stainless steel powders were analyzed by Mastersizer 2000. The morphology and microstructure of samples was observed by SEM. The experiments for preparation of 430L nanocrystalline stainless steel powders with different weight ratio of balls to powders and the same ball milling time were performed. The research results indicated the crystalline grain size of the powders reduced rapidly with the increasing of weight ratio of balls to powders, the average crystalline grain size reduced from 32nm to 23nm as weight ratio of balls to powders increased from 5:1 to 20:1. As the weight ratio of balls to powders increased further, the crystalline grain size reduced slowly. It was 19nm as the weight ratio of balls to powders reached to 30:1. The experiments with various ball milling time and the same weight ratio of balls to powders were also performed. The research results showed that the crystalline grain size of the powders decreased drastically at the early stage (0-10h), which rapidly reduced to 23nm, then decreased slowly. After 50h ball milling, it reached to 15nm. The observation results of SEM and MS2000 indicate that cold welding, fragmentation and work harden occurred during high energy ball milling. The changes of particles size of 430L stainless steel powders could be divided into four stages: at the initial stage (0-10h), the particle size of the powders increased quickly because of cold welding, and the average particle size of the powders reached to 330μm; in the second stage(10-20h), the particle size of the powders decreased because of fragmentation, the average particle size reduced to 100μm.; in the third stage (20-30h), the particle size of the powders has less change, the average particle size was about 98μm, the dynamical equilibrium was held between cold welding and fragmentation; in the final stage(30-50h), the particle size of the powders decreased slowly, the average particle size reduced to 55μm, the dominative role was also fragmentation at this stage .
Nanocrystalline 430L stainless steel cermets produced using spark plasma sintering was also investigated. Bulk densities of the samples were determined by Archimedes method in distilled water, the hardness and the tensile strength were measured using Vickers hardness tester and MTS810 materials testing machine, the crystalline grain size was observed by TEM. Nanocrystalline 430L stainless steel powders prepared by high-energy ball milling(weight ratio of balls to powders 20:1 for ball milling time of 30h) were sintered by spark plasma sintering at 800-1000℃for holding time of 3 to 15min. Comparison with sample sintered at 800℃, the properties of samples sintered at 900℃has improved much. After having sintered at 900℃for
引文
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