CN112404425A - 一种高强度12Cr钢及其制备方法 - Google Patents
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Abstract
本发明公开一种高强度12Cr钢及其制备方法。先用放电等离子烧结方法制备出成分Fe‑12Cr‑1Mo‑1.1W‑1Mn‑0.2V‑0.15Ta‑0.03Ti‑0.1C‑0.07N‑0.15Si‑0.4Y2O3的样品，再将样品进行热轧，轧制前保温时间为30‑60min，保温温度为1100℃‑1200℃。轧制速度为100m/s‑200m/s，变形量为75%‑90%。将轧制后的样品在1000‑1200℃下进行30‑60min的退火处理，即可得到晶粒尺寸为50nm‑200μm的组织，硬度最高可达到565HV。
Description
技术领域
能源是人类生存和发展的物质基础，随着国民经济的发展和人民生活水平的较快提高，人类对能源的需求量越来越大。现在大多数专家认为，核能是目前唯一现实的、可大规模代替化石燃料的能源。而在核电发展的近几十年里，快堆燃料包壳材料先后出现了多种不同候选材料。如：奥氏体不锈钢（304和316型不锈钢）、Zr合金、ODS钢和铁素体/马氏体钢等。
氧化物弥散强化钢制备主要包括机械合金化、SPS烧结成型、热变形加工以及后续热处理等步骤。含Y的弥散氧化物具有较强的抗辐照分解能力，添加Y2O3的合金也具有更好的高温强度和抗氧化层剥落性能。这种弥散分布的氧化物颗粒可以阻碍位错运动，起到弥散强化的作用，提高合金的高温强度，其应用温度可达600℃。热轧能改善金属及合金的加工工艺性能,即将铸造状态的粗大晶粒破碎,显著裂纹愈合,减少或消除铸造缺陷,将铸态组织转变为变形组织,提高合金的加工性能。但是热轧后，材料内部会沿着轧制方向拉成薄片形成板条状结构，导致材料内部应变不均匀。而一定温度的热处理一般情况下会降低材料硬度，改善切削加工性；降低残余应力，稳定尺寸，减少变形与裂纹倾向；均匀化晶粒，调整组织，消除组织缺陷，提高材料的力学性能。
发明内容
本发明公开一种高强度12Cr 钢及其制备方法，利用放电等离子烧结技术制备出成分为Fe-12Cr-1Mo-1.1W-1Mn-0.2V-0.15Ta-0.03Ti-0.1C-0.07N-0.15Si-0.4Y2O3 的样品。本发明通过适当的热变形及热处理工艺, 得到不同的12Cr 钢的微观组织及相应的材料强度。
为实现上述目的，本发明提供如下技术方案：
1）本发明使用高纯Fe粉、Cr粉、Mo粉、W粉、Mn粉、V粉、Ta粉、Ti粉、C粉、N粉、Si粉和Y粉为基体，按照合金成分Fe-12Cr-1Mo-1.1W-1Mn-0.2V-0.15Ta-0.03Ti-0.1C-0.07N-0.15Si-0.4Y2O3 (质量分数% )比例混合。混合后的金属粉末在行星式高能研磨机中通过球磨完成机械合金化过程。球磨后的合金粉末经SPS烧结成块体，烧结时间为5 min、烧结压力40MPa、烧结温度为1050 ℃并随炉冷却至室温。烧结能够使粉末颗粒之间发生粘结，增加烧结体的强度，把粉末颗粒的聚集体变成为晶粒的聚结体，从而获得较强的物理、机械性能的制品。
所述样品Fe-12Cr-1Mo-1.1W-1Mn-0.2V-0.15Ta-0.03Ti-0.1C-0.07N-0.15Si-0.4Y2O3 中
Fe、Cr、Mo、W、Mn、V、Ta、Ti、C、N、Si和Y2O3的质量比为1:12:1:1.1:1：0.2:0.15:0.03:0.1:0.07:0.15:0.4。
2)轧制前保温时间为30-60min，保温温度为1100℃-1200℃。从热处理炉中取出样品完成热轧，轧制速度为100m/s-200m/s，总变形量为75%-90%。热轧会将烧结态的粗大晶粒破碎，显著裂纹愈合，减少或消除烧结缺陷，将烧结态组织转变为变形组织并进一步细化晶粒，均匀材料尺寸分布。
3)将轧制后的样品在1000-1200℃下退火处理30-60min，即可得到晶粒尺寸为50nm-200μm的样品。退火的目的是为了消除内应力，使变形晶粒发生回复再结晶使材料内部组织均匀化，通过控制退火参数，可减少晶粒内部形变带，提高材料的强度。
有益效果：本发明通过适当的热变形及热处理工艺, 得到不同的12Cr 钢的微观组织及相应的材料强度。
附图说明
图1为85%变形1000℃空冷的显微组织图；
图2为75%变形1200℃空冷的显微组织图；
图3为90变形1200℃水冷的显微组织图；
图4为三种实施例的的硬度对比图。
具体实施方式
下面对本发明的实施例作详细说明，本实施例在以本发明技术方案为前提下进行实施，给出了详细的实施方式和具体操作过程，但本发明的保护范围不限于下述的实施例。
实施例一：（1000℃空冷 85%）
使用高纯Fe粉、Cr粉、Mo粉、W粉、Mn粉、V粉、Ta粉、Ti粉、C粉、N粉、Si粉和Y粉为基体，按照合金成分Fe-12Cr-1Mo-1.1W-1Mn-0.2V-0.15Ta-0.03Ti-0.1C-0.07N-0.15Si-0.4Y2O3 (质量分数%) 比例混合。混合后的金属粉末在行星式高能研磨机中通过球磨完成机械合金化过程。球磨后的合金粉末经放电等离子烧结成块体，烧结时间为5min、烧结压力40 MPa、烧结温度为1050℃，随炉冷却至室温。随后样品在1200℃热处理炉中保温60min。从热处理炉中取出样品完成热轧。轧制速度为200m/s，变形量约为85%。将轧制后的样品在1000℃下退火保温60min并进行空冷，即可得到晶粒尺寸为50nm-200μm混晶组织样品，如图1所示，其硬度值为274.5HV。
实施例二（1200℃空冷 75%）
使用高纯Fe粉、Cr粉、Mo粉、W粉、Mn粉、V粉、Ta粉、Ti粉、C粉、N粉、Si粉和Y粉为基体，按照金成分Fe-12Cr-1Mo-1.1W-1Mn-0.2V-0.15Ta-0.03Ti-0.1C-0.07N-0.15Si-0.4Y2O3 (质量分数%) 比例混合。混合后的金属粉末在行星式高能研磨机中通过球磨完成机械合金化过程。球磨后的合金粉末经放电等离子烧结成块体，烧结时间为5min、烧结压力40 MPa、烧结温度为1050℃，随炉冷却至室温。随后样品在1200℃热处理炉中保温60min。从热处理炉中取出样品完成热轧。轧制速度为100m/s，变形量约为75%。将轧制后的样品在1200℃下退火处理60min并进行空冷，即可得到晶粒尺寸为50μm的等轴晶组织样品，如图2所示，其硬度值为565.0HV。
实施例三（1200℃水冷 90%）
使用高纯Fe粉、Cr粉、Mo粉、W粉、Mn粉、V粉、Ta粉、Ti粉、C粉、N粉、Si粉和Y粉为基体，按照金成分Fe-12Cr-1Mo-1.1W-1Mn-0.2V-0.15Ta-0.03Ti-0.1C-0.07N-0.15Si-0.4Y2O3 (质量分数%) 比例混合。混合后的金属粉末在行星式高能研磨机中通过球磨完成机械合金化过程。球磨后的合金粉末经放电等离子烧结成块体，烧结时间为5min、烧结压力40 MPa、烧结温度为1050℃，随炉冷却至室温。随后样品在热处理炉中于1300℃加热30min。从热处理炉中取出样品完成热轧。轧制速度为150m/s，变形量约为90%。将轧制后的样品在1100℃下退火处理60min并进行水冷，即可得到晶粒尺寸为30-60μm的混晶组织样品，如图3所示，其硬度值为455.5HV。
对比例一：（1000℃空冷 60%）
使用高纯Fe粉、Cr粉、Mo粉、W粉、Mn粉、V粉、Ta粉、Ti粉、C粉、N粉、Si粉和Y粉为基体，按照合金成分Fe-12Cr-1Mo-1.1W-1Mn-0.2V-0.15Ta-0.03Ti-0.1C-0.07N-0.15Si-0.4Y2O3 比例混合。混合后的金属粉末在行星式高能研磨机中通过球磨完成机械合金化过程。球磨后的合金粉末经放电等离子烧结成块体，烧结时间为5min、烧结压力40 MPa、烧结温度为1050℃，随炉冷却至室温。随后样品在1200℃热处理炉中保温60min。从热处理炉中取出样品完成热轧。轧制速度为200m/s，变形量约为60%。将轧制后的样品在1000℃下退火保温60min并进行空冷，即可得到晶粒尺寸为50nm-200μm混晶组织样品，如图1所示，其硬度值为174.5HV。
对比例二（800℃空冷 75%）
使用高纯Fe粉、Cr粉、Mo粉、W粉、Mn粉、V粉、Ta粉、Ti粉、C粉、N粉、Si粉和Y粉为基体，按照金成分Fe-12Cr-1Mo-1.1W-1Mn-0.2V-0.15Ta-0.03Ti-0.1C-0.07N-0.15Si-0.4Y2O3 (质量分数%) 比例混合。混合后的金属粉末在行星式高能研磨机中通过球磨完成机械合金化过程。球磨后的合金粉末经放电等离子烧结成块体，烧结时间为5min、烧结压力40 MPa、烧结温度为1050℃，随炉冷却至室温。随后样品在1200℃热处理炉中保温60min。从热处理炉中取出样品完成热轧。轧制速度为100m/s，变形量约为75%。将轧制后的样品在1200℃下退火处理60min并进行空冷，即可得到晶粒尺寸为50μm的等轴晶组织样品，如图2所示，其硬度值为170.5HV。
对比例三（1200℃水冷 60%）
使用高纯Fe粉、Cr粉、Mo粉、W粉、Mn粉、V粉、Ta粉、Ti粉、C粉、N粉、Si粉和Y粉为基体，按照金成分Fe-12Cr-1Mo-1.1W-1Mn-0.2V-0.15Ta-0.03Ti-0.1C-0.07N-0.15Si-0.4Y2O3 (质量分数%) 比例混合。混合后的金属粉末在行星式高能研磨机中通过球磨完成机械合金化过程。球磨后的合金粉末经放电等离子烧结成块体，烧结时间为5min、烧结压力40 MPa、烧结温度为1050℃，随炉冷却至室温。随后样品在热处理炉中于1300℃加热30min。从热处理炉中取出样品完成热轧。轧制速度为150m/s，变形量约为90%。将轧制后的样品在1100℃下退火处理60min并进行水冷，即可得到晶粒尺寸为30-60μm的混晶组织样品，如图3所示，其硬度值为360.5HV。
以上所述仅为本发明的较佳实施例，凡依本发明申请专利范围所做的均等变化与修饰，皆应属本发明的涵盖范围。
Claims (6)
1.一种高强度12Cr 钢的制备方法，其特征在于：具体包括以下步骤：
（1）12Cr 钢放电等离子烧结制备工艺：使用高纯Fe粉、Cr粉、Mo粉、W粉、Mn粉、V粉、Ta粉、Ti粉、C粉、N粉、Si粉和Y粉为基体，混合后的金属粉末通过球磨完成机械合金化过程，球磨后的合金粉末经放电等离子烧结成块体，并随炉冷却至室温，制备出Fe-12Cr-1Mo-1.1W-1Mn-0.2V-0.15Ta-0.03Ti-0.1C-0.07N-0.15Si-0.4Y2O3 样品；
（2）12Cr 钢轧制工艺：将步骤（1）的块体放在热处理炉中保温后进行轧制变形；
（3）12Cr 钢退火工艺：将轧制后的样品在1000-1200℃下进行30-60min的退火处理得到高强度12Cr 钢。
2.根据权利要求1所述的高强度12Cr 钢的制备方法，其特征在于：所述样品Fe-12Cr-1Mo-1.1W-1Mn-0.2V-0.15Ta-0.03Ti-0.1C-0.07N-0.15Si-0.4Y2O3 中Fe、Cr、Mo、W、Mn、V、Ta、Ti、C、N、Si和Y2O3的质量比为1:12:1:1.1:1：0.2:0.15:0.03:0.1:0.07:0.15:0.4。
3.根据权利要求1所述的高强度12Cr 钢的制备方法，其特征在于：步骤（1）所述烧结温度为1050℃，烧结压力为40MPa，烧结时间为5min。
4.根据权利要求1所述的高强度12Cr 钢的制备方法，其特征在于：步骤（2）所述保温时间为30-60min，保温温度为1200-1300℃。
5.根据权利要求1所述的高强度12Cr 钢的制备方法，其特征在于：步骤（2）所述轧制速度为100-200m/s，变形量为75%-90%。
6.一种如权利要求1-5任一项所述12Cr 钢的制备方法制得的高强度12Cr 钢，其特征在于：所述高强度12Cr 钢中晶粒尺寸为50nm-200μm的组织，硬度最高达到565HV。
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