CN111230115A - 一种微米银颗粒增强316l不锈钢基复合材料及其制备方法 - Google Patents

一种微米银颗粒增强316l不锈钢基复合材料及其制备方法 Download PDF

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CN111230115A
CN111230115A CN202010153865.7A CN202010153865A CN111230115A CN 111230115 A CN111230115 A CN 111230115A CN 202010153865 A CN202010153865 A CN 202010153865A CN 111230115 A CN111230115 A CN 111230115A
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stainless steel
powder
composite material
spherical
based composite
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林开杰
顾冬冬
全景峰
方亚美
葛庆
庄杰
刘洋
董伟菘
帅朋江
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Nanjing University of Aeronautics and Astronautics
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Priority to US17/263,876 priority patent/US11946122B2/en
Priority to PCT/CN2020/103772 priority patent/WO2021174750A1/zh
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Abstract

本发明涉及一种微米银颗粒增强316L不锈钢基复合材料，包括316L不锈钢基体和均匀分布于316L不锈钢基体中的银颗粒，所述银颗粒占复合材料总重量的1～5％；所述复合材料的密度为7.9～8.2g/cm3，致密度为98％以上。制备方法：以球形银粉和球形316L不锈钢粉末作为原料，混合后进行机械球磨，得到混合粉末，过筛后，加入到SLM成形机的粉料缸中，然后通入惰性保护气体进行打印，即得。本发明通过SLM技术将银颗粒均匀分布于316L不锈钢基体中，工艺简单、节省时间、成本低，制得的复合材料具有优异的导电性和耐蚀性能，适合用于燃料电池双极板等对耐蚀性和导电性有较高要求的技术领域。

Description

一种微米银颗粒增强316L不锈钢基复合材料及其制备方法
技术领域
本发明涉及一种微米银颗粒增强316L不锈钢基复合材料及其制备方法，属于材料制备技术领域。
背景技术
316L不锈钢由于具有良好的耐蚀性、易加工性、低成本等优点，被广泛用于食品加工、医疗器械及燃料电池双极板等领域。然而，质子交换膜燃料电池双极板对材料的耐蚀性和导电性有较高的要求，单纯的316L不锈钢还不能满足要求。这一缺陷可以通过在316L不锈钢中引入能增强耐蚀性和导电性的颗粒形成颗粒增强不锈钢基复合材料来克服。
颗粒增强不锈钢基复合材料由于其增强相成本低、微观结构均匀、材料性能各向同性、可以采用传统的金属加工工艺进行加工，因此引起了人们的广泛关注。以前颗粒增强不锈钢基复合材料的制造工艺的研究往往侧重于传统的外加增强体复合法，但人们却发现传统的复合技术存在着许多问题，如增强体与基体结合不良、增强体易于偏聚，工艺复杂，成本昂贵等。与传统的复合技术相比，选区激光熔化(SLM)技术由于具有熔凝速度快、成形材料组织细小、增强相分布均匀等优点，能够节省时间、节约材料、实现复杂结构一体化成形，因此受到人们的重视。相对于传统材料表面改性处理，通过SLM技术进行材料合金化改性处理不但能简化工艺、降低成本，还能够提高材料的使用寿命。
本发明人选用银颗粒作为增强相，并对用量进行优化，通过SLM技术使其均匀分布于316L不锈钢基体中，制得的复合材料优异的导电性和耐蚀性能，这对于扩大316L不锈钢在燃料电池双极板等领域(以及其他对耐蚀性和导电性有较高的要求的技术领域)的应用具有重要的意义。
发明内容
本发明的目的在于克服上述现有技术的不足，提供一种微米银颗粒增强316L不锈钢基复合材料及其制备方法。
技术方案
一种微米银颗粒增强316L不锈钢基复合材料，包括316L不锈钢基体和均匀分布于316L不锈钢基体中的银颗粒，所述银颗粒占复合材料总重量的1～5％；所述复合材料的密度为7.9～8.2g/cm3，致密度为98％以上。
本发明将微米银颗粒作为合金化元素引入到316L不锈钢基体中，提高了316L不锈钢的耐蚀性和导电性。
上述微米银颗粒增强316L不锈钢基复合材料的制备方法，包括如下步骤：
(1)以球形银粉和球形316L不锈钢粉末作为原料，混合后进行机械球磨，得到混合粉末；混合粉末中，球形银粉的质量分数为1～5％；
(2)将混合粉末过筛后，加入到SLM成形机的粉料缸中，然后通入惰性保护气体进行打印，即得。
进一步，步骤(1)中，所述球形银粉的纯度为99.99％，球形银粉的粒度为1～5μm。
进一步，步骤(1)中，所述球形316L不锈钢粉末的粒度为30～60μm。
进一步，步骤(1)中，所述机械球磨以氧化锆为研磨球，球形银粉和球形316L不锈钢粉末的总质量与研磨球的质量比为1：1，球磨时间为4～6小时。
进一步，步骤(2)中，所述过筛为过200目筛。
进一步，步骤(2)中，所述SLM成形机的打印参数为：激光功率为300～325W，扫描速度为1500～2000mm/s，层厚为30um，扫描间距为50um，岛状扫描，起始角度为0°，旋转角度为90°。
本发明的有益效果：本发明通过SLM技术将银颗粒均匀分布于316L不锈钢基体中，工艺简单、节省时间、成本低，制得的复合材料具有优异的导电性和耐蚀性能，本发明对于扩大316L不锈钢在燃料电池双极板等领域(以及其他对耐蚀性和导电性有较高的要求的技术领域)的应用具有重要的意义。
附图说明
图1为实施例1中球形银粉的SEM图；
图2为实施例1中球形316L不锈钢粉末的SEM图；
图3为实施例1中混合粉末的SEM图；
图4为实施例1制得的微米银颗粒增强316L不锈钢基复合材料成形件的光学显微镜图；
图5为实施例1制得的微米银颗粒增强316L不锈钢基复合材料成形件的SEM图。
具体实施方式
下面结合附图和具体实施例对本发明的技术方案作进一步说明。
下述实施例中，球形银粉购自上海超威纳米科技有限公司，纯度为99.99％；球形316L不锈钢粉末购自Powder Alloy corporation；SLM成形机，采用的是南京航空航天大学的SLM成形机，最大功率为500W，聚焦光斑直径为70um。但均不限于此。
实施例1
一种微米银颗粒增强316L不锈钢基复合材料的制备方法，包括如下步骤：
(1)以球形银粉(粒度为4μm)和球形316L不锈钢粉末(粒度为40μm)作为原料，混合后进行机械球磨(以氧化锆为研磨球，球形银粉和球形316L不锈钢粉末的总质量与研磨球的质量比为1：1，球磨时间为5小时)，得到混合粉末；混合粉末中，球形银粉的质量分数为5％；
(2)将混合粉末过筛后，加入到SLM成形机的粉料缸中，然后通入惰性保护气体进行打印(SLM成形机的打印参数为：激光功率为325W，扫描速度为2000mm/s，层厚为30um，扫描间距为50um，岛状扫描，起始角度为0°，旋转角度为90°)，即得微米银颗粒增强316L不锈钢基复合材料成形件。测得密度为7.94g/cm3，致密度为98.34％。
球形银粉的SEM图见图1，球形316L不锈钢粉末的SEM图见图2，混合粉末的SEM图见图3，微米银颗粒增强316L不锈钢基复合材料成形件的光学显微镜图和SEM图分别见图4和图5，从图1-5可以看出，原始银粉和316L不锈钢发粉末具有较高的球形度。球磨后，银粉和316L不锈钢粉末混合均匀，且部分银粉被挤压成片状附在316L不锈钢粉末的表面。在微米银颗粒增强316L不锈钢基复合材料成形件中同时存在微米级的银颗粒和纳米级的银颗粒，微米级的银颗粒均匀分布在316L不锈钢的基体中而纳米级的银颗粒倾向于沿着316L不锈钢亚晶的晶界处分布。
实施例2
一种微米银颗粒增强316L不锈钢基复合材料的制备方法，包括如下步骤：
(1)以球形银粉(粒度为4μm)和球形316L不锈钢粉末(粒度为60μm)作为原料，混合后进行机械球磨(以氧化锆为研磨球，球形银粉和球形316L不锈钢粉末的总质量与研磨球的质量比为1：1，球磨时间为6小时)，得到混合粉末；混合粉末中，球形银粉的质量分数为5％；
(2)将混合粉末过筛后，加入到SLM成形机的粉料缸中，然后通入惰性保护气体进行打印(SLM成形机的打印参数为：激光功率为325W，扫描速度为1500mm/s，层厚为30um，扫描间距为50um，岛状扫描，起始角度为0°，旋转角度为90°)，即得微米银颗粒增强316L不锈钢基复合材料成形件。
测得密度为7.91g/cm3，致密度为98％。
实施例3
一种微米银颗粒增强316L不锈钢基复合材料的制备方法，包括如下步骤：
(1)以球形银粉(粒度为4μm)和球形316L不锈钢粉末(粒度为30μm)作为原料，混合后进行机械球磨(以氧化锆为研磨球，球形银粉和球形316L不锈钢粉末的总质量与研磨球的质量比为1：1，球磨时间为4小时)，得到混合粉末；混合粉末中，球形银粉的质量分数为5％；
(2)将混合粉末过筛后，加入到SLM成形机的粉料缸中，然后通入惰性保护气体进行打印(SLM成形机的打印参数为：激光功率为300W，扫描速度为1500mm/s，层厚为30um，扫描间距为50um，岛状扫描，起始角度为0°，旋转角度为90°)，即得微米银颗粒增强316L不锈钢基复合材料成形件。
测得密度为7.98g/cm3，致密度为98.87％。
将实施例1-3制得的微米银颗粒增强316L不锈钢基复合材料成形件进行耐蚀性和导电性的测试，并与316L不锈钢进行对比：
1.耐蚀性测试
测试方法：采用传统的三电极体系(以铂电极作为对电极，饱和甘汞电极作为参比电极)，利用辰华电化学工作站chi760e测试试样的动电位极化曲线来分析试样的耐蚀性能。将试样表面打磨抛光成镜面，最后将试样浸入电解液液(0.5mol/L H2SO4+2ppm HF)中进行的测试。测试条件为：起始电位＝-0.6V，终止电位＝1.2V，扫描速度＝0.001V/s。
测试结果见表1：
表1
Figure BDA0002402471250000041
2.导电性测试
测试方法：利用Wang文中所采用的方法和步骤测试表面接触电阻(参考文献：WangH,Sweikart MA,Turner JA.Stainless steel as bipolar plate material for polymerelectrolyte membrane fuel cells.2003；115:243-251.doi:10.1016/S0378-7753(03)00023-5)，测试参数如下：加载压力＝1.4Mpa，加载速度＝1N/s。测试结果见表2：
表2
Figure BDA0002402471250000042
由表1和表2的测试结果可以看出，本发明的微米银颗粒增强316L不锈钢基复合材料具有优异的导电性和耐蚀性能。

Claims (7)

1.一种微米银颗粒增强316L不锈钢基复合材料，其特征在于，包括316L不锈钢基体和均匀分布于316L不锈钢基体中的银颗粒，所述银颗粒占复合材料总重量的1～5％；所述复合材料的密度为7.9～8.2g/cm3，致密度为98％以上。
2.权利要求1所述微米银颗粒增强316L不锈钢基复合材料的制备方法，其特征在于，包括如下步骤：
(1)以球形银粉和球形316L不锈钢粉末作为原料，混合后进行机械球磨，得到混合粉末；混合粉末中，球形银粉的质量分数为1～5％；
(2)将混合粉末过筛后，加入到SLM成形机的粉料缸中，然后通入惰性保护气体进行打印，即得。
3.如权利要求2所述微米银颗粒增强316L不锈钢基复合材料的制备方法，其特征在于，步骤(1)中，所述球形银粉的纯度为99.99％，球形银粉的粒度为1～5μm。
4.如权利要求2所述微米银颗粒增强316L不锈钢基复合材料的制备方法，其特征在于，步骤(1)中，所述球形316L不锈钢粉末的粒度为30～60μm。
5.如权利要求2所述微米银颗粒增强316L不锈钢基复合材料的制备方法，其特征在于，步骤(1)中，所述机械球磨以氧化锆为研磨球，球形银粉和球形316L不锈钢粉末的总质量与研磨球的质量比为1：1，球磨时间为4～6小时。
6.如权利要求2所述微米银颗粒增强316L不锈钢基复合材料的制备方法，其特征在于，步骤(2)中，所述过筛为过200目筛。
7.如权利要求2至6任一项所述微米银颗粒增强316L不锈钢基复合材料的制备方法，其特征在于，步骤(2)中，所述SLM成形机的打印参数为：激光功率为300～325W，扫描速度为1500～2000mm/s，层厚为30um，扫描间距为50um，岛状扫描，起始角度为0°，旋转角度为90°。
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