CN109516809A - 一种基于i-wp曲面的铜碳化硅复合材料的制备方法 - Google Patents
一种基于i-wp曲面的铜碳化硅复合材料的制备方法 Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims description 60
- 229910010271 silicon carbide Inorganic materials 0.000 title claims description 60
- 239000010949 copper Substances 0.000 title claims description 44
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims description 13
- 229910052802 copper Inorganic materials 0.000 title claims description 13
- 239000000919 ceramic Substances 0.000 claims abstract description 62
- 239000002184 metal Substances 0.000 claims abstract description 14
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- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 10
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
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Abstract
本发明公开一种基于I‑WP曲面的Cu/SiC复合材料的制备方法，是一种金属相Cu和陶瓷相SiC以三周期极小曲面I‑WP结构为基础，在三维空间网络结构连续并且互相缠绕在一起的三维网络结构复合材料。I‑WP曲面结构能有效避免应力集中，增加复合材料的力学性能，Cu/SiC复合材料既具有金属的塑形、导电导热性，又具备陶瓷的高硬度、高耐磨性及化学稳定性等特点。所述制备方法具体是设计并3D打印I‑WP曲面的结构；多孔SiC陶瓷预制体的制备；金属Cu的浸渗。本发明可以通过改变I‑WP曲面结构的打印参数，控制金属和陶瓷的含量，使制备的Cu/SiC复合材料更适合工业的需要。
Description
技术领域
本发明涉及一种Cu/SiC复合材料的制备方法，具体的涉及一种基于I-WP曲面的Cu/SiC复合材料及其制备方法
背景技术
铜的导电导热性能较好，但硬度耐磨性较差；而碳化硅陶瓷硬度相当高，仅次于几种超硬材料，且具有较好的机械性能，但碳化硅陶瓷脆性较大。SiC陶瓷材料弹性模量高、抗氧化性能好、高温强度大等优越性能，是用于强化电接触基体材料的最理想原料之一。因此将金属铜和碳化硅陶瓷复合起来制成复合材料能充分发挥两种材料的性能优点，弥补各自的不足，使Cu/SiC复合材料成为一种综合性能更为优良的新型导电耐磨复合材料。常用的制备方法主要包括：内氧化法、粉末冶金法、机械合金化法、搅拌铸造法，但是这些传统制备方法不能形成规则的三维联通结构，为了保证导电性能，需要大量加入Cu形成三维网络导电结构，但是过多的铜会使强度和耐磨性下降，易产生裂纹，坍塌等缺陷。
发明内容
本发明提供一种基于I-WP曲面的Cu/SiC复合材料的制备方法，这种三周期极小曲面结构除了能保证力学性能外，而且还具备光滑连续、连通性良好、三维贯通的金属Cu结构，保证导电导热等性能。通过该方法可以对金属铜的结构、分布及含量的任意调整，便于获取特定工况下的最佳金属Cu含量，以及具有特定要求的结构，可以制备力学性能和导电性能好的Cu/SiC复合材料。其中，该制备方法包含以下几个步骤：
(1)PLA骨架的制备：利用熔融沉积式3D打印机打印所设计的PLA材料的I-WP曲面结构，分层厚度0.1～0.2mm，打印速度60mm/s，周期参数1～4，曲面厚度0.5～2mm；
(2)陶瓷粉体的制备：将SiC粉，滑石粉，Al2O3粉和Y2O3粉、纤维素按质量比88.5～91.5：3.6～5.5：0.9～2.2：0.5～1.5：1.5～3.0比例称量混合(所述的陶瓷浆料中SiC粉，滑石粉，Al2O3粉和Y2O3粉、纤维素优选质量比为90.5：4.0：1.5：1.0：3.0)，球磨4h后，过筛得到颗粒粒度≤1μm的陶瓷粉体；
(3)陶瓷浆料的制备：将步骤(2)所述的陶瓷粉体倒入无水乙醇中，粉末与无水乙醇的质量比2：0.8-1.2，用氨水调节pH至9～11。置于滚筒式球磨机中混料2-4h，回转速度250～300r/min，使各种物料混合均匀，成泥浆状，再陈腐1-2d后得到碳化硅陶瓷浆料；
(4)陶瓷胚体的制备：将步骤(1)所述的PLA结构放置于铸造模具内，再将得到的碳化硅陶瓷浆料加入催化剂和引发剂，按陶瓷浆料、催化剂四甲基乙二胺和引发剂过硫酸铵的质量比为100：1.0～1.5：0.5～1.0的比例添加，快速搅拌后注入模具使浆料固化，将固化浆料放在真空干燥箱中进行冷冻干燥，温度为-140～-120℃，预冻2～3h，待完全结晶后抽真空，然后在-5～0℃，真空度10～20Pa下冷冻干燥24h，即可得到基于I-WP曲面的PLA/碳化硅陶瓷材料胚体；
(5)多孔SiC陶瓷的制备：将步骤(4)所得到的陶瓷胚体置于高温炉中烧结，先在10℃/min升温至200-220℃；再以5～10℃/min升温至550-600℃，保温1～2h，排出有机添加剂；最后以10℃/min升温至1400-1450℃，保温2h，然后随炉冷却至室温，去除PLA残渣，再进行超声波清洗，反复三次，即可得到基于I-WP曲面反向结构的多孔SiC陶瓷。
(6)浸渗法制备Cu/SiC复合材料：将金属铜块置于步骤(5)所述的多孔SiC陶瓷预制体上方，在真空条件下进行熔渗，熔渗压力为0.5-0.6MPa，升温至1100～1200℃，保温时间2～3小时，冷却后取出，即得到基于I-WP曲面的Cu/SiC复合材料。
本发明具有如下有益效果：
本发明的技术方案提供了一种基于I-WP曲面结构的Cu/SiC复合材料的制备方法，该模型的I-WP曲面是一种三周期极小曲面结构，是一种光滑连续、连通性良好、三维贯通的结构，相较于一般多孔结构如蜂窝结构，受力更加均匀，整体更加稳定以及空间排列更加多样。同时在设计过程中可以通过调整I-WP曲面结构的参数，如周期参数、曲率和曲面厚度等来控制金属Cu的结构参数，赋予该复合材料不同的性能。
通过本发明的步骤制备出的基于I-WP曲面的Cu/SiC复合材料，其中金属Cu为I-WP曲面的结构，该结构为三维网状光滑连通结构，具有优良特质如高比强度、耐冲击性、导电性、热声隔离性能等相等优点，陶瓷具有高的强度、耐磨性、耐腐蚀性等优点，光滑过渡的曲面结构有利于避免应力集中，且通过对I-WP曲面结构的参数化设计，可以构造相互连通并且规则金属Cu结构，从而调节Cu含量及分布，进而性能优化，有助于促进Cu/SiC复合材料的发展和应用。
附图说明
下面结合附图对本发明进一步的说明：
图1为I-WP曲面结构示意图。
图2结构一制备Cu/SiC复合材料示意图。
图3为结构二制备Cu/SiC复合材料示意图。
具体实施方式
下面结合具体实施例对本发明做进一步说明。
实施例一
(1)PLA骨架的制备：利用熔融沉积式3D打印机直接打印所设计的PLA材料的I-WP曲面结构，分层厚度0.1mm，边长为4×4×4cm的立方体，周期参数2，曲面厚度1mm；
(2)陶瓷粉体的制备：将SiC粉，滑石粉，Al2O3粉和Y2O3粉、纤维素按90.5：4.0：1.5：1.0：3.0比例称量混合，球磨4h后，过筛得到颗粒粒度≤1μm的陶瓷粉体；
(3)陶瓷浆料的制备：将步骤(2)所述的陶瓷粉体倒入无水乙醇中，粉末与无水乙醇的质量比2：1，用氨水调节pH至10。置于滚筒式球磨机中混料3h，回转速度250r/min，使各种物料混合均匀，成泥浆状，再陈腐1d后得到碳化硅陶瓷浆料；
(4)陶瓷胚体的制备：将步骤(1)所述的PLA结构放置于铸造模具内，再将得到的碳化硅陶瓷浆料加入催化剂和引发剂，按陶瓷浆料、催化剂四甲基乙二胺和引发剂过硫酸铵的质量比为100：1.0：0.5的比例添加，快速搅拌后注入模具使浆料固化，将固化浆料放在真空干燥箱中进行冷冻干燥，温度为-140℃，预冻2h，待完全结晶后抽真空，然后在-5℃，真空度10Pa下冷冻干燥24h，即可得到基于I-WP曲面的PLA/碳化硅陶瓷材料胚体；
(5)多孔SiC陶瓷的制备：将步骤(4)得到的陶瓷胚体置于高温炉中烧结，先在10℃/min升温至220℃；再以5℃/min升温至600℃，保温2h，排出有机添加剂；最后以10℃/min升温至1450℃，保温2h，然后随炉冷却至室温，去除PLA残渣，再进行超声波清洗，反复三次，即可得到基于I-WP曲面反向结构的多孔SiC陶瓷。
(6)浸渗法制备Cu/SiC复合材料：将金属铜块置于步骤(5)所述的多孔SiC陶瓷预制体上方，在真空条件下进行熔渗，熔渗压力为0.5MPa，升温至1100℃，保温时间3小时，冷却后取出，即得到基于I-WP曲面的Cu/SiC复合材料，其中铜的体积分数为10.79％，SiC陶瓷的体积分数为89.21％，如图2所示。
实施例二
(1)PLA骨架的制备：利用熔融沉积式3D打印机直接打印所设计的PLA材料的I-WP曲面结构，分层厚度0.1mm，边长为4×4×4cm的立方体，周期参数3，曲面厚度1mm；
(2)陶瓷粉体的制备：将SiC粉，滑石粉，Al2O3粉和Y2O3粉、纤维素按90.5：4.0：1.5：1.0：3.0比例称量混合，球磨4h后，过筛得到颗粒粒度≤1μm的陶瓷粉体；
(3)陶瓷浆料的制备：将步骤(2)所述的陶瓷粉体倒入无水乙醇中，粉末与无水乙醇的质量比2：1，用氨水调节pH至10。置于滚筒式球磨机中混料3h，回转速度250r/min，使各种物料混合均匀，成泥浆状，再陈腐1d后得到碳化硅陶瓷浆料；
(4)陶瓷胚体的制备：将步骤(1)所述的PLA结构放置于铸造模具内，再将得到的碳化硅陶瓷浆料加入催化剂和引发剂，按陶瓷浆料、催化剂四甲基乙二胺和引发剂过硫酸铵的质量比为100：1.0：0.5的比例添加，快速搅拌后注入模具使浆料固化，将固化浆料放在真空干燥箱中进行冷冻干燥，温度为-140℃，预冻2h，待完全结晶后抽真空，然后在0℃，真空度10Pa下冷冻干燥24h，即可得到基于I-WP曲面的PLA/碳化硅陶瓷材料胚体；
(5)多孔SiC陶瓷的制备：将步骤(4)得到的陶瓷胚体置于高温炉中烧结，先在10℃/min升温至220℃；再以5℃/min升温至600℃，保温2h，排出有机添加剂；最后以10℃/min升温至1450℃，保温2h，然后随炉冷却至室温，去除PLA残渣，再进行超声波清洗，反复三次，即可得到基于I-WP曲面反向结构的多孔SiC陶瓷
(6)浸渗法制备Cu/SiC复合材料：将金属铜块置于步骤(5)所述的多孔SiC陶瓷预制体上方，在真空条件下进行熔渗，熔渗压力为0.5MPa，升温至1100℃，保温时间3小时，冷却后取出，即得到基于I-WP曲面的Cu/SiC复合材料，铜的体积分数为13.63％，SiC陶瓷的体积分数为86.37％，如图3所示。
Claims (8)
1.一种基于I-WP曲面的Cu/SiC复合材料的制备方法，其特征在于，包括以下步骤：
(1)PLA骨架的制备：采用3D打印机对PLA材料打印成I-WP曲面结构；
(2)陶瓷粉体的制备：将SiC粉，滑石粉，Al2O3粉和Y2O3粉、纤维素混合，球磨后，过筛得到颗粒粒度≤1μm的陶瓷粉体；
(3)陶瓷浆料的制备：将步骤(2)所述的陶瓷粉体倒入无水乙醇中，球磨混料成泥浆后，陈腐得到碳化硅陶瓷浆料；
(4)陶瓷胚体的制备：将步骤(1)所述的PLA结构放置于铸造模具内，再将得到的碳化硅陶瓷浆料加入催化剂四甲基乙二胺和引发剂过硫酸铵，快速搅拌后注入模具使其固化，将固化的浆料放在真空干燥箱中抽真空排除气泡，进行真空冷冻干燥，即可得到基于I-WP曲面的PLA/碳化硅陶瓷材料胚体；
(5)多孔SiC陶瓷的制备：将步骤(4)所得到的胚体置于高温炉中烧结，随炉冷却并去除PLA残渣，再进行超声波清洗，反复三次，即可得到基于I-WP曲面反向结构的多孔SiC陶瓷；
(6)浸渗法制备Cu/SiC复合材料：将金属铜块置于步骤(5)所述的多孔SiC陶瓷预制体上方，在真空条件下进行熔渗后取出，即得到基于I-WP曲面的Cu/SiC复合材料。
2.根据权利要求1所述的基于I-WP曲面的Cu/SiC复合材料的制备方法，其特征在于，步骤(1)中，3D打印I-WP曲面结构的参数为分层厚度0.1～0.2mm，打印速度60mm/s，周期参数1～4，曲面厚度0.5～2mm。
3.根据权利要求1所述的基于I-WP曲面的Cu/SiC复合材料的制备方法，其特征在于，步骤(2)中，SiC粉，滑石粉，Al2O3粉和Y2O3粉、纤维素的质量比88.5～91.5：3.6～5.5：0.9～2.2：0.5～1.5：1.5～3.0。
4.根据权利要求1所述的基于I-WP曲面的Cu/SiC复合材料的制备方法，其特征在于，步骤(3)中，将步骤(2)所述的陶瓷粉体倒入无水乙醇中，粉末与无水乙醇的质量比2：0.8-1.2，用氨水调节pH至9～11，置于滚筒式球磨机中混料2-4h，回转速度250～300r/min，使各种物料混合均匀，成泥浆状，再陈腐1-2d后得到碳化硅陶瓷浆料。
5.根据权利要求1所述的基于I-WP曲面的Cu/SiC复合材料的制备方法，其特征在于，步骤(4)中，采用真空冷冻干燥陶瓷胚体，将胚体放入真空冷冻干燥机以-140～-120℃预冻2～3h，待完全结晶后抽真空,然后在-5～0℃，真空度10～20Pa下冷冻干燥24h。
6.根据权利要求1所述的基于I-WP曲面的Cu/SiC复合材料的制备方法，其特征在于，步骤(4)中，按陶瓷浆料、催化剂四甲基乙二胺和引发剂过硫酸铵的质量比为100：1.0～1.5：0.5～1.0。
7.根据权利要求1所述的基于I-WP曲面的Cu/SiC复合材料的制备方法，其特征在于，步骤(5)中，烧结过程中采用阶梯升温、分段保温、慢速焙烧的工艺，具体为先在10℃/min升温至200-220℃；再以5～10℃/min升温至550-600℃，保温1～2h，排出有机添加剂；最后以10℃/min升温至1400-1450℃，保温2h，然后随炉冷却至室温。
8.根据权利要求1所述的基于I-WP曲面的Cu/SiC复合材料的制备方法，其特征在于，步骤(6)中，将金属铜块置于步骤(5)所述的多孔SiC陶瓷预制体上方，在真空条件下，熔渗压力为0.5-0.6MPa，升温至1100～1200℃，保温时间2～3小时进行熔渗，冷却后取出，即得到基于I-WP曲面的Cu/SiC复合材料。
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