CN106116534A - 一种制备拉拔模具的纳米晶陶瓷材料 - Google Patents

一种制备拉拔模具的纳米晶陶瓷材料 Download PDF

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CN106116534A
CN106116534A CN201610471081.2A CN201610471081A CN106116534A CN 106116534 A CN106116534 A CN 106116534A CN 201610471081 A CN201610471081 A CN 201610471081A CN 106116534 A CN106116534 A CN 106116534A
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aluminium oxide
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drawing mould
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徐淑波
张琳娜
徐爱青
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Shandong Jianzhu University
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Abstract

本发明属于拉拔模具材料领域，涉及一种制备拉拔模具的纳米晶陶瓷材料，特别是一种氧化铝和碳化锆纳米晶须增强拉拔模具的纳米晶陶瓷材料的制备方法。原位生成氧化铝和碳化锆晶须增强纳米拉拔模具材料粉末由氧化铝、氧化锆和氧化镁基体材料粉末和氧化铝和碳化锆纳米晶须粉末组成，然后采用机械混合法使氧化铝、氧化锆和氧化镁基体粉末与氧化铝和碳化锆晶须粉末均匀混合，混合粉末冷等静压实后在10‑6托真空条件下逐步加热除气，然后在1500‑1600℃，50‑200Mpa条件下真空烧结1‑4小时。增强纳米晶须直径尺寸细小，分布均匀，组织稳定性高，表面无污染，拉拔模具的纳米晶陶瓷材料的强度、韧性、硬度、耐磨性和良疲劳性能得到显著提高。

Description

一种制备拉拔模具的纳米晶陶瓷材料
技术领域
本发明属于拉拔模具材料领域，涉及一种制备拉拔模具的纳米晶陶瓷材料，特别是一种氧化铝和碳化锆纳米晶须增强拉拔模具的纳米晶陶瓷材料的制备方法。
背景技术
拉拔工艺是工业生产中重要的环节，目前，拉拔工艺在毛坯的下料、零件的制备以及装备制造业的使用中不可或缺，在工业生产中使用量非常大，拉拔模具要求高的硬度和耐磨性，其中硬度高（HRC≥58-64），才能保证拉拔模具在被加工材料产生变形时，拉拔模具本身不产生变形和开裂，高的耐磨性是模具长期使用不变形，高耐磨性是以高硬度为基础的。同时要求有足够的强度与韧性，高的强度会提高拉拔模具的变形抗力，高的韧性防止冲击载荷下的脆断。还要求有良好的疲劳性能和良好的抗咬合能力。
拉拔模具材料主要分为高速钢、硬质合金和新型拉拔模具材料， 本发明拉拔模具材料的基体为氧化铝、氧化锆和氧化镁，针对要求的高硬度与耐磨性、高的耐热性、高的化学稳定性以及较低的摩擦系数，本发明为新型拉拔模具材料，在氧化铝、氧化锆和氧化镁的基体上采用氧化铝和碳化锆晶须增强，在高温下获得的一种新型拉拔模具材料。
目前我国现有的拉拔模具材料在专利申请号为2010106005000中，采用氧化铝和碳化钛等化合物制备拉拔模具材料，同时添加钼、镍等金属元素细化晶粒，增加制备材料的强度、韧性、耐热性、耐腐蚀性、抗酸性等。但是合金元素细化晶粒的程度是有限制的，而进一步提高拉拔模具硬度与耐磨性、耐热性需要进一步研究，采用晶须增强与纳米晶粒材料相结合的方法获得高性能材料近年来取得了很大的进步，本发明利用氧化铝和碳化锆两种物质的优良特性，通过生成两种物质的纳米晶须，通过纳米晶须达到增韧增强拉拔模具材料，同时拉拔模具材料的基体为氧化铝、氧化锆和氧化镁材料，从而，本发明可以显著提高拉拔模具的强度、韧性、硬度、耐磨性和良疲劳性能，具有重要的工业应用价值和广泛的应用领域。
发明内容
本发明专利的目的是：在于克服上述现有技术不足，提供一种加工工艺稳定、生产成本低廉、无污染排放、可在常规条件下组织生产的氧化铝和碳化锆纳米晶须增强氧化铝、氧化锆和氧化镁拉拔模具材料，较传统的陶瓷拉拔模具有高的硬度与耐磨性、高的耐热性、高的化学稳定性以及较低的摩擦系数。
本发明提供了一种生成氧化铝和碳化锆晶须增强纳米拉拔模具材料，其特征在于：该材料沿挤压流线形成定向排列的碳化锆、氧化锆晶须和氧化铝、氧化锆和氧化镁基体材料组成，晶须直径为200-800nm。
本发明是通过以下技术方案如下：生成氧化铝和碳化锆晶须增强拉拔模具材料粉末由氧化铝、氧化锆和氧化镁基体材料粉末和氧化铝和氧化锆晶须粉末组成，然后采用机械混合法使氧化铝、氧化锆和氧化镁基体粉末与氧化铝和氧化锆晶须粉末均匀混合，混合粉末冷等静压实后在10-6托真空条件下逐步加热除气，然后在1500-1600℃，50-200Mpa条件下真空烧结1-4小时。
测试表明所获得的生成氧化铝和碳化锆纳米晶须增强拉拔模具材料具有高强韧性。
方案所需材料按如下具体步骤制备：
（1）和氧化锆晶须的制备：
生成碳化锆和氧化铝晶须粉末的制备工艺为：氧化铝和氧化锆晶须前驱体材料化学成分及重量百分比为：ZrO2：46.4～52.2％，Al：46.4～52.2％，Mn：0.1～0.9％，NaCl：1.0～8.1％。将按比例配制的能够生成碳化锆和氧化铝晶须的先驱体复合粉末加无水乙醇于球磨机中进行机械化球磨48小时，获得具有200-600nm晶粒尺寸超细先驱体复合粉末，将粉末装入石墨容器中，在氩气气氛保护和1550℃-1800℃的温度条件下，保温90min-180min合成。
ZrO2+3C=（加热）ZrC+2CO↑
4Al+3O2=（加热）2Al2O3
（2）氧化铝、氧化锆和氧化镁基体材料粉末制备：
氧化铝、氧化锆和氧化镁基体材料的化学成分及重量百分比为：Al2O3：46％，ZrO2：46％，MgO：8％。本发明为获得最佳的综合力学性能和生物学腐蚀性能，严格控制Fe、Cu、Al等杂质的含量：Al2O3、ZrO2和MgO的纯净度大于等于99.99％。氧化铝、氧化锆和氧化镁粉末加无水乙醇于球磨机中进行机械化球磨48小时，获得具有50-100μm晶粒尺寸超细粉末。
（3）碳化锆和氧化铝纳米晶须与氧化铝、氧化锆和氧化镁基体材料混合粉末：
氧化铝和碳化锆在氧化铝、氧化锆和氧化镁基体材料中的重量含量为5-10%，将碳化锆和氧化锆晶须与氧化铝、氧化锆和氧化镁基体材料按重量百分比为（5-10）: （95-90）的比例配制为氧化铝和碳化锆晶须增强拉拔模具材料粉末。
该生成氧化铝和氧化锆晶须增强拉拔模具材料无需专用设备，在常规氧化铝厂即可组织生产，本发明投资少，见效快，能快速收回投资成本。
与现有氧化铝陶瓷拉拔模具材料相比，生成氧化铝和碳化锆晶须增韧氧化铝的制备方法具有如下优点：
（1）韧性、耐磨性、强度显著提高，间隔2小时挤压试样的力学性能差小于6%，这将有利于大批量、小尺寸口腔医学材料的稳定生产。增强颗粒尺寸细小，分布均匀，组织稳定性高，与在氧化铝基体结合良好。拉拔模具材料的强度、韧性、硬度、耐磨性和良疲劳性能得到显著提高。
（2）化学稳定性好，不会分解有毒气体或有毒溶解物，本发明因氧化铝和碳化锆增强晶须是与氧化锆颗粒、铝颗粒在真空中反应生成，生产的工艺稳定性高。
附图说明
图1 是最佳实施例的氧化铝和碳化锆纳米晶须增强拉拔模具材料的透射电镜照片。
利用本发明配方和制备方法制备的拉拔模具的纳米晶陶瓷材料，晶须与晶粒尺寸均小于400nm，本制备方法工艺简单，低成本，适用于工业化生产。
具体实施方式
下面给出本发明的最佳实施例：按氧化铝基体材料的化学成分及重量百分比为：Al2O3：46％，ZrO2：46％，MgO：8％。严格控制Fe、Cu、Al 等杂质的含量：Al2O3、ZrO2和MgO的纯净度大于等于99.99％，将按比例配制的氧化铝、氧化锆和氧化镁粉末加无水乙醇于球磨机中进行机械化球磨48小时，获得具有50-150μm晶粒尺寸超细粉末。将氧化铝和碳化锆晶须前驱体材料化学成分及重量百分比为：ZrO2：46.4～52.2％，Al：46.4～52.2％，Mn：0.1～0.9％，NaCl：1.0～8.1％。将按比例配制的能够生成氧化铝和碳化锆晶须的先驱体复合粉末加无水乙醇于球磨机中进行机械化球磨48小时，获得具有200-800nm晶粒尺寸超细先驱体复合粉末。将氧化铝和碳化锆晶须与氧化铝、氧化锆和氧化镁基体材料按重量百分比为8:92的比例配制为氧化铝和氧化锆晶须增韧氧化铝、氧化锆和氧化镁材料粉末。然后采用机械混合法使氧化铝基体粉末与氧化铝和氧化锆晶须粉末均匀混合，混合粉末冷等静压实后在10-6托真空条件下逐步加热除气，然后在550℃，100Mpa条件下真空烧结2小时，获得一种制备拉拔模具的纳米晶陶瓷材料然后进行T6处理，并进行性能测试，抗弯强度765MPa、断裂韧性10.76MPa·m1/2、维氏硬度20.7GPa。

Claims (3)

1.一种制备拉拔模具的纳米晶陶瓷材料，其特征是氧化铝和碳化锆晶须增强拉拔模具材料粉末由氧化铝、碳化锆和氧化镁基体材料粉末和氧化铝和氧化锆晶须粉末组成，然后采用机械混合法使氧化铝、碳化锆和氧化镁基体粉末与氧化铝和碳化锆晶须粉末均匀混合，混合粉末冷等静压实后在10-6托真空条件下逐步加热除气，然后在1500-1600℃，50-200Mpa条件下真空烧结1-4小时。
2.根据权利要求1所述的一种制备拉拔模具的纳米晶陶瓷材料，其特征是氧化铝和碳化锆晶须纳米晶须的先驱体复合粉末加无水乙醇于球磨机中进行机械化球磨48小时，获得具有200-600nm晶粒尺寸超细先驱体复合粉。
3.将先驱体粉末装入石墨容器中，在氩气气氛保护和1550℃-1800℃的温度条件下，保温90min-180min合成氧化铝和碳化锆纳米晶须。
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CN105272329A (zh) * 2015-10-29 2016-01-27 山东建筑大学 一种氧化铝-碳化硅-碳化锆纳米晶须增强切割刀具材料的制备方法

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CN101289313A (zh) * 2008-05-29 2008-10-22 大连理工大学 一种氧化铝基纳米复相陶瓷拉丝模及其制备方法
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