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CN108409327A - 一种碳热还原法合成wc基纳米复合粉末的方法 - Google Patents

一种碳热还原法合成wc基纳米复合粉末的方法 Download PDF

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CN108409327A
CN108409327A CN201810242868.0A CN201810242868A CN108409327A CN 108409327 A CN108409327 A CN 108409327A CN 201810242868 A CN201810242868 A CN 201810242868A CN 108409327 A CN108409327 A CN 108409327A
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赵志伟
郑娟
毛淑芳
王艳荣
陈艳
胡余沛
关春龙
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Henan University of Technology
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Abstract

一种碳热还原法合成WC基纳米复合粉末的方法,其特征包括以下步骤:a、按重量比取纳米氧化钨6.41 g~7.58 g、纳米氧化钴0.65~0.76g、纳米氧化钒、纳米氧化铬混合物0.048g~0.057g、纳米碳质还原剂1.60g~2.90 g,将它们置于混料机中,采用湿混的方法,充分混合后,制得混合料。b、将步骤a所得混合料置于干燥箱中,在200℃条件下干燥1h~3h。c、将步骤b所得干燥后的混合料置于高温反应炉中,在真空或氩气气氛条件下,制得平均粒径<100nm、粒度分布均匀的WC基纳米复合粉末。本发明具有制备过程简便、周期短、能耗低,能大幅度降低成本,适合工业生产。

Description

一种碳热还原法合成WC基纳米复合粉末的方法
技术领域
本发明涉及一种碳热还原法合成WC基纳米复合粉末的方法,属于纳米金属陶瓷复合粉体制备技术领域。
背景技术
近年来,超细/纳米WC-Co复合粉末因其优异的物理机械性能广泛应用于超细/纳米晶硬质合金制备、热喷涂、金属快速成形、表面贴装、材料表面强化等领域。如纳米WC-Co复合粉末制备的硬质合金比传统混合料制备的硬质合金晶粒更细、更均匀,力学性能好,使用寿命长。硬质合金在现代工具材料、耐磨材料、耐高温和耐腐蚀材料等领域占有重要地位,很大程度上取代了高速钢,引起了金属切削加工工业的技术革命,被誉为“工业的牙齿”。其中,WC-Co 硬质合金主要成分 WC 硬度相当高,其粘结相 Co 与 WC之间具有良好的润湿性,接触角基本为 0℃,因此 WC-Co 复合材料在受力的情况下,由碳化物颗粒形成的骨架可以承受很大的应力,显示出高的强度,而作为粘结相的 Co 通过形变吸收能量,抑制裂纹延伸,呈现出较好的断裂韧性。因而,WC-Co 系硬质合金占整个硬质合金产品的一半以上。
现代工业对硬质合金的性能要求越来越高,硬质合金中 WC 的晶粒尺寸越小,粘结相 Co 的平均自由程(即硬质相 WC 晶粒间钴层的厚度)越短,合金的硬度和强度越高。WC 晶粒为 0.5μm 以下的超细硬质合金因其具有优良的综合性能,在难加工材料领域、微电子工业、精密模具加工业、木材加工、医学等领域得到广泛应用。WC 晶粒在 100nm 以下的纳米硬质合金具有更优良的性能。因此,它已经成为“难熔金属与硬质材料”领域内各国科学家竞相研究的热点之一。超细硬质合金的一个关键制备技术便是粉末的制备,合金的晶粒尺寸首先取决于粉末的颗粒大小,制备出颗粒细小、粒度均匀的粉末是制备超细硬质合金的必要条件。理论与实践表明, 当 WC-Co合金的WC晶粒尺寸减少到亚微米以下时,材料的硬度、韧性、强度、耐磨性都能得到提高,同时达到完全致密化所需的烧结温度较低。因此,由传统硬质合金向超细或纳米硬质合金的发展已成为当今硬质合金行业的一大趋势。
发明内容
本发明的目的在于提供一种新型纳米WC基复合粉末的合成方法,以便更好的满足WC基复合粉末在超细/纳米硬质合金制造、材料表面强化喷涂等领域的应用。本发明采用的原位还原碳化法,该方法所需设备简单,反应原料价格低廉,制备过程简便、周期短、能耗低,能大幅度降低制备成本,保证合成的WC基复合粉末在粒度、分散性、颗粒形状等方面满足工业需求。
本发明的WC基纳米复合粉末的合成方法包括以下步骤:
a、按重量比取纳米氧化钨6.41 g~7.58 g、纳米氧化钴0.65~0.76g、纳米氧化钒、纳米氧化铬混合物0.048g~0.057g、纳米碳质还原剂1.60g~2.90 g,将它们置于混料机中,采用湿混的方法,充分混合后,制得混合料。
b、将步骤a所得混合料置于干燥箱中,在200℃条件下干燥1h~3h。
c、将步骤b所得干燥后的混合料置于高温反应炉中,在真空或氩气气氛条件下,在1000~1300℃、0.5~2h的条件下进行碳热还原碳化,制得平均粒径<100nm、粒度分布均匀的WC基纳米复合粉末。
所述纳米氧化钨为纳米三氧化钨或纳米二氧化钨中的任意一种。
所述纳米氧化钴为纳米四氧化三钴、纳米三氧化二钴或纳米氧化亚钴中的任意一种。
所述纳米氧化钒为纳米五氧化二钒、纳米二氧化钒或纳米三氧化二钒中的任意一种。
所述纳米氧化铬为纳米三氧化二铬。
所述纳米碳质还原剂为纳米碳黑或纳米活性碳中的任意一种。
所述高温反应炉为管式炉或微波炉中的任意一种。
本发明相比现有制备WC基复合粉末的方法,具有如下有益效果:
(1)工艺简单。原料经混料、干燥后,即可进行碳热还原碳化,而且一次完成,简化了制备工艺,操作方便,适合工业化生产。
(2)反应温度低,反应时间短,节约能源。以纳米氧化钨、纳米氧化钴、纳米氧化钒、纳米氧化铬混合物、纳米碳质还原剂为原料,具有较高的比表面积,颗粒之间的接触面积较大,界面原子数较多,界面区域原子扩散系数较高,使得纳米材料具有较高的化学活性,可以加速碳热还原碳化反应的进行。相对传统WC基纳米复合粉末的合成方法,本合成方法可以大幅度降低反应温度,缩短反应时间,有效节约能源。
(3)性能优异:反应生成的多元WC基纳米复合粉末,杂质含量少,粉末粒度<100nm,粒度均匀,粒径分布范围较窄,在硬质合金、电子材料、涂层材料等领域具有广阔应用前景。
具体实施方式
本发明以下将结合实施例作进一步描述:
实施例1:
按重量比取纳米三氧化钨6.41 g、纳米四氧化三钴0.76g、纳米碳黑2.77 g、纳米五氧化二钒0.027g、纳米三氧化二铬0.030g,将它们置于混料机中,采用湿混方式,分散介质为无水乙醇,充分混合后,制得混合料。将所得混合料置于干燥箱中,在200℃条件下干燥1h。将干燥后的混合料置于管式炉中,在真空条件下,在1000~1300℃、0.5~2h的条件下进行碳热还原碳化,制得平均粒径<100nm、粒度分布均匀的WC基复合粉末。
实施例2:
按重量比取纳米二氧化钨7.58 g、纳米三氧化二钴0.65g、纳米活性碳1.72 g、纳米二氧化钒0.020g、纳米三氧化二铬0.028g,将它们置于混料机中,采用湿混方式,分散介质为无水丙酮,充分混合后,制得混合料。将所得混合料置于干燥箱中,在200℃条件下干燥2h。将干燥后的混合料置于微波炉中,在氩气气氛条件下,在1000~1300℃、0.5~2h的条件下进行碳热还原碳化,制得平均粒径<100nm、粒度分布均匀的WC基复合粉末。
实施例3:
按重量比取纳米三氧化钨7.50 g、纳米氧化亚钴0.70g、纳米碳黑1.65 g、纳米三氧化二钒0.020g、纳米三氧化二铬0.030g,将它们置于混料机中,采用湿混方式,分散介质为无水乙醇,充分混合后,制得混合料。将所得混合料置于干燥箱中,在200℃条件下干燥3h。将干燥后的混合料置于管式炉中,在真空条件下,在1000~1300℃、0.5~2h的条件下进行碳热还原碳化,制得平均粒径<100nm、粒度分布均匀的WC基复合粉末。
实施例4:
按重量比取纳米二氧化钨6.45 g、纳米三氧化二钴0.68g、纳米活性碳2.90 g、纳米五氧化二钒0.037g、纳米三氧化二铬0.020g,将它们置于混料机中,采用湿混方式,分散介质为无水丙酮,充分混合后,制得混合料。将所得混合料置于干燥箱中,在200℃条件下干燥1.5h。将干燥后的混合料置于微波炉中,在氩气气氛条件下,在1000~1300℃、0.5~2h的条件下进行碳热还原碳化,制得平均粒径<100nm、粒度分布均匀的WC基复合粉末。

Claims (7)

1.一种碳热还原法合成WC基纳米复合粉末的方法,其特征在于:所述合成方法包括以下步骤:
a、按重量比取纳米氧化钨6.41 g~7.58 g、纳米氧化钴0.65~0.76g、纳米氧化钒、纳米氧化铬混合物0.048g~0.057g、纳米碳质还原剂1.60g~2.90 g,将它们置于混料机中,采用湿混的方法,充分混合后,制得混合料;
b、将步骤a所得混合料置于干燥箱中,在200℃条件下干燥1h~3h;
c、将步骤b所得干燥后的混合料置于高温反应炉中,在真空或氩气气氛条件下,在1000~1300℃、0.5~2h的条件下进行碳热还原碳化,制得平均粒径<100nm、粒度分布均匀的WC基纳米复合粉末。
2.根据权利要求1所述纳米氧化钨为纳米三氧化钨或纳米二氧化钨中的任意一种。
3.根据权利要求1所述纳米氧化钴为纳米四氧化三钴、纳米三氧化二钴或纳米氧化亚钴中的任意一种。
4.根据权利要求1所述纳米氧化钒为纳米五氧化二钒、纳米二氧化钒或纳米三氧化二钒中的任意一种。
5.根据权利要求1所述纳米氧化铬为纳米三氧化二铬。
6.根据权利要求1所述纳米碳质还原剂为纳米碳黑或纳米活性碳中的任意一种。
7.根据权利要求1所述高温反应炉为管式炉或微波炉中的任意一种。
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