等离子原位冶金碳化钨结晶过程研究
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摘要
为突破粉末冶金硬质合金技术瓶颈,本文采用等离子原位冶金技术制备碳化钨复合材料。讨论了原位冶金碳化钨复合材料的的显微组织结构和机械性能,研究了原位冶金碳化钨工艺中在等离子弧高温和富碳液相条件下钨碳反应及碳化钨相结晶长大的现象与规律性。
组织分析结果表明,电流的大小直接影响最终得到复合材料的成型性；等离子原位冶金碳化钨中相组成主要为WC、W2C、M6C (Fe3W3C)、γ-Fe以及少量的Cr7C3和(Fe, Ni)3C,组织均匀,具有三角形或四边形的硬质相颗粒尺寸约为5-30μm。
等离子在原位冶金加热过程中,在等离子束高温作用下同步送入的粉末与基体共同形成熔池。冶金区剧烈反应产生的气体、熔渣上浮。WC成核后,以具有平滑固液界面的形式成长。在WC结晶过程中,由于晶面的各向异性等原因引起WC晶粒各晶面表面能的差异,决定了特定的截断因子r和伸长率k,生成具有特殊形貌的WC晶粒。晶粒的特殊结构和复杂的界面环境使WC晶粒以(0001)面为基面,沿<0001>方向生长形成多层堆垛结构。
得到的WC复合材料的平均硬度都能达到HRA82以上。对合金内部不同物相的显微硬度分别进行分析发现,WCp相的硬度最高,能达到2000 HV0.2以上,而组织中的η相—Fe3 W3C相的硬度也能达到1100 HV0.2以上,而基体相由于固溶了一定的合金元素也表现较高的显微硬度,达到600-800 HV0.2左右。耐磨性能能够接近甚至达到粉末冶金硬质合金水平。
WC-based composite material was successfully fabricated by plasma in-situ metallurgy to break through the bottleneck of powder metallurgy cemented carbide in this paper. Microstructure and mechanical property were analyzed, reaction between W and C and the crystallizing process of WCP in a high temperature and C-rich situation were discussed.
The structure analysis results reveal that level of electric current would influence the mouldability of the final composite; Main phases in the composite obtained by plasma in-situ metallurgy are WC,W2C,M6C (Fe3W3C),y-Fe and small amount of Cr7C3 and (Fe, Ni)3C.The composite has a uniform microstructure and the triangle and rectangle shape hard phase is with the length of 5-30μm.
During the heating process of plasma in-situ metallurgy, the synchronously feeding powder and the matrix melst and form a molten bath together. Gases and slag produced by the intense reactions in the metallurgy area float upon. Once the crystal nucleus formed, it would grow up with a smooth solid-liquid interface.During the crystallization of WC, the anisotropy of crystal faces causes different surface energy of different crystal faces, then determine specific guillotine factor r and elongation k,then WC grain with characteristic of special morphological formed. WC crystal grow up along the crystal orientation<0001> based on (0001) crystal face because of the special construction of crystal and complex interfaces.
The average hardness of all the prepared WC composite materials could exceed HRA82. The WCP phase has the highest hardness and the microhardness of it can reach above 2000HV0.2; the microhardness of Fe3W3C phase can reach above 1100 HV0.2; the microhardness of the matrix can reach around 600-800 HV0.2 because of high solid solubility of alloy elements. And the property of wear-resisting could approach or even achieve the level of powder metallurgy cemented carbide.
组织分析结果表明,电流的大小直接影响最终得到复合材料的成型性；等离子原位冶金碳化钨中相组成主要为WC、W2C、M6C (Fe3W3C)、γ-Fe以及少量的Cr7C3和(Fe, Ni)3C,组织均匀,具有三角形或四边形的硬质相颗粒尺寸约为5-30μm。
等离子在原位冶金加热过程中,在等离子束高温作用下同步送入的粉末与基体共同形成熔池。冶金区剧烈反应产生的气体、熔渣上浮。WC成核后,以具有平滑固液界面的形式成长。在WC结晶过程中,由于晶面的各向异性等原因引起WC晶粒各晶面表面能的差异,决定了特定的截断因子r和伸长率k,生成具有特殊形貌的WC晶粒。晶粒的特殊结构和复杂的界面环境使WC晶粒以(0001)面为基面,沿<0001>方向生长形成多层堆垛结构。
得到的WC复合材料的平均硬度都能达到HRA82以上。对合金内部不同物相的显微硬度分别进行分析发现,WCp相的硬度最高,能达到2000 HV0.2以上,而组织中的η相—Fe3 W3C相的硬度也能达到1100 HV0.2以上,而基体相由于固溶了一定的合金元素也表现较高的显微硬度,达到600-800 HV0.2左右。耐磨性能能够接近甚至达到粉末冶金硬质合金水平。
WC-based composite material was successfully fabricated by plasma in-situ metallurgy to break through the bottleneck of powder metallurgy cemented carbide in this paper. Microstructure and mechanical property were analyzed, reaction between W and C and the crystallizing process of WCP in a high temperature and C-rich situation were discussed.
The structure analysis results reveal that level of electric current would influence the mouldability of the final composite; Main phases in the composite obtained by plasma in-situ metallurgy are WC,W2C,M6C (Fe3W3C),y-Fe and small amount of Cr7C3 and (Fe, Ni)3C.The composite has a uniform microstructure and the triangle and rectangle shape hard phase is with the length of 5-30μm.
During the heating process of plasma in-situ metallurgy, the synchronously feeding powder and the matrix melst and form a molten bath together. Gases and slag produced by the intense reactions in the metallurgy area float upon. Once the crystal nucleus formed, it would grow up with a smooth solid-liquid interface.During the crystallization of WC, the anisotropy of crystal faces causes different surface energy of different crystal faces, then determine specific guillotine factor r and elongation k,then WC grain with characteristic of special morphological formed. WC crystal grow up along the crystal orientation<0001> based on (0001) crystal face because of the special construction of crystal and complex interfaces.
The average hardness of all the prepared WC composite materials could exceed HRA82. The WCP phase has the highest hardness and the microhardness of it can reach above 2000HV0.2; the microhardness of Fe3W3C phase can reach above 1100 HV0.2; the microhardness of the matrix can reach around 600-800 HV0.2 because of high solid solubility of alloy elements. And the property of wear-resisting could approach or even achieve the level of powder metallurgy cemented carbide.
引文
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2. 李勇,谢淑华.WC粗晶硬质合金的研究进展[J].材料研究与应用,2009(2)：77-80
3. 王淑峰,李惠琪,迟静,李敏.等离子原位冶金快速制备钨基硬质合金的研究[J].山东科技大学学报(自然科学版),2010(1)：85-89
4. 崔洪芝,李惠琪,孙宏飞,孙玉宗,李敏,王灿明,赵增玉,姬强,张启明,姚树玉,宋强,陈聚武.等离子控制原位冶金反应技术与工程应用.中国科技奖励,2008(9)：53
5. 任莹.原位合成碳化钨增强金属陶瓷涂层的基础研究[D].天津：天津大学,2008
6. 迟静,李惠琪,王淑峰,李敏.矿用WC硬质合金的研究进展与趋势[J].矿山机械,2010(8)：23-28
7. 周建华,卢伟民.国内外硬质合金生产现状及近期发展动向分析[J].稀有金属与硬质合金,2006(1)：36-41
8. 张启修,赵秦生主编.钨钼冶金[M].北京：冶金工业出版社,2005
9. 王国栎.硬质合金原理[M].北京：冶金工业出版社,1988
10.饶岩岩,张久兴,王澈,张国珍.钨／钻氧化物SPS直接碳化原位合成超细WC-Co硬质合金[J].稀有金属与硬质合金,2006(1)：18-21
11. Jiuxing Zhang, Guozhen Zhang, Shixian Zhao. Binder-free WC bulk synthesized by spark plasma sintering[J]. Journal of Alloys and Compounds,2009,479(1-2):427-431
12. Anklekar R. M, Agrawal D. K, Roy R. Microwave sintering and mechanical Properties of PM copper steel[J]. Powder Metallurgy,2001,44(4):355-362
13.周建华,卢伟民.G413型矿用截齿的开发与应用[J].凿岩机械气动工具,2009(1)：27-30
14.李沐山.八十年代世界硬质合金技术进展[M].株洲：硬质合金编辑部,1992
15.孙东平.我国矿用硬质合金的发展现状与趋势[J].粉末冶金材料科学与工程,1998(4)：281-284
16. He Xianeng, Shi Jianhua. Study on technology for carburization of high quality coarse-grained WC[J]. Rare Metal Letters,2005(10):28-31
17.罗斌辉,张华明.不同氧化钨原料对钨粉性能的影响研究[J].硬质合金,2006(3)： 139-142
18.孙宝琦,陈一鸣.锂活化钨氧化物氢还原制取粗结晶钨粉过程的初步探讨[J].稀有金属与硬质合金,1999(1)
19.高辉.钨粉分级在粗晶碳化钨粉生产中的应用[J].硬质合金,2006(2)：92-96
20.黄新.优质粗晶WC粉末及合金的研制[D].重庆大学,2004
21.黄新,孙亚丽,颜态,唐凯,刘清才,何宪峰,李伟.两步碳化法生产优质粗颗粒WC粉末[J].中国钨业,2007(6)：39-42
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