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热压工艺对硅掺杂碳复合靶材的性能影响研究

Performance of Silicon-Doped Carbon Composite Target with Hot Pressing Process
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摘要 以碳粉、碳化硅粉体为原料,添加不同含量的硅粉为烧结助剂,在不同的热压工艺参数下制备C/Si 80%/20%(原子分数)复合靶材,通过扫描电镜(SEM)分析微观形貌、四探针测试电阻率、X射线衍射(XRD)分析晶体结构、压汞法测试气孔分布,分析Si粉的添加量、液相保温时间、原料预处理工艺对靶材致密化和均匀性的影响,优化硅碳复合(C/Si 80%/20%)靶材的热压烧结工艺。结果如下:(1)随着Si粉添加量增加,体系中液相含量增加,扩散传质速率加快,硅碳化合反应生成3C-SiC,体系中的Si元素全部以3C-SiC的形式存在,靶材的致密度逐渐增加,Si粉添加量为14%时,靶材的密度达到2.51 g·cm^(-3);开孔孔径分布随Si粉添加量的增加而逐渐减小至20 nm以下;靶材电阻率随Si粉添加量的增加而逐渐降低,Si粉添加量为14%时,电阻率降低50%。(2)在1350~1450℃,随着液相保温时间的增加,硅元素挥发并逸出,产生反致密化的现象,Si含量越高,反致密化越明显,密度降低至2.2 g·cm^(-3)。(3)采用SiC/C/Si 6%/74%/14%组分体系,C/Si预球磨48 h后再添加纳米SiC粉体继续球磨2 h制备复合原料粉体,在1980℃,70 MPa下,液相保温时间为1 h 15 min所制备靶材致密度达到2.51 g·cm^(-3),组织结构均匀,形貌呈层片状生长,无闭合气孔,电阻率最低为2.06×10^(-3)Ω·cm。 With high resistivity,high hardness,wear resistance,corrosion resistance,high thermal conductivity and other excellent properties like diamond,diamond-like carbon(DLC)films have been widely used in mechanical,optical,electrical,acoustic and thermal fields.The DLC film prepared by magnetron sputtering has the advantages of simple process,fast deposition rate,low deposition temperature,smooth and flat film surface during large-area film formation,which has attracted widespread attention in scientific research and commercial fields.Through liquid phase sintering technology,raw material pretreatment process and high temperature and pressure process,silicon doped carbon composite target with excellent performance was prepared by hot pressing method.Using carbon and silicon carbide powder as raw materials,silicon powder as sintering additives,C/Si 80%/20%(atom fraction)composite targets were prepared under different process parameters.The details were as follows:(1)Added 5%and 10%Si powders,respectively,mixed the powders evenly and put them in a mold.Then placed the mold in hot-pressing furnace.Kept holding time 1 h 15 min and 2 h 15 min at 1380~140℃,1 h 30 min at 1980℃and pressure 30 MPa,comparing the influence of different liquid-phase heat preservation time on target densification.(2)Raw materials with 0,5%,10%,12%and 14%silicon added respectively were mixing evenly and then hot-pressed under the following parameters:1380~1450℃for 1 h 15 min,1980℃for 1 h 30 min with pressure of 70 MPa.(3)SiC/C/Si 6%/74%/14%system was used as the research object.After C/Si powder was pre-ball milled for 48 h,nanoβ-SiC powder was added for another 2 h ball milling.Using this pretreatment powder,the silicon doped carbon target was prepared by hot pressing at 1380~1450℃for 1 h 15 min,1980℃for 1 h 30 min with pressure of 70 MPa.The microstructure was analyzed by scanning electron microscope(SEM),resistivity was measured by four probe method,crystal structure was analyzed by X-ray diffraction(XRD),pore distribution was measur
作者 白雪 刘宇阳 桂涛 王星奇 杨磊 王星明 Bai Xue;Liu Yuyang;Gui Tao;Wang Xingqi;Yang Lei;Wang Xingming(GRINM Resources and Environment Tech.Co.,Ltd,Beijing 101407,China)
出处 《稀有金属》 EI CAS CSCD 北大核心 2022年第4期538-544,共7页 Chinese Journal of Rare Metals
基金 国家自然科学基金项目(51674035) 有研科技集团有限公司青年基金项目(13161)资助。
关键词 硅粉 液相烧结 靶材 热压 C/Si silicon powder liquid phase sintering target hot pressing C/Si
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