CN1096061A - 溅射法沉积难熔金属碳化物纳米晶 - Google Patents
溅射法沉积难熔金属碳化物纳米晶 Download PDFInfo
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- CN1096061A CN1096061A CN 93111176 CN93111176A CN1096061A CN 1096061 A CN1096061 A CN 1096061A CN 93111176 CN93111176 CN 93111176 CN 93111176 A CN93111176 A CN 93111176A CN 1096061 A CN1096061 A CN 1096061A
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- sputtering
- torr
- argon gas
- applying argon
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- 238000004544 sputter deposition Methods 0.000 title claims abstract description 32
- 238000000151 deposition Methods 0.000 title claims description 6
- 239000013078 crystal Substances 0.000 title description 6
- 230000008021 deposition Effects 0.000 title description 2
- 238000002844 melting Methods 0.000 title description 2
- 230000008018 melting Effects 0.000 title description 2
- 229910052751 metal Inorganic materials 0.000 title description 2
- 239000002184 metal Substances 0.000 title description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052786 argon Inorganic materials 0.000 claims abstract description 15
- 239000007789 gas Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000009792 diffusion process Methods 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- 239000003870 refractory metal Substances 0.000 claims abstract description 6
- 239000002159 nanocrystal Substances 0.000 claims abstract description 5
- 239000010955 niobium Substances 0.000 claims abstract description 5
- 238000004062 sedimentation Methods 0.000 claims abstract description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 3
- 239000011733 molybdenum Substances 0.000 claims abstract description 3
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 3
- 239000010936 titanium Substances 0.000 claims abstract description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 3
- 239000010937 tungsten Substances 0.000 claims abstract description 3
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 6
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 239000000758 substrate Substances 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 229910021419 crystalline silicon Inorganic materials 0.000 description 4
- 239000002932 luster Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002707 nanocrystalline material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000005546 reactive sputtering Methods 0.000 description 1
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- Physical Vapour Deposition (AREA)
Abstract
一种金属碳化物纳米晶的制备方法,适合于难熔
金属如钛、铌、钽、钼、钨,其特征在于工艺过程和参数
如下:用机械泵和扩散泵将真空抽到10-5—
10-6Torr;充氩气;用纯难熔金属作靶,靶极距50~
80mm,无外界加热和冷却,直接溅射沉积。本发明
工艺简单易行。
Description
本发明涉及纳米材料的制备,特别是难熔金属碳化物纳米晶的制备技术。
纳米晶材料是近几年新发展起来的亚稳材料,由于其晶粒非常细小,因而其内部晶界所占的比例非常大,从而表现出与常规晶体材料截然不同的性能,这主要体现在机械强度、热膨胀系数、磁学性能、蠕变性能,光学性能、电子性能等。碳化物本身具有较高的强度,纳米晶碳化物的机械性能则更加优越。纳米材料一般可通过气相沉积方法得到,但用此法得到的纳米晶大多为单组元材料,对其它合金材料和化合物材料则存在很大的局限性。溅射沉积通常被有效地用来制备合金以及化合物材料,对碳化物来说,通常利用反应溅射方法得到,但这种方法工艺较复杂。
本发明的目的在于提供一种制备难熔金属碳化物的方法,其工艺简单易行。
本发明所提供的金属碳化物纳米晶的制备方法,适合于难熔金属如钛、铌、钽、钼、钨,其特征在于工艺过程和参数如下:
-用机械泵和扩散泵将真空抽到10-5-10-6Torr;
-充氩气;
-用纯难熔金属作靶,靶极距50~80mm,无外界加热和冷却,直接溅射沉积。
当用直流溅射法进行沉积时,充氩气到10-4-10-5Torr,溅射电压0.7~2KV,电流30~80mA。当用磁控溅射法进行沉积时,充氩气到10-2-10-3Torr,溅射电压300~500V,电流2~4A,功率密度为5~20w/cm2。
实施例1
用机械泵和扩散泵将真空抽到9×10-5Torr,充氩气到5×10-4Torr,用Nb(99%)作靶,靶极距70mm,采用直流溅射,溅射电压1KV,电流50mA,溅射时间40分钟,基板为抛光单晶硅,得到厚度1微米、表面光泽度很好的薄膜,薄膜结构由X-射线衍射、透射电镜分析得到结构为NbC,晶粒尺寸5纳米左右。成分沿深度方向均匀性由俄歇电子能谱结合离子剥落分析,结果表明成分分布均匀。
实施例2
用机械泵和扩散泵将真空抽到8×10-5Torr,充氩气到3×10-4Torr,用纯Mo(99%)作靶,靶极距70mm,采用直流溅射,溅射电压1.2KV,电流40mA,溅射时间为60分钟,基板为单晶Si,得到膜厚度为1微米、表面光泽度较好。薄膜结构由X-射线衍射,透射电镜分析得到为Mo2C,晶粒尺寸约为8纳米。纳米晶Mo2C膜的成分均匀性由俄歇电子能谱结合离子剥落进行分析,结果表明此膜成分很均匀。
实施例3
用机械泵和扩散泵将真空抽到8×10-5Torr,充氩气到7×10-4Torr,用纯Ta(99.9%)靶,靶极距75mm。采用直流溅射,溅射电压0.9KV,电流为50mA,溅射时间为45分钟,基板为玻璃,得到膜厚度为0.8微米,表面光泽度很好。薄膜结构由X-射线衍射,透射电镜分析为TaC,晶粒尺寸为10纳米。
实施例4
用机械泵和扩散泵将真空抽到7×10-5Torr,充氩气到5×10-4Torr,用纯W(99%)靶,靶极距50mm。采用直流溅射,溅射电压1KV,电流45mA。溅射时间为50分钟,基板为单晶硅(Si),得到膜厚度为0.8微米,表面光泽度较好。薄膜结构由X-射线衍射,透射电镜分析得到为WC,晶粒尺寸约为5纳米。
实施例5
用机械泵和扩散泵将真空抽到5×10-5Torr,充氩气到3×10-3Torr,用Mo(99%)靶,靶极距80mm,采用磁控溅射,溅射电压460V,电流4A,溅射时间为50分钟,基板为单晶Si,得到膜厚度为0.9微米,表面光泽。薄膜经X-射线衍射和电镜观察被确定为Mo2C,晶粒尺寸约为7纳米。
实施例6
用机械泵和扩散泵将真空抽到7×10-5Torr,充氩气到9×10-2Torr,用Nb(99%)靶,靶极距80mm,采用磁控溅射,溅射电压420V,电流3A,溅射时间为40分钟,基板为单晶Si,得到膜厚度为0.7微米,表面光泽。薄膜经X-射线衍射和电镜观察被确定为NbC,晶粒尺寸约为9纳米。
实施例7
用机械泵和扩散泵将真空抽到3×10-5Torr,充氩气到8×10-3Torr,用Ta(99.9%)靶,靶极距75mm,采用磁控溅射,溅射电压400V,电流3.2A,溅射时间为50分钟,基板为单晶Si,得到膜厚度为0.8微米,表面光泽。薄膜经X-射线衍射和电镜观察被确定为TaC,晶粒尺寸约为12纳米。
实施例8
用机械泵和扩散将真空抽到9×10-6Torr,充氩气到2×10-3Torr,用W(99%)靶,靶极距70mm,采用磁控溅射,溅射电压420V,电流3.1A,溅射时间为50分钟,基板为玻璃,得到膜厚度为0.7微米,表面光泽。薄膜经X-射线衍射和电镜观察被确定为WC,晶粒尺寸为9纳米。
Claims (3)
1、一种金属碳化物纳米晶的制备方法,适合于难熔金属如钛、铌、钽、钼、钨,其特征在于工艺过程和参数如下:
--用机械泵和扩散泵将真空抽到10-5-10-6Torr;
--充氩气;
--用纯难熔金属作靶,靶极距50~80mm,无外界加热和冷却,直接溅射沉积。
2、按权利要求1所述金属碳化物纳米晶的制备方法,其特征在于,当用直流溅射法进行沉积时,充氩气到10-4-10-5Torr,溅射电压0.7~2KV,电流30~80mA。
3、按权利要求1所述金属碳化物纳米晶的制备方法,其特征在于当用磁控溅射法进行沉积时,充氩气到10-2-10-3Torr,溅射电压300~500V,电流2~4A,功率密度为5~20w/cm2。
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CN 93111176 CN1096061A (zh) | 1993-05-29 | 1993-05-29 | 溅射法沉积难熔金属碳化物纳米晶 |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN100500924C (zh) * | 2006-08-10 | 2009-06-17 | 中国科学院微电子研究所 | 一种金属纳米晶薄膜的制备方法 |
CN105862131A (zh) * | 2016-06-03 | 2016-08-17 | 武汉工程大学 | 一种利用mpcvd制备碳化钼晶体时钼的引入方法 |
CN113436946A (zh) * | 2021-06-25 | 2021-09-24 | 广东粤港澳大湾区国家纳米科技创新研究院 | 一种金属碳化物针尖及其制备方法和应用、电子枪 |
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1993
- 1993-05-29 CN CN 93111176 patent/CN1096061A/zh active Pending
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN100500924C (zh) * | 2006-08-10 | 2009-06-17 | 中国科学院微电子研究所 | 一种金属纳米晶薄膜的制备方法 |
CN105862131A (zh) * | 2016-06-03 | 2016-08-17 | 武汉工程大学 | 一种利用mpcvd制备碳化钼晶体时钼的引入方法 |
CN113436946A (zh) * | 2021-06-25 | 2021-09-24 | 广东粤港澳大湾区国家纳米科技创新研究院 | 一种金属碳化物针尖及其制备方法和应用、电子枪 |
CN113436946B (zh) * | 2021-06-25 | 2022-12-30 | 广东粤港澳大湾区国家纳米科技创新研究院 | 一种金属碳化物针尖及其制备方法和应用、电子枪 |
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