CN107109633A - 铜合金溅射靶及其制造方法 - Google Patents
铜合金溅射靶及其制造方法 Download PDFInfo
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- CN107109633A CN107109633A CN201680004589.XA CN201680004589A CN107109633A CN 107109633 A CN107109633 A CN 107109633A CN 201680004589 A CN201680004589 A CN 201680004589A CN 107109633 A CN107109633 A CN 107109633A
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- 238000000034 method Methods 0.000 title claims abstract description 65
- 238000005477 sputtering target Methods 0.000 title claims abstract description 59
- 229910000881 Cu alloy Inorganic materials 0.000 title claims abstract description 41
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 239000010949 copper Substances 0.000 claims abstract description 75
- 238000002844 melting Methods 0.000 claims abstract description 69
- 230000008018 melting Effects 0.000 claims abstract description 69
- 229910052802 copper Inorganic materials 0.000 claims abstract description 66
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 61
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000001301 oxygen Substances 0.000 claims abstract description 43
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 43
- 239000007789 gas Substances 0.000 claims abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 35
- 229910052751 metal Inorganic materials 0.000 claims abstract description 35
- 239000002184 metal Substances 0.000 claims abstract description 35
- 238000005275 alloying Methods 0.000 claims abstract description 21
- 239000012298 atmosphere Substances 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000011261 inert gas Substances 0.000 claims abstract description 7
- 238000005223 charged particle activation analysis Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000003723 Smelting Methods 0.000 claims description 15
- 239000000956 alloy Substances 0.000 claims description 14
- 230000006698 induction Effects 0.000 claims description 14
- 229910045601 alloy Inorganic materials 0.000 claims description 13
- 239000001257 hydrogen Substances 0.000 claims description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 12
- 238000010894 electron beam technology Methods 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- 238000005096 rolling process Methods 0.000 claims description 4
- 238000005242 forging Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000010309 melting process Methods 0.000 claims description 2
- 229960004424 carbon dioxide Drugs 0.000 claims 1
- 229910002090 carbon oxide Inorganic materials 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 28
- 238000004544 sputter deposition Methods 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 description 26
- 125000004429 atom Chemical group 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 14
- 229910052782 aluminium Inorganic materials 0.000 description 8
- 238000009792 diffusion process Methods 0.000 description 8
- 229910052748 manganese Inorganic materials 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 239000010408 film Substances 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 238000007711 solidification Methods 0.000 description 6
- 230000008023 solidification Effects 0.000 description 6
- 238000007670 refining Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001036 glow-discharge mass spectrometry Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- DBGSRZSKGVSXRK-UHFFFAOYSA-N 1-[2-[5-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]acetyl]-3,6-dihydro-2H-pyridine-4-carboxylic acid Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NN=C(O1)CC(=O)N1CCC(=CC1)C(=O)O DBGSRZSKGVSXRK-UHFFFAOYSA-N 0.000 description 1
- AWFYPPSBLUWMFQ-UHFFFAOYSA-N 2-[5-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]-1-(1,4,6,7-tetrahydropyrazolo[4,3-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NN=C(O1)CC(=O)N1CC2=C(CC1)NN=C2 AWFYPPSBLUWMFQ-UHFFFAOYSA-N 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052765 Lutetium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000005097 cold rolling Methods 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 229910052571 earthenware Inorganic materials 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000007499 fusion processing Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- -1 so Afterwards Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D7/00—Casting ingots, e.g. from ferrous metals
- B22D7/005—Casting ingots, e.g. from ferrous metals from non-ferrous metals
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
- C22C9/01—Alloys based on copper with aluminium as the next major constituent
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
- C22C9/05—Alloys based on copper with manganese as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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- H01—ELECTRIC ELEMENTS
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- H01J37/32—Gas-filled discharge tubes
- H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
- H01J37/3411—Constructional aspects of the reactor
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- H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
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- H01L21/28512—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic Table
- H01L21/2855—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic Table by physical means, e.g. sputtering, evaporation
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- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
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Abstract
一种铜合金溅射靶,其特征在于,通过带电粒子活化分析而测定的、氧含量为0.6重量ppm以下、或者、氧含量为2重量ppm以下且碳含量为0.6重量ppm以下。另外,一种铜合金溅射靶的制造方法,其特征在于,对铜原料在真空或惰性气体气氛中进行熔炼,然后向熔炼中的气氛中加入还原气体,接着,向熔融金属中添加合金元素而进行合金化,并将所得到的锭加工为靶形状。本发明的课题是提供一种溅射时粉粒的产生少的铜合金溅射靶及其制造方法。
Description
技术领域
本发明涉及铜合金溅射靶及其制造方法,特别是适合于形成用作半导体集成电路中的布线的包含铜合金的薄膜的溅射靶及其制造方法。
背景技术
以往,使用Al(电阻率:约3.1μΩ·cm)作为半导体集成电路的布线材料,但是随着布线的微细化,电阻更低的Cu(电阻率:约1.7μΩ·cm)得以实用化。作为铜布线的形成工艺,多数情况下在布线层或布线槽形成Ta、TaN等扩散阻挡层,然后电镀铜。为了进行该电镀,作为基底层(籽晶层),一般进行将铜或铜合金溅射成膜。
但是,对于布线宽度为0.130nm以下、例如90nm、65nm、45nm、20nm这样的微细布线而言,籽晶层的厚度为小于布线宽度的极薄膜,在形成这样的极薄膜的籽晶层的情况下,存在因溅射时产生的粉粒引起的无法形成良好的籽晶层的问题。这样的籽晶层的形成是重要的,如果在籽晶层中存在粉粒,则会形成断线等缺陷。
作为半导体集成电路的布线形成用途,迄今为止,本申请人提出了涉及高纯度的铜或铜合金溅射靶的发明(参见专利文献1~3)。这些发明能够防止空隙、突起、断线等缺陷的产生、电阻率低、并且能够具有耐EM性、耐氧化性,但是,对于近年来更进一步的超微细布线而言,因极微量地含有的杂质引起的粉粒等越来越被视为问题。需要说明的是,虽然与本申请没有直接相关性,但是在专利文献4~6中公开了高纯度铜的制造方法。
现有技术文献
专利文献
专利文献1:国际公开第2004/083482号
专利文献2:国际公开第2008/041535号
专利文献3:日本特愿2013-045838
专利文献4:日本专利第4680325号
专利文献5:日本特开平8-92662号公报
专利文献6:日本特开2000-17345号公报
发明内容
发明所要解决的问题
本发明涉及适合于形成用作半导体集成电路的布线的包含铜合金的薄膜的铜合金溅射靶,其课题在于提供一种溅射时粉粒的产生少的铜合金溅射靶及其制造方法。
用于解决问题的手段
为了解决上述问题,本发明人进行了深入研究,结果发现:通过对作为溅射靶的原材料的铜合金锭的制造方法进行设计,能够减少铜合金溅射靶中所含的氧、碳,溅射时能够显著地抑制因该杂质引起的粉粒的产生。为了解决上述课题,本发明提供下述发明。
1)一种铜合金溅射靶,其特征在于,通过带电粒子活化分析而测定的、氧含量为0.6重量ppm以下、或者、氧含量为2重量ppm以下且碳含量为0.6重量ppm以下。
2)如上述1)所述的铜合金溅射靶,其特征在于,合金元素为与氧或碳的亲和力比Cu高的元素中的一种以上。
3)一种铜合金溅射靶的制造方法,其特征在于,对铜原料在真空或惰性气体气氛中进行熔炼,然后向熔炼中的气氛中加入还原气体,接着,向熔融金属中添加合金元素而进行合金化,并将所得到的锭加工为靶形状。
4)如上述3)所述的铜合金溅射靶的制造方法,其特征在于,还原气体包含氢气或一氧化碳。
5)如上述3)或4)所述的铜合金溅射靶的制造方法,其特征在于,熔炼工序通过等离子体电弧熔炼法、电子束熔炼法、感应熔炼法等进行。
6)如上述3)~5)中任一项所述的铜合金溅射靶的制造方法,其特征在于,各熔炼处理在不同的坩埚内进行熔炼。
7)如上述3)~6)中任一项所述的铜合金溅射靶的制造方法,其特征在于,将铜引入水冷铜坩埚中,在氩气气氛中通过等离子体电弧熔炼法进行熔炼,然后向熔炼中的气氛中加入氢气,接着,将熔融金属引入下一阶段的水冷铜坩埚中,添加合金元素,然后通过等离子体电弧熔炼法进行合金化,使所得到的锭经过锻造、轧制、热处理,从而制成溅射靶原材料,对该靶原材料进行机械加工,从而加工成靶形状。
发明效果
本发明具有如下优良的效果:能够显著地减少铜合金溅射靶中所含的杂质、特别是氧、碳,能够抑制溅射时粉粒的产生。
具体实施方式
本发明的铜合金溅射靶的特征在于,通过带电粒子活化分析而测定的、氧含量为0.6重量ppm以下、或者、氧含量为2重量ppm以下且碳含量为0.6重量ppm以下。以往,已知对铜原料进行熔炼而除去金属、气体等杂质从而制作高纯度铜的技术,但是在想要制作高纯度铜合金的情况下,有时铜中所含的氧、碳会转移至合金元素而残留。本发明通过对制造方法进行设计从而对于铜合金而言也能够极其有效地减少氧、碳。
本发明中,带电粒子活化分析是化学分析的一种方法,利用氘核、中子、γ射线等照射试样而使其活化,并对其放射性同位素进行跟踪,由此进行试样中所含的各种元素的定性、定量。在本发明中,能够显著减少铜合金溅射靶中所含的氧、碳,由此,能够有效地抑制溅射时的粉粒的产生。需要说明的是,利用该分析方法的定量下限为氧:0.1重量ppm、碳:0.1重量ppm。
不言而喻,本发明的铜合金是高纯度的,纯度优选为99.999重量%(5N)以上。纯度使用辉光放电质谱法(GDMS分析)对靶中含有的除铜和合金元素以外的金属杂质的含量进行测定并通过差值法(将100重量%减去金属杂质后的量作为纯度重量%)求出。杂质为Ag、Al、Ca、Cr、Fe、K、Na、Ni、P、S、Th、U。
作为构成本发明的铜合金溅射靶的合金元素,优选为与氧或碳的亲和力比铜高的元素中的任意一种以上。可以列举例如:Al、Mn、Co、Ni、Mg、Ti、Si、In、Sn、Ge、Bi、B、Cr、Nd、Zr、La、Er、Gd、Dy、Yb、Lu、Hf、Ta。这些合金元素是能够改善半导体元件的布线的特性的公知材料,为了改善特性,也可以将多种材料组合添加。它们的添加量根据所要求的特性而不同,优选例如为:Al:0.1~15.0原子%、Mn:0.1~30.0原子%。
接着,对本发明的铜合金溅射靶的制造方法进行说明。首先,准备作为原料的铜和合金材料(Al、Mn等)。这些原料优选使用尽可能高纯度的材料,铜使用纯度6N以上的铜、合金元素使用纯度4N以上的合金元素是有效的。接着,称量这些原料以得到期望的组成,然后,仅将铜原料引入水冷铜坩埚(包括熔炉(ハース))中。作为坩埚材料,有氧化铝、氧化镁、石墨等耐火材料,但是有时会以杂质的形式混入熔融金属中,因此,可以使用与被熔炼材料相同材质的铜。由此,即使坩埚材料熔出至熔融金属中,也不会成为杂质。
接着,将铜原料在真空或惰性气体(Ar、He等)气氛中对铜进行熔炼。此时,通过在惰性气体气氛中进行熔炼,能够抑制成分的挥发。熔炼可以使用等离子体电弧熔炼法、电子束熔炼法、感应熔炼法等。然后,向该熔炼过程中的气氛中加入还原气体(氢气、一氧化碳等)。由此,能够有效地除去铜中所含的氧。作为所引入的气体量,在等离子体熔炼法的情况下,优选在惰性气体中加入0.1体积%~20体积%的还原气体。在电子束熔炼法的情况下,优选以400ml/分钟以上的流量向真空中加入还原气体。
在此,还原气体的加入优选在真空或惰性气体气氛中进行熔炼而使铜中所含的氧和碳以一氧化碳的形式充分脱离后进行。充分地除去碳后,可以利用还原气体使多余的氧以水蒸气(H2O)、二氧化碳(CO2)的形式脱离,能够极其有效地减少作为杂质在铜中含有的碳和氧。当然,并不限于在对铜进行熔炼的相对初期(未充分地除去碳)的阶段加入还原气体。
接着,将所得到的铜的熔融金属引入下一阶段的水冷铜坩埚(包括熔炉)中,添加合金元素,然后,使用等离子体电弧熔炼法、电子束熔炼法、感应熔炼法等制成铜合金。特别重要的是:对除去氧、碳后的铜的熔融金属添加合金元素,并进行熔炼。这是因为:如果向进行脱气前的铜中添加合金元素并进行熔炼,则铜中所含的氧、碳纳入合金元素中,从而形成氧化物、碳化物,熔炼后这些杂质也会残留在合金锭中。因此,添加合金元素的时机非常重要。
接着,将铜合金的熔融金属引入水冷铜模具中,通过感应熔炼法等进行熔炼,并且从模具的底部拉出凝固的锭。然后,除去所制造的锭的表面层,经过塑性加工、热处理工序,从而制成溅射靶原材料。然后,可以通过机械加工将该靶原材料加工成规定的靶形状,从而得到铜合金溅射靶。
实施例
接着,基于实施例对本发明进行说明。以下所示的实施例是为了易于理解,并不是通过这些实施例来限制本发明。即,基于本发明的技术构思的变形和其它实施例当然也包含在本发明中。
(实施例1)
准备纯度6N以上的Cu,将其引入水冷铜坩埚中,利用等离子体电弧熔炼法在引入了4体积%氢气的氩气气氛下照射等离子体而进行熔炼。然后,将该熔融金属引入水冷铜坩埚中,添加纯度4N以上的Al使得其达到1原子%,并通过等离子体电弧熔炼法进行熔炼。接着,将铜合金的熔融金属浇注到水冷铜模具中,通过真空感应熔炼进行熔炼,并且从模具的底部拉出凝固的锭。
接着,将该锭制成直径180mm×厚度160mm,然后在700℃进行热锻,然后通过冷轧轧制至直径460mm×厚度24.5mm。然后,在400℃进行热处理,然后进行骤冷而制作出轧制板。对该轧制板进行机械加工,由此制造出直径440mm、厚度16.5mm的溅射靶。然后,通过扩散接合将该溅射靶与背衬板接合。
对于切割出的锭的一部分考察杂质浓度。需要说明的是,对于金属成分使用GDMS法,对于气体成分(氧、碳)使用带电粒子活化分析。其结果是,金属杂质的合计含量为1重量ppm以下,气体成分中碳为0.7重量ppm、氧为0.3重量ppm,特别是能够显著地降低氧的气体成分的浓度。
对靶进行溅射直到100kWh,在输入功率为38kW下在12英寸的硅基板上进行5秒钟成膜。对于所形成的膜,对0.088μm以上的尺寸的粉粒数进行测量,结果为8个,是良好的结果。然后,对于200kWh、300kWh、500kWh、800kWh的寿命位置分别对基板上的粉粒数进行测量,结果遍及整个寿命为10个以下,得到了良好的结果。
(实施例2)
准备纯度6N以上的Cu,将其引入水冷铜坩埚中,通过等离子体电弧熔炼法在氩气气氛下照射等离子体而进行熔炼。然后,向熔炼中的气氛中加入4体积%的氢气,再进行熔炼。然后,将该熔融金属引入下一阶段的水冷铜坩埚中,添加纯度4N以上的Al使得其达到1原子%,通过等离子体电弧熔炼法进行熔炼。接着,将熔融金属浇注到水冷铜模具中,通过真空感应熔炼进行熔炼,并且从模具的底部拉出凝固的锭。
接着,通过与实施例1同样的方法、条件将该合金锭加工成溅射靶,然后,通过扩散接合将该溅射靶与背衬板接合。对切割出的锭的一部分考察杂质浓度,结果是金属杂质的合计含量为1重量ppm以下,气体成分中碳为0.2重量ppm、氧为0.3重量ppm,能够显著地降低碳、氧两者的气体成分的浓度。另外,与实施例1同样地实施溅射、并测量粉粒数,结果遍及整个寿命为8个以下,得到了良好的结果。
(实施例3)
准备纯度6N以上的Cu,将其引入水冷铜坩埚中,在向真空中以400ml/分钟以上的流量加入氢气的气氛下,通过电子束熔炼法进行熔炼。然后,将该熔融金属引入下一阶段的水冷铜坩埚中,添加纯度4N以上的高纯度Al使得其达到1原子%,通过电子束熔炼法进行熔炼。接着,将熔融金属浇注到水冷铜模具中,通过真空感应熔炼进行熔炼,并且从模具的底部拉出凝固的锭。
接着,通过与实施例1同样的方法、条件将该合金锭加工成溅射靶,然后,通过扩散接合将该溅射靶与背衬板接合。对切割出的锭的一部分考察杂质浓度,结果是金属杂质的合计含量为1重量ppm以下,气体成分中碳为0.6重量ppm、氧为0.8重量ppm,特别是能够显著地降低碳的气体成分的浓度。另外,与实施例1同样地实施溅射、并测量粉粒数,结果得到了遍及整个寿命为12个以下这样的结果。将上述结果示于表1中。
(实施例4)
准备纯度6N以上的Cu,将其引入水冷铜坩埚中,在真空中通过电子束熔炼法进行熔炼。然后,向熔炼中的气氛中以400ml/分钟以上的流量加入氢气,再进行熔炼。然后,将该熔融金属引入下一阶段的水冷铜坩埚中,添加纯度4N以上的高纯度Al使得其达到1原子%,通过电子束熔炼法进行熔炼。接着,将熔融金属浇注到水冷铜模具中,通过真空感应熔炼进行熔炼,并且从模具的底部拉出凝固的锭。
接着,通过与实施例1同样的方法、条件将该合金锭加工成溅射靶,然后,通过扩散接合将该溅射靶与背衬板接合。对切割出的锭的一部分考察杂质浓度,结果是金属杂质的合计含量为1重量ppm以下,气体成分中碳为0.2重量ppm、氧为0.9重量ppm,特别是能够显著地降低碳的气体成分的浓度。另外,与实施例1同样地实施溅射、并测量粉粒数,结果得到了遍及整个寿命为10个以下这样的结果。将上述结果示于表1中。
[表1]
(实施例5-12)
如表1所记载的,将Al的添加量变为2原子%(实施例5-8)、4原子%(实施例9-12),分别使用与实施例1同样的方法,制作出合金锭和溅射靶。其结果均是金属杂质的合计含量为1重量ppm以下、碳为1重量ppm以下、氧为1重量ppm以下,能够显著地降低气体成分的浓度。另外,与实施例1同样地实施溅射、并测量粉粒数,结果得到了遍及整个寿命为13个以下这样良好的结果。
(实施例13-24)
如表1所记载的,将添加元素设定为Mn,将Mn的添加量变为1原子%(实施例13-16)、2原子%(实施例17-20)、4原子%(实施例21-24),分别使用与实施例1同样的方法,制作出合金锭和溅射靶。其结果均是金属杂质的总含量为1重量ppm以下、碳为0.6重量ppm以下、氧为2重量ppm以下,能够显著地降低气体成分的浓度。另外,与实施例1同样地实施溅射、并测量粉粒数,结果得到了遍及整个寿命为9个以下这样良好的结果。
(比较例1)
准备纯度6N以上的高纯度Cu,将其引入水冷铜坩埚中,通过等离子体电弧熔炼法在氩气气氛下照射等离子体,由此进行熔炼。需要说明的是,未进行还原气体的加入。然后,将该熔融金属引入下一阶段的水冷铜坩埚中,添加纯度4N以上的高纯度Al使得其达到1原子%,通过等离子体电弧熔炼法进行熔炼。接着,将该熔融金属浇注到水冷铜模具中,通过真空感应熔炼进行熔炼,并且从模具的底部拉出凝固的锭。
接着,通过与实施例1同样的方法、条件将该锭加工成溅射靶,然后,通过扩散接合将该溅射靶与背衬板接合。对切割出的锭的一部分考察杂质浓度,结果是气体成分中碳为0.2重量ppm、氧为10重量ppm,关于氧值,为与引入了氢气时相比较高的结果。另外,与实施例1同样地实施溅射、并测量粉粒数,结果发现了偶尔最多30个的大量粉粒。
(比较例2)
准备纯度6N以上的Cu、1原子%的纯度5N以上的Al,将其引入水冷铜坩埚中,对Cu、Al同时利用等离子体电弧熔炼法通过在引入了4体积%氢气的氩气气氛下照射等离子体而进行熔炼。然后,将该熔融金属浇注到水冷铜模具中,通过真空感应熔炼进行熔炼,并且从模具的底部拉出凝固的锭。
接着,通过与实施例1同样的方法、条件将该合金锭加工成溅射靶,然后,通过扩散接合将该溅射靶与背衬板接合。对切割出的锭的一部分考察杂质浓度,结果是气体成分中碳为0.9重量ppm、氧为0.8重量ppm,与之后添加Al的情况相比,为略高的值。另外,与实施例1同样地实施溅射、并测量粉粒数,结果发现了偶尔最多20个的大量粉粒。
(比较例3)
准备纯度6N以上的Cu、1原子%的纯度5N以上的Al,将其引入水冷铜坩埚中,对Cu、Al同时利用等离子体电弧熔炼法通过在氩气气氛下照射等离子体而进行熔炼。然后,向熔炼中的气氛中加入4体积%的氢气,再进行熔炼。接着,将熔融金属浇注到水冷铜模具中,通过真空感应熔炼进行熔炼,并且从模具的底部拉出凝固的锭。
接着,通过与实施例1同样的方法、条件将该合金锭加工成溅射靶,然后,通过扩散接合将该溅射靶与背衬板接合。对切割出的锭的一部分考察杂质浓度,结果是气体成分中碳为0.9重量ppm、氧为1重量ppm,与之后添加Al的情况相比,为略高的值。另外,与实施例1同样地实施溅射、并测量粉粒数,结果发现了偶尔最多为19个的大量粉粒。
(比较例4)
准备纯度6N以上的Cu、1原子%的纯度5N以上的Al,将其引入水冷铜坩埚中,对Cu、Al同时在向真空中以400ml/分钟以上的流量加入氢气的气氛下通过电子束熔炼法进行熔炼。接着,将熔融金属浇注到水冷铜模具中,通过真空感应熔炼进行熔炼,并且从模具的底部拉出凝固的锭。
接着,通过与实施例1同样的方法、条件将该合金锭加工成溅射靶,然后,通过扩散接合将该溅射靶与背衬板接合。对切割出的锭的一部分考察杂质浓度,结果是气体成分中碳为1重量ppm、氧为3重量ppm,与加入了还原气体的情况相比,为较高的值。另外,与实施例1同样地实施溅射、并测量粉粒数,结果发现了偶尔最多为23个的大量粉粒。
(比较例5)
准备纯度6N以上的Cu,将其引入水冷铜坩埚中,在真空中通过电子束熔炼法进行熔炼。需要说明的是,未进行还原气体的加入。然后,将该熔融金属引入下一阶段的水冷铜坩埚中,添加纯度4N以上的高纯度Al使得其达到1原子%,通过电子束熔炼法进行熔炼。接着,将熔融金属浇注到水冷铜模具中,通过真空感应熔炼进行熔炼,并且从模具的底部拉出凝固的锭。
接着,通过与实施例1同样的方法、条件将该合金锭加工成溅射靶,然后,通过扩散接合将该溅射靶与背衬板接合。对切割出的锭的一部分考察杂质浓度,结果是气体成分中碳为0.2重量ppm、氧为4重量ppm,与加入了还原气体的情况相比,氧值为较高的值。另外,与实施例1同样地实施溅射、并测量粉粒数,结果发现了偶尔最多为26个的大量粉粒。
(比较例6-15)
如表1所记载的,将Al的添加量变为2原子%(比较例6-10)、4原子%(比较例11-15),分别使用与比较例1同样的方法制作出合金锭和溅射靶。其结果是,氧为1重量ppm以上,氧的降低不充分。另外,与实施例1同样地实施溅射、并测量粉粒数,结果增加至遍及整个寿命最多为18个以上。
(比较例16-30)
如表1所记载的,将添加元素设定为Mn,将Mn的添加量变为1原子%(比较例16-20)、2原子%(比较例21-25)、4原子%(比较例26-30),分别使用与比较例1同样的方法制作出合金锭和溅射靶。其结果均是氧为3重量ppm以上,氧的降低不充分。另外,与实施例1同样地实施溅射、并测量粉粒数,结果增加到遍及整个寿命最多为14个以上。
产业实用性
本发明能够制造氧、碳极少的铜合金溅射靶,在使用这样的靶进行溅射的情况下,能够显著地抑制粉粒的产生。通过本发明制造的铜合金溅射靶特别是对于半导体集成电路的布线膜形成是有用的。
Claims (7)
1.一种铜合金溅射靶,其特征在于,通过带电粒子活化分析而测定的、氧含量为0.6重量ppm以下、或者、氧含量为2重量ppm以下且碳含量为0.6重量ppm以下。
2.如权利要求1所述的铜合金溅射靶,其特征在于,合金元素为与氧或碳的亲和力大于Cu的元素中的一种以上。
3.一种铜合金溅射靶的制造方法,其特征在于,对铜原料在真空或惰性气体气氛中进行熔炼,然后向熔炼中的气氛中加入还原气体,接着,向熔融金属中添加合金元素而进行合金化,并将所得到的合金锭加工为靶形状。
4.如权利要求3所述的铜合金溅射靶的制造方法,其特征在于,还原气体包含氢气或一氧化碳。
5.如权利要求3或4所述的铜合金溅射靶的制造方法,其特征在于,熔炼工序通过等离子体电弧熔炼法、电子束熔炼法、感应熔炼法进行。
6.如权利要求3~5中任一项所述的铜合金溅射靶的制造方法,其特征在于,各熔炼处理在不同的坩埚内进行熔炼。
7.如权利要求3~6中任一项所述的铜合金溅射靶的制造方法,其特征在于,将铜引入水冷铜坩埚中,在氩气气氛中通过等离子体电弧熔炼法进行熔炼,然后向熔炼中的气氛中加入氢气,接着,将熔融金属引入下一阶段的水冷铜坩埚中,添加合金元素,然后通过等离子体电弧熔炼法进行合金化,使所得到的锭经过锻造、轧制、热处理,从而得到溅射靶原材料,对该靶原材料进行机械加工,从而加工成靶形状。
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US20170342546A1 (en) | 2017-11-30 |
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