TWI651426B - 鉭濺鍍靶及其製造方法 - Google Patents
鉭濺鍍靶及其製造方法 Download PDFInfo
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- TWI651426B TWI651426B TW104108593A TW104108593A TWI651426B TW I651426 B TWI651426 B TW I651426B TW 104108593 A TW104108593 A TW 104108593A TW 104108593 A TW104108593 A TW 104108593A TW I651426 B TWI651426 B TW I651426B
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- 238000005477 sputtering target Methods 0.000 title claims abstract description 52
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 206010036790 Productive cough Diseases 0.000 title 1
- 210000003802 sputum Anatomy 0.000 title 1
- 208000024794 sputum Diseases 0.000 title 1
- 238000004544 sputter deposition Methods 0.000 claims abstract description 109
- 238000003490 calendering Methods 0.000 claims abstract description 24
- 239000013078 crystal Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000000137 annealing Methods 0.000 claims abstract description 15
- 238000001953 recrystallisation Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 3
- 150000004767 nitrides Chemical class 0.000 claims description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 10
- 238000005266 casting Methods 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 28
- 238000005242 forging Methods 0.000 abstract description 20
- 238000001354 calcination Methods 0.000 abstract description 12
- 230000001186 cumulative effect Effects 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 5
- 238000005096 rolling process Methods 0.000 description 27
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 18
- 229910052707 ruthenium Inorganic materials 0.000 description 18
- 229910052715 tantalum Inorganic materials 0.000 description 18
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 18
- 230000004888 barrier function Effects 0.000 description 12
- 238000009792 diffusion process Methods 0.000 description 12
- 239000010410 layer Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 8
- 239000010949 copper Substances 0.000 description 8
- 239000007789 gas Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 6
- 238000005097 cold rolling Methods 0.000 description 6
- 229910052750 molybdenum Inorganic materials 0.000 description 6
- 239000011733 molybdenum Substances 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000010955 niobium Substances 0.000 description 4
- 229910052758 niobium Inorganic materials 0.000 description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 4
- 239000010937 tungsten Substances 0.000 description 4
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 235000012431 wafers Nutrition 0.000 description 4
- 230000005611 electricity Effects 0.000 description 3
- 210000001161 mammalian embryo Anatomy 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010273 cold forging Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
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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
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- B21B—ROLLING OF METAL
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- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
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- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
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- C21D8/0273—Final recrystallisation annealing
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
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- 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
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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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
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- H—ELECTRICITY
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- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
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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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- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
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Abstract
一種鉭濺鍍靶,其特徵在於:濺鍍面之(100)面的位向率為30~90%,(111)面的位向率在50%以下。一種鉭濺鍍靶之製造方法,其特徵在於:係對經熔解鑄造之鉭鑄錠進行鍛造及再結晶退火後,進行壓延及熱處理,形成鉭濺鍍靶之(100)面的位向率為30~90%,(111)面的位向率在50%以下的結晶組織。
藉由控制靶之結晶位向,具有下述效果:減少鉭靶之預燒累積電力消耗量,使電漿容易產生,使成膜速度穩定化,減少膜之電阻變動。
Description
本發明係關於一種鉭濺鍍靶及其製造方法。尤其是關於一種用於形成LSI中作為銅配線之擴散阻擋層的Ta膜或TaN膜的鉭濺鍍靶及其製造方法。
以往,一直使用鋁作為半導體元件之配線材料,但隨著元件之微細化、高積集化,浮現出配線延遲之問題,而開始使用電阻較小之銅來代替鋁。銅作為配線材料非常有效,但由於銅本身為活潑之金屬,故會有擴散至層間絕緣膜而造成污染之問題,必須於銅配線與層間絕緣膜之間形成Ta膜或TaN膜等擴散阻擋層。
通常,Ta膜或TaN膜係藉由對鉭靶進行濺鍍來形成。迄今為止對於鉭靶,關於對濺鍍時之性能造成之影響,已知靶所含有之各種雜質、氣體成分、結晶之面方位或結晶粒徑等會對成膜速度、膜厚之均勻性、顆粒(particle)產生等造成影響。
例如,於專利文獻1記載有:自靶厚之30%的位置朝向靶之中心面,形成為(111)位向優先的結晶組織,藉此提升膜之均勻性。
又,於專利文獻2記載有:使鉭靶之結晶位向為無規(未統一於特定之結晶方位),藉此提高成膜速度,提升膜之均勻性。
又,於專利文獻3記載有:於濺鍍面選擇性地增多原子密度高之(110)、
(100)、(211)之面方位,藉此提升成膜速度,且藉由抑制面方位之變動來提升均勻性。
並且,於專利文獻4記載有:使利用X射線繞射求出之(110)面強度比因濺鍍表面部分之位置所造成之變動在20%以內,藉此提升膜厚均勻性。
又,於專利文獻5記述有:將型鍛(swaging)、擠出、旋轉鍛造、無潤滑之鍛粗鍛造與時脈軋製(clock rolling)組合使用,可製作具有非常強之(111)、(100)等之結晶學織構的圓形金屬靶。
其他,於下述專利文獻6,記載有一種鉭濺鍍靶之製造方法,係對鉭鑄錠實施鍛造、退火、壓延加工,於最後組成加工後,進一步以1173K以下之溫度進行退火,使未再結晶組織在20%以上90%以下。
又,於專利文獻7,揭示有如下之技術:藉由鍛造、冷壓延等加工與熱處理,使靶濺鍍面之波峰的相對強度為(110)>(211)>(100),使濺鍍特性穩定化。通常,(110)由於會因加工應變而變高,故經以此方式加工之表面其濺鍍速率會變快,藉由預燒去除表層會提早結束,具有早點露出穩定區域之效果,故具有採用此種(110)之傾向。
又,於專利文獻8記載有:對鉭鑄錠進行鍛造,於此鍛造步驟進行2次以上之熱處理,進一步實施冷壓延,並進行再結晶化熱處理。
又,專利文獻9記載有一種鉭濺鍍靶,其特徵在於:含有1massppm以上、100massppm以下之鉬作為必須成分,不計鉬及氣體成分之純度在99.998%以上。並記載有如上述之鉭濺鍍靶,其特徵在於:進一步含有0~100massppm(惟不包括0massppm)之鈮,不計鉬、鈮及氣體成分之
純度在99.998%以上。記載有得到具備均一微細之組織、電漿穩定、膜之均勻性(uniformity)優異的高純度鉭濺鍍靶。
並且,專利文獻10記載有一種鉭濺鍍靶,其特徵在於:含有1massppm以上、100massppm以下之鎢作為必須成分,不計鎢及氣體成分之純度在99.998%以上。並記載有如上述之鉭濺鍍靶,其特徵在於:進一步含有0~100massppm(惟不包括0massppm)之鉬及/或鈮,鎢、鉬、鈮之合計含量在1massppm以上、150massppm以下,不計鎢、鉬、鈮及氣體成分之純度在99.998%以上。記載有得到具備均一微細之組織、電漿穩定、膜之均勻性(uniformity)優異的高純度鉭濺鍍靶。
使用於半導體之鉭濺鍍靶,一直以此方式開發多種類之靶。靶材雖主要採用10mm左右之厚度,但藉由增加每1片靶之成膜數(晶圓數),以謀求降低成本。此時,增加靶之厚度,由於能夠降低靶之替換頻率,減少裝置之停止時間,故對於降低成本,可說是有效的。
想要增加靶之使用累積時間,只要增加靶之厚度,可更長久地使用即可,但鉭靶之情形,卻具有獨特的問題。一般會於靶之濺鍍時,被膜形成於晶圓周邊機器,或因逆濺鍍而使被膜形成於靶周圍。
因此採用下述方法,藉此,以謀求成膜之延長:於使用靶之中途,大氣解放濺鍍裝置(真空機器),替換受到污染之機器,再次開始濺鍍。
然而,於高真空中進行過濺鍍之鉭靶,會露出非常活性化之表面,若解放真空機器,而使靶暴露於大氣,則會快速地形成牢固之氧化膜。此種氧化膜之形成,係即使不是刻意導入氧,亦會因大氣中之氧引起的現象。
形成有此種氧化膜之鉭靶,會發生下述問題:即使想要再次抽真空,重新進行濺鍍,表面之氧化膜亦會使成膜特性不穩定,成膜速度混亂,且將此表面氧化膜濺鍍去除而露出穩定之靶新生面的預燒時間亦會變長。結果,而成為時間與電力、材料之浪費及材料(成膜)特性惡化的原因。
然而,於上述所說明之一連串的專利文獻,並未揭示解決此問題之方法,甚至連其線索亦無法發現。
專利文獻1:日本特開2004-107758號公報
專利文獻2:國際公開2005/045090號
專利文獻3:日本特開平11-80942號公報
專利文獻4:日本特開2002-363736號公報
專利文獻5:日本特表2008-532765號公報
專利文獻6:日本特許第4754617號
專利文獻7:國際公開2011/061897號
專利文獻8:日本特許第4714123號
專利文獻9:國際公開2011/018970號
專利文獻10:國際公開2011/08971號
本發明對於鉭濺鍍靶,控制靶濺鍍面之結晶位向,使氮化膜容易形成,當採用「於使用靶之中途,解放濺鍍裝置(真空機器),替換受到污染之機器,再次開始濺鍍」此方法時,若鉭靶活性化之表面直接暴露於大氣,則會有形成牢固之氧化膜之問題。
因此,本發明事先形成氮化膜。亦即,在解放於大氣之前,在鉭靶的表面形成氮化膜。藉此,可有效地抑制「因與空氣中之氧快速反應而形成氧化膜」。並且,可使成膜特性及成膜速度穩定化,且亦可縮短預燒時間,可使時間與電力之浪費及材料(成膜)特性為良好。
並且,可增加靶之使用累積時間,增加靶的厚度,且可更長久地使用靶,有效降低成本。以此方式,可提供一種適用於形成由Ta膜或TaN膜等構成之擴散阻擋層之有效率的鉭濺鍍靶。
為了解決上述課題,本發明提供以下發明。
1)一種鉭濺鍍靶,其特徵在於:濺鍍面之(100)面的位向率為30~90%,(111)面的位向率在50%以下。
2)如上述1)之鉭濺鍍靶,其於濺鍍面具備氮化膜。
3)如上述2)之鉭濺鍍靶,其中,氮化膜之厚度在200Å以上。
4)一種擴散阻擋層用薄膜,係使用上述1)至3)中任一項之濺鍍靶形成。
5)如上述4)之擴散阻擋層用薄膜,其中,濺鍍膜之電阻變動在15%以下。
6)如上述4)或5)記載之擴散阻擋層用薄膜,其中,為100kwh以下之預燒累積電力消耗量。
7)一種半導體元件,具有上述4)至6)中任一項之擴散阻擋層用薄膜。
又,本發明提供以下之發明。
8)一種鉭濺鍍靶之製造方法,其特徵在於:係對經熔解鑄造之鉭鑄錠
進行鍛造及再結晶退火後,進行壓延及熱處理,形成鉭濺鍍靶之(100)面的位向率為30~90%,(111)面的位向率在50%以下的結晶組織。
9)如上述8)之鉭濺鍍靶之製造方法,其中,對預定再使用濺鍍之靶,暫時停止濺鍍操作,於大氣解放真空容器之前,在該靶之表面供給氮氣,形成氮化膜。
10)如上述9)之鉭濺鍍靶之製造方法,其中,形成之氮化膜的厚度在200Å以上。
本發明之鉭濺鍍靶,藉由控制靶濺鍍面之結晶位向,而可使氮化膜容易形成於鉭靶表面。藉此,當採用「於使用靶之中途,解放濺鍍裝置(真空機器),替換受到污染之機器,再次開始濺鍍」此方法時,即使是鉭靶活性化之表面暴露於大氣的情形,亦可抑制形成牢固之氧化膜,使成膜特性及成膜速度穩定化,且亦可縮短預燒時間,可使時間與電力之浪費及材料(成膜)特性為良好。
結果,可使靶的厚度增加,增加靶之使用累積時間,且可更長久地使用靶,故對於降低靶之使用成本極為有效。藉此,可提供一種適用於形成由Ta膜或TaN膜等構成之擴散阻擋層之有效率的鉭濺鍍靶。
另,預燒累積電力消耗量,係以濺鍍時間h乘以預燒時之輸入功率kW即kWh表示之用電量。通常於濺鍍裝置,輸入功率、濺鍍時間係受到管理,故濺鍍基本上係一直藉由累積電量來加以管理。
本發明之鉭濺鍍靶,於通常之步驟實施濺鍍,但當於使用靶之中途,解放濺鍍裝置(真空機器),替換受到污染之機器,再次開始濺鍍的情形時,具有本發明之(100)面的位向率為30~90%且(111)面的位向率在50%以下的結晶之面位向率者,具有下述特徴:容易藉由氮氣形成氮化膜。
並且,事先形成之氮化膜,由於可有效地抑制「因與空氣中之氧快速反應而形成氧化膜」,故可解決以往之問題。
另,具有本發明之(100)面的位向率為30~90%且(111)面的位向率在50%以下的結晶之面位向率者,作為鉭靶,由於具備有特殊位向,故其本身可稱為具有新穎性之鉭靶。鉭靶通常具有5mm以上之厚度。
由於上述,對預定再使用濺鍍之靶,暫時停止濺鍍操作,於大氣解放真空容器之前,對該靶之表面供給氮氣,形成氮化膜,使氮化膜之厚度在200Å以上。
當形成氮化膜時,可對預定再使用濺鍍之靶,暫時停止濺鍍操作,於大氣解放真空容器之前,對該靶之表面供給氮氣,形成氮化膜。
濺鍍裝置雖獨立地具有N2與Ar之供給線路,但此操作之目的在於表面之氮化,不進行濺鍍,並不需要Ar混合氣體,故僅供給氮氣。亦可視需要,使用含N2(Ar 1%)氣體。
於替換受到污染之機器,再次開始濺鍍之情形時,表面具備有氮化膜之鉭濺鍍靶的氮化膜,可有效地抑制形成氧化膜,但再使用時之預燒時間,具有只需相對較短之時間即可的特徴。因此,具備有下述效果:時間與電力之消費及因預燒而消耗之材料少,且使成膜特性良好。結果,
能夠使鉭靶的厚度增加,能夠增加靶之使用累積時間,且可更長久地使用靶,故可說對於降低靶之使用成本極為有效。
以此方式,可使再使用時之鉭濺鍍膜的電阻變動為使用中斷前之15%以下,且可為100kwh以下之預燒累積電力消耗量。此種擴散阻擋層用薄膜,對於製造半導體元件有效。另,電阻變動,係將濺鍍裝置之大氣開放前後的成膜晶圓之片電阻加以比較,大氣開放後之片電阻宜自解放前之片電阻值的85%進入115%的範圍。
為了形成鉭濺鍍靶之(100)面的位向率為30~90%,(111)面的位向率在50%以下的結晶組織,能以對經熔解鑄造之鉭鑄錠重複進行至少2次以上鍛造-退火之循環,較佳為重複3次以上的條件,進行鍛造及再結晶退火後,進行壓延及熱處理來製造。另,前述(100)面或(111)面包含從靶表面至內部自濺鍍初期至濺鍍最後階段所露出之全部部位。
本發明之鉭濺鍍靶,可用於形成銅配線中之Ta膜或TaN膜等擴散阻擋層。即使於將氮導入濺鍍時之環境來形成TaN膜之情形時,本發明之濺鍍靶藉由控制靶濺鍍面之結晶位向,亦具有可降低鉭靶之放電電壓、使電漿容易產生且提升電漿之穩定性的優異效果,故在形成具備有該Ta膜或TaN膜等擴散阻擋層之銅配線,以及在製造具備有該銅配線之半導體元件時,可提升製品產率。
本發明之鉭濺鍍靶,係藉由下述步驟製造。若顯示其例,首先,通常使用4N(99.99%)以上之高純度鉭作為鉭原料。藉由電子束熔解等將其熔解,並對其進行鑄造製作鑄錠或小胚(billet)。接著,對該鑄錠或小胚進行鍛造、再結晶退火。具體而言,例如進行如下操作:鑄錠或小胚
-合模鍛造-1100~1400℃之溫度的退火-冷鍛造(一次鍛造)-再結晶溫度~1400℃之溫度的退火-冷鍛造(二次鍛造)-再結晶溫度~1400℃之溫度的退火。
接著,進行冷壓延。藉由調整此冷壓延之條件,可控制本發明之鉭濺鍍靶的位向率。具體而言,壓延輥宜為輥直徑小者,較佳在500mm 以下。又,壓延速度宜儘可能地慢,較佳在10m/min以下。並且,於僅實施1次壓延之情形時,壓延率較佳為高且超過80%,於重複進行2次以上之壓延的情形時,係使壓延率在60%以上,必須使靶之最終厚度與壓延1次之情形相同。壓延率總計宜超過80%。又壓延1道次之軋縮率設計成不超過10%。
接著,進行熱處理。藉由一併調整冷壓延之條件及冷壓延後所進行之熱處理條件,可控制本發明之鉭濺鍍靶的位向率。具體而言,熱處理溫度以較高為佳,較佳為800~1200℃。該溫度雖亦取決於壓延所導入之變形量,但為了獲得再結晶組織,必須於800℃以上之溫度進行熱處理。另一方面,以超過1200℃之溫度進行熱處理,會助長粗大粒成長,且在經濟上並不佳。然後,藉由對靶表面進行機械加工、研磨加工等精加工,製成最後之製品。
藉由上述之製造步驟製造鉭靶,於本發明中尤其重要的是對於靶濺鍍面之結晶位向,提高(100)面之位向率,且降低(111)面之位向率。
與控制位向大有關係的主要是壓延步驟。於壓延步驟中,藉由控制壓延輥之直徑、壓延速度、壓延率等參數,可改變壓延時所導入之變形量或
分佈,而可控制(100)面之位向率及(111)面之位向率。
想要有效地進行面位向率之調整,需要某程度之重複設定條件,若一旦可調整(100)面之位向率及(111)面之位向率,則藉由設定其製造條件,而可製造恆常特性(具有一定程度之特性)之靶。
於製造具有本發明之位向特性之靶的情形時,使用壓延輥直徑在500mm以下之壓延輥,且使壓延速度在10m/min以下,1道次之壓延率在10%以下是有效的。然而,只要為可達成本發明之結晶位向的製造步驟,則並不一定僅限定於此製造步驟。下述之條件設定是有效的:於一連串之加工中,以鍛造、壓延破壞鑄造組織,且充分地進行再結晶化。
並且,宜在對經熔解鑄造之鉭鑄錠或小胚進行鍛造並施以壓延等加工之後,進行再結晶退火,使組織微細且均勻化。
實施例
接著,基於實施例說明本發明。以下所示之實施例係為了容易理解,本發明並不受此等實施例之限制。亦即,本發明當然包含基於本發明之技術思想的變形及其他實施例。
對純度99.995%之鉭原料進行電子束熔解,對其進行鑄造製成直徑195mm 之鑄錠。接著,以室溫對該鑄錠進行合模鍛造製成直徑150mm ,並以1100~1400℃之溫度對其進行再結晶退火。
再次以室溫重複對其進行初鍛-鍛粗鍛造製成厚度100mm、直徑150mm (一次鍛造),並以再結晶溫度~1400℃之溫度對其進行再結晶退火。進一步以室溫重複對其進行初鍛-鍛粗鍛造製成厚度70~100mm、直徑150~185mm (二次鍛造),並以再結晶溫度~1400℃之溫度對其進行
再結晶退火,而製得靶原材料。
(實施例1)
於實施例1,使用壓延輥直徑為400mm之壓延輥,以壓延速度10m/min、壓延率86%,並使1道次之最大軋縮率為10%,對所製得之靶原材料進行冷壓延,製成厚度14mm、直徑520mm ,以1000℃之溫度對其進行熱處理。然後,對表面進行切削、研磨而製成靶。
藉由以上步驟,可獲得具有(100)面之位向率為30%、(111)面之位向率為50%之結晶組織的鉭濺鍍靶。使用此濺鍍靶實施濺鍍。
接著,於靶之濺蝕最深部厚度成為8mm左右之時點,暫時停止濺鍍,花費60秒將氮氣導入濺鍍裝置(真空容器)內。藉此,在靶之表面形成厚度為200Å左右的氮化膜。
接著,將濺鍍裝置解放於大氣,實施內部機器之替換或清洗。然後,再次密閉濺鍍裝置,重新進行濺鍍。預燒之電力消耗量低至75kwh,於短時間可進行濺鍍,且濺鍍後之膜的電阻變動為14%,膜特性之變化少。
鉭膜之成膜係以下述條件進行(以下之實施例、比較例亦同)。
電源:直流方式
功率:15kW
到達真空度:5×10-8Torr
環境氣體組成:Ar
濺鍍氣壓:5×10-3Torr
濺鍍時間:15秒
(實施例2)
於實施例2,使用壓延輥直徑為400mm之壓延輥,以壓延速度8m/min、壓延率88%,並使1道次之最大軋縮率為10%,對所製得之靶原材料進行冷壓延,製成厚度14mm、直徑520mm ,以900℃之溫度對其進行熱處理。然後,對表面進行切削、研磨而製成靶。
藉由以上步驟,可獲得具有(100)面之位向率為50%、(111)面之位向率為20%之結晶組織的鉭濺鍍靶。使用此濺鍍靶實施濺鍍。
接著,於靶之濺蝕最深部厚度成為8mm左右之時點,暫時停止濺鍍,花費60秒將氮氣導入濺鍍裝置(真空容器)內。藉此,在靶之表面形成厚度為320Å左右的氮化膜。
接著,將濺鍍裝置解放於大氣,實施內部機器之替換或清洗。然後,再次密閉濺鍍裝置,重新進行濺鍍。預燒之電力消耗量低至50kwh,於短時間可進行濺鍍,且濺鍍後之膜的電阻變動為10%,膜特性之變化少。
(實施例3)
於實施例3,使用壓延輥直徑為400mm之壓延輥,以壓延速度5m/min、壓延率85%,並使1道次之最大軋縮率為10%,對所製得之靶原材料進行冷壓延,製成厚度14mm、直徑520mm ,以1100℃之溫度對其進行熱處理。然後,對表面進行切削、研磨而製成靶。
藉由以上步驟,可獲得具有(100)面之位向率為70%、(111)面之位向率為15%之結晶組織的鉭濺鍍靶。使用此濺鍍靶實施濺鍍。
接著,於靶之濺蝕最深部厚度成為8mm左右之時點,暫時
停止濺鍍,花費60秒將氮氣導入濺鍍裝置(真空容器)內。藉此,在靶之表面形成厚度為450Å左右的氮化膜。
接著,將濺鍍裝置解放於大氣,實施內部機器之替換或清洗。然後,再次密閉濺鍍裝置,重新進行濺鍍。預燒之電力消耗量低至35kwh,於短時間可進行濺鍍,且濺鍍後之膜的電阻變動為7%,膜特性之變化少。
(實施例4)
於實施例4,使用壓延輥直徑為500mm之壓延輥,以壓延速度5m/min、壓延率90%,並使1道次之最大軋縮率為5%,對所製得之靶原材料進行冷壓延,製成厚度14mm、直徑520mm ,以800℃之溫度對其進行熱處理。然後,對表面進行切削、研磨而製成靶。
藉由以上步驟,可獲得具有(100)面之位向率為90%、(111)面之位向率為5%之結晶組織的鉭濺鍍靶。使用此濺鍍靶實施濺鍍。
接著,於靶之濺蝕最深部厚度成為8mm左右之時點,暫時停止濺鍍,花費60秒將氮氣導入濺鍍裝置(真空容器)內。藉此,在靶之表面形成厚度為500Å左右的氮化膜。
接著,將濺鍍裝置解放於大氣,實施內部機器之替換或清洗。然後,再次密閉濺鍍裝置,重新進行濺鍍。預燒之電力消耗量低至25kwh,於短時間可進行濺鍍,且濺鍍後之膜的電阻變動為5%,膜特性之變化少。
(比較例1)
於比較例1,使用壓延輥直徑為400mm之壓延輥,以壓延速度5m/min、壓延率85%,並使1道次之最大軋縮率為10%,對所製得之靶原材料進行冷壓延,製成厚度14mm、直徑520mm ,以1100℃之溫度對其進行
熱處理。然後,對表面進行切削、研磨而製成靶。
藉由以上步驟,可獲得具有(100)面之位向率為70%、(111)面之位向率為15%之結晶組織的鉭濺鍍靶。使用此濺鍍靶實施濺鍍。
接著,於靶之濺蝕最深部厚度成為8mm左右之時點,暫時停止濺鍍,將濺鍍裝置解放於大氣,實施內部機器之替換或清洗。然後,再次密閉濺鍍裝置,重新進行濺鍍。預燒之電力消耗量低至300kwh,於短時間可進行濺鍍,且濺鍍後之膜的電阻變動為35%,膜特性之變化最大。此被認為是因為沒有形成氮化膜,氧化快速地進行的緣故。
(比較例2)
於比較例2,使用壓延輥直徑為500mm之壓延輥,以壓延速度15m/min、壓延率78%,並使1道次之最大軋縮率為15%,對所製得之靶原材料進行冷壓延,製成厚度14mm、直徑520mm ,以800℃之溫度對其進行熱處理。然後,對表面進行切削、研磨而製成靶。
藉由以上步驟,可獲得具有(100)面之位向率為20%、(111)面之位向率為60%之結晶組織的鉭濺鍍靶。另,此結晶位向脫離本發明。使用此濺鍍靶實施濺鍍。
接著,於靶之濺蝕最深部厚度成為8mm左右之時點,暫時停止濺鍍,花費60秒將氮氣導入濺鍍裝置(真空容器)內。藉此,在靶之表面形成厚度為150Å左右的氮化膜。
接著,將濺鍍裝置解放於大氣,實施內部機器之替換或清洗。然後,再次密閉濺鍍裝置,重新進行濺鍍。預燒之電力消耗量增加至275kwh,至穩定之濺鍍需要長時間。且濺鍍後之膜的電阻變動為32%,膜特性之變化
大,呈不佳之結果。此被認為是因為結晶位向率不適當的緣故。
(比較例3)
於比較例3,使用壓延輥直徑為400mm之壓延輥,以壓延速度5m/min、壓延率85%,並使1道次之最大軋縮率為10%,對所製得之靶原材料進行冷壓延,製成厚度14mm、直徑520mm ,以1100℃之溫度對其進行熱處理。然後,對表面進行切削、研磨而製成靶。
藉由以上步驟,可獲得具有(100)面之位向率為70%、(111)面之位向率為15%之結晶組織的鉭濺鍍靶。使用此濺鍍靶實施濺鍍。
接著,於靶之濺蝕最深部厚度成為8mm左右之時點,暫時停止濺鍍,花費30秒將氮氣導入濺鍍裝置(真空容器)內。藉此,在靶之表面形成厚度為150Å左右的氮化膜。
接著,將濺鍍裝置解放於大氣,實施內部機器之替換或清洗。然後,再次密閉濺鍍裝置,重新進行濺鍍。預燒之電力消耗量增加至105kwh,至可穩定之濺鍍需要長時間。且濺鍍後之膜的電阻變動為24%,膜特性之變化亦變大。此被認為是因為用以形成氮化膜之氮氣流動時間不足夠的緣故。
如以上之實施例及比較例所示,位於本發明之條件範圍者,可使鉭靶之成膜特性及成膜速度穩定化,且亦可縮短預燒時間,可使時間與電力之浪費及材料(成膜)特性為良好。又,具有下述優異之效果:可將放電電壓之變動抑制得較低,並且可減低放電異常發生率。
產業上之可利用性
本發明提供一種鉭濺鍍靶,藉由控制靶之濺鍍面的結晶位向,而可使氮化膜容易形成於鉭靶表面。因此,當採用「於使用靶之中途,
解放濺鍍裝置(真空機器),替換受到污染之機器,再次開始濺鍍」此方法時,即使於鉭靶活性化之表面暴露於大氣之情形時,亦可抑制形成牢固之氧化膜,可使成膜特性及成膜速度穩定化,且亦可縮短預燒時間,可使時間與電力之浪費及材料(成膜)特性為良好。結果,可使靶的厚度增加,增加靶之使用累積時間,且可更長久地使用靶,故對於降低靶之使用成本極為有效。藉此,可提供一種適用於形成由Ta膜或TaN膜等構成之擴散阻擋層之有效率的鉭濺鍍靶。
Claims (4)
- 一種鉭濺鍍靶,其濺鍍面之(100)面的位向率為30~90%,(111)面的位向率在50%(含)以下,於濺鍍面具備氮化膜。
- 如申請專利範圍第1項之鉭濺鍍靶,其中,氮化膜之厚度在200A以上。
- 一種鉭濺鍍靶之製造方法,係對經熔解鑄造之鉭鑄錠進行鍛造及再結晶退火後,進行壓延及熱處理,形成鉭濺鍍靶之(100)面的位向率為30~90%,(111)面的位向率在50%(含)以下的結晶組織,對預定再使用濺鍍之靶,暫時停止濺鍍操作,於大氣解放真空容器之前,對該靶之表面供給氮氣,形成氮化膜。
- 如申請專利範圍第3項之鉭濺鍍靶之製造方法,其中,氮化膜的厚度在200Å以上。
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2015
- 2015-03-04 US US14/914,385 patent/US20160208377A1/en not_active Abandoned
- 2015-03-04 CN CN201580001927.XA patent/CN105555997B/zh active Active
- 2015-03-04 KR KR1020167002643A patent/KR20160027122A/ko active Search and Examination
- 2015-03-04 KR KR1020187002988A patent/KR102112937B1/ko active IP Right Grant
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JPWO2015146516A1 (ja) | 2017-04-13 |
JP6009683B2 (ja) | 2016-10-19 |
TW201602379A (zh) | 2016-01-16 |
KR20160027122A (ko) | 2016-03-09 |
CN105555997A (zh) | 2016-05-04 |
US20160208377A1 (en) | 2016-07-21 |
WO2015146516A1 (ja) | 2015-10-01 |
CN105555997B (zh) | 2017-09-26 |
KR102112937B1 (ko) | 2020-05-19 |
KR20180014869A (ko) | 2018-02-09 |
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