TW202039919A - 附著物之去除方法及成膜方法 - Google Patents
附著物之去除方法及成膜方法 Download PDFInfo
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- TW202039919A TW202039919A TW108144635A TW108144635A TW202039919A TW 202039919 A TW202039919 A TW 202039919A TW 108144635 A TW108144635 A TW 108144635A TW 108144635 A TW108144635 A TW 108144635A TW 202039919 A TW202039919 A TW 202039919A
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- 238000000034 method Methods 0.000 title claims abstract description 42
- 239000007789 gas Substances 0.000 claims abstract description 118
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 57
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000011593 sulfur Substances 0.000 claims abstract description 55
- 238000004140 cleaning Methods 0.000 claims abstract description 41
- 150000001875 compounds Chemical class 0.000 claims abstract description 32
- 239000001257 hydrogen Substances 0.000 claims abstract description 30
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 30
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000002161 passivation Methods 0.000 claims description 79
- 239000000758 substrate Substances 0.000 claims description 35
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical group S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 13
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 7
- 150000002431 hydrogen Chemical class 0.000 claims description 5
- 239000004215 Carbon black (E152) Substances 0.000 claims description 3
- 229930195733 hydrocarbon Natural products 0.000 claims description 3
- 150000002430 hydrocarbons Chemical class 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 15
- 239000004065 semiconductor Substances 0.000 description 15
- 239000000463 material Substances 0.000 description 14
- 239000011261 inert gas Substances 0.000 description 13
- 239000002245 particle Substances 0.000 description 12
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 230000007547 defect Effects 0.000 description 5
- 229910052732 germanium Inorganic materials 0.000 description 5
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- 125000004434 sulfur atom Chemical group 0.000 description 3
- 238000011144 upstream manufacturing Methods 0.000 description 3
- 229910000530 Gallium indium arsenide Inorganic materials 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- KXNLCSXBJCPWGL-UHFFFAOYSA-N [Ga].[As].[In] Chemical compound [Ga].[As].[In] KXNLCSXBJCPWGL-UHFFFAOYSA-N 0.000 description 2
- 230000001464 adherent effect Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 150000004770 chalcogenides Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- 229910052774 Proactinium Inorganic materials 0.000 description 1
- 229910018503 SF6 Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- -1 for example Inorganic materials 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 1
- 229960000909 sulfur hexafluoride Drugs 0.000 description 1
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
本發明提供附著物之去除方法及成膜方法,該附著物之去除方法係可在不將腔室解體下去除含硫的附著物,該含硫的附著物係附著於腔室之內面或腔室所連接的配管之內面。藉由使含有含氫化合物氣體的清洗氣體與含硫的附著物反應而去除附著物,該含硫的附著物係附著於腔室(10)之內面及腔室(10)所連接的排氣用配管(15)之內面的至少一者。
Description
本發明關於附著物之去除方法及成膜方法。
近年來,於半導體領域中,含有矽(Si)以外的元素之半導體材料係受到注目。作為含有矽以外的元素之半導體材料,例如可舉出含有鍺(Ge)、銦鎵砷(InGaAs)等III-V族元素之半導體材料或含有金屬硫屬化物之半導體材料。
此等之半導體材料雖然具有移動率(移動度)比矽材料高之優點,但是有成膜困難之情況或材料間的界面之缺陷密度變高之情況。
因此,為了減低材料間的界面之缺陷密度,有提案在鍺、鉬等的基板之上,使用硫化氫(H2
S)氣體形成鈍化膜之方法(例如參照專利文獻1)。又,作為金屬硫屬化物之成膜方法,有提案以硫化氫氣體來處理鉬氧化物層、鎢氧化物層,形成硫化鉬層、硫化鎢層之方法(例如參照專利文獻2)。先前技術文獻 專利文獻
專利文獻1:日本發明專利公開公報2016年第207789號
專利文獻2:日本發明專利公開公報2017年第61743號
專利文獻3:日本發明專利公開公報2011年第189338號
發明所欲解決的課題
於減低材料間的界面之缺陷密度的上述方法中,由於在高溫下進行反應,故在進行該反應的腔室之內面或在腔室之下游側所配置的配管之內面,有附著因硫化氫之分解所生成之含硫的附著物之情況。
於含硫的附著物附著於腔室之內面或在腔室之下游側所配置的配管之內面的狀態下,若將晶圓等的基板導入至腔室內,於使腔室內成為真空,以惰性氣體置換之際,有硫的顆粒附著於晶圓等的基板上之虞。而且,若硫的顆粒附著於基板,則有所製造的半導體構造之性能降低之虞。
例如專利文獻3中,揭示使用電漿洗淨裝置來洗淨基板之技術。於此技術中,由於來自基板之洗淨中使用的六氟化硫氣體之硫係附著於基板,故藉由氬的濺射而去除該附著的硫。
然而,於專利文獻3所揭示的技術中,由於物理地去除硫,有所去除的硫係再附著於電漿洗淨裝置內的另一場所,或再附著於在電漿洗淨裝置之下游側所配置之配管。
因此,於含硫的附著物附著於腔室之內面或腔室之下游側所配置的配管之內面時,必須將腔室解體,進行洗淨。
本發明之課題在於提供附著物之去除方法及成膜方法,該附著物之去除方法係可在不將腔室解體下去除含硫的附著物,該含硫的附著物係附著於腔室之內面或腔室所連接的配管之內面。解決課題的手段
為了解決前述課題,本發明之一態樣係如以下之[1]~[6]。
[1]一種附著物之去除方法,其係藉由使含有含氫化合物氣體的清洗氣體與含硫的附著物反應而去除附著物,該含硫的附著物係附著於腔室之內面及前述腔室所連接的配管之內面的至少一者。
[2]如[1]記載之附著物之去除方法,其中在溫度20℃以上800℃以下、壓力20Pa以上101kPa以下之條件下,使前述清洗氣體接觸前述附著物。
[3]如[1]或[2]記載之附著物之去除方法,其中前述含氫化合物氣體係選自由氫氣、烴氣及氨氣所成之群組的至少1種。
[4]如[1]或[2]記載之附著物之去除方法,其中前述含氫化合物氣體係氫氣。
[5]一種成膜方法,其具備:
鈍化步驟,係將含有含硫化合物氣體的鈍化氣體供給至收容有基板的腔室,使前述基板與前述鈍化氣體反應,將鈍化膜成膜在前述基板之表面;與
附著物去除步驟,係在進行前述鈍化步驟後去除含硫的附著物,該含硫的附著物係附著於腔室之內面及前述腔室所連接的配管之內面的至少一者;
其中,藉由如[1]~[4]中任一項記載之附著物之去除方法,進行前述附著物去除步驟。
[6]如[5]記載之成膜方法,其中前述含硫化合物氣體係硫化氫氣體。發明的效果
依照本發明,可在不將腔室解體下去除含硫的附著物,該含硫的附著物係附著於腔室之內面或腔室所連接的配管之內面。
實施發明的形態
以下說明本發明之一實施形態。還有,本實施形態係顯示本發明之一例者,不是將本發明限定於本實施形態。又,對於本實施形態可加以各種的變更或改良,加以如此的變更或改良之形態亦可被包含於本發明中。
[第一實施形態]
本發明之第一實施形態係附著物去除方法的實施形態,為藉由使含有含氫化合物氣體的清洗氣體與含硫的附著物(以下亦有僅記載為「附著物」之情形)反應而去除附著物之方法,該含硫的附著物係附著於腔室之內面及腔室所連接的配管之內面的至少一者。還有,含氫化合物氣體與清洗氣體係不含硫原子。
於腔室中進行使用硫的反應之情況等中,有含硫的附著物附著於腔室之內面或腔室所連接的配管(例如,連接於腔室的上游側之清洗氣體的供氣用配管或連接於腔室的下游側之排氣用配管)之內面的情況。若附著物維持附著而進行下一個反應,則有對於反應造成不良影響之虞,故較佳為在去除附著物後進行下一個反應。
第一實施形態的附著物之去除方法係藉由使清洗氣體接觸附著物,使附著物中的硫與清洗氣體中的含氫化合物氣體反應,生成硫化氫氣體而去除附著物,故可在不將腔室解體下去除附著於腔室之內面或腔室所連接的配管之內面的附著物。因此,可容易地進行附著物之去除。
清洗氣體與附著物之接觸較佳為在溫度20℃以上800℃以下之條件下進行,更佳為在溫度40℃以上600℃以下之條件下進行。若為800℃以下之溫度,則清洗氣體中的含氫化合物氣體或所生成的硫化氫氣體係不易腐蝕形成腔室或配管的不鏽鋼等金屬材料,除此之外藉由附著物中的硫與清洗氣體中的含氫化合物氣體之反應所生成的硫化氫氣體係不易發生變回硫的逆反應。另一方面,若為20℃以上之溫度,則附著物中的硫與清洗氣體中的含氫化合物氣體之反應係容易進行。
又,清洗氣體與附著物之接觸,較佳為在絕對壓力之壓力20Pa以上101kPa以下之條件下進行,更佳為在壓力60Pa以上90kPa以下之條件下進行。若為101kPa以下之壓力,則在腔室或配管不易發生不良狀況。例如,腔室為使基板與鈍化氣體反應而在基板之表面上形成鈍化膜之成膜裝置的反應容器時,由於以在減壓環境下的使用為前提,壓力條件較佳為101kPa以下。另一方面,若為20Pa以上之壓力,則附著物中的硫與清洗氣體中的含氫化合物氣體之反應係容易進行。
含氫化合物氣體係具有氫原子的化合物之氣體,再者為不具有硫原子及鹵素原子之氣體,例如可舉出氫氣(H2
)、烴氣及氨氣(NH3
)。於此等之中,較佳為選自由氫氣(H2
)、甲烷氣體(CH4
)、乙烷氣體(C2
H6
)、丙烷氣體(C3
H8
)、丁烷氣體(C4
H10
)及氨氣(NH3
)所成之群組的至少一種氣體,更佳為氫氣及甲烷氣體之至少一者。
由於氫氣係在101kPa之壓力下、300℃以上之溫度下與硫反應,當清洗氣體中含有氫氣時,較佳為在300℃以上800℃以下之溫度下使清洗氣體與硫(附著物)接觸。還有,當清洗氣體中含有氫氣時,為了有效率地去除附著物,較佳為一邊加熱腔室的內部或配管,一邊進行附著物之去除。由於甲烷氣體係在101kPa之壓力下、140℃以上之溫度下與硫反應,故當清洗氣體中含有甲烷氣體時,較佳為在140℃以上800℃以下之溫度下使清洗氣體與硫(附著物)接觸。
清洗氣體中的含氫化合物氣體之含有比率,只要能去除硫(附著物)的充分量,則沒有特別的限定,但較佳為5體積%以上,更佳為20體積%以上,尤佳為90體積%以上,特佳為100體積%。清洗氣體中所含有的含氫化合物氣體以外之成分,只要是不具有硫原子的化合物之氣體,則沒有特別的限定,例如可舉出氮氣、氬氣等之惰性氣體。
腔室只要由具有對於硫化氫之耐性的材料所形成,則沒有特別的限定,但較佳為具有能減壓至特定的壓力之構造,作為材料,例如可舉出表面經防蝕鋁處理的鋁等。又,對於腔室所連接的配管,亦只要由具有對於硫化氫之耐性的材料所形成,則沒有特別的限定,但較佳為具有能耐得住特定壓力的構造。例如,可在半導體之成膜裝置作為反應容器所具備的腔室,及對於該腔室所連接的配管,適宜使用第一實施形態的附著物之去除方法。
[第二實施形態]
本發明之第二實施形態係成膜方法之實施形態,其為一種具備以下步驟之方法:鈍化步驟,係將含有含硫化合物氣體的鈍化氣體供給至收容有基板的腔室,使基板與鈍化氣體反應,將鈍化膜成膜在基板之表面;及,附著物去除步驟,係在進行鈍化步驟後去除含硫的附著物,該含硫的附著物係附著於腔室之內面及腔室所連接的配管之內面的至少一者。而且,該附著物去除步驟係藉由第一實施形態的附著物之去除方法進行者。
於使用鈍化氣體,將鈍化膜成膜在基板之表面之鈍化步驟中,有含硫的附著物附著於腔室之內面或腔室所連接的配管(例如,連接於腔室的上游側之鈍化氣體或清洗氣體的供氣用配管或連接於腔室的下游側之排氣用配管)之內面的情況。
於附著物附著於腔室之內面或配管之內面的狀態下,若將基板導入至腔室內,則於使腔室內成為真空,以惰性氣體置換之際,有硫的顆粒附著於基板之虞。而且,若硫的顆粒附著於基板,則有所製造的半導體構造之性能降低之虞。又,若硫的顆粒附著基板而直接進行下一個鈍化步驟,則有發生鈍化膜的成膜速度或膜質的降低等之不良狀況之虞。因此,較佳為在去除附著物後進行下一個鈍化步驟。
第二實施形態之成膜方法係藉由使清洗氣體接觸附著物,使附著物中的硫與清洗氣體中的含氫化合物氣體反應,生成硫化氫氣體而去除附著物,故可在不將腔室解體下去除附著於腔室之內面或腔室所連接的配管之內面的附著物。因此,可容易地進行附著物之去除。又,依照第二實施形態之成膜方法,由於可藉由附著物之去除而抑制硫的顆粒附著於基板,故可製造具有優異的性能之半導體構造。
再者,於第二實施形態之成膜方法中,並非在每次進行鈍化步驟後必須進行附著物去除步驟,而可在每進行複數次的鈍化步驟後,進行附著物去除步驟。相對於進行鈍化步驟之次數,若減少進行附著物去除步驟之次數,則可提高成膜裝置的利用效率。
含有含硫化合物氣體的鈍化氣體之種類,只要是具有硫的化合物之氣體,則沒有特別的限定,但從鈍化性能為良好來看,較佳為硫化氫氣體。
鈍化氣體中的含硫化合物氣體之含有比率,只要是鈍化膜之成膜所需之充分的量,則沒有特別的限定,但較佳為1體積%以上,更佳為2體積%以上,尤佳為10體積%以上,特佳為100體積%。鈍化氣體中含有的含硫化合物氣體以外之成分係沒有特別的限定,例如可舉出氮氣、氬氣等之惰性氣體。
形成基板的材料之種類,只要是半導體材料,則沒有特別的限定,例如可舉出含有矽、鍺、III-V族化合物、鉬、鎢等元素之材料。作為矽,半導體元件之形成中使用的矽係合適,例如可舉出非晶矽、多晶矽、單晶矽等。關於鍺、III-V族化合物、鉬、鎢,亦半導體元件之形成中使用者亦合適。
鈍化步驟中將鈍化膜成膜時的腔室內之壓力係沒有特別的限定,但較佳為1Pa以上101kPa以下,更佳為10Pa以上90kPa以下,尤佳為100Pa以上80kPa以下。
鈍化步驟中使基板與鈍化氣體反應之際的基板之溫度係沒有特別的限定,但為了得到基板之表面的藉由鈍化氣體所致之處理的高面內均勻性,較佳為20℃以上1500℃以下,更佳為50℃以上1200℃以下,尤佳為100℃以上1000℃以下。
鈍化步驟中鈍化時間的長度係沒有特別的限定,但若考慮半導體元件製程之效率,則較佳為120分鐘以內。還有,所謂鈍化時間,就是指從將鈍化氣體供給至收容有基板的腔室起,到為了結束鈍化氣體所致的基板之表面處理而藉由真空泵等將腔室內的鈍化氣體予以排氣為止之時間。
第二實施形態之成膜方法係可對於將鈍化膜成膜在基板之表面上的半導體之成膜裝置,可較宜適用。此成膜裝置之構造係沒有特別的限定,反應容器之腔室內所收容的基板與腔室所連接的配管之位置關係亦沒有特別的限定。實施例
以下顯示實施例及比較例,更詳細地說明本發明。
(實施例1)
使用圖1所示的成膜裝置1,重複進行:將鈍化膜成膜在前述基板之表面上的鈍化步驟,與去除含硫的附著物之附著物去除步驟。成膜裝置1具備進行鈍化步驟或附著物去除步驟的腔室10,與調整腔室10的內部之溫度的溫度調整裝置(未圖示)。於腔室10之內部,具備支撐試料20的載台11。作為試料20,使用在矽基板上形成厚度150nm的矽氧化膜,且更在其上形成有厚度80nm的鍺膜者。
於腔室10中,在其上游側,分別介由閥32、33、34連接:將含有含硫化合物氣體的鈍化氣體供給至腔室10的鈍化氣體供氣用配管12、將含有含氫化合物氣體的清洗氣體供給至腔室10的清洗氣體供氣用配管13、與將惰性氣體供給至腔室10的惰性氣體供氣用配管14。
又,於腔室10中,在其下游側,連接將腔室10內的氣體排出外部之排氣用配管15,在排氣用配管15之下游側,介由閥35而連接真空泵38。腔室10的內部之壓力係藉由能控制閥35的壓力控制器37而被控制。
使用如此的成膜裝置1,首先進行鈍化步驟。在載台11上設置試料20,將腔室10內的壓力減壓到未達10Pa後,將腔室10內的溫度升溫到800℃。然後,使閥32成為開狀態,從鈍化氣體供氣用配管12以101kPa之壓力將作為鈍化氣體的硫化氫氣體供給至腔室10內。此時的鈍化氣體之流量係設為100sccm,將鈍化膜成膜在試料20之表面上時的腔室10內之壓力係設為67kPa。還有,sccm表示0℃、101.3kPa下的流量(mL/min)。
進行30分鐘的鈍化氣體之導入,在溫度800℃、壓力67kPa之條件下將試料20之表面予以硫化而形成鈍化膜後,停止鈍化氣體之導入。然後,以真空泵38使腔室10的內部成為真空,從惰性氣體供氣用配管14將惰性氣體供給至腔室10內,以惰性氣體置換腔室10之內部。然後,將腔室10內的溫度降低到室溫,將形成有鈍化膜的試料20從腔室10取出。
接著,使用成膜裝置1,進行附著物去除步驟。將取出試料20後的腔室10內之壓力減壓到未達10Pa後,將腔室10內的溫度升溫到500℃。然後,使閥33成為開狀態,從清洗氣體供氣用配管13將作為清洗氣體的氫氣供給至腔室10之內部及排氣用配管15。此時的清洗氣體之流量係設為100sccm,去除附著物時的腔室10內之壓力係設為67kPa。
進行5分鐘的清洗氣體之導入,在溫度500℃、壓力67kPa之條件下使附著物與氫氣反應而進行附著物之去除後,停止清洗氣體之導入。然後,以真空泵38使腔室10的內部成為真空,從惰性氣體供氣用配管14將惰性氣體供給至腔室10內,以惰性氣體置換腔室10之內部。
於附著物去除步驟結束後,與上述同樣地進行鈍化步驟,將鈍化膜成膜在新的試料20上。然後,與上述同樣地進行附著物去除步驟。重複如此的操作,製造合計100片的形成有鈍化膜之試料20。
(實施例2)
除了將附著物去除步驟中的腔室10內之溫度設為350℃,將壓力設為100Pa之點以外,與實施例1同樣地製造100片的形成有鈍化膜之試料20。
(實施例3)
除了將附著物去除步驟中的腔室10內之溫度設為20℃之點以外,與實施例1同樣地製造100片的形成有鈍化膜之試料20。
(實施例4)
除了將附著物去除步驟中的腔室10內之溫度設為800℃之點以外,與實施例1同樣地製造100片的形成有鈍化膜之試料20。
(實施例5)
除了將附著物去除步驟中的腔室10內之壓力設為20Pa之點以外,與實施例1同樣地製造100片的形成有鈍化膜之試料20。
(實施例6)
除了將附著物去除步驟中的腔室10內之壓力設為101kPa之點以外,與實施例1同樣地製造100片的形成有鈍化膜之試料20。
(實施例7)
除了將附著物去除步驟中的從清洗氣體供氣用配管13供給的清洗氣體設為甲烷氣體之點以外,與實施例1同樣地製造100片的形成有鈍化膜之試料20。
(實施例8)
除了將附著物去除步驟中的從清洗氣體供氣用配管13供給的清洗氣體設為氨氣之點以外,與實施例1同樣地製造100片的形成有鈍化膜之試料20。
(比較例1)
除了不進行附著物去除步驟而僅重複進行鈍化步驟之點以外,與實施例1同樣地製造100片的形成有鈍化膜之試料20。
對於實施例1~8及比較例1之試料20,在第1片至第100片的各試料20之鈍化步驟每次結束時,測定試料20之表面上附著的硫之顆粒的個數。顆粒的個數之測定係使用KLA-Tencor公司製的晶圓檢查裝置Surfscan(註冊商標)6240進行。表1與圖2之圖表中顯示測定結果。
如由表1與圖2之圖表可知,於不進行附著物去除步驟而僅重複進行鈍化步驟之比較例1中,隨著所進行的鈍化步驟之次數變多,即隨著形成有鈍化膜之試料20的製造片數變多,試料20上附著的顆粒之個數變多,在第30次為1000個/m2
以上,在第100次為6000個/m2
以上。
相對於其,於鈍化步驟之後進行附著物去除步驟之實施例1~8中,試料20上附著的顆粒之個數少,即使鈍化步驟之次數為第100次,也於實施例1中為100個/m2
以下,於實施例2中為300個/m2
以下,於其他的實施例中為1000個/m2
以下。
如此地,藉由進行附著物去除步驟,顯示可在不將腔室解體洗淨下,保持低的附著顆粒之個數,重複進行鈍化步驟。
1:成膜裝置
10:腔室
11:載台
12:鈍化氣體供氣用配管
13:清洗氣體供氣用配管
14:惰性氣體供氣用配管
15:排氣用配管
20:試料
[圖1]係說明本發明之成膜方法的一實施形態之成膜裝置之概略圖。
[圖2]係顯示測定矽基板上附著的顆粒之個數的結果之圖表。
1:成膜裝置
10:腔室
11:載台
12:鈍化氣體供氣用配管
13:清洗氣體供氣用配管
14:惰性氣體供氣用配管
15:排氣用配管
20:試料
32,33,34,35:閥
37:壓力控制
38:真空泵
Claims (6)
- 一種附著物之去除方法,其係藉由使含有含氫化合物氣體的清洗氣體與含硫的附著物反應而去除附著物,該含硫的附著物係附著於腔室之內面及前述腔室所連接的配管之內面的至少一者。
- 如請求項1之附著物之去除方法,其中在溫度20℃以上800℃以下、壓力20Pa以上101kPa以下之條件下,使前述清洗氣體接觸前述附著物。
- 如請求項1或2之附著物之去除方法,其中前述含氫化合物氣體係選自由氫氣、烴氣及氨氣所成之群組的至少1種。
- 如請求項1或2之附著物之去除方法,其中前述含氫化合物氣體係氫氣。
- 一種成膜方法,其具備: 鈍化步驟,係將含有含硫化合物氣體的鈍化氣體供給至收容有基板的腔室,使前述基板與前述鈍化氣體反應,將鈍化膜成膜在前述基板之表面;與 附著物去除步驟,係在進行前述鈍化步驟後去除含硫的附著物,該含硫的附著物係附著於腔室之內面及前述腔室所連接的配管之內面的至少一者; 其中,藉由如請求項1~4中任一項之附著物之去除方法,進行前述附著物去除步驟。
- 如請求項5之成膜方法,其中前述含硫化合物氣體係硫化氫氣體。
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