CN113228235B - 附着物除去方法和成膜方法 - Google Patents
附着物除去方法和成膜方法 Download PDFInfo
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- CN113228235B CN113228235B CN201980083535.0A CN201980083535A CN113228235B CN 113228235 B CN113228235 B CN 113228235B CN 201980083535 A CN201980083535 A CN 201980083535A CN 113228235 B CN113228235 B CN 113228235B
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- 238000000034 method Methods 0.000 title claims abstract description 48
- 239000007789 gas Substances 0.000 claims abstract description 121
- 238000004140 cleaning Methods 0.000 claims abstract description 44
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 42
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000011593 sulfur Substances 0.000 claims abstract description 40
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000001257 hydrogen Substances 0.000 claims abstract description 26
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 26
- 150000001875 compounds Chemical class 0.000 claims abstract description 21
- 238000002161 passivation Methods 0.000 claims description 81
- 239000000758 substrate Substances 0.000 claims description 34
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 13
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 12
- 150000003464 sulfur compounds Chemical class 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 7
- 230000001464 adherent effect Effects 0.000 claims description 7
- 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
- 239000000463 material Substances 0.000 description 15
- 239000002245 particle Substances 0.000 description 15
- 239000004065 semiconductor Substances 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 13
- 239000011261 inert gas Substances 0.000 description 13
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 10
- 239000000126 substance Substances 0.000 description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 229910052732 germanium Inorganic materials 0.000 description 4
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 150000002431 hydrogen Chemical class 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
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 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
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 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
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 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
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000004770 chalcogenides Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- -1 hydrogen compound Chemical class 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000005259 measurement 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
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-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
- 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
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Abstract
提供能够在不拆解腔室的状态下将附着在腔室的内表面或者与腔室连接的配管的内表面的含硫的附着物除去的附着物除去方法和成膜方法。使附着在腔室(10)的内表面以及与腔室(10)连接的排气用配管(15)的内表面中的至少一者的含硫的附着物,与含有含氢化合物气体的清洁气体反应,由此将该附着物除去。
Description
技术领域
本发明涉及附着物除去方法和成膜方法。
背景技术
近年来,在半导体领域中,含有硅(Si)以外的元素的半导体材料受到关注。作为含有硅以外的元素的半导体材料,例如可举出锗(Ge)、砷化铟镓(InGaAs)等含有III-V族元素的半导体材料、含有金属硫属化物的半导体材料。
这些半导体材料与硅材料相比,虽然具有移动性(mobility)高的优点,但存在成膜困难的情况、材料之间的界面的缺陷密度变高的情况。
因此,为了降低材料之间的界面的缺陷密度,提出了在锗、钼等基板上使用硫化氢(H2S)气体形成钝化膜的方法(例如参照专利文献1)。另外,作为金属硫属化物的成膜方法,已提出利用硫化氢气体对钼氧化物层、钨氧化物层进行处理而形成硫化钼层、硫化钨层的方法(例如参照专利文献2)。
在先技术文献
专利文献1:日本特许公开公报2016年第207789号
专利文献2:日本特许公开公报2017年第61743号
专利文献3:日本特许公开公报2011年第189338号
发明内容
发明要解决的课题
在降低材料之间的界面的缺陷密度的上述方法中,由于在高温下进行反应,因此在进行该反应的腔室的内表面、配置于腔室的下游侧的配管的内表面,有时会附着含有由硫化氢分解生成的硫的附着物。
如果在腔室的内表面、配置于腔室的下游侧的配管的内表面附着有含硫的附着物的状态下,将晶片等基板导入腔室内,则在使腔室内成为真空并用惰性气体置换时,硫的颗粒(particle)有可能附着在晶片等基板上。如果硫的颗粒附着于基板,则制造出的半导体结构的性能有可能降低。
例如专利文献3公开了一种使用等离子体清洗装置清洗基板的技术。该技术中,来自用于清洗基板的六氟化硫气体的硫附着在基板上,因此通过利用氩气进行溅射来除去该附着的硫。
但是,专利文献3公开的技术属于物理性地除去硫,因此存在被除去的硫再次附着于等离子体清洗装置内的其他位置、或者再次附着于配置在等离子体清洗装置的下游侧的配管这样的问题。
因此,在腔室的内表面、配置于腔室的下游侧的配管的内表面附着有含硫的附着物的情况下,需要将腔室拆解进行清洗。
本发明的课题在于提供能够在不拆解腔室的状态下将附着在腔室的内表面或者与腔室连接的配管的内表面的含硫的附着物除去的附着物除去方法和成膜方法。
用于解决课题的手段
为解决上述课题,本发明的一个技术方案如以下的[1]~[6]所述。
[1]一种附着物除去方法,使附着在腔室的内表面以及与所述腔室连接的配管的内表面中的至少一者的含硫的附着物,与含有含氢化合物气体的清洁气体反应,由此将所述附着物除去。
[2]根据[1]所述的附着物除去方法,在温度20℃以上且800℃以下、压力20Pa以上且101kPa以下的条件下,使所述清洁气体与所述附着物接触。
[3]根据[1]或[2]所述的附着物除去方法,所述含氢化合物气体是选自氢气、烃气和氨气中的至少一种。
[4]根据[1]或[2]所述的附着物除去方法,所述含氢化合物气体是氢气。
[5]一种成膜方法,具备钝化工序和附着物除去工序,
所述钝化工序中,将含有含硫化合物气体的钝化气体供给到收纳有基板的腔室,使所述基板与所述钝化气体反应,在所述基板的表面形成钝化膜,
所述附着物除去工序中,在进行所述钝化工序之后,将附着在所述腔室的内表面以及与所述腔室连接的配管的内表面中的至少一者的含硫的附着物除去,
采用[1]~[4]中任一项所述的附着物除去方法进行所述附着物除去工序。
[6]根据[5]所述的成膜方法,所述含硫化合物气体是硫化氢气体。
发明的效果
根据本发明,能够在不拆解腔室的状态下将附着在腔室的内表面或者与腔室连接的配管的内表面的含硫的附着物除去。
附图说明
图1是用于说明本发明涉及的成膜方法的一个实施方式的成膜装置的概略图。
图2是表示附着在硅基板上的颗粒个数的结果的图表。
具体实施方式
以下,对本发明的一个实施方式进行说明。再者,本实施方式表示本发明的一个例子,本发明并不限定于本实施方式。另外,可以对本实施方式施加各种变更或改良,施加了这样的变更或改良而得到的方案也包含在本发明中。
〔第一实施方式〕
本发明的第一实施方式是附着物除去方法的实施方式,是使附着在腔室的内表面以及与腔室连接的配管的内表面中的至少一者的含硫的附着物(以下有时也简称为“附着物”),与含有含氢化合物气体的清洁气体反应,由此将所述附着物除去的方法。再者,含氢化合物气体和清洁气体不含硫原子。
在腔室中进行使用硫的反应的情况等,有时在腔室的内表面、与腔室连接的配管(例如与腔室的上游侧连接的清洁气体的供气用配管、与腔室的下游侧连接的排气用配管)的内表面会附着含硫的附着物。如果在附着有附着物的状态下进行接下来的反应,则有可能对反应造成不良影响,因此优选在除去附着物后再进行接下来的反应。
第一实施方式涉及的附着物除去方法,通过使附着物与清洁气体接触,使附着物中的硫与清洁气体中的含氢化合物气体反应而生成硫化氢气体,从而除去附着物,因此能够在不拆解腔室的状态下将附着在腔室的内表面、与腔室连接的配管的内表面的附着物除去。由此,能够容易地进行附着物的除去。
清洁气体与附着物的接触,优选在温度为20℃以上且800℃以下的条件下进行,更优选在温度为40℃以上且600℃以下的条件下进行。如果是800℃以下的温度,则清洁气体中的含氢化合物气体、生成的硫化氢气体难以腐蚀形成腔室、配管的不锈钢等金属材料,而且难以引起由附着物中的硫与清洁气体中的含氢化合物气体的反应而生成的硫化氢气体恢复为硫的逆反应。另一方面,如果是20℃以上的温度,则附着物中的硫与清洁气体中的含氢化合物气体的反应容易进行。
另外,清洁气体与附着物的接触,优选在以绝对压力计压力为20Pa以上且101kPa以下的条件下进行,更优选在压力为60Pa以上且90kPa以下的条件下进行。如果是101kPa以下的压力,则腔室、配管难以产生不良情况。例如,在腔室是使基板与钝化气体反应而在基板的表面形成钝化膜的成膜装置的反应容器的情况下,由于以减压环境下的使用为前提,因此压力条件优选为101kPa以下。另一方面,如果是20Pa以上的压力,则附着物中的硫与清洁气体中的含氢化合物气体的反应容易进行。
含氢化合物气体是具有氢原子的化合物的气体,并且是不具有硫原子和卤素原子的气体,例如可举出氢气(H2)、烃气和氨气(NH3)。其中,优选为选自氢气(H2)、甲烷气体(CH4)、乙烷气体(C2H6)、丙烷气体(C3H8)、丁烷气体(C4H10)和氨气(NH3)中的至少一种气体,更优选为氢气和甲烷气体中的至少一者。
氢气在101kPa的压力下,在300℃以上的温度下与硫反应,因此在清洁气体中含有氢气的情况下,优选在300℃以上且800℃以下的温度下使清洁气体与硫(附着物)接触。再者,在清洁气体中含有氢气的情况下,为了有效地除去附着物,优选一边对腔室的内部、配管进行加热,一边除去附着物。甲烷气体在101kPa的压力下,在140℃以上的温度下与硫反应,因此在清洁气体中含有甲烷气体的情况下,优选在140℃以上且800℃以下的温度下使清洁气体与硫(附着物)接触。
关于清洁气体中的含氢化合物气体的含有比率,只要是足以除去硫(附着物)的量就没有特别限定,优选为5体积%以上,更优选为20体积%以上,进一步优选为90体积%以上,特别优选为100体积%。关于清洁气体所含有的含氢化合物气体以外的成分,只要是不具有硫原子的化合物的气体就没有特别限定,例如可举出氮气、氩气等惰性气体。
腔室只要由对于硫化氢具有耐性的材料形成就没有特别限定,优选具有能够减压至预定压力的结构,作为材料例如可举出表面进行了氧化铝膜处理的铝等。另外,关于与腔室连接的配管,只要由对于硫化氢具有耐性的材料形成就没有特别限定,优选具有能够承受预定压力的结构。例如,对于在半导体的成膜装置中作为反应容器而具备的腔室以及与该腔室连接的配管,能够很好地应用第一实施方式涉及的附着物除去方法。
〔第二实施方式〕
本发明的第二实施方式是成膜方法的实施方式,该方法具备钝化工序和附着物除去工序,在钝化工序中,将含有含硫化合物气体的钝化气体供给到收纳有基板的腔室,使基板与钝化气体反应,在基板的表面形成钝化膜,在附着物除去工序中,在进行钝化工序之后,将附着在腔室的内表面以及与腔室连接的配管的内表面中的至少一者的含硫的附着物除去。并且,该附着物除去工序采用第一实施方式的附着物除去方法进行。
在使用钝化气体在基板的表面形成钝化膜的钝化工序中,有时在腔室的内表面、与腔室连接的配管(例如与腔室的上游侧连接的钝化气体或清洁气体的供气用配管、与腔室的下游侧连接的排气用配管)的内表面会附着含硫的附着物。
如果在腔室的内表面、配管的内表面附着有附着物的状态下将基板导入腔室内,则在使腔室内成为真空并用惰性气体置换时,硫的颗粒有可能附着在基板上。如果硫的颗粒附着在基板上,则制造出的半导体结构的性能有可能降低。另外,如果在硫的颗粒附着于基板的状态下进行接下来的钝化工序,则有可能产生钝化膜的成膜速度、膜质量的降低等不良状况。由此,优选在除去附着物后再进行接下来的钝化工序。
第二实施方式涉及的成膜方法,通过使附着物与清洁气体接触,使附着物中的硫与清洁气体中的含氢化合物气体反应而生成硫化氢气体,从而除去附着物,因此能够在不拆解腔室的状态下将附着在腔室的内表面、与腔室连接的配管的内表面的附着物除去。由此,能够容易地进行附着物的除去。另外,根据第二实施方式涉及的成膜方法,能够通过附着物的除去来抑制硫的颗粒附着于基板,因此能够制造具有优异性能的半导体结构。
再者,第二实施方式涉及的成膜方法中,并不是每次进行钝化工序都必须进行附着物除去工序,也可以每当进行多次钝化工序时进行附着物除去工序。如果相对于钝化工序的次数而减少附着物除去工序的次数,则能够提高成膜装置的利用效率。
关于含有含硫化合物气体的钝化气体的种类,只要是具有硫的化合物的气体就没有特别限定,从钝化性能良好出发,优选硫化氢气体。
关于钝化气体中的含硫化合物气体的含有比率,只要是足以形成钝化膜的量就没有特别限定,优选为1体积%以上,更优选为2体积%以上,进一步优选为10体积%以上,特别优选为100体积%。对于钝化气体所含有的含硫化合物气体以外的成分没有特别限定,例如可举出氮气、氩气等惰性气体。
关于形成基板的材料的种类,只要是半导体材料就没有特别限定,例如可举出含有硅、锗、III-V族化合物、钼、钨等元素的材料。作为硅,优选半导体元件的形成所使用的硅,例如可举出非晶硅、多晶硅、单晶硅等。关于锗、III-V族化合物、钼、钨,也优选半导体元件的形成所使用的材料。
对于在钝化工序中形成钝化膜时的腔室内的压力没有特别限定,优选为1Pa以上且101kPa以下,更优选为10Pa以上且90kPa以下,进一步优选为100Pa以上且80kPa以下。
对于在钝化工序中使基板与钝化气体反应时的基板的温度没有特别限定,为了对基板表面进行钝化气体处理得到高的面内均匀性,优选为20℃以上且1500℃以下,更优选为50℃以上且1200℃以下,进一步优选为100℃以上且1000℃以下。
对于在钝化工序中钝化时间的长度没有特别限定,考虑到半导体元件制造工艺的效率,优选为120分钟以内。再者,钝化时间是指从向收纳有基板的腔室供给钝化气体开始,直到为了完成利用钝化气体对基板表面的处理而通过真空泵等排出腔室内的钝化气体为止的时间。
第二实施方式涉及的成膜方法,能够很好地应用于在基板表面形成钝化膜的半导体的成膜装置。对于该成膜装置的结构没有特别限定,对于在作为反应容器的腔室内收纳的基板与连接到腔室的配管之间的位置关系也没有特别限定。
实施例
以下示出实施例和比较例,对本发明进行更详细的说明。
(实施例1)
使用图1所示的成膜装置1,反复进行在基板的表面形成钝化膜的钝化工序和除去含硫的附着物的附着物除去工序。成膜装置1具有进行钝化工序、附着物除去工序的腔室10,以及调整腔室10的内部的温度的温度调整装置(未图示)。在腔室10的内部具备支撑试料20的平台11。作为试料20,使用在硅基板上形成厚度150nm的硅氧化膜,再在其上形成厚度80nm的锗膜而得到的试料。
腔室10中,在其上游侧分别经由阀32、33、34连接有:将含有含硫化合物气体的钝化气体向腔室10供给的钝化气体供气用配管12、将含有含氢化合物气体的清洁气体向腔室10供给的清洁气体供气用配管13、以及将惰性气体向腔室10供给的惰性气体供气用配管14。
另外,腔室10中,在其下游侧连接有将腔室10内的气体向外部排出的排气用配管15,在排气用配管15的下游侧经由阀35连接有真空泵38。腔室10的内部的压力由对阀35进行控制的压力控制器37控制。
使用这样的成膜装置1,首先进行钝化工序。在平台11上设置试料20,将腔室10内的压力减压至小于10Pa之后,将腔室10内的温度升温至800℃。然后,使阀32成为打开状态,从钝化气体供气用配管12向腔室10内以101kPa的压力供给作为钝化气体的硫化氢气体。此时的钝化气体的流量为100sccm,在试料20的表面形成钝化膜时的腔室10内的压力为67kPa。再者,sccm表示0℃、101.3kPa时的流量(mL/min)。
进行30分钟钝化气体的导入,在温度800℃、压力67kPa的条件下使试料20的表面硫化而形成钝化膜后,停止钝化气体的导入。接着,利用真空泵38使腔室10的内部成为真空,从惰性气体供气用配管14向腔室10内供给惰性气体,用惰性气体置换腔室10的内部。然后,使腔室10内的温度降低至室温,将形成有钝化膜的试料20从腔室10中取出。
接着,使用成膜装置1进行了附着物除去工序。将取出了试料20的腔室10内的压力减压至小于10Pa后,将腔室10内的温度升温至500℃。然后,使阀33成为打开状态,从清洁气体供气用配管13向腔室10的内部和排气用配管15供给作为清洁气体的氢气。此时的清洁气体的流量为100sccm,除去附着物时的腔室10内的压力为67kPa。
进行5分钟清洁气体的导入,在温度500℃、压力67kPa的条件下使附着物与氢气反应而除去附着物后,停止清洁气体的导入。接着,利用真空泵38使腔室10的内部成为真空,从惰性气体供气用配管14向腔室10内供给惰性气体,用惰性气体置换腔室10的内部。
附着物除去工序结束后,与上述同样地进行钝化工序,在新的试料20上形成钝化膜。然后,与上述同样地进行了附着物除去工序。反复进行这样的操作,合计制造100个形成有钝化膜的试料20。
(实施例2)
将附着物除去工序中的腔室10内的温度设为350℃、将压力设为100Pa,除此以外与实施例1同样地制造了100个形成有钝化膜的试料20。
(实施例3)
将附着物除去工序中的腔室10内的温度设为20℃,除此以外与实施例1同样地制造了100个形成有钝化膜的试料20。
(实施例4)
将附着物除去工序中的腔室10内的温度设为800℃,除此以外与实施例1同样地制造了100个形成有钝化膜的试料20。
(实施例5)
将附着物除去工序中的腔室10内的压力设为20Pa,除此以外与实施例1同样地制造了100个形成有钝化膜的试料20。
(实施例6)
将附着物除去工序中的腔室10内的压力设为101kPa,除此以外与实施例1同样地制造了100个形成有钝化膜的试料20。
(实施例7)
将附着物除去工序中的从清洁气体供气用配管13供给的清洁气体设为甲烷气体,除此以外与实施例1同样地制造了100个形成有钝化膜的试料20。
(实施例8)
将附着物除去工序中的从清洁气体供气用配管13供给的清洁气体设为氨气,除此以外与实施例1同样地制造了100个形成有钝化膜的试料20。
(比较例1)
不进行附着物除去工序,仅反复进行钝化工序,除此以外与实施例1同样地制造了100个形成有钝化膜的试料20。
关于实施例1~8和比较例1的试料20,每当从第1个到第100个的各试料20的钝化工序结束时,测定附着在试料20表面的硫的颗粒个数。颗粒个数的测定是使用KLATencor公司制的晶片检查装置surfscan(注册商标)6240进行的。测定结果示于表1和图2中。
表1
由表1和图2可知,在不进行附着物除去工序,仅反复进行钝化工序的比较例1中,随着进行的钝化工序的次数变多,即、随着形成有钝化膜的试料20的制造个数变多,附着于试料20的颗粒的个数变多,在第30次为1000个/m2以上,在第100次为6000个/m2以上。
与此相对,在钝化工序之后进行附着物除去工序的实施例1~8中,附着于试料20的颗粒的个数少,即使钝化工序的次数是第100次,在实施例1中也为100个/m2以下,在实施例2中也为300个/m2以下,在其他实施例中也为1000个/m2以下。
这就表示,通过进行附着物除去工序,无需将腔室拆解进行清洗,能够在保持低的附着颗粒个数的状态下反复进行钝化工序。
附图标记说明
1···成膜装置
10···腔室
11···平台
12···钝化气体供气用配管
13···清洁气体供气用配管
14···惰性气体供气用配管
15···排气用配管
20···试料
Claims (5)
1.一种附着物除去方法,使附着在腔室的内表面以及与所述腔室连接的配管的内表面中的至少一者的含硫的附着物,与含有含氢化合物气体的清洁气体反应,由此将所述附着物除去,其中,在温度20℃以上且800℃以下、压力20Pa以上且101kPa以下的条件下,使所述清洁气体与所述附着物接触。
2.根据权利要求1所述的附着物除去方法,所述含氢化合物气体是选自氢气、烃气和氨气中的至少一种。
3.根据权利要求1或2所述的附着物除去方法,所述含氢化合物气体是氢气。
4.一种成膜方法,具备钝化工序和附着物除去工序,
所述钝化工序中,将含有含硫化合物气体的钝化气体供给到收纳有基板的腔室,使所述基板与所述钝化气体反应,在所述基板的表面形成钝化膜,
所述附着物除去工序中,在进行所述钝化工序之后,将附着在所述腔室的内表面以及与所述腔室连接的配管的内表面中的至少一者的含硫的附着物除去,
采用权利要求1~3中任一项所述的附着物除去方法进行所述附着物除去工序。
5.根据权利要求4所述的成膜方法,所述含硫化合物气体是硫化氢气体。
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