TWI687548B - 釔系溶射被膜以及其製造方法 - Google Patents
釔系溶射被膜以及其製造方法 Download PDFInfo
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- TWI687548B TWI687548B TW105124154A TW105124154A TWI687548B TW I687548 B TWI687548 B TW I687548B TW 105124154 A TW105124154 A TW 105124154A TW 105124154 A TW105124154 A TW 105124154A TW I687548 B TWI687548 B TW I687548B
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- yttrium
- acid
- spray coating
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- based spray
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- 229910052727 yttrium Inorganic materials 0.000 title claims abstract description 65
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 238000005507 spraying Methods 0.000 title claims abstract description 51
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 56
- 238000000034 method Methods 0.000 claims abstract description 17
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 14
- CHBIYWIUHAZZNR-UHFFFAOYSA-N [Y].FOF Chemical compound [Y].FOF CHBIYWIUHAZZNR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000007921 spray Substances 0.000 claims abstract description 10
- 229940105963 yttrium fluoride Drugs 0.000 claims abstract description 10
- RBORBHYCVONNJH-UHFFFAOYSA-K yttrium(iii) fluoride Chemical compound F[Y](F)F RBORBHYCVONNJH-UHFFFAOYSA-K 0.000 claims abstract description 10
- 239000011248 coating agent Substances 0.000 claims description 27
- 238000000576 coating method Methods 0.000 claims description 27
- 239000007864 aqueous solution Substances 0.000 claims description 19
- 238000004140 cleaning Methods 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 16
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 10
- 150000007524 organic acids Chemical class 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 150000007522 mineralic acids Chemical class 0.000 claims description 9
- 239000000758 substrate Substances 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 150000001735 carboxylic acids Chemical class 0.000 claims description 8
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 7
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 150000001261 hydroxy acids Chemical class 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 5
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 5
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 5
- 239000011975 tartaric acid Substances 0.000 claims description 5
- 235000002906 tartaric acid Nutrition 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 3
- 239000004310 lactic acid Substances 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 3
- 239000011976 maleic acid Substances 0.000 claims description 3
- 229940098779 methanesulfonic acid Drugs 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 2
- KVBCYCWRDBDGBG-UHFFFAOYSA-N azane;dihydrofluoride Chemical compound [NH4+].F.[F-] KVBCYCWRDBDGBG-UHFFFAOYSA-N 0.000 claims description 2
- 239000004065 semiconductor Substances 0.000 abstract description 14
- 238000005530 etching Methods 0.000 abstract description 12
- 230000007797 corrosion Effects 0.000 abstract description 6
- 238000005260 corrosion Methods 0.000 abstract description 6
- 238000010410 dusting Methods 0.000 abstract description 4
- 229910052736 halogen Inorganic materials 0.000 abstract description 4
- 150000002367 halogens Chemical class 0.000 abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 16
- 239000007789 gas Substances 0.000 description 9
- 229910052786 argon Inorganic materials 0.000 description 8
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000428 dust Substances 0.000 description 5
- -1 Cl 2 Chemical compound 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 229910021642 ultra pure water Inorganic materials 0.000 description 4
- 239000012498 ultrapure water Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000007750 plasma spraying Methods 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- MBXOOYPCIDHXGH-UHFFFAOYSA-N 3-butylpentane-2,4-dione Chemical compound CCCCC(C(C)=O)C(C)=O MBXOOYPCIDHXGH-UHFFFAOYSA-N 0.000 description 1
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 102220043159 rs587780996 Human genes 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 150000003746 yttrium Chemical class 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
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Abstract
一種釔系溶射被膜，其特徵係由氧化釔、氟化釔以及氧氟化釔之1種或2種以上所成之厚度10~500μm之釔系溶射被膜，於該被膜表面存在之粒徑300nm以下之粒子數每1mm2為5個以下。
本發明之釔系溶射被膜即使在鹵系氣體電漿氛圍中亦發揮優異之耐腐蝕性，且於半導體製造步驟中之蝕刻處理中可盡可能防止釔系粒子之剝落所致之發塵，可有效地提高半導體製造之良率。
Description
本發明係有關溶射氧化釔、氟化釔以及氧氟化釔之1種或2種以上而成膜而成之釔系溶射被膜，尤其是可作為在半導體製造步驟中於腐蝕性電漿氛圍下使用之零件或物品之低發塵性被膜而較好地採用之釔系溶射被膜。
以往，半導體製品之製造中，在腐蝕性高的鹵系氣體電漿氛圍下進行處理，作為該鹵系腐蝕性氣體係使用SF6、CF4、CHF3、ClF3、HF等之氟系氣體，或使用Cl2、BCl3、HCl等之氯系氣體。於此等處理中所用之裝置之零件或構件係進行於表面形成耐腐蝕被膜者，例如於由金屬鋁或氧化鋁陶瓷所成之基材表面溶射氧化釔(日本專利第4006596號公報)或氟化釔(日本專利第3523222號公報，日本特表2011-514933號公報)而成膜之零件或構件之耐腐蝕性優異係為已知，而被採用。
近幾年來，隨著半導體之積體化進展，而使配線亦逐漸成為20nm以下，但於其製造過程之蝕刻中釔
系粒子自零件之釔系被膜表面剝落而掉落於Si晶圓上成為蝕刻處理之障礙，此成為使半導體裝置之良率惡化之原因。且，於蝕刻時間之初期自釔系被膜表面剝落之釔系粒子較多，隨著蝕刻時間拉長，有減少之傾向。又，作為先前技術文獻除上述以外亦舉例下述專利文獻4及5。
[專利文獻1]日本專利第4006596號公報
[專利文獻2]日本專利第3523222號公報
[專利文獻3]日本特表2011-514933號公報
[專利文獻4]日本特開2008-133528號公報
[專利文獻5]日本專利第4591722號公報
本發明係鑑於上述情況而完成者，目的在於提供溶射氧化釔、氟化釔以及氧氟化釔之1種或2種以上而成膜而成之釔系溶射被膜之中，尤其是於蝕刻處理中等可盡可能防止自被膜表面之釔系粒子之剝落，可作為在半導體製造步驟中於腐蝕性電漿氛圍下使用之零件或物品之低發塵性被膜而較好地採用之釔系溶射被膜。
本發明人等為解決上述課題而進行積極探討之結果，獲得下述見解。首先，以電漿溶射法成膜氧化釔、氟化釔以及氧氟化釔時，係成為將其材料粒子於電漿火焰中溶解、成為液滴，於基材上凝固而成膜，但若材料粒子粒徑小則不會進入火焰中，有以未溶解粉末之狀態附著於膜上之情形。且，即使暫時溶解，亦有於膜上彈開，而成為細小液滴，作為細小的粒子附著於膜上之情況。如此，於被膜表面附著之粒子若在成膜途中則在之後由液滴被覆而變為緻密之膜，於成膜結束之際附著於膜表面之細小的粒子變成直接殘留。而且，該附著粒子以超純水洗淨或超音波洗淨等去除係困難，認為此為於蝕刻處理中剝落而成為發塵原因。該情況下，雖提案有將以超純水洗淨或超音波洗淨無法去除之粒子藉由研磨或噴射處理而物理性去除之方法(日本專利第4591722號公報)，但研磨等之物理去除由於其處理本身會發生微粒子，故難以獲得有效結果。
因此，本發明人等進一步進行檢討之結果，發現藉由將溶射氧化釔、氟化釔以及氧氟化釔之1種或2種以上而成膜之釔系溶射被膜，以由，有機酸水溶液或無機酸水溶液或有機酸/無機酸混合水溶液所成之洗淨液化學性地洗淨，可有效地去除於被膜表面附著之釔系粒子，該情況下進行洗淨至厚度10~500μm之釔系溶射被膜中，於被膜表面每1mm2存在之粒徑300nm以下之粒子數成為5個以下，藉此可獲得在蝕刻處理中不會產生因釔系粒子
之剝落所致之缺陷，可作為在半導體製造步驟中於腐蝕性電漿氛圍下使用之零件或物品之低發塵性被膜而較好地採用的釔系溶射被膜，因而完成本發明。
因此，本發明提供下述請求項1~3之釔系溶射被膜及下述請求項4~7之釔系溶射被膜之製造方法。
請求項1：
一種釔系溶射被膜，其特徵係由氧化釔、氟化釔以及氧氟化釔之1種或2種以上所成之厚度10~500μm之釔系溶射被膜，於該被膜表面存在之粒徑300nm以下之粒子數每1mm2為5個以下。
請求項2：
如請求項1之釔系溶射被膜，其中膜厚為80~400μm。
請求項3：
如請求項1或2之釔系溶射被膜，其係於由金屬鋁、氧化鋁或金屬矽所成之基材表面成膜之溶射被膜。
請求項4：
一種釔系溶射被膜之製造方法，其特徵係以由有機酸水溶液或無機酸水溶液或有機酸/無機酸混合水溶液所成之洗淨液，化學性地洗淨使含有氧化釔、氟化釔以及氧氟化釔之1種或2種以上之粒子之溶射材料溶射而成膜之厚度10~500μm之釔系溶射被膜之表面，使於該被膜表面存在之粒徑300nm以下之粒子數成為每1mm2為5個以下。
請求項5：如請求項4之釔系溶射被膜之製造方法，其中上述洗淨液係自一價羧酸、二價羧酸、三價羧酸、羥基酸、磺酸、硝酸、硫酸、碳酸、氟化氫酸及酸性氟化銨選出之1種水溶液或2種以上之混合水溶液。
請求項6：如請求項5之釔系溶射被膜之製造方法，其中上述洗淨液中，上述一價羧酸為甲酸、乙酸，上述二價羧酸為馬來酸、酒石酸、鄰苯二甲酸，上述三價羧酸為檸檬酸，上述羥基酸為乳酸，上述磺酸為甲烷磺酸。
請求項7：如請求項4~6中任一項之釔系溶射被膜之製造方法，其中將釔系溶射被膜浸漬於上述洗淨液中，使該被膜自表面溶解0.01μm以上，而去除該被膜表面之粒徑300nm以下之粒子。
依據本發明，可獲得在腐蝕性高的鹵系氣體電漿氛圍下進行處理時發揮優異耐腐蝕性、且例如於半導體製造步驟之蝕刻處理中，不會產生釔系粒子之剝落所致之發塵，可有效提高半導體製造之良率，且可作為於腐蝕性電漿氛圍下使用之零件或物品之低發塵性被膜而較好地採用之釔系溶射被膜。
圖1係顯示實施例1製作之釔系溶射被膜表面之SEM照片。
圖2係顯示實施例2製作之釔系溶射被膜表面之SEM照片。
圖3係顯示實施例3製作之釔系溶射被膜表面之SEM照片。
圖4係顯示實施例4製作之釔系溶射被膜表面之SEM照片。
圖5係顯示比較例1製作之釔系溶射被膜表面之SEM照片。
圖6係顯示比較例2製作之釔系溶射被膜表面之SEM照片。
本發明之釔系溶射被膜係如上述，將氧化釔、氟化釔以及氧氟化釔之1種或2種以上溶射於期望之基材上而成膜者。
對基材之溶射可藉由大氣壓電漿溶射或減壓電漿溶射而進行。該情況下，作為電漿氣體並未特別限定而可適當選擇，舉例為例如氮/氫、氬/氫、氬/氦、氬/氮、氬單體、氮氣單體等。對溶射之基材並未限制而可根據用途等適當選擇。例如作為半導體製造裝置之零件或構件，舉例為不銹鋼、鋁、鎳、鉻、鋅及該等之合金、金屬
矽、氧化鋁、氮化鋁、氮化矽、碳化矽、石英玻璃等。又，關於溶射氧化釔、氟化釔以及氧氟化釔時之條件等，並未特別限定，只要根據基材、溶射材料之粒徑或具體材質、所得之溶射構件之用途等適當設定即可。
若例示具體例，若為於金屬鋁基材上成膜氧化釔被膜時，只要例如使用氬氣40L/min、氫氣5L/min之混合氣體將平均粒徑D50=約20μm左右之氧化釔粉末進行氬/氫大氣壓電漿溶射而成膜氧化釔被膜即可。該情況下，溶射距離或電流值、電壓值等之溶射條件只要根據溶射構件之用途等適當設定即可，進而上述氬氣供給量或氫氣供給量亦同樣可適當調整。
此處，溶射層厚度，亦即本發明釔系溶射被膜厚度為10~500μm。該情況下，厚度未達10μm時，有無法獲得充分耐腐蝕性之情況，且亦有因後述之洗淨操作露出部分基材表面之可能性。另一方面即使厚超過500μm，並不特別能期望耐腐蝕性提高效果僅是導致成本增高。又，被膜之較佳厚度為80~400μm，更好為100~400μm，又更好為100~300μm。
本發明中，以特定洗淨液洗淨成膜之上述釔系溶射被膜表面來去除附著於被膜表面之釔系粒子，調整為存在於被膜表面之粒徑300nm以下之釔系粒子成為每1mm2為5個以下。該情況下，存在於被膜表面之粒徑300nm以下之釔系粒子當然較好為0個，但若為每1mm2為5個以下，則於上述半導體製造之蝕刻處理時亦不會產
生導致實質良率降低之發塵。此處所謂釔系粒子之粒徑，係藉由SEM等之顯微鏡法等實測之各個粒子之最大徑。又，關於超過粒徑300nm之粒子，如觀看圖5、6所明瞭，於溶射被膜表面幾乎不存在，倘若存在亦為極少量，若去除粒徑300nm以下之粒子，則可去除大部分的阻礙粒子。
上述洗淨液係使用有機酸水溶液或無機酸水溶液或有機酸與無機酸水溶液之混合水溶液。該情況下，作為有機酸只要為水溶性者即可，例示有例如甲酸、乙酸等之一價羧酸，馬來酸或酒石酸、鄰苯二甲酸等之二價羧酸，檸檬酸等之三價羧酸，乳酸等之羥基酸，甲烷磺酸等之磺酸，但未特別限制，該等中尤其是酒石酸或檸檬酸，由於在食用亦無毒性且易於處理故較好使用。且無機酸亦若為水溶性者則未特別限制，但可較好地使用例如硝酸、硫酸、碳酸、氟化氫酸、酸性氟化銨。
洗淨方法並未特別限制，就效果與效率方面而言，較好為將於零件或構件之基材表面成膜形成之上述釔系溶射被膜連同該零件或構件一起浸漬於上述洗淨液之方法。該情況下，基材若為金屬鋁或金屬Si，則由於於酸中易溶解，故使用強酸性之酸時，不欲受酸腐蝕之處期望以樹脂膠帶或薄片遮蔽。若為鄰苯二甲酸、酒石酸、檸檬酸等之弱酸性羧酸或羥基酸等之有機酸不須遮蔽即可洗淨。又，若基材為對酸抗性較強之石英玻璃或A1203陶瓷，則即使為硝酸等之強酸性溶液亦不須遮蔽即可洗淨。
且根據情況，亦可使用組合酸與鹽作成緩衝溶液之洗淨液。
如此以上述洗淨液化學性地洗淨釔系溶射被膜而薄薄地溶解該被膜表面，而去除成為發塵原因之粒徑300nm以下之粒子。被膜之溶解量較好為自被膜表面起0.01μm以上。該情況下，溶解量上限並未特別限制，但較好為自被膜表面起20μm以下，更好之溶解量為自被膜表面起1~20μm。溶解量未達0.01μm時，無法充分去除粒徑300nm以下之粒子，而有無法達成5個/1mm2以下之情況，另一方面，即使溶解超過20μm之被膜，僅是使被膜變薄，對粒子去除幾無影響。
洗淨後，以超純水充分洗淨酸後，進行真空乾燥或常壓乾燥。乾燥後之被膜表面例如藉由將掃描型電子顯微鏡(SEM)之二次電子像進行10000倍以上觀察，可確認被膜表面之300nm以下之釔系粒子，本發明係藉由上述洗淨操作自被膜表面去除該釔系粒子，而調整為每1mm2為5個以下者。
以下顯示實施例與比較例，具體說明本發明，但本發明不受限於下述實施例。
於由表1記載之材質所成之基材(試驗片)表面成膜表
1記載之溶射被膜，將其連同基材一起浸漬於表1記載之洗淨劑之水溶液所成之洗淨液中而洗淨被膜表面，以超純水充分洗淨後，真空乾燥獲得釔系溶射被膜。所得釔系被膜之表面以掃描型電子顯微鏡(SEM)觀察，確認該表面上存在之粒徑300nm以下之釔系粒子之存在及個數。結果示於表1，各SEM照片分別示於圖1~6。又，溶射所致之釔系被膜之成膜，係藉由使用氬40L/min、氫8L/min之混合氣體的大氣壓電漿溶射進行。
如表1及圖1~6所示，確認於本發明之實施例1~4之釔系溶射被膜表面完全不存在粒子，但於未進行酸水溶液(洗淨劑)之洗淨的比較例1、2之釔系溶射被膜表面附著無數粒子，容易預測該粒子於蝕刻處理中等成為發塵原因。
因此，藉由使用形成有實施例1~4之釔系溶射被膜之零件或構件，於半導體製造步驟之蝕刻處理中可盡可能防止釔系粒子剝落所致之發塵，而可提高半導體製造之良率。
Claims (7)
- 一種釔系溶射被膜，其特徵係由氧化釔、氟化釔以及氧氟化釔之1種或2種以上所成之厚度10~500μm之釔系溶射被膜，於該被膜表面存在之粒徑300nm以下之粒子數每1mm2為5個以下。
- 如請求項1之釔系溶射被膜，其中膜厚為80~400μm。
- 如請求項1或2之釔系溶射被膜，其係於由金屬鋁、氧化鋁或金屬矽所成之基材表面成膜之溶射被膜。
- 一種釔系溶射被膜之製造方法，其特徵係以由有機酸水溶液或無機酸水溶液或有機酸/無機酸混合水溶液所成之洗淨液，由含有氧化釔、氟化釔以及氧氟化釔之1種或2種以上之粒子之溶射材料溶射而成膜之厚度10~500μm之釔系溶射被膜之表面溶解0.01μm，去除於該溶射被膜之表面存在之粒徑300nm以下之粒子，使其數量成為每1mm2為5個以下。
- 如請求項4之釔系溶射被膜之製造方法，其中上述洗淨液係自一價羧酸、二價羧酸、三價羧酸、羥基酸、磺酸、硝酸、硫酸、碳酸、氟化氫酸及酸性氟化銨選出之1種水溶液或2種以上之混合水溶液。
- 如請求項5之釔系溶射被膜之製造方法，其中上述洗淨液中，上述一價羧酸為甲酸、乙酸，上述二價羧酸為馬來酸、酒石酸、鄰苯二甲酸，上述三價羧酸為檸檬酸，上述羥基酸為乳酸，上述磺酸為甲烷磺酸。
- 如請求項4~6中任一項之釔系溶射被膜之製造方法，其中將釔系溶射被膜浸漬於上述洗淨液中，使該被膜自表面溶解0.01μm以上，而去除該被膜表面之粒徑300nm以下之粒子。
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| CN112831744A (zh) * | 2020-12-31 | 2021-05-25 | 沈阳富创精密设备股份有限公司 | 一种应用于半导体设备的陶瓷涂层的制备方法 |
| JP7214935B1 (ja) * | 2021-06-07 | 2023-01-30 | 株式会社新菱 | イットリウム系薄膜の密着性を改善する方法 |
| CN116018669A (zh) * | 2021-08-23 | 2023-04-25 | 株式会社日立高新技术 | 等离子处理装置用保护皮膜的清洗方法 |
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| US20130202990A1 (en) * | 2012-02-02 | 2013-08-08 | Vibhu Jindal | Coating of shield surfaces in deposition systems |
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| KR20170015236A (ko) | 2017-02-08 |
| US20170253955A1 (en) | 2017-09-07 |
| KR20230011461A (ko) | 2023-01-20 |
| KR20210114371A (ko) | 2021-09-23 |
| TW201718912A (zh) | 2017-06-01 |
| US20170029628A1 (en) | 2017-02-02 |
| JP6500681B2 (ja) | 2019-04-17 |
| JP2017031457A (ja) | 2017-02-09 |
| KR102602620B1 (ko) | 2023-11-16 |
| CN106399896A (zh) | 2017-02-15 |
| US20240043983A1 (en) | 2024-02-08 |
| CN116695048A (zh) | 2023-09-05 |
| KR20210009410A (ko) | 2021-01-26 |
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