TWI650301B - 氧化鎂系陶瓷膜、半導體製造裝置用元件及氧化鎂系陶瓷膜之製法 - Google Patents
氧化鎂系陶瓷膜、半導體製造裝置用元件及氧化鎂系陶瓷膜之製法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 41
- 238000004519 manufacturing process Methods 0.000 title claims description 16
- 239000004065 semiconductor Substances 0.000 title claims description 11
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title description 238
- 239000000395 magnesium oxide Substances 0.000 title description 113
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 title description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 24
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 6
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 6
- 239000006104 solid solution Substances 0.000 claims abstract description 6
- 239000007921 spray Substances 0.000 claims description 40
- 239000002994 raw material Substances 0.000 claims description 32
- 239000002245 particle Substances 0.000 claims description 16
- 238000005259 measurement Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 10
- 238000002347 injection Methods 0.000 claims 1
- 239000007924 injection Substances 0.000 claims 1
- 229910020068 MgAl Inorganic materials 0.000 abstract description 27
- 239000013078 crystal Substances 0.000 abstract description 11
- 238000005260 corrosion Methods 0.000 description 28
- 230000007797 corrosion Effects 0.000 description 28
- 238000007751 thermal spraying Methods 0.000 description 15
- 239000000463 material Substances 0.000 description 14
- 238000005507 spraying Methods 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 239000000758 substrate Substances 0.000 description 10
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- 238000005422 blasting Methods 0.000 description 7
- 238000005530 etching Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 210000002381 plasma Anatomy 0.000 description 7
- SXAMGRAIZSSWIH-UHFFFAOYSA-N 2-[3-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,2,4-oxadiazol-5-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NOC(=N1)CC(=O)N1CC2=C(CC1)NN=N2 SXAMGRAIZSSWIH-UHFFFAOYSA-N 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 6
- WZFUQSJFWNHZHM-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 WZFUQSJFWNHZHM-UHFFFAOYSA-N 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 230000007423 decrease Effects 0.000 description 5
- 239000011777 magnesium Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- ZRPAUEVGEGEPFQ-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]pyrazol-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C=1C=NN(C=1)CC(=O)N1CC2=C(CC1)NN=N2 ZRPAUEVGEGEPFQ-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000004453 electron probe microanalysis Methods 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000007750 plasma spraying Methods 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 229910052596 spinel Inorganic materials 0.000 description 3
- 239000011029 spinel Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
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- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000013585 weight reducing agent Substances 0.000 description 2
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- YJLUBHOZZTYQIP-UHFFFAOYSA-N 2-[5-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-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=N2 YJLUBHOZZTYQIP-UHFFFAOYSA-N 0.000 description 1
- 238000007088 Archimedes method Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 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
- GSWGDDYIUCWADU-UHFFFAOYSA-N aluminum magnesium oxygen(2-) Chemical compound [O--].[Mg++].[Al+3] GSWGDDYIUCWADU-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- UAMZXLIURMNTHD-UHFFFAOYSA-N dialuminum;magnesium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Mg+2].[Al+3].[Al+3] UAMZXLIURMNTHD-UHFFFAOYSA-N 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000227 grinding 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
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
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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
本發明的MgO系陶瓷膜,係Al固溶於MgO,使用CuKα線的XRD測定,MgO(200)面的繞射峰向較2θ=42.92°高角側偏移,結晶相包含MgO與MgAl2O4。MgO(200)面的繞射波峰於高角側具有肩峰為佳。此外,將Mg與Al以氧化物換算時的MgO與Al2O3的質量比(MgO/Al2O3)較2.33大為佳。
Description
本發明係關於氧化鎂系陶瓷膜、半導體製造裝置用元件及氧化鎂系陶瓷膜之製法。
用於半導體製造的乾式製程或電漿塗層等的半導體製造裝置,作為蝕刻用及清潔用,使用反應性及腐蝕性高的F、Cl等的鹵素系電漿。組入如此之半導體製造裝置的元件需要很高的抗蝕性。該等材料,由於長時間的使用會漸漸地進行腐蝕,而因發塵等成為對半導體的污染原因,故需要很高的抗蝕性。抗蝕性高的材料,已知有氧化鋁、氮化鋁、氧化釔等,使用於半導體製造裝置。此外,抗蝕性高的材料,已知例如,專利文獻1~2所述之材料。
於專利文獻1,揭示一種陶瓷熔射膜,其特徵在於:主要成分係由MgO與Al2O3所組成的尖晶石質的陶瓷熔射膜,MgO與Al2O3的質量比(MgO/Al2O3)為0.25~1.5,體積電阻率為1×108~1×1014Ωcm,尖晶石結晶的晶格常數a=8.084Å以上。於該專利文獻1,記載含較多氧化鎂在抗蝕性方面較佳,但由於有吸水性而難以處理,此外吸水會使抗蝕性惡化,故上述質量比為1.50以下。
於專利文獻2,揭示一種抗蝕性陶瓷材料,其特徵在於,其係以MgO與Al2O3為主成分的尖晶石質陶瓷材料,MgO與Al2O3的組成比及重量比在1~2.33的範圍,且結晶晶粒的平均粒徑未滿3μm。於該專利文獻2,記載上述重量比超過2.33則MgO的量過多而會降低抗蝕性。
[專利文獻1]日本專利第5188898號公報
[專利文獻2]日本專利第4368021號公報
但是,至今並無多含MgO而抗蝕性高的陶瓷膜。例如,於專利文獻1,記載於陶瓷熔射膜多含MgO則因會吸水而使抗蝕性惡化,實際上,MgO/Al2O3的質量比超過1.5的陶瓷熔射膜,蝕刻速率高而抗蝕性會下降。此外於專利文獻2,亦記載當MgO的量過多則抗蝕性會下降,實際上,MgO/Al2O3的質量比為2.4或2.57的燒結體的蝕刻速率高而抗蝕性會下降。
本發明係為解決如此的課題而完成,以提供抗蝕性高的MgO系陶瓷膜為主要目標。
本發明者們,以各種比例混合MgO與Al2O3作成顆粒狀之後,以既定溫度熱處理者作為熔射原料,研究將該熔
射原料熔射而得之MgO系陶瓷膜的抗蝕性,結果發現某種MgO系陶瓷膜抗蝕性優良,而達至完成本發明。
即,本發明的MgO系陶瓷膜,係Al固溶於MgO,使用CuKα線的XRD測定,MgO(200)面的繞射峰向較2θ=42.92°高角側偏移,結晶相包含MgO與MgAl2O4。
此外,本發明的MgO系陶瓷膜之製法,係將MgO與Al2O3作成顆粒狀之後製作以1200℃以上的熱處理者作為熔射原料,藉由將該熔射原料對既定的基板熔射製造上述MgO系陶瓷膜。
第1圖係實驗例2之熔射原料的XRD分析圖表。
第2圖係實驗例4-1之熔射膜的XRD分析圖表。
第3圖係第2圖之部分放大圖。
第4圖係實驗例7-1之熔射膜的XRD波峰放大圖。
第5圖係實驗例7-1之熔射膜的XRD波峰放大圖。
本發明的MgO系陶瓷膜,係Al固溶於MgO,使用CuKα線的XRD測定,MgO(200)面的繞射峰向較2θ=42.92°高角側偏移,結晶相包含MgO與MgAl2O4。在此,所謂「MgO系陶瓷膜」係指包含在陶瓷膜中的化合物之中MgO的質量%最大者,例如MgO超過50質量%。本發明的MgO系陶瓷膜,抗蝕性優良。其理由之一個原因可認為是本發明的MgO系陶瓷膜的吸水性較MgO單體的陶瓷相低。
此外,在使用CuKα線的XRD測定,MgO(200)面的繞射波峰向高角側偏移為佳,向2θ=42.96°以上的高角側偏移為佳。由於藉由向高角側偏移,增加Al的固溶量,提升MgO的耐水性。
本發明的MgO系陶瓷膜,在使用CuKα線的XRD測定,亦可在MgO(200)面的繞射波峰的高角側具有新的繞射波峰或肩峰。該新的繞射波峰或肩峰,可認為是來自結晶結構相同而Al進一步固溶而使晶格常數變化的MgO,例如藉由熔射而被急速冷卻等的熱力學上的非平衡狀態而生成。由於該新的繞射波峰或肩峰,可分峰,則可觀察到抗蝕性的下降的趨勢,故以無法看作是完全的繞射波峰或無法分峰的程度的肩峰呈現為佳。另一方面,由提升耐水性的觀點,該新的繞射波峰或肩峰可明確地分峰有降低在吸水時的重量減少的趨勢而佳。該新的繞射波峰或肩峰,可認為是藉由Al固溶於MgO而改善MgO的低耐水性的特性。
本發明的MgO系陶瓷膜,係將Mg與Al以氧化物換算時的MgO與Al2O3的質量比MgO/Al2O3較2.33大為佳。在該質量比2.33以下時,由於可觀察到抗蝕性下降的趨勢,該質量比較2.33大為佳。
本發明的MgO系陶瓷膜,以熔射膜為佳。熔射方法,只要可將熔射用原料熔融,該方法並無特別限定,可舉例如,電漿熔射法、氣體式熔射法、氣體爆炸熔射法等。
本發明的MgO系陶瓷膜,MgO(200)面的繞射波峰(以下,稱為繞射波峰(A))與出現在較MgO(200)面的繞射波峰
高角側的新繞射波峰或肩峰(以下,稱為繞射波峰(B))的峰高比IB/IA以0.33以下為佳,較0.22小更佳。繞射波峰(B)的結晶相可認為是經由熱力學的非平衡狀態生成,故可預測其結晶性低,而抗蝕性亦低。但是,由於Al固溶於MgO結晶,故在保持耐水性的觀點,可存在不對抗蝕性造成不良影響的程度。
本發明的MgO系陶瓷膜,繞射波峰(A)、(B)及MgAl2O4的(220)方面的繞射波峰(以下,稱為繞射波峰(C))的峰高比IC/(IA+IB)以0.2以下為佳,以0.1以下更佳。該值高,則相對於MgO,抗蝕性低的MgAl2O4會增加,而降低陶瓷膜的抗蝕性。
本發明的MgO系陶瓷膜,孔隙率以20%以下為佳,以15%以下更佳,進一步以13%以下更佳。求得孔隙率的方法可舉根據膜的剖面照片的影像處理,由膜與孔洞的面積比求得。已知膜的真密度時,可以阿基米德法求得膜的孔隙率。此外,只要可求得孔隙率,其方法並無限制。孔隙率超過20%,則熔射膜的強度有下降之虞或因材料本身的脫粒而容易發塵之虞,再者有腐蝕性高的鹵素系電漿腐蝕抗蝕性低的基材部分之虞而不佳。此外,孔隙率,越接近零越佳。因此,並無特定下限值。
本發明的MgO系陶瓷膜,可利用於作為披覆半導體製造裝置用元件的表面的披膜。半導體製造裝置用元件,可舉例如,靜電吸盤或晶舟、加熱器、盤、腔體、內壁材、監視窗、微波導入窗、微波藕合天線等。該等,由於需要對含有鹵素的腐蝕性氣體的電漿具有優良的抗蝕性,以本發明的MgO
系陶瓷膜披覆為佳。
本發明的MgO系陶瓷膜之製法,係將MgO與Al2O3作成顆粒狀之後製作以1200℃以上的熱處理者作為熔射原料,藉由將該熔射原料對既定的基板熔射而得。熔射原料,係將MgO與Al2O3的顆粒熱處理者,結晶相包含MgO與MgAl2O4。如此的熔射原料,係MgO與MgAl2O4良好接觸的狀態,與僅將MgO與MgAl204混合者相比,Al較容易固溶於MgO且可相對容易製造更殘留MgO的MgO系陶瓷膜。再者,使用如此的熔射原料熔射之點,在於上述專利文獻1、2並無表示。熔射法,只要可將熔射原料熔融,其方法並無特別限定,可舉例如電漿熔射法、氣體式熔射法、氣體爆炸熔射法等。電漿氣體,並無特別限定,可採用氬、氦、氮、氫、氧氣及該等的複數組合。關於熔射條件,並無特別限定,只要按照熔射用原料或形成披膜的基板的種類適宜設定即可。
[實施例]
以下表示本發明的實施例。再者,以下的實施例並非限定本發明。此外,實驗例1~9係熔射原料的具體例,實驗例1-1~9-1係熔射膜的具體例。其中,實驗例1-1~7-1係實施例,實驗例8-1~9-1係比較例。
[實驗例1~9]
(熔射原料的製作)
實驗例1~7的熔射原料,係以如下方法製作。首先,如第1表所示質量%秤量MgO原料(純度99.9質量%以上,粒度(D50)3μm以下),Al2O3原料(純度99.9質量以上,粒度(D50)1μm
以下),以粉末30質量%、水70質量%、及對粉末1質量%的分散劑(優墾工業製Serander)加入水及分散劑。以直徑20mm的內含鐵芯的尼龍球作為磨球,以尼龍製的罐將該等濕式混合。將混合後的漿料,使用噴霧乾燥機噴霧,製作顆粒。將如此的顆粒稱為「SD顆粒」。之後,在大氣氣氛以1600℃熱處理。所得熱處理粉末,以75μm網目的篩網振動過篩,將篩落所得原料作為熔射原料。
此外,於實驗例8,係將粉碎製作的市售MgO原料(粒度(D50)34μm)與市售的MgAl2O4(粒度(D50)約4μm),以與實驗例4相同的MgO/Al2O3比調配,以與實驗例1~7同樣地製作SD顆粒之後沒有處理熱的作為熔射原料。於實驗例9,將實驗例8所使用的市售MgO原料單體作為熔射原料。
(熔射原料的評估)1)
1)XRD測定
藉由X射線繞射裝置鑑定結晶相。測定條件為CuKα,40kv,40mA,2θ=10-70°,使用封管式X射線繞射裝置(BRUKER AXS D8 ADVANCE)。測定的行進間隔為0.02°,為特定波峰峰頂的繞射角添加NIST製Si標準樣品粉末(SRM640C),修正波峰位置。將其結果示於第1表。
2)粒度分佈
對所得熔射原料的粉末求粒度分佈。測定係以日機裝製MicrotracMT3300EX II進行,求累積粒徑10%(D10)及90%(D90)。將其結果示於第1表。
3)SEM觀察
對所得熔射原料進行SEM觀察。
(熔射用原料的評估結果)
於第1圖表示實驗例2的熔射原料的XRD測定結果。由第1圖可知結晶相係由MgO與MgAl2O4構成。雖未示於圖,實驗例1、3~8亦相同。進行SEM觀察的結果,確認到關於實驗例1~7一次粒徑有變得較原來的MgO及MgAl2O4大,粒子相互以頸部連接,藉由熱處理MgO與Al2O3反應生成MgO與MgAl2O4,而一部分進行燒結而使MgO與MgAl2O4接觸良好。另一方面,在於實驗例8,並未觀察到MgO與MgAl2O4晶粒成長,並未觀察到粒子相互以頸部連結的樣子。
[實驗例1-1~9-1]
(熔射膜的製作)
準備Ra>1μm的鋁基板作為熔射基板。將實驗例1~9所得
的熔射原料,在大氣氣氛以第2表所示條件對熔射基板實施電漿熔射。
如於實驗例1-1係以實驗例1的熔射原料,於實驗例2-1係以實驗例2的熔射原料,使用實驗例N(N係1~9的整數)的熔射原料所製作的熔射膜為實驗例N-1。於實驗例1-1~7-1的熔射膜,得到厚度30~210μm的熔射膜。使用實驗例8的熔射原料時,由於得到較實驗例1~7更薄的熔射膜,故增加熔射次數得到厚度30μm的熔射膜。使用實驗例9的熔射原料時,即使以與實驗例1-1~7-1的實施例大致相同的粉末供應量重複相同次數的成膜,亦無法在基板上得到熔射膜。
(熔射膜的評估)
1)XRD測定
藉由X射線繞射裝置鑑定結晶相。將所得熔射膜由基板剝離,以研缽粉碎成粉末狀。測定條件係以CuKα,40kV,40mA,2θ=10-70°,使用封管式X設限時機裝置(BRUKER AXS D8 ADVANCE)。測定的行進間隔為0.02°,為特定波峰峰頂的繞射角添加NIST製Si標準樣品粉末(SRM640C),修正波峰位置。確認在ICDD78-0430所示的MgO(111)面、(200)面、(220)面附近分別檢測出繞射波峰之後,求各熔射膜的MgO(200)面的繞射角的波峰峰頂的位置。此外,以市售的軟體MDI公司製JADE7的波峰搜尋功能求得各個峰高。JADE7的波峰搜尋條件,關於過濾類型為可變,關於拋物線過濾器、波峰位置的決定係以波峰峰頂、限值的範圍,係線值σ=3.0,波峰強度%切除=0.1,決定BG的範圍=1.0,BG平均化的點數=7,消除Kα2
波峰ON、消除現存的波峰清單ON。將各熔射膜的結晶相、MgO(200)面的繞射角的波峰峰頂位置、繞射波峰(A)~(C)的高度示於第2表。再者,關於繞射波峰(A)~(C)將於後述。
2)成分分析
將所得熔射膜由基板剝離,以研缽作成粉末,進行化學分析。將試料溶解之後,將Mg及Al以螯合物滴定法定量。將結果示於第2表。
3)抗蝕性試驗
將所得熔射膜的表面鏡面研磨,將一部分掩蓋使用ICP電漿抗腐試驗裝置,以如下條件進行抗蝕試驗。藉由段差計測定掩蓋面與暴露面的段差以試驗時間商除算出各材料的蝕刻速率。將結果示於第2表。
ICP:800W,偏壓:450W,導入氣體:NF3/O2/Ar=75/35/140sccm 0.05Torr,暴露時間:5h,試料溫度:室溫
4)吸水性試驗
關於實驗例1-1~7-1,將熔射膜由基板剝離,以30℃、95%濕度的環境下保管4天之後,以TG-DTA於大氣加熱至500℃求重量減少。將結果示於第2表。關於MgO沒有得到熔射膜,故將市售的MgO粉末以壓制機成形,以1600℃熱處理之後,作成厚度約200μm,假定成熔射膜,以同樣的方法求得重量減少。將所得重量減少以熔射膜(關於MgO係以燒給體的膜面)的單邊的面積換算。將結果示於第2表。
5)構成元素
將實驗例1-1~7-1的熔射膜剖面,邊以真空脫泡邊鑲埋於環氧樹脂中使環氧樹脂固化之後進行鏡面研磨,使用EPMA進行構成元素的感測及鑑定。
6)孔隙率
藉由將熔射膜鑲埋於樹脂(環氧樹脂),將熔射膜的氣孔以樹脂填埋之後,將熔射膜的剖面切出研磨,之後以SEM(掃描式電子顯微鏡)取得熔射膜剖面的SEM影像。SEM影像,係倍率500倍,712×532像素的影像。所得影像,係以影像分析軟體(Media Cybernetics公司製Image-Pro Plus 7.0J),首先變換為16位元灰階之後(以增值定標),進行2值化處理,計算出膜的孔隙率。2值化時的限值,係使用大津的2值化設定判定方法。
[第2表]
(熔射膜的評估)
以XRD測定實驗例1-1~8-1的熔射膜的結果,確認可以檢測到包含MgO(200)面,ICDD78-0430所示的MgO附近的繞射波峰,此外亦檢測到鎂鋁氧化物(MgAl2O4)。
作為XRD測定的代表例,第2圖係表示實驗例4-1的XRD分析圖表,第3圖係其放大圖,第4圖係表示實驗例7-1的XRD波峰放大圖。由第2圖可知實驗例4-1的熔射膜係由MgO及鎂鋁氧化物(MgAl2O4)組成。雖未示於圖,實驗例1-1~實驗例8-1之其他熔射膜亦同樣地係由MgO與MgAl2O4組成。此外,由第3圖、第4圖,確認實驗例4-1、7-1的MgO(200)面的繞射波峰(以下,稱為繞射波峰(A)),峰值向較MgO(ICDD78-0430)高角側偏移。雖未示於圖,如第2表實驗例1-1~7-1之其他的實驗例,亦確認到同樣地峰值往高角側偏移。於第4圖,在MgO(200)面的高角側,與MgAl2O4(400)面之間,確認到在原料沒有看到的新繞射波峰(以下,稱為繞射波峰(B))。此外,於第5圖表示實驗例7-1的MgO(220)面的放大波峰。與MgO(200)面同樣地,在MgO(220)面的高角側確認到在原料沒有看到的繞射波峰。再者,關於MgO(111)面,由於波峰與MgAl2O4的(311)面的繞射波峰位置非常接近而無法分離,而高角側的波峰無法明確地確認。關於後述的EPMA,幾乎沒有檢測到Mg、Al、O之外的元素來看,該新繞射波峰(B)、繞射波峰(A),雖然晶格常數不同,可知係與MgO具有相同結晶結構的物質。關於第3圖的實驗例4-1,於MgO(200)面的繞射波峰的高角側可看到些微的肩峰,可認為是存在極少
量與實驗例7-1同樣地具有與MgO相同的結晶結構的結晶相,於上述波峰分離中無法將繞射波峰(B)分離,推測其峰高非常的小。於第2表彙整繞射波峰(B)的高度。雖均確認到繞射波峰(B),但是關於一部分的樣品無法明確分離。此外,於第2表表示做為MgAl2O4(220)面的繞射波峰(以下,稱為繞射波峰(C))時的峰高。繞射波峰(C)係出現在2θ=31.27°附近。熔射原料Al的量越少該值的變化越小,可知原料的Al量越少MgAl2O4的生成量越少。此外,在於實驗例8-1,雖然檢測到MgO及MgAl2O4,但幾乎沒有觀察到向MgO的高角側的峰值偏移。此外,於實驗例8-1,MgAl2O4的繞射波峰(C)變得較MgO的繞射峰(A)大。由以上,可推測如實驗例1-1~7-1由微粒的MgO與MgAl2O4經熱處理反應,使MgO與MgAl2O4頸部連結等良好地使MgO與MgAl2O4接觸的熔射原料,可較如實驗例8-1僅為混合MgO與MgAl2O4的粉末,得到使Al固溶於MgO且更殘留MgO的MgO系陶瓷熔射膜。
測定EPMA的結果,可知係由主要包含Mg與O及微量的Al的部分,與較此包含較多Al的部分所組成。可認為前者為MgO,後者為MgAl2O4,與XRD的測定結果彙整,則顯示Al固溶於MgO。此外,亦確認到Al,較Al固溶於MgO中的Al的量多,較MgAl2O4中的Al的量少的相,顯示此係相當於繞射波峰(B)的部分。
於第2表表示熔射膜的化學分析的結果,及由此所得Mg與Al以氧化物換算時的MgO與Al2O3的質量比(MgO/Al2O3)。實驗例1-1~5-1之質量比較2.33大,實驗例6-1~7-1
則為2.33以下。
於第2表表示實驗例1-1~7-1之熔射膜的蝕刻速率的結果。任一熔射膜均蝕刻速率小而抗蝕性高。其中,實驗例1-1~5-1相對於實驗例6-1~7-1蝕刻速率較小。由此,可知MgO與Al2O3的質量比(MgO/Al2O3)較2.33大可提升抗蝕性。
此外,關於熔射膜的孔隙率,實驗例2-1為14.5%,實驗例4-1為12.7%,實驗例6-1為8.1%,實驗例7-1為7.3%。
於第2表表示根據TG-DTA測定的每面積當量的重量減少(mg/cm2)。實驗例1-1~7-1的重量減少,由顯示較第2表所沒有記載的MgO燒結體的重量減少1.5mg/cm2更小的值來看,本熔射膜的吸水性較MgO低,即耐水性優良。
本發明係主張以日本專利申請編號2014-133870為優先權其申請日為西元2014年6月30日,且其全部內容以參考資料包含於此。
再者,上述實施例當然並非有任何限定本發明者。
本發明,例如可利用於在半導體製造的乾式製程或電漿塗層等的半導製造裝置。
Claims (7)
- 一種MgO系陶瓷膜,固溶於MgO的是Al而不是AlN,使用CuKα線的XRD測定,MgO(200)面的繞射峰向較2θ=42.92°高角側偏移,結晶相包含MgO與MgAl2O4。
- 根據申請專利範圍第1項之MgO系陶瓷膜,其中在於上述XRD測定,MgO(200)面的繞射波峰在高角側具有繞射波峰或肩峰。
- 根據申請專利範圍第1或2項之MgO系陶瓷膜,其中將Mg與Al以氧化物換算時的MgO與Al2O3的質量比(MgO/Al2O3)較2.33大。
- 根據申請專利範圍第1或2項所述的MgO系陶瓷膜,其中孔隙率為20%以下。
- 根據申請專利範圍第1或2項所述的MgO系陶瓷膜,其係熔射膜。
- 一種半導體製造裝置用元件,以申請專利範圍第1至5項中任一項所述的MgO系陶瓷膜披覆。
- 一種MgO系陶瓷膜之製法,將MgO與Al2O3作成顆粒狀之後製作以1200℃以上的熱處理者作為熔射原料,藉由將該熔射原料對既定的基板熔射製造申請專利範圍第5項之MgO系陶瓷膜。
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