TWI753574B - 耐蝕性構件 - Google Patents
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- TWI753574B TWI753574B TW109131782A TW109131782A TWI753574B TW I753574 B TWI753574 B TW I753574B TW 109131782 A TW109131782 A TW 109131782A TW 109131782 A TW109131782 A TW 109131782A TW I753574 B TWI753574 B TW I753574B
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Abstract
本發明提供一種耐蝕性構件,其即使遭受熱歷程,耐蝕性被膜也不易從基材剝離。耐蝕性構件具備金屬製的基材(10)與形成在基材(10)之表面上的耐蝕性被膜(30)。耐蝕性被膜(30)係從基材(10)側起層合有含有氟化鎂的氟化鎂層(31)與含有氟化鋁的氟化鋁層(32)者。氟化鋁層(32)係從氟化鎂層(31)側起層合有含有的氟化鋁為結晶質的第一結晶質層(32A)、含有的氟化鋁為非晶質的非晶質層(32B)與含有的氟化鋁為結晶質的第二結晶質層(32C)者。第一結晶質層(32A)與第二結晶質層(32C)係在電子線繞射圖像中被觀察到繞射斑點之層,非晶質層(32B)係在電子線繞射圖像中被觀察到光暈圖型之層。
Description
本發明關於耐蝕性構件。
於半導體製程中,由於有使用氯氣、氟氣等腐蝕性強的氣體之情況,故在構成半導體製造裝置的構件,要求耐蝕性。作為構成半導體製造裝置的構件之例,可舉出腔室、配管、氣體儲存裝置、閥、基座(susceptor)、噴淋頭(shower head)等。
專利文獻1中揭示半導體製程中所使用的噴淋頭等之構件。此構件具有經由氟化鋁及氟化鎂之至少一者所成之耐蝕性被膜所被覆之鋁表面。
又,專利文獻2中揭示在基材之表面上形成耐蝕性被膜而成之真空室構件。耐蝕性被膜之表面側係以鋁氧化物為主體之層,或以鋁氧化物與鋁氟化物為主體之層,耐蝕性被膜之基材側係以鎂氟化物為主體之層,或以鎂氟化物與鋁氧化物為主體之層。
[先前技術文獻]
[專利文獻]
[專利文獻1]日本發明專利公表公報2005年第533368號
[專利文獻2]日本發明專利公開公報平成11年第61410號
[發明所欲解決的課題]
然而,專利文獻1、2中揭示的構件係有因熱歷程而耐蝕性被膜容易從基材剝離之問題點。
本發明之課題在於提供即使遭受熱歷程,耐蝕性被膜也不易從基材剝離之耐蝕性構件。
[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]~[4]。
[1]一種耐蝕性構件,其具備金屬製的基材與形成在前述基材之表面上的耐蝕性被膜,
前述耐蝕性被膜係從前述基材側起依序層合有含有氟化鎂的氟化鎂層與含有氟化鋁的氟化鋁層者,
前述氟化鋁層係從前述氟化鎂層側起依序層合有含有的氟化鋁為結晶質的第一結晶質層、含有的氟化鋁為非晶質的非晶質層與含有的氟化鋁為結晶質的第二結晶質層者,
前述第一結晶質層及前述第二結晶質層係在藉由電子線的照射所得之電子線繞射圖像中被觀察到繞射斑點之層,
前述非晶質層係在藉由電子線的照射所得之電子線繞射圖像中被觀察到光暈圖型之層。
[2]如[1]記載之耐蝕性構件,其中前述金屬製的基材為鋁製或鋁合金製。
[3]如[1]或[2]記載之耐蝕性構件,其中前述氟化鎂層之厚度為100nm以上1000nm以下。
[4]如[1]~[3]中任一項記載之耐蝕性構件,其中前述氟化鋁層之合計厚度為200nm以上50000nm以下。
[發明的效果]
本發明之耐蝕性構件係即使遭受熱歷程,耐蝕性被膜也不易從基材剝離。
[實施發明的形態]
以下說明本發明之一實施形態。尚且,本實施形態係顯示本發明之一例者,本發明係不受本實施形態所限定。又,於本實施形態,可加以各種的變更或改良,施加有如此的變更或改良之形態亦可被包含於本發明中。
本實施形態之耐蝕性構件係如圖1所示,具備金屬製的基材10與形成在基材10之表面上的耐蝕性被膜30。此耐蝕性被膜30係從基材10側起依序層合有含有氟化鎂(MgF2
)的氟化鎂層31與含有氟化鋁(AlF3
)的氟化鋁層32者。
又,氟化鋁層32係從氟化鎂層31側起依序層合有含有的氟化鋁為結晶質的第一結晶質層32A、含有的氟化鋁為非晶質的非晶質層32B與含有的氟化鋁為結晶質的第二結晶質層32C者。
而且,如圖2、4所示,第一結晶質層32A及第二結晶質層32C係在藉由電子線的照射所得之電子線繞射圖像中被觀察到繞射斑點之層。又,如圖3所示,非晶質層32B係在藉由電子線的照射所得之電子線繞射圖像中被觀察到光暈圖型之層,較佳為被觀察到僅光暈圖型之層。
尚且,第一結晶質層32A及第二結晶質層32C只要含有的氟化鋁之至少一部分為結晶質即可,不必要全部為結晶質。又,第一結晶質層32A及第二結晶質層32C之氟化鋁只要是由氟化鋁(AlF3
)、氟化鋁水合物(AlF3
・nH2
O)、一部分含有羥基的氟化鋁(AlF3-X
(OH)X
)、一部分含有羥基的氟化鋁水合物(AlF3-X
(OH)X
・nH2
O)、一部分含有氧的氟化鋁(AlF3(1-X)
O3/2X
)及一部分含有氧的氟化鋁水合物(AlF3(1-X)
O3/2X
・nH2
O)所選出的至少一個即可。又,非晶質層32B所含有的非晶質氟化鋁只要是由氟化鋁(AlF3
)、氟化鋁水合物(AlF3
・nH2
O)、一部分含有羥基的氟化鋁(AlF3-X
(OH)X
)、一部分含有羥基的氟化鋁水合物(AlF3-X
(OH)X
・nH2
O)、一部分含有氧的氟化鋁(AlF3(1-X)
O3/2X
)及一部分含有氧的氟化鋁水合物(AlF3(1-X)
O3/2X
・nH2
O)所選出的至少一個即可。
本實施形態之耐蝕性構件由於具備耐蝕性被膜30,故即使在腐蝕性強的氣體或電漿之中也具有優異的耐蝕性。又,由於在氟化鋁層32與基材10之間隔著氟化鎂層31,故氟化鋁層32與基材10之密著性高。再者,氟化鋁層32由於具有在第一結晶質層32A與第二結晶質層32C之間夾住非晶質層32B之三明治構造,故即使遭受熱歷程,耐蝕性被膜30也不易從基材10剝離,且不易發生破裂。例如,即使遭受重複升溫與降溫之熱歷程,也不易發生耐蝕性被膜30之剝離或破裂。結果,本實施形態之耐蝕性構件係即使遭受熱歷程,耐蝕性也優異,同時可抑制源自耐蝕性被膜30之剝離所造成的粒子發生。
如此的本實施形態之耐蝕性構件係適合作為需要耐蝕性及耐熱性的構件,例如適合作為構成半導體製造裝置(尤其使用化學蒸鍍法的成膜裝置)的構件。舉出具體例,適合作為以使電漿產生之狀態下在晶圓上形成薄膜之成膜裝置的基座或噴淋頭。作為構成半導體製造裝置的構件,若使用本實施形態之耐蝕性構件,則由於粒子之發生係被抑制,故可以高良率製造半導體。
本實施形態之耐蝕性構件,例如可藉由在基材10之表面上形成氟化鎂層31,更在氟化鎂層31之上,依序形成第一結晶質層32A、非晶質層32B、第二結晶質層32C而形成氟化鋁層32來製造。
氟化鎂層31例如可藉由真空蒸鍍或濺鍍等方法而形成。又,氟化鋁層32的第一結晶質層32A與第二結晶質層32C,亦例如可藉由真空蒸鍍或濺鍍等之方法而形成,尤其藉由將形成氟化鋁層的對象物控制在高溫,可提高氟化鋁層之結晶性。非晶質層32B例如可藉由蒸鍍法(物理蒸鍍(PVD)、化學蒸鍍(CVD)等)等之方法而形成,尤其藉由將形成氟化鋁層的對象物控制在低溫,可抑制氟化鋁層之結晶性。
以下,更詳細地說明本實施形態之耐蝕性構件。
構成基材10的金屬係沒有特別的限定,可為單質的金屬(含有不可避免的雜質),也可為合金。例如,可為鋁或鋁合金。
氟化鎂層31之厚度較佳為100nm以上1000nm以下。若氟化鎂層31之厚度為上述範圍內,則氟化鋁層32與基材10之密著性變更高。
氟化鋁層32之厚度,亦即第一結晶質層32A與第二結晶質層32C與非晶質層32B之合計厚度,較佳為200nm以上50000nm以下。若氟化鋁層32之厚度為上述範圍內,則遭受熱歷程時的耐蝕性被膜30之剝離困難度變更高。
氟化鎂層31及氟化鋁層32之厚度的測定方法係沒有特別的限定,但例如可舉出穿透型電子顯微鏡(TEM)、掃描型透過電子顯微鏡(STEM)、掃描型電子顯微鏡(SEM)等之方法。第一結晶質層32A、非晶質層32B、第二結晶質層32C之厚度亦各自可用同樣的方法測定。
氟化鎂層31及氟化鋁層32中存在的鎂、鋁等之各元素,例如可藉由、能量分散型X射線分析(EDS分析)進行定量。
第一結晶質層32A、非晶質層32B、第二結晶質層32C中存在結晶質或非晶質的氟化鋁者,係可藉由電子線繞射法(藉由電子線的照射所得之電子線繞射圖像)進行分析。本發明中的電子線繞射法之條件係如以下。即,使用以離子切片機加工成厚度40nm以上100nm以下之樣品,將電子線的束徑設為10nm以上20nm以下,以TEM得到電子線繞射圖像之方法。
[實施例]
以下顯示實施例及比較例,更具體地說明本發明。
[實施例1]
對於基材,首先進行前處理,然後進行真空蒸鍍,在基材之表面上形成氟化鎂層後,於氟化鎂層之上依序形成第一結晶質層、非晶質層、第二結晶質層,而形成氟化鋁層,得到耐蝕性構件。第一結晶質層及第二結晶質層係藉由加熱蒸鍍而形成,非晶質層係藉由常溫蒸鍍而形成。
構成基材的金屬係含有2.55質量%的鎂之鋁合金A5052。對於基材之前處理係如以下地進行。首先,將S-Clean AL-13(佐佐木化學藥品股份有限公司製)70g溶於水1L中,將溫度成為50℃者當作脫脂液,於此脫脂液中浸漬基材10分鐘而進行脫脂,以純水洗淨。其次,將S-Clean AL-5000(佐佐木化學藥品股份有限公司製)500g加熱至70℃,當作蝕刻液,於此蝕刻液中浸漬上述經脫脂的基材1分鐘而進行蝕刻,以純水洗淨。然後,將Smutclean(RAIKI股份有限公司)200g溶於水400g中,將溫度成為25℃者當作污垢去除液,於此污垢除去液中,浸漬上述經蝕刻的基材30秒而進行污垢去除,以純水洗淨。然後,使上述經污垢去除的基材真空乾燥,完成前處理。
形成氟化鎂層時的真空蒸鍍之條件係如以下。首先,將施有前處理的基材設置於真空室內後。將真空室內排氣直到真空度成為2×10-4
Pa為止。然後,將施有前處理的基材加熱至380℃。使用氟化鎂燒結體材料作為蒸鍍材料,對於此燒結體材料,照射電子束,打開快門,在已進行前處理的基材上形成厚度約235nm的氟化鎂層。此時的電子束之投入電力係5kV的加速電壓、40mA左右,蒸鍍時的真空度為5×10-4
Pa。
形成第一結晶質層時的蒸鍍之條件係如以下。首先,將形成有氟化鎂層的基材設置於真空室內後,將真空室內排氣直到真空度成為2×10-4
Pa為止。然後,將形成有氟化鎂層的基材加熱至400℃。使用氟化鋁燒結體材料作為蒸鍍材料,對於此燒結體材料,照射電子束,打開快門,在經加熱至400℃的基材之氟化鎂層上,形成236 nm的膜厚之氟化鋁層作為第一結晶質層。此時的電子束之投入電力係5kV的加速電壓、40mA左右,蒸鍍時的真空度為5×10-4
Pa。
形成非晶質層時的蒸鍍之條件係如以下。首先,將形成有第一結晶質層的基材設置於真空室內後,將真空室內排氣直到真空度成為2×10-4
Pa為止,保持在常溫。使用氟化鋁燒結體材料作為蒸鍍材料,對於此燒結體材料,照射電子束,打開快門,在經保持在常溫的基材之第一結晶質層上,形成厚度約451nm的氟化鋁層作為非晶質層。此時的電子束之投入電力係5kV的加速電壓、40mA左右,蒸鍍時的真空度為5×10-4
Pa。
形成第二結晶質層時的蒸鍍之條件係與第一結晶質層之情況同樣,將在第一結晶質層上形成有非晶質層的基材加熱至400℃,在經加熱至400℃的基材之非晶質層上,形成厚度約249nm的氟化鋁層作為第二結晶質層。
形成第一結晶質層、非晶質層及第二結晶質層後,在20%氟氣(剩餘80%為氮氣)環境中將基材加熱至350℃,補充上述蒸鍍中所發生的氟原子之缺損。
所形成的氟化鎂層及氟化鋁層中存在的鎂、鋁等之各元素係藉由EDS進行分析。詳細而言,對於以離子切片機加工成厚度40nm以上100nm以下之樣品,以加速電壓200V進行各層的點分析,進行鎂、鋁等各元素之分析。
所形成的第一結晶質層、非晶質層、第二結晶質層中存在結晶質或非晶質的氟化鋁者,係藉由電子線繞射法確認。詳細而言,對於以離子切片機加工成厚度40nm以上100nm以下之樣品,照射束徑10nm以上20nm以下的電子線,將以TEM得到電子線繞射圖像,將第一結晶質層、非晶質層、第二結晶質層之電子線繞射圖像分別顯示於圖2、圖3及圖4中。
對於所得之實施例1的耐蝕性構件,進行加熱試驗,評價耐蝕性被膜的剝離狀態。加熱試驗之條件係將於氮氣環境中在300℃下保持300min後,自然冷卻到室溫為止的步驟當作1個循環,進行10個循環的該者。
加熱試驗結束後,以掃描型電子顯微鏡觀察耐蝕性構件的耐蝕性被膜,評價剝離的程度。表1中顯示結果。表1中,耐蝕性被膜中剝離的部分之面積未達耐蝕性被膜之面積的1%之情況係以A表示,1%以上且未達10%之情況係以B表示,10%以上且未達50%之情況係以C表示,50%以上之情況係以D表示。
又,對於所得之實施例1的耐蝕性構件,進行腐蝕試驗,評價耐蝕性被膜的剝離狀態。腐蝕試驗係在含有氟氣(F2
)的惰性氣體環境下進行熱處理者,其條件係惰性氣體環境中的氟氣濃度為1體積%,熱處理溫度為300℃,熱處理時間為300min。
腐蝕試驗結束後,以掃描型電子顯微鏡觀察耐蝕性構件的耐蝕性被膜之表面,評價剝離的程度。表1中顯示結果。表1中,耐蝕性被膜中剝離的部分之面積未達耐蝕性被膜之面積的1%之情況係以A表示,1%以上且未達10%之情況係以B表示,10%以上且未達50%之情況係以C表示,50%以上之情況係以D表示。尚且,表1中之數值表示各層之厚度,「-」表示未形成該層。
[比較例1]
除了於氟化鎂層之上,僅形成第一結晶質層及非晶質層作為氟化鋁層,不形成第二結晶質層之點以外,與實施例1同樣地製造耐蝕性構件,進行評價。表1中顯示結果。
[比較例2]
除了於氟化鎂層之上,僅形成第一結晶質層及第二結晶質層作為氟化鋁層,不形成非晶質層之點以外,與實施例1同樣地製造耐蝕性構件,進行評價。表1中顯示結果。
[比較例3]
除了於氟化鎂層之上,僅形成非晶質層及第二結晶質層作為氟化鋁層,不形成第一結晶質層之點以外,與實施例1同樣地製造耐蝕性構件,進行評價。表1中顯示結果。
[比較例4]
除了於基材之表面上不形成氟化鎂層之點以外,與實施例1同樣地製造耐蝕性構件,進行評價。表1中顯示結果。
[比較例5]
除了於氟化鎂層之上,僅形成第一結晶質層作為氟化鋁層,不形成非晶質層及第二結晶質層之點以外,與實施例1同樣地製造耐蝕性構件,進行評價。表1中顯示結果。
[比較例6]
除了於氟化鎂層之上不形成氟化鋁層之點以外,與實施例1同樣地製造耐蝕性構件,進行評價。表1中顯示結果。
如由表1可知,實施例1係即使遭受加熱試驗的熱歷程,耐蝕性被膜之剝離也幾乎不發生。又,即使遭受腐蝕試驗的腐蝕,耐蝕性被膜之剝離也幾乎不發生。
相對於其,在表面上無氟化鋁的結晶質層之比較例1、6係發生腐蝕試驗所致的耐蝕性被膜之剝離。尤其可知非晶質層在最表面的比較例1係對於氟氣容易腐蝕。又,相較於最表面為氟化鋁的結晶質層之實施例1,可知最表面為氟化鎂層之比較例6係耐腐蝕性低。
於金屬製的基材之上,不隔著氟化鎂層,直接形成有氟化鋁層之比較例4,係在重複升溫與降溫時從界面發生剝離。
於第一結晶層與第二結晶層之間不存在非晶質層之比較例2,係在重複升溫與降溫時,在氟化鋁層的層合方向中發生裂痕,結果發生剝離。由此結果可預料:非晶質層係有助於緩和因溫度變化所發生的應力。
相較於實施例1,於氟化鎂層之上僅存在第一結晶層之比較例5係有容易發生因重複升溫與降溫所造成的裂痕之傾向,以此裂痕為起點而發生剝離。由此結果亦可預料:非晶質層係有助於緩和因溫度變化所發生的應力。
於氟化鎂層之上存在非晶質層之比較例3,係因重複升溫與降溫而在界面容易發生剝離。
10:基材
30:蝕性被膜
31:氟化鎂層
32:氟化鋁層
32A:第一結晶質層
32B:非晶質層
32C:第二結晶質層
[圖1]係說明本發明之一實施形態的耐蝕性構件之構成之剖面圖。
[圖2]係對圖1之耐蝕性構件所具有的第一結晶質層,照射電子線而得之電子線繞射圖像。
[圖3]係對圖1之耐蝕性構件所具有的非晶質層,照射電子線而得之電子線繞射圖像。
[圖4]係對圖1之耐蝕性構件所具有的第二結晶質層,照射電子線而得之電子線繞射圖像。
10:基材
30:蝕性被膜
31:氟化鎂層
32:氟化鋁層
32A:第一結晶質層
32B:非晶質層
32C:第二結晶質層
Claims (3)
- 一種耐蝕性構件,其具備金屬製的基材與形成在前述基材之表面上的耐蝕性被膜,前述耐蝕性被膜係從前述基材側起依序層合有含有氟化鎂的氟化鎂層與含有氟化鋁的氟化鋁層者,前述氟化鋁層係從前述氟化鎂層側起依序層合有含有的氟化鋁為結晶質的第一結晶質層、含有的氟化鋁為非晶質的非晶質層與含有的氟化鋁為結晶質的第二結晶質層者,前述第一結晶質層及前述第二結晶質層係在藉由電子線的照射所得之電子線繞射圖像中被觀察到繞射斑點之層,前述非晶質層係在藉由電子線的照射所得之電子線繞射圖像中被觀察到光暈圖型之層,其中前述氟化鎂層之厚度為100nm以上1000nm以下。
- 如請求項1之耐蝕性構件,其中前述金屬製的基材為鋁製或鋁合金製。
- 如請求項1或2之耐蝕性構件,其中前述氟化鋁層之合計厚度為200nm以上50000nm以下。
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- 2020-09-03 JP JP2021550483A patent/JPWO2021065327A1/ja active Pending
- 2020-09-03 CN CN202080040248.4A patent/CN113924381B/zh active Active
- 2020-09-03 EP EP20871764.5A patent/EP4039845B1/en active Active
- 2020-09-03 WO PCT/JP2020/033461 patent/WO2021065327A1/ja unknown
- 2020-09-03 US US17/595,413 patent/US20220195605A1/en active Pending
- 2020-09-16 TW TW109131782A patent/TWI753574B/zh active
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EP4039845B1 (en) | 2023-11-29 |
EP4039845A4 (en) | 2023-01-11 |
WO2021065327A1 (ja) | 2021-04-08 |
US20220195605A1 (en) | 2022-06-23 |
JPWO2021065327A1 (zh) | 2021-04-08 |
CN113924381A (zh) | 2022-01-11 |
CN113924381B (zh) | 2023-11-28 |
KR20220035202A (ko) | 2022-03-21 |
EP4039845A1 (en) | 2022-08-10 |
TW202124734A (zh) | 2021-07-01 |
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