TWI751701B - 耐蝕性構件 - Google Patents

耐蝕性構件 Download PDF

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TWI751701B
TWI751701B TW109131778A TW109131778A TWI751701B TW I751701 B TWI751701 B TW I751701B TW 109131778 A TW109131778 A TW 109131778A TW 109131778 A TW109131778 A TW 109131778A TW I751701 B TWI751701 B TW I751701B
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corrosion
resistant
base material
mass
buffer layer
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宮石壮
大久保雅裕
吉村真幸
坂根航
田中鉄兵
中村冴子
山木沙織
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日商昭和電工股份有限公司
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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)、形成在基材(10)之表面上的耐蝕性被膜(30)與形成在基材(10)及耐蝕性被膜(30)之間的緩衝層(20)。基材(10)含有在基材(10)所含有的元素之中質量含有率最高的元素之主元素與質量含有率為1質量%以下的元素之微量元素。耐蝕性被膜(30)係以選自氟化鎂、氟化鋁及氧化鋁的至少1種所構成。緩衝層(20)含有與微量元素同種的元素，緩衝層(20)中所含有之與微量元素同種的元素之藉由能量分散型X射線分析的含有率為2質量%以上99質量%以下。

Description

耐蝕性構件
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中揭示一種耐蝕性構件，其係在由金屬所成的基材之表面上形成由鎂氟化物膜所成的耐蝕性被膜而成者。又，專利文獻2中揭示一種耐蝕性鋁合金材，其係由含有鎂的鋁合金所成之基材的表面被由含有氟化鎂的氟化鈍態膜所成之耐蝕性被膜所被覆者。 [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2000年第169953號 [專利文獻2]日本發明專利公開公報平成4年第66657號
[發明所欲解決的課題]
然而，專利文獻1、2中揭示的耐蝕性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]～[5]。 [1]一種耐蝕性構件，其具備金屬製的基材、形成在前述基材之表面上的耐蝕性被膜與形成在前述基材及前述耐蝕性被膜之間的緩衝層， 前述基材含有在前述基材所含有的元素之中質量含有率最高的元素之主元素與質量含有率為1質量%以下的元素之微量元素， 前述耐蝕性被膜係以選自氟化鎂、氟化鋁及氧化鋁的至少1種所構成， 前述緩衝層含有與前述微量元素同種的元素，前述緩衝層中所含有之與前述微量元素同種的元素之藉由能量分散型X射線分析的含有率為2質量%以上99質量%以下。
[2]如[1]記載之耐蝕性構件，其中前述主元素為鋁。 [3]如[1]或[2]之耐蝕性構件，其中前述微量元素係選自鉻、鎳、鐵及銅的至少1種。
[4]如[1]～[3]中任一項記載之耐蝕性構件，其中前述緩衝層之厚度為5nm以上100nm以下。 [5]如[1]～[4]中任一項記載之耐蝕性構件，其中前述耐蝕性被膜之厚度為100nm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、形成在基材10之表面上的耐蝕性被膜30與形成在基材10及耐蝕性被膜30之間的緩衝層20。即，在基材10之表面上形成緩衝層20，在緩衝層20之上形成耐蝕性被膜30。
基材10含有在基材10所含有的元素之中質量含有率最高的元素之主元素與質量含有率為1質量%以下的元素之微量元素(例如，雜質元素、形成合金的元素)。此處，基材10中的主元素之質量含有率較佳為50質量%以上。 耐蝕性被膜30係以選自氟化鎂(MgF2 )、氟化鋁(AlF3 )及氧化鋁(Al2 O3 )的至少1種所構成。
緩衝層20含有與上述微量元素同種的元素。而且，緩衝層20中所含有之與微量元素同種的元素之藉由能量分散型X射線分析(EDS分析)的含有率為2質量%以上99質量%以下。 即，緩衝層20係藉由與基材10所含有之微量元素同種的元素而構成之層，或含有與基材10所含有之微量元素同種的元素且其濃度高之層。尚且，緩衝層20可含有與微量元素同種的元素作為金屬、金屬間化合物、合金、氧化物及氟化物之至少1種。
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，由於具有緩衝層20，即使遭受熱歷程，耐蝕性被膜30也不易從基材10剝離。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。再者，即使基材10所含有的微量元素擴散至基材10之表面，也由於該微量元素被緩衝層20所捕捉，故可抑制含有微量元素的粒子從耐蝕性構件產生。
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，例如可藉由濺鍍等之方法，在基材10之表面上形成由與微量元素同種的元素所成之層或含有與微量元素同種的元素之層(緩衝層20)，更在緩衝層20之上，藉由電泳堆積法、蒸鍍法等之方法，形成耐蝕性被膜30而製造。
構成基材10的金屬，可為單質的金屬(含有不可避免的雜質)，也可為合金。基材10所含有的元素之中質量含有率最高的元素之主元素較佳為鋁，微量元素較佳為選自鉻、鎳、鐵、銅、矽、鈦及錳的至少1種。於主元素及微量元素以外，作為基材10所含有的元素之例，可舉出鎂。
再者，緩衝層20之厚度較佳為5nm以上100nm以下。還有，耐蝕性被膜30之厚度較佳為100nm以上50000nm以下。若緩衝層20之厚度為5nm以上100nm以下，則即使遭受熱歷程，耐蝕性被膜30也不易從基材10剝離的效果變更高。若耐蝕性被膜30之厚度為100nm以上50000nm以下，則耐蝕性更優異。緩衝層20及耐蝕性被膜30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)、掃描穿透型電子顯微鏡(STEM)、掃描型電子顯微鏡(SEM)等。
耐蝕性被膜之氟化鎂只要是由氟化鎂(MgF2 )、氟化鎂水合物(MgF2 ・nH2 O)、一部分含有羥基的氟化鎂(MgF2-X (OH)X )、一部分含有羥基的氟化鎂水合物(MgF2-X (OH)X ・nH2 O)、一部分含有氧的氟化鎂(MgF2(1-X) OX )及一部分含有氧的氟化鎂水合物(MgF2(1-X) OX ・nH2 O)所選出的至少一個即可。
同樣地，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。
同樣地，氧化鋁只要是由氧化鋁(Al2 O3 )、氧化鋁水合物(Al2 O3 ・nH2 O)、一部分含有羥基的氧化鋁(Al2 O3-X (OH)2X )、一部分含有羥基的氧化鋁水合物 (Al2 O3-X (OH)2X ・nH2 O)、一部分含有氟的氧化鋁 (Al2 O3-X F2X )及一部分含有氟的氧化鋁水合物(Al2 O3-X F2X ・nH2 O)所選出的至少一個即可。
尚且，耐蝕性構件係如圖2所示的變形例，耐蝕性被膜30可以複數的層(圖2之例中2個層31、32)所構成。此等複數的層係以不同種類的化合物所構成。例如，如圖2之例，於耐蝕性被膜30以2個層31、32所構成時，層31可以氟化鎂所構成，層32可以氟化鋁所構成。 [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] 對於基材進行濺鍍而在基材之表面上形成緩衝層後，藉由電泳堆積法在緩衝層之上形成耐蝕性被膜。然後，對於耐蝕性被膜施予後處理而得到耐蝕性構件。
構成基材的金屬係含有2.55質量%的鎂之鋁合金A5052。此鋁合金A5052含有鉻0.23質量%、鎳0.04質量%、鐵0.26質量%及銅0.07質量%作為微量元素。
首先，進行上述基材之前處置。於水1L中溶解有S-Clean AL-13(佐佐木化學藥品股份有限公司製)70g之50℃的脫脂液中，浸漬上述基材10分鐘，以純水洗淨。其次，於經加熱至70℃的S-Clean AL-5000(佐佐木化學藥品股份有限公司製)500g之蝕刻液中，浸漬如上述經洗淨的基材1分鐘，以純水洗淨。然後，於水400g中溶解有Smutclean(RAIKI股份有限公司製)200g之25℃的污垢去除液中，浸漬上述基材30秒，以純水洗淨，使其真空乾燥，完成基材的前處理。
接著，於已進行前處理的上述基材上，以形成緩衝層為目的，進行濺鍍。構成緩衝層的金屬係與微量元素同種的元素，為鉻、鎳、鐵及銅。作為靶，準備含有鉻、鎳、鐵及銅之合金，在直流磁控濺鍍裝置的陰極上配置靶。於靶之對向位置，配置已進行前處理之基材，將靶與已進行前處理的基材之間的距離設為50mm。真空抽吸到1×10-3 Pa以下的壓力後，導入氬氣而使壓力成為10Pa，將直流電力投入至靶，處理30秒。尚且，直流放電電力係設為50W。
接著，藉由電泳堆積法，形成耐蝕性被膜。構成耐蝕性被膜的化合物為氟化鎂。電泳堆積法之條件係如以下。首先，使純度為99.99%以上的MgF2 粉末(富士軟片和光純藥股份有限公司製)5g分散於加有0.15g的Esleam(註冊商標)C-2093I(日油股份有限公司製)作為分散材料之495g的乙醇中，進行珠磨處理，製作一次粒徑為30nm的MgF2 懸浮液。於此懸浮液中，使由已進行上述濺鍍的基材所成之尺寸20mm×25mm×2mm的負極與由碳所成的正極以電極間距離30mm浸漬，施加50V的恆定電壓120秒，在負極表面上形成厚度約2μm的由MgF2 所成之粒子膜。 耐蝕性被膜之後處理的方法係在含有氟氣(F2 )的環境下之熱處理。後處理之條件係環境中的氟氣濃度為1體積%，氮氣濃度為99體積%，熱處理溫度為350℃，熱處理時間為900min。
對於所得之耐蝕性構件，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下從室溫到300℃為止以3小時升溫，在300℃下保持5小時後，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30%之情況係以C表示，30%以上之情況係以D表示。
又，於加熱試驗之前後各自中，以感應耦合電漿質量分析法(ICP-MS)測定耐蝕性被膜之表面上存在的元素(與微量元素同種的元素)之量。首先，將加熱試驗前的耐蝕性構件浸漬於濃度0.3質量%的硝酸100mL中5分鐘，萃取耐蝕性被膜之表面上存在的元素，得到溶液。對於所得之溶液，進行ICP-MS分析，而測定加熱試驗前的元素量。對於加熱試驗後的耐蝕性構件，亦進行同樣的操作，測定加熱試驗後的元素量。
然後，藉由下述式，算出加熱試驗之前後的各元素之增加率(%)。 (加熱試驗之前後的元素之增加率)=100×{(加熱試驗後的元素之量)-(加熱試驗前的元素之量)}/(加熱試驗前的元素之量) 表1中顯示結果。表1中，藉由上述式所算出的「加熱試驗之前後的元素之增加率」未達200%之情況係以A表示，200%以上且未達500%之情況係以B表示，500%以上且未達1000%之情況係以C表示，1000%以上之情況係以D表示。
Figure 02_image001
[實施例2] 除了構成基材的金屬為含有鎂0.84質量%及矽0.78質量%之鋁合金A6061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。尚且，鋁合金A6061含有鉻0.16質量%、鎳0.04質量%、鐵0.52質量%及銅0.25質量%作為微量元素。
[實施例3] 除了將後處理之條件中的氮氣之濃度設為100體積%，將熱處理溫度設為450℃之點，及構成耐蝕性被膜的化合物為氧化鋁之點以外，與實施例1同樣地製造耐蝕性構件，進行評價。尚且，耐蝕性被膜之形成方法係與實施例1同樣，使用電泳堆積法，使用5g的氫氧化氧化鋁(富士軟片和光化學股份有限公司製)來形成粒子膜。尚且，珠磨處理後的一次粒徑為21nm。此處，前述氫氧化氧化鋁係藉由在450℃下熱處理，而成為經燒結的氧化鋁膜。表1中顯示結果。
[實施例4] 除了構成耐蝕性被膜的化合物為氟化鋁之點以外，與實施例1同樣地製造耐蝕性構件，進行評價。尚且，耐蝕性被膜之形成方法係與實施例1同樣，使用電泳堆積法，使用5g的氟化鋁粉末(富士軟片和光化學股份有限公司製)來形成粒子膜。尚且，珠磨處理後的一次粒徑為27nm。表1中顯示結果。
[實施例5] 除了構成耐蝕性被膜的化合物為氟化鎂及氟化鋁之點以外，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。尚且，於實施例5中，耐蝕性被膜係與圖2所示的變形例同樣，以由氟化鎂所成之層與由氟化鋁所成之層的2層所構成。尚且，耐蝕性被膜之形成方法係與實施例1同樣，使用電泳堆積法，使用5g的氟化鎂粉末(與實施例1相同)與5g的氟化鋁粉末(與實施例4相同)來形成粒子膜。尚且，珠磨處理後的一次粒徑分別為33nm、24nm。
[實施例6] 除了形成耐蝕性被膜之方法為真空蒸鍍法之點以外，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。尚且，實施例6中的耐蝕性被膜之形成方法係如以下。首先，將已進行濺鍍的基材設置於真空室內後，將真空室內排氣直到壓力成為2×10-4 Pa為止。然後，將已進行濺鍍的基材加熱到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，在已進行濺鍍的基材上形成厚度2.0μm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，真空蒸鍍時的真空度為5×10-4 Pa。
[比較例1] 除了不形成緩衝層，在基材之表面上直接形成耐蝕性被膜之點以外，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] 除了不形成緩衝層，在基材之表面上直接形成耐蝕性被膜之點以外，與實施例2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1～6係即使遭受熱歷程也耐蝕性被膜之剝離幾乎不發生。又，即使遭受熱歷程，基材所含有的微量元素也幾乎沒有擴散到耐蝕性被膜之表面。
10:基材 20:緩衝層 30:耐蝕性被膜
[圖1]係說明本發明之一實施形態的耐蝕性構件之構成的剖面圖。 [圖2]係說明圖1之耐蝕性構件的變形例之構成的剖面圖。
10:基材
20:緩衝層
30:耐蝕性被膜

Claims (4)

  1. 一種耐蝕性構件，其具備金屬製的基材、形成在前述基材之表面上的耐蝕性被膜與形成在前述基材及前述耐蝕性被膜之間的緩衝層，前述基材含有在前述基材所含有的元素之中質量含有率最高的元素之主元素與質量含有率為1質量%以下的元素之微量元素，前述耐蝕性被膜係以選自氟化鎂、氟化鋁及氧化鋁的至少1種所構成，前述緩衝層含有與前述微量元素同種的元素，前述緩衝層中所含有之與前述微量元素同種的元素之藉由能量分散型X射線分析的含有率為2質量%以上99質量%以下，其中前述微量元素係選自鉻、鎳、鐵及銅的至少1種。
  2. 如請求項1之耐蝕性構件，其中前述主元素為鋁。
  3. 如請求項1或2之耐蝕性構件，其中前述緩衝層之厚度為5nm以上100nm以下。
  4. 如請求項1或2之耐蝕性構件，其中前述耐蝕性被膜之厚度為100nm以上50000nm以下。
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