TWI804787B - 鈍化膜之製造方法 - Google Patents

鈍化膜之製造方法 Download PDF

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TWI804787B
TWI804787B TW109142762A TW109142762A TWI804787B TW I804787 B TWI804787 B TW I804787B TW 109142762 A TW109142762 A TW 109142762A TW 109142762 A TW109142762 A TW 109142762A TW I804787 B TWI804787 B TW I804787B
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passivation
substrate
gas
film
passivation film
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TW202136544A (zh
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谷本陽祐
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日商昭和電工股份有限公司
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Abstract

本發明提供可再現性良好地製造氧原子濃度低之鈍化膜的鈍化膜之製造方法。藉由具備下述步驟之方法製造鈍化膜：將表面具有鍺及鉬之至少一者的基板，以含有分子中具有氧原子之化合物的含氧化合物與硫化氫之鈍化氣體處理，於基板表面上形成含有硫原子之鈍化膜之鈍化步驟。鈍化氣體中之含氧化合物之濃度為0.001莫耳ppm以上且未達75莫耳ppm。

Description

鈍化膜之製造方法
本發明有關鈍化膜之製造方法。
近幾年來，於半導體領域中，含有矽(Si)以外之元素的半導體材料備受矚目。作為含有矽以外之元素的半導體材料，舉例為含有例如鍺(Ge)、銦鎵砷(InGaAs)等III-V族元素之半導體材料，或含有硫化鉬(IV)(MoS2 )等之金屬硫屬化物(chalcogenide)的半導體材料。 該等半導體材料與矽材料比較，雖具有移動度(mobility)較高之優點，但有成膜困難之情況，或因材料間之界面缺陷密度高而使移動度降低之情況。
因此，為了減低材料間之界面缺陷密度，提案有於鍺、鉬等之基板上使用硫化氫(H2 S)氣體形成鈍化膜之方法(例如參考專利文獻1)。又，作為金屬硫屬化物之成膜方法，提案有以硫化氫氣體處理鉬氧化物層、鎢氧化物層而形成硫化鉬層、硫化鎢層之方法(例如參考專利文獻2)。 [先前技術文獻] [專利文獻]
[專利文獻1] 日本專利公開公報2016年第207789號 [專利文獻2] 日本專利公開公報2017年第61743號
[發明欲解決之課題]
然而，根據硫化氫氣體之品質，而有鈍化膜所含之氧原子濃度變高而使鈍化膜性能降低之情況。 本發明之課題在於提供可再現性良好地製造氧原子濃度低之鈍化膜的鈍化膜之製造方法。 [用以解決課題之手段]
為了解決前述課題，本發明之一態樣係如以下之[1]~[5]。 [1] 一種鈍化膜之製造方法，其具備下述步驟：將表面具有鍺及鉬之至少一者的基板，以含有分子中具有氧原子之化合物的含氧化合物與硫化氫之鈍化氣體處理，於前述基板表面上形成含有硫原子之鈍化膜之鈍化步驟， 前述鈍化氣體中之前述含氧化合物之濃度為0.001莫耳ppm以上且未達75莫耳ppm。
[2] 如[1]之鈍化膜之製造方法，其中前述鈍化氣體中之前述含氧化合物之濃度為0.5莫耳ppm以上且65莫耳ppm以下。 [3] 如[1]或[2]之鈍化膜之製造方法，其中前述含氧化合物係氧氣及水之至少一者。 [4] 如[1]至[3]中任一項之鈍化膜之製造方法，其中前述基板於表面具有含有鍺及鉬之至少一者的膜。 [5] 如[1]至[4]中任一項之鈍化膜之製造方法，其中於溫度20℃以上1500℃以下、壓力1Pa以上101kPa以下之條件下，以前述鈍化氣體處理前述基板。 [發明效果]
依據本發明，可再現性良好地製造氧原子濃度低之鈍化膜。
以下針對本發明之一實施形態加以說明。尚且，本實施形態係顯示本發明之一例者，本發明不受本實施形態之限制。又，本實施形態中，可加入各種變更或改良，此等加入變更或改良之形態亦可包含於本發明。
本實施形態之鈍化膜之製造方法具備下述步驟：將表面具有鍺及鉬之至少一者的基板，以含有分子中具有氧原子之化合物的含氧化合物與硫化氫之鈍化氣體處理，於基板表面上形成含有硫原子之鈍化膜之鈍化步驟。而且鈍化氣體中之含氧化合物之濃度為0.001莫耳ppm以上且未達75莫耳ppm。
依據本實施形態之鈍化膜之製造方法，由於可抑制非預期之氧化膜生成且可生成安定之硫化膜，故可再現性良好地製造氧原子濃度低之鈍化膜。 為了充分抑制非預期之氧化膜生成且再現性良好地製造氧原子濃度低之鈍化膜，鈍化氣體中之含氧化合物之濃度必須為0.001莫耳ppm以上且未達75莫耳ppm，但上限較佳為65莫耳ppm以下，更佳為40莫耳ppm以下，又更佳為5莫耳ppm以下，下限可為0.5莫耳ppm以上。又，鈍化氣體中之含氧化合物之濃度越低越佳，但低於0.001莫耳ppm之濃度難以測定。
含氧化合物之種類並未特別限定，但舉例為例如氧氣(O2 )、水(H2 O)、一氧化碳(CO)、二氧化碳(CO2 )、羰基硫(COS)及二氧化硫(SO2 )。該等含氧化合物中，較佳為氧氣及水之至少一者。
以鈍化氣體處理之基板，係於表面具有鍺及鉬之至少一者的基板，但基板表面以何種形態具有鍺及鉬之至少一者並未特別限定。例如基板可於表面具有含有鍺及鉬之至少一者之膜。
又，於表面具有含有鍺及鉬之至少一者之膜的基板，若膜含有鍺及鉬之至少一者，則任何基板都無妨，但例如適宜為半導體元件之形成所使用之基板。尤其較佳為以物理蒸鍍(PVD)或化學蒸鍍(CVD)於表面成膜含有鍺及鉬之至少一者的膜之單晶矽基板。
鈍化氣體中之硫化氫濃度若為鈍化膜可充分成膜之量，則未特別限定，但較佳為1體積%以上，更佳為2體積%以上，又更佳為10體積%以上，特佳為100體積%。鈍化氣體所含有之成分中硫化氫及含氧化合物以外之成分並未特別限定，但可舉例為例如氮氣、氬氣等之惰性氣體。
鈍化步驟中以鈍化氣體處理基板時之壓力(例如以鈍化氣體進行處理之腔室內壓力)並未特別限定，但較佳為1Pa以上101kPa以下，更佳為10Pa以上90kPa以下，又更佳為100Pa以上80kPa以下。
又，鈍化步驟中以鈍化氣體處理基板時之溫度(例如配置於腔室內之基板溫度)並未特別限定，但為了獲得鈍化氣體對基板表面處理之高面內均一性，較佳為20℃以上1500℃以下，更佳為50℃以上1200℃以下，又更佳為100℃以上1000℃以下。
再者，鈍化步驟以鈍化氣體處理基板之時間長度並未特別限定，但若考慮半導體元件製造製程之效率，較佳為120分鐘以內。又，以鈍化氣體處理基板之時間係指自對收容基板之腔室供給鈍化氣體起，至為了使鈍化氣體對基板之表面處理結束而以真空泵等將腔室內之鈍化氣體排氣為止之時間。
本實施形態之鈍化膜之製造方法可較佳地適用於在基板表面成膜鈍化膜之半導體的成膜裝置。該成膜裝置之構造並未特別限定，收容於反應容器的腔室內之基板與連接於腔室之配管之位置關係亦未特別限定。 [實施例]
以下顯示實施例及比較例，更詳細說明本發明。 (實施例1) 使用圖1所示之成膜裝置1，於基板表面成膜鈍化膜。成膜裝置1具有進行鈍化步驟之腔室10及調整腔室10內部溫度之溫度調整裝置(未圖示)。於腔室10內部具備支撐試料20之載台11。作為試料20係使用於矽基板上形成厚150nm之氧化矽膜，進而於其上形成厚80nm之鍺膜者。
對腔室10，於其上游側分別經由閥32、33連接對腔室10供給含有含氧化合物及硫化氫之鈍化氣體之鈍化氣體供氣用配管12，與對腔室10供給惰性氣體之惰性氣體供氣用配管13。
又，對腔室10，於其下游側連接將腔室10內之氣體排出至外部之排氣用配管15，於排氣用配管15之下游側經由閥35連接真空泵38。腔室10內部之壓力係藉由控制閥35之壓力控制器37控制。
使用此成膜裝置1進行鈍化步驟。於載台11上設置試料20，將腔室10內之壓力減壓至未達10Pa後，將腔室10內之溫度升溫至800℃。隨後，將閥32設為打開狀態，自鈍化氣體供氣用配管12對腔室10內以101kPa之壓力供給鈍化氣體。該鈍化氣體為氧氣與硫化氫氣體之混合氣體，鈍化氣體中之氧氣濃度為60莫耳ppm。此時之鈍化氣體流量設為100sccm，於試料20表面成膜鈍化膜時之腔室10內之壓力設為67kPa。又，sccm表示0℃、101.3kPa下之流量(mL/min)。
鈍化氣體之導入進行30分鐘，於溫度800℃、壓力67kPa之條件下使試料20表面硫化而成膜鈍化膜後，停止鈍化氣體之導入。接著，以真空泵38將腔室10內部抽真空，自惰性氣體供氣用配管13於腔室10內供給惰性氣體的氮氣將腔室10內部以氮氣置換。隨後，使腔室10內之溫度降低至室溫，將成膜有鈍化膜之試料20自腔室10取出。
(實施例2) 除了鈍化氣體中氧氣濃度設為30莫耳ppm之方面以外，與實施例1同樣於基板表面成膜鈍化膜。 (實施例3) 除了鈍化氣體中氧氣濃度設為3.8莫耳ppm之方面以外，與實施例1同樣於基板表面成膜鈍化膜。 (實施例4) 除了鈍化氣體中氧氣濃度設為0.75莫耳ppm之方面以外，與實施例1同樣於基板表面成膜鈍化膜。
(比較例1) 除了鈍化氣體中氧氣濃度設為75莫耳ppm之方面以外，與實施例1同樣於基板表面成膜鈍化膜。 (比較例2) 除了鈍化氣體中氧氣濃度設為150莫耳ppm之方面以外，與實施例1同樣於基板表面成膜鈍化膜。
(實施例5) 除了使用於矽基板上形成有厚150nm之氧化矽膜，進而於其上形成厚80nm之鉬膜者作為試料20之方面以外，與實施例1同樣於基板表面成膜鈍化膜。 (實施例6) 除了鈍化氣體中氧氣濃度設為30莫耳ppm之方面以外，與實施例5同樣於基板表面成膜鈍化膜。
(實施例7) 除了鈍化氣體中氧氣濃度設為3.8莫耳ppm之方面以外，與實施例5同樣於基板表面成膜鈍化膜。 (實施例8) 除了鈍化氣體中氧氣濃度設為0.75莫耳ppm之方面以外，與實施例5同樣於基板表面成膜鈍化膜。
(比較例3) 除了鈍化氣體中氧氣濃度設為75莫耳ppm之方面以外，與實施例5同樣於基板表面成膜鈍化膜。 (比較例4) 除了鈍化氣體中氧氣濃度設為150莫耳ppm之方面以外，與實施例5同樣於基板表面成膜鈍化膜。
對於實施例1~8及比較例1~4之成膜有鈍化膜之試料20，進行飛行時間二次離子質量分析法(TOF-SIMS：Time-of-Flight Secondary Ion Mass Spectrometry)之分析，分析形成有鈍化膜之鍺膜或鉬膜之表面狀態。各鈍化膜中之氧化鍺(GeOx)、硫化鍺(GeSx)、氧化鉬(MoOx)、硫化鉬(MoSx)之量示於表1、2及圖2、3之圖表。
Figure 02_image001
Figure 02_image003
如由表1、2及圖2、3之圖表所了解，鈍化氣體中氧氣濃度為75莫耳ppm以上的比較例1、2、3、4係試料20之鈍化膜中氧化物之量相對於硫化物之量的比率較大。相對於此，鈍化氣體中氧氣濃度未達75莫耳ppm的實施例1~8，試料20之鈍化膜中氧化物之量相對於硫化物之量的比率，與比較例相比顯著較小，係顯示於實施例及比較例之間存在臨界條件之結果。如此，藉由使用氧氣濃度較低之鈍化氣體進行處理，顯示可抑制氧化膜生成並且可成膜硫化膜。
1:成膜裝置 10:腔室 11:載台 12:鈍化氣體供氣用配管 13:惰性氣體供氣用配管 15:排氣用配管 20:試料
[圖1]係說明本發明之鈍化膜之製造方法的一實施形態之成膜裝置之概略圖。 [圖2]係顯示形成鈍化膜之鍺膜表面狀態之分析結果的圖表。 [圖3]係顯示形成鈍化膜之鉬膜表面狀態之分析結果的圖表。
1:成膜裝置
10:腔室
11:載台
12:鈍化氣體供氣用配管
13:惰性氣體供氣用配管
15:排氣用配管
20:試料
32,33,35:閥
37:壓力控制器
38:真空泵

Claims (4)

  1. 一種鈍化膜之製造方法，其具備下述步驟：將表面具有鍺及鉬之至少一者的基板，以鈍化氣體處理，於前述基板表面上形成含有硫原子之鈍化膜之鈍化步驟，其中前述鈍化氣體係實質上由氧氣(O2)與硫化氫組成，或實質上由氧氣(O2)、硫化氫及惰性氣體組成，前述鈍化步驟中以鈍化氣體處理前述基板時之溫度為800℃以上1500℃以下，前述鈍化氣體中之前述氧氣(O2)之濃度為0.001莫耳ppm以上且未達75莫耳ppm。
  2. 如請求項1之鈍化膜之製造方法，其中前述鈍化氣體中之前述氧氣(O2)之濃度為0.5莫耳ppm以上且65莫耳ppm以下。
  3. 如請求項1或2之鈍化膜之製造方法，其中前述基板於表面具有含有鍺及鉬之至少一者的膜。
  4. 如請求項1或2之鈍化膜之製造方法，其中於壓力1Pa以上101kPa以下之條件下，以前述鈍化氣體處理前述基板。
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WO2016170988A1 (ja) * 2015-04-20 2016-10-27 東京エレクトロン株式会社 パッシベーション処理方法、半導体構造の形成方法及び半導体構造

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