TW201938783A - 用以去除乾蝕刻殘渣之洗淨液及使用此洗淨液之半導體基板之製造方法 - Google Patents

用以去除乾蝕刻殘渣之洗淨液及使用此洗淨液之半導體基板之製造方法 Download PDF

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TW201938783A
TW201938783A TW108108147A TW108108147A TW201938783A TW 201938783 A TW201938783 A TW 201938783A TW 108108147 A TW108108147 A TW 108108147A TW 108108147 A TW108108147 A TW 108108147A TW 201938783 A TW201938783 A TW 201938783A
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cleaning solution
water
dry etching
semiconductor substrate
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菊永孝裕
堀江宏彰
青山公洋
田島恒夫
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日商三菱瓦斯化學股份有限公司
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Abstract

根據本發明，可提供一種洗淨液，含有胺化合物(A)0.2~20質量%、水溶性有機溶劑(B)40~70質量%及水，該胺化合物(A)含有選自於由正丁胺、己胺、辛胺、1,4-丁二胺、二丁胺、3-胺基-1-丙醇、N,N-二乙基-1,3-二胺基丙烷、及雙(六亞甲基)三胺構成之群組中之1種以上，且該水溶性有機溶劑(B)於20℃之黏度為10mPa･s以下，且該洗淨液之pH為9.0~14之範圍。

Description

用以去除乾蝕刻殘渣之洗淨液及使用此洗淨液之半導體基板之製造方法
本發明係關於在半導體基板之製造步驟中，抑制含有鈷之金屬配線層及層間絕緣膜的損傷，且除去被處理表面之乾蝕刻殘渣及乾蝕刻阻擋層的清洗液及使用此清洗液之半導體基板之製造方法。
在半導體基板之製造步驟中包含乾蝕刻步驟，係相對於其他材料，選擇性地除去特定之材料的步驟。此時，被稱為乾蝕刻殘渣的蝕刻殘留物或金屬殘渣等會殘留於蝕刻處理後的表面，為了除去此等物質會使用洗淨液。
在近年之半導體基板中，使用銅作為配線材料，使用低介電係數膜（以下稱為「Low-k膜」）作為層間絕緣膜。然而，伴隨著配線之微細化的進展，容易產生電遷移(electromigration)，銅配線之可靠性降低而被視為問題。因此，作為改善電遷移耐性的替代材料，有人提倡鈷。另一方面，將含有該配線材料之基板進行乾蝕刻時，在處理後之基板表面會殘留有機系或矽系的乾蝕刻殘渣。此外，在半導體基板，為了防止乾蝕刻所致之對於配線材料的損傷，有時會包含氧化鋁等的乾蝕刻阻擋層。
因此，有在防止腐蝕基板之配線材料及層間絕緣膜的同時，將乾蝕刻殘渣及乾蝕刻阻擋層予以除去的洗淨技術的需求。另外，有必要抑制氧化鋁等乾蝕刻阻擋層的側蝕，該側蝕現象對於洗淨後之製膜步驟較不理想。
為了使乾蝕刻殘渣變脆弱，有時會於洗淨液中使用氧化還原劑。然而，氧化還原劑會有誘發洗淨液中之成分分解所致之性能變差、基板表面之材質變化等的問題。
此外，為了防止配線材料之損傷，有時會使用抗蝕劑，但有必要除去吸附於配線材料表面的抗蝕劑以避免在清洗後之製膜步驟中發生不良情況。含氮雜環化合物係具代表性的鈷的抗蝕劑，但以一般的洗淨液並不容易將其從配線材料表面除去。
就適合含有鈷配線材料之基板的洗淨液而言，已知有使用由羥基胺化合物、特定結構之含氮化合物、有機溶劑及水構成之藥液進行洗淨之方法(專利文獻1)。然而，其為了使殘渣溶解而使用了為還原劑的羥基胺化合物。此外，若不添加為抗蝕劑的含氮雜環化合物，則無法充分抑制對於鈷的損傷。
就適合含有鈷配線材料之基板的洗淨液，已知有使用由鹼金屬化合物、過氧化物、鹼土金屬及水構成之藥液進行洗淨之技術(專利文獻2)。然而，為了使乾蝕刻殘渣溶解而使用了過氧化物作為氧化劑，且若不添加抗蝕劑則無法抑制對於鈷的損傷。
[先前技術文獻]
[專利文獻]
[專利文獻1] 國際公開第2017-119350號
[專利文獻2] 國際公開第2016-076033號
[發明所欲解決之課題]
本發明之課題係難以使用以往的方法來應對，本案發明者係提供可防止含有鈷之金屬配線層及層間絕緣膜的腐蝕，且可除去乾蝕刻殘渣及乾蝕刻阻擋層的洗淨液，及使用此清洗液之含有鈷的半導體基板的製造方法。
[解決課題之手段]
本案發明者們深入研究之結果，發現藉由使用含有特定之胺化合物(A)、水溶性有機溶劑(B)及水的洗淨液可解決上述課題。
亦即，本發明如同下述。
＜1＞ 一種洗淨液，含有胺化合物(A)0.2~20質量%、水溶性有機溶劑(B)40~70質量%、及水；
該胺化合物(A)含有選自於由正丁胺、己胺、辛胺、1,4-丁二胺、二丁胺、3-胺基-1-丙醇、N,N-二乙基-1,3-二胺基丙烷、及雙(六亞甲基)三胺構成之群組中之1種以上，且該水溶性有機溶劑(B)於20℃之黏度為10mPa･s以下，且該洗淨液之pH為9.0~14之範圍。
＜2＞ 如＜1＞之洗淨液，其中，該胺化合物(A)之含量為0.2~4.0質量%。
＜3＞ 如＜1＞或＜2＞之洗淨液，其中，該水之含量為28~59質量%。
＜4＞ 如＜1＞至＜3＞中任一項之洗淨液，其中，該水溶性有機溶劑(B)含有選自於由二乙二醇單甲醚、二乙二醇單丁醚、三乙二醇單甲醚、二丙二醇單甲醚、及N,N-二甲基異丁醯胺構成之群組中之1種以上。
＜5＞ 如＜1＞至＜4＞中任一項之洗淨液，其中，該胺化合物(A)含有選自於由3-胺基-1-丙醇、N,N-二乙基-1,3-二胺基丙烷、及雙(六亞甲基)三胺構成之群組中之1種以上。
＜6＞ 如＜1＞至＜5＞中任一項之洗淨液，係用以除去乾蝕刻殘渣。
＜7＞ 一種半導體基板之製造方法，包含下述步驟：使用如＜1＞至＜6＞中任一項之洗淨液，將含有鈷之半導體基板予以洗淨。
＜8＞ 如＜7＞之半導體基板之製造方法，其中，該半導體基板包含：含有鈷之金屬配線層、層間絕緣膜、及含有氧化鋁之乾蝕刻阻擋層。
[發明之效果]
藉由本發明，可提供在半導體基板之製造步驟中，可抑制含有鈷之金屬配線層及層間絕緣膜的損傷，且可選擇性地除去基板表面之乾蝕刻殘渣及乾蝕刻阻擋層的洗淨液，及使用此洗淨液的半導體基板的製造方法。
本發明之洗淨液係含有特定之胺化合物(A)、水溶性有機溶劑(B)、及水。以下詳細地進行說明。
[胺化合物(A)]
本發明中使用之胺化合物(A)考慮鈷之抗蝕性之觀點，係含有選自特定之胺化合物中的一種以上。
具體而言，可列舉正丁胺、己胺、辛胺、1,4-丁二胺、二丁胺、3-胺基-1-丙醇、N,N-二乙基-1,3-二胺基丙烷、及雙(六亞甲基)三胺。此等之中，宜為即使於高溫條件下仍揮發少的3-胺基-1-丙醇、N,N-二乙基-1,3-二胺基丙烷、及雙(六亞甲基)三胺。此等係容易取得市售商品且可適當地使用市售商品。
洗淨液中之胺化合物(A)的含量係0.2~20質量%之範圍，宜為0.2~8.0質量%之範圍，更宜為0.2~4.0質量%之範圍，尤其宜為0.5~4.0質量%之範圍，藉由為此等之範圍，可兼顧乾蝕刻殘渣的除去性及含有氧化鋁之乾蝕刻阻擋層之除去性。
使用量過多時，有時有含有氧化鋁之乾蝕刻阻擋層的除去性變高，含有氧化鋁之乾蝕刻阻擋層的側蝕增大的情況。另一方面，使用量過少時，有時有乾蝕刻殘渣及含有氧化鋁之乾蝕刻阻擋層的除去性無法令人滿意的情況。
[水溶性有機溶劑(B)]
本發明中使用之水溶性有機溶劑(B)係在20℃之黏度為10mPa・s以下之可溶於水的溶劑。
具體而言，可列舉二乙二醇單甲醚(以下簡稱為DGME)、二乙二醇單丁醚(以下簡稱為DGMB)、三乙二醇單甲醚(以下簡稱為TGME)、二丙二醇單甲醚(以下簡稱為DPGME)、及N,N-二甲基異丁醯胺(以下簡稱為DMIB)較為理想。此等係容易取得市售商品且可適當地使用市售商品，亦可組合2種以上來使用。
洗淨液中之水溶性有機溶劑(B)之含量係40~70質量%之範圍，宜為45~65質量%之範圍。使用量過少時，有時有含有氧化鋁之乾蝕刻阻擋層之除去性變高，含有氧化鋁之乾蝕刻阻擋層之側蝕增加的情況。此外，有時也有鈷之抗蝕性無法令人滿意之情況。另一方面，使用量過多時，有時有含有氧化鋁之乾蝕刻阻擋層之除去性降低，洗淨時間變長的情況。
[水]
就本發明中使用之水而言，可為自來水、工業用水、地下水、蒸餾水、離子交換水、超純水等而沒有特別之限定，宜為離子交換水，更宜為超純水。
洗淨液中之水的含量宜為28~59質量%之範圍，更宜為34~54質量%之範圍。
[洗淨液]
本發明之洗淨液可將上述胺化合物(A)、水溶性有機溶劑(B)、及水藉由通常方法攪拌均勻來製備。
洗淨液之pH係9.0~14，宜為11~13。若pH過低，則含有氧化鋁之乾蝕刻阻擋層的除去性或鈷之抗蝕降低，若pH過高則有時有含有氧化鋁之乾蝕刻阻擋層之除去性變高，含有氧化鋁之乾蝕刻阻擋層之側蝕增加的情況。
pH調整可只藉由胺化合物(A)之含量來進行調整，亦可在不損害本發明之目的的範圍內添加酸。
[半導體基板]
使用本發明之洗淨液的半導體基板宜具有含有鈷之金屬配線層、層間絕緣膜、及乾蝕刻阻擋層，於基板表面會存在蝕刻後的殘渣。尤其，在半導體基板具有為乾蝕刻殘渣之掩模圖案殘渣(有機物系化合物殘渣)時具有效果。此外，上述層間絕緣膜可包含低介電係數膜(Low-k膜)。此外，上述乾蝕刻阻擋層宜含有氧化鋁。
[半導體基板之製造方法]
本發明之半導體基板之製造方法係包含下述步驟：使用上述本發明之洗淨液，洗淨含有鈷之半導體基板。
例如，可對於乾蝕刻處理後的半導體基板，以浸漬處理或單片處理的方法來使用本發明之洗淨液。處理溫度通常為10~70℃，宜為40~60℃。處理時間通常為0.5~10分鐘，宜為1~5分鐘。就使用了本發明之洗淨液後的潤洗液而言，只使用水進行潤洗即可，但亦可使用如醇般的有機溶劑或氨水。
[實施例]
以下，藉由實施例來具體地說明本發明，但本發明不限於以下的實施例。
＜評價基板＞
乾蝕刻殘渣除去性評價用(評價I)：由有機物(碳、氫、氧、氮)構成之下層抗反射膜(膜厚：400埃)、
乾蝕刻阻擋層除去性評價用(評價II)：氧化鋁膜(膜厚：3000埃)、
金屬配線抗蝕性評價用(評價III)：使用鈷膜(膜厚：2000埃)。
層間絕緣膜抗蝕性評價用(評價IV)：由矽、碳、氫、氧構成之Low-k膜(膜厚：3000埃)
＜評價基板之製作方法＞
下層抗反射膜及Low-k膜係各別旋塗於矽晶圓成膜而得。
氧化鋁膜係於矽晶圓上藉由物理氣相沉積法成膜而得。
鈷膜係於矽晶圓上按5000埃之氧化矽、250埃之鈦的順序堆疊，且在其上以化學氣相沉積法成膜而得。
＜評價方法＞
[處理條件]
將1×1cm、或2×2cm尺寸之上述評價基板的試驗片浸漬於60℃之洗淨液10g，並將處理後的試驗片以水潤洗。
[膜厚測定]
下層抗反射膜、氧化鋁膜、及Low-k膜之膜厚係藉由光學式膜厚計n&k1280(n&k Technology, Inc.製)進行測定。鈷之膜厚減少量係使用ICP-AES iCAP6300(Thermo Scientific製)，從處理後之洗淨液中的金屬濃度算出。
(膜厚減少量[埃]=洗淨液中之金屬溶解量[g]×108 ÷密度[g/cm3 ]÷試驗片的表面積[cm2 ])
蝕刻速率[埃/min]係將膜厚減少量除以處理時間(氧化鋁膜為1分鐘，鈷膜為4分鐘，Low-k膜為5分鐘)來算出。
判定：
(評價I)：乾蝕刻殘渣之除去性
藉由下層抗反射膜的除去時間(下層抗反射膜剝離並可目視到基底材之時間點的時間)進行判定。
G：未達15分鐘
A：15分鐘~未達30分鐘
P：30分鐘~60分鐘
(評價II)：氧化鋁膜之除去性
藉由氧化鋁膜之蝕刻速率進行判定。
G：15~未達50埃/min
A1：10~未達15埃/min
A2：50~60埃/min
P1：未達10埃/min。
P2：超過60埃/min。
判定為G、A1及A2者則認定為合格。
(評價III)：鈷之抗蝕性
以鈷膜之蝕刻速率進行判定。
G：未達1埃/min。
P：1埃/min以上。
判定為G則認定為合格。
(評價IV)：Low-k膜之抗蝕性
以Low-k膜之蝕刻速率進行判定。
G：未達1埃/min。
P：1埃/min以上。
判定為G則認定為合格。
[pH]
洗淨液之pH以HORIBA製pH METER F-52進行測定。測定溫度設為25℃。
[黏度]
洗淨液之黏度以柴田科學製烏氏黏度計(Ubbelohde viscometer)進行測定。測定溫度設為20℃。
[實施例1~22及比較例1~9]
使用表1或表2所示之組成的洗淨液，處理上述評價基板並進行評價。表1或表2中之濃度的單位係表示質量%。評價IV係針對實施例1~22進行評價，全部皆為G判定。
【表1】 DGME：二乙二醇單甲醚(在20℃之黏度為4mPa･s)
DGMB：二乙二醇單丁醚(在20℃之黏度為7mPa･s)
TGME：三乙二醇單甲醚(在20℃之黏度為8mPa･s)
DPGME：二丙二醇單甲醚(在20℃之黏度為4mPa･s)
DMIB：N,N-二甲基異丁醯胺(在20℃之黏度為1mPa･s)
【表2】 甘油：(在20℃之黏度為1500mPa･s)
1‧‧‧乾蝕刻殘渣
2‧‧‧乾蝕刻阻擋層
3‧‧‧金屬配線層(鈷)
4‧‧‧層間絕緣膜
[圖1] 係展示除去乾蝕刻殘渣前之含有鈷的半導體基板的一例的概略剖面圖。

Claims (8)

  1. 一種洗淨液，含有胺化合物(A)0.2~20質量%、水溶性有機溶劑(B)40~70質量%、及水； 該胺化合物(A)含有選自於由正丁胺、己胺、辛胺、1,4-丁二胺、二丁胺、3-胺基-1-丙醇、N,N-二乙基-1,3-二胺基丙烷、及雙(六亞甲基)三胺構成之群組中之1種以上，且該水溶性有機溶劑(B)於20℃之黏度為10mPa･s以下，且該洗淨液之pH為9.0~14之範圍。
  2. 如申請專利範圍第1項之洗淨液，其中，該胺化合物(A)之含量為0.2~4.0質量%。
  3. 如申請專利範圍第1或2項之洗淨液，其中，該水之含量為28~59質量%。
  4. 如申請專利範圍第1至3項中任一項之洗淨液，其中，該水溶性有機溶劑(B)含有選自於由二乙二醇單甲醚、二乙二醇單丁醚、三乙二醇單甲醚、二丙二醇單甲醚、及N,N-二甲基異丁醯胺構成之群組中之1種以上。
  5. 如申請專利範圍第1至4項中任一項之洗淨液，其中，該胺化合物(A)含有選自於由3-胺基-1-丙醇、N,N-二乙基-1,3-二胺基丙烷、及雙(六亞甲基)三胺構成之群組中之1種以上。
  6. 如申請專利範圍第1至5項中任一項之洗淨液，係用以除去乾蝕刻殘渣。
  7. 一種半導體基板之製造方法，包含下述步驟：使用如申請專利範圍第1至6項中任一項之洗淨液，將含有鈷之半導體基板予以洗淨。
  8. 如申請專利範圍第7項之半導體基板之製造方法，其中，該半導體基板包含：含有鈷之金屬配線層、層間絕緣膜、及含有氧化鋁之乾蝕刻阻擋層。
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