CN111837218A - 用于去除干蚀刻残渣的清洗液及使用其的半导体基板的制造方法 - Google Patents

用于去除干蚀刻残渣的清洗液及使用其的半导体基板的制造方法 Download PDF

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CN111837218A
CN111837218A CN201980018203.4A CN201980018203A CN111837218A CN 111837218 A CN111837218 A CN 111837218A CN 201980018203 A CN201980018203 A CN 201980018203A CN 111837218 A CN111837218 A CN 111837218A
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dry etching
water
semiconductor substrate
cleaning solution
mass
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菊永孝裕
堀江宏彰
青山公洋
田岛恒夫
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Mitsubishi Gas Chemical Co Inc
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Abstract

根据本发明，可以提供如下清洗液，其含有：胺化合物(A)0.2～20质量％、水溶性有机溶剂(B)40～70质量％及水，前述胺化合物(A)含有选自由正丁胺、己胺、辛胺、1,4‑丁二胺、二丁胺、3‑氨基‑1‑丙醇、N,N‑二乙基‑1,3‑二氨基丙烷、及双(六亚甲基)三胺组成的组中的1者以上，并且前述水溶性有机溶剂(B)在20℃下的粘度为10mPa·s以下，所述清洗液的pH为9.0～14的范围。

Description

用于去除干蚀刻残渣的清洗液及使用其的半导体基板的制造 方法
技术领域
本发明涉及：在半导体基板的制造工序中，抑制含有钴的金属布线层及层间绝缘膜的损伤、去除被处理表面的干蚀刻残渣和干蚀刻阻挡层的清洗液及使用其的半导体基板的制造方法。
背景技术
半导体基板的制造工序中有干蚀刻工序，包括相对于其他材料选择性地去除特定的材料的工序。此时，被称为干蚀刻残渣的蚀刻的溶解残留物、金属渣等残存在蚀刻处理后的表面，为了将其去除而使用清洗液。
近年的半导体基板中，作为布线材料使用铜，作为层间绝缘膜使用低介电常数膜(以下称为“Low-k膜”)。但是，随着布线的微细化的进展，变得容易引起电迁移，铜布线的可靠性降低的问题受到关注。因此，作为提高电迁移耐性的代替材料，提倡钴。另一方面，在对包含该布线材料的基板进行干蚀刻时，有机系、硅系的干蚀刻残渣残留在处理后的基板表面。另外，为了防止干蚀刻导致的对布线材料的损伤，半导体基板有时包含氧化铝等干蚀刻阻挡层。
因此，要求防止基板的布线材料及层间绝缘膜腐蚀、并且将干蚀刻残渣和干蚀刻阻挡层去除的清洗技术。进而，需要抑制作为清洗后的制膜工序中不优选的现象的、氧化铝等干蚀刻阻挡层的侧蚀刻(side etching)。
为了使干蚀刻残渣脆弱化，有时清洗液中使用氧化还原剂。但是，氧化还原剂存在诱发清洗液中的成分分解导致的性能劣化、基板表面的材质变化等的问题。
另外，为了防止布线材料的损伤，有时也使用防腐蚀剂，需要将吸附于布线材料表面的防腐蚀剂去除以使清洗后的制膜工序不产生不良情况。含氮杂环式化合物为代表性的防钴腐蚀剂，用通常的清洗液不容易从布线材料表面去除。
对于包含钴布线材料的基板用的清洗液，已知有使用包含羟基胺化合物、特定结构的含氮化合物、有机溶剂和水的化学溶液进行清洗的方法(专利文献1)。但是，为了使残渣溶解，使用了作为还原剂的羟基胺化合物。另外，如果不添加作为防腐蚀剂的含氮杂环式化合物，则不能充分抑制对钴的损伤。
对于包含钴布线材料的基板用的清洗液，已知有使用包含碱金属化合物、过氧化物、碱土金属及水的化学溶液进行清洗的技术(专利文献2)。但是，为了使干蚀刻残渣溶解，使用过氧化物作为氧化剂，若不添加防腐蚀剂，则不能抑制对钴的损伤。
现有技术文献
专利文献
专利文献1：国际公开第2017-119350号
专利文献2：国际公开第2016-076033号
发明内容
发明要解决的问题
本发明的课题在于，提供：通过以往的方法难以应对的、防止含有钴的金属布线层及层间绝缘膜腐蚀、可进行干蚀刻残渣及干蚀刻阻挡层的去除的清洗液及使用其的包含钴的半导体基板的制造方法。
用于解决问题的方案
本发明人等进行了深入研究，结果发现，通过使用含有特定的胺化合物(A)、水溶性有机溶剂(B)及水的清洗液，能够解决上述课题。
即，本发明如下。
<1>一种清洗液，其含有：胺化合物(A)0.2～20质量％、水溶性有机溶剂(B)40～70质量％、及水，
前述胺化合物(A)含有选自由正丁胺、己胺、辛胺、1,4-丁二胺、二丁胺、3-氨基-1-丙醇、N,N-二乙基-1,3-二氨基丙烷、及双(六亚甲基)三胺组成的组中的1者以上，并且前述水溶性有机溶剂(B)在20℃下的粘度为10mPa·s以下，前述清洗液的pH为9.0～14的范围。
<2>为上述<1>所述的清洗液，其中，前述胺化合物(A)的含量为0.2～4.0质量％。
<3>为上述<1>或<2>所述的清洗液，其中，前述水的含量为28～59质量％。
<4>为上述<1>～<3>中任一项所述的清洗液，其中，前述水溶性有机溶剂(B)含有选自由二乙二醇单甲醚、二乙二醇单丁醚、三乙二醇单甲醚、二丙二醇单甲醚、及N,N-二甲基异丁酰胺组成的组中的1者以上。
<5>为上述<1>～<4>中任一项所述的清洗液，其中，前述胺化合物(A)含有选自由3-氨基-1-丙醇、N,N-二乙基-1,3-二氨基丙烷、及双(六亚甲基)三胺组成的组中的1者以上。
<6>为上述<1>～<5>中任一项所述的清洗液，其用于去除干蚀刻残渣。
<7>为一种半导体基板的制造方法，其包括使用上述<1>～<6>中任一项所述的清洗液对包含钴的半导体基板进行清洗的工序。
<8>为上述<7>所述的半导体基板的制造方法，其中，前述半导体基板包含：含有钴的金属布线层、层间绝缘膜、和含有氧化铝的干蚀刻阻挡层。
发明的效果
根据本发明，可以提供：半导体基板的制造工序中，可抑制含有钴的金属布线层及层间绝缘膜的损伤、可将基板表面的干蚀刻残渣和干蚀刻阻挡层选择性地去除的清洗液及使用其的半导体基板的制造方法。
附图说明
图1为示出干蚀刻残渣去除前的含有钴的半导体基板的一例的截面示意图。
具体实施方式
本发明的清洗液含有特定的胺化合物(A)、水溶性有机溶剂(B)、及水。以下，详细地进行说明。
[胺化合物(A)]
从防钴腐蚀性的观点出发，本发明中使用的胺化合物(A)含有选自特定的胺化合物中的1者以上。
具体而言，可列举出正丁胺、己胺、辛胺、1,4-丁二胺、二丁胺、3-氨基-1-丙醇、N,N-二乙基-1,3-二氨基丙烷及双(六亚甲基)三胺。这些之中，优选即使在高温条件下挥发也少的3-氨基-1-丙醇、N,N-二乙基-1,3-二氨基丙烷、及双(六亚甲基)三胺。这些可以容易地获得市售品，而且可以适当地使用。
清洗液中的胺化合物(A)的含量为0.2～20质量％的范围，优选0.2～8.0质量％的范围，更优选0.2～4.0质量％的范围，特别优选0.5～4.0质量％的范围，通过处于所述范围，能够兼顾干蚀刻残渣的去除性和包含氧化铝的干蚀刻阻挡层的去除性。
用量过多的情况下，有时包含氧化铝的干蚀刻阻挡层的去除性变高，包含氧化铝的干蚀刻阻挡层的侧蚀刻增大。另一方面，用量过少的情况下，有时干蚀刻残渣和包含氧化铝的干蚀刻阻挡层的去除性变得不充分。
[水溶性有机溶剂(B)]
本发明中使用的水溶性有机溶剂(B)为在20℃下的粘度为10mPa·s以下的在水中可溶的溶剂。
具体而言，优选可列举出二乙二醇单甲醚(以下记为DGME)、二乙二醇单丁醚(以下记为DGMB)、三乙二醇单甲醚(以下记为TGME)、二丙二醇单甲醚(以下记为DPGMG)、及N,N-二甲基异丁酰胺(以下记为DMIB)。这些可以容易地获得市售品，而且可以适当地使用，也可以将2种以上组合使用。
清洗液中的水溶性有机溶剂(B)的含量为40～70质量％的范围，优选45～65质量％的范围。用量过少的情况下，有时包含氧化铝的干蚀刻阻挡层的去除性变高、包含氧化铝的干蚀刻阻挡层的侧蚀刻增大。另外，有时钴的防腐蚀性也变得不充分。另一方面，用量过多的情况下，有时包含氧化铝的干蚀刻阻挡层的去除性降低、清洗时间变长。
[水]
作为本发明中使用的水，没有特别限定，有自来水、工业用水、地下水、蒸馏水、离子交换水、超纯水等，优选为离子交换水、更优选为超纯水。
清洗液中的水的含量优选28～59质量％的范围，更优选34～54质量％的范围。
[清洗液]
本发明的清洗液可以通过通常的方法将前述胺化合物(A)、水溶性有机溶剂(B)、及水均匀地搅拌来制备。
清洗液的pH为9.0～14，优选11～13。若pH变得过低，则有时包含氧化铝的干蚀刻阻挡层的去除性、钴的防腐蚀性降低，若pH变得过高，则有时包含氧化铝的干蚀刻阻挡层的去除性变高，包含氧化铝的干蚀刻阻挡层的侧蚀刻增大。
对于pH调节，可以仅通过胺化合物(A)的含量来进行调节，也可以在不损害本发明目的的范围内添加酸。
[半导体基板]
使用本发明的清洗液的半导体基板优选具有：含有钴的金属布线层、层间绝缘膜、及干蚀刻阻挡层，干蚀刻后的残渣存在于基板表面。特别是在半导体基板具有掩模图案残渣(有机物系化合物残渣)作为干蚀刻残渣的情况下是有效的。另外，上述层间绝缘膜可以包含低介电常数膜(Low-k膜)。另外，上述干蚀刻阻挡层优选包含氧化铝。
[半导体基板的制造方法]
本发明的半导体基板的制造方法包括使用上述本发明的清洗液对包含钴的半导体基板进行清洗的工序。
例如，可以通过浸渍处理或单片处理的方法对干蚀刻处理后的半导体基板使用本发明的清洗液。处理温度通常为10～70℃，优选40～60℃。处理时间通常为0.5～10分钟，优选1～5分钟。作为使用本发明的清洗液后的冲洗液，仅用水进行冲洗就足够，但也可以使用醇那样的有机溶剂、氨水。
实施例
以下，通过实施例具体地对本发明进行说明，但本发明不受以下实施例的任何限定。
<评价基板>
干蚀刻残渣去除性评价用(评价I)：由有机物(碳、氢、氧、氮)形成的下层防反射膜(膜厚：
Figure BDA0002673314470000061
)、
干蚀刻阻挡层去除性评价用(评价II)：氧化铝膜(膜厚：
Figure BDA0002673314470000062
)、金属布线防腐蚀性评价用(评价III)：使用钴膜(膜厚：
Figure BDA0002673314470000063
)。
层间绝缘膜防腐蚀性评价用(评价IV)：由硅、碳、氢、氧形成的Low-k膜(膜厚：
Figure BDA0002673314470000064
)
<评价基板的制作方法>
对于下层防反射膜及Low-k膜，各自在硅晶圆上进行旋转涂布而成膜。
对于氧化铝膜，在硅晶圆上通过物理气相沉淀法进行成膜。
对于钴膜，在硅晶圆上按照
Figure BDA0002673314470000071
的氧化硅、
Figure BDA0002673314470000072
的钛的顺序进行堆积并在其上通过化学气相沉积法进行成膜。
<评价方法>
[处理条件]
使1×1cm、或2×2cm尺寸的上述评价基板的试验片在60℃的清洗液10g中浸渍，对处理后的试验片进行水冲洗。
[膜厚测定]
对于下层防反射膜、氧化铝膜、及Low-k膜的膜厚，用光学式膜厚计n&k1280(n&kTechnology Inc.制)进行测定。对于钴的膜厚减少量，使用ICP-AES iCAP6300(ThermoScientific制)，由处理后的清洗液中的金属浓度来算出。
Figure BDA0002673314470000073
蚀刻速率[
Figure BDA0002673314470000074
/分钟]通过用膜厚减少量除以处理时间(氧化铝膜为1分钟、钴膜为4分钟、Low-k膜为5分钟)来算出。
判定：
(评价I)：干蚀刻残渣的去除性
通过下层防反射膜的去除时间(下层防反射膜剥离、可以目视到基底材料的时刻的时间)进行判定。
G：小于15分钟
A：15分钟～小于30分钟
P：30分钟～60分钟
(评价II)：氧化铝膜的去除性
通过氧化铝膜的蚀刻速率进行判定。
G：
Figure BDA0002673314470000081
/分钟～小于
Figure BDA0002673314470000082
/分钟
A1：
Figure BDA0002673314470000083
/分钟～小于
Figure BDA0002673314470000084
/分钟
A2：
Figure BDA0002673314470000085
/分钟～
Figure BDA0002673314470000086
/分钟
P1：小于
Figure BDA0002673314470000087
/分钟。
P2：超过
Figure BDA0002673314470000088
/分钟。
将G、A1及A2判定记为合格。
(评价III)：钴的防腐蚀性
通过钴膜的蚀刻速率进行判定。
G：小于
Figure BDA0002673314470000089
/分钟。
P：
Figure BDA00026733144700000810
/分钟以上。
将G判定记为合格。
(评价IV)：Low-k膜的防腐蚀性
通过Low-k膜的蚀刻速率进行判定。
G：小于
Figure BDA00026733144700000811
/分钟。
P：
Figure BDA00026733144700000812
/分钟以上。
将G判定记为合格。
[pH]
用HORIBA制pH METER F-52对清洗液的pH进行测定。测定温度设为25℃。
[粘度]
用柴田科学制乌氏粘度计测定清洗液的粘度。测定温度设为20℃。
[实施例1～22及比较例1～9]
使用表1或表2所示的组成的清洗液，对上述评价基板进行处理并进行评价。表1或表2中的浓度的单位表示质量％。对于评价IV，对实施例1～22进行评价，全部为G判定。
[表1]
Figure BDA0002673314470000091
DGME：二乙二醇单甲醚(20℃下的粘度为4mPa·s)
DGBE：二乙二醇单丁醚(20℃下的粘度为7mPa·s)
TGME：三乙二醇单甲醚(20℃下的粘度为8mPa·s)
DPGME：二丙二醇单甲醚(20℃下的粘度为4mPa·s)
DMIB：N,N-二甲基异丁酰胺(20℃下的粘度为1mPa·s)
[表2]
Figure BDA0002673314470000101
甘油：(20℃下的粘度为1500mPa·s)
附图标记说明
1：干蚀刻残渣
2：干蚀刻阻挡层
3：金属布线层(钴)
4：层间绝缘膜

Claims (8)

1.一种清洗液，其含有：胺化合物(A)0.2～20质量％、水溶性有机溶剂(B)40～70质量％、及水，
所述胺化合物(A)含有选自由正丁胺、己胺、辛胺、1,4-丁二胺、二丁胺、3-氨基-1-丙醇、N,N-二乙基-1,3-二氨基丙烷、及双(六亚甲基)三胺组成的组中的1者以上，并且所述水溶性有机溶剂(B)在20℃下的粘度为10mPa·s以下，所述清洗液的pH为9.0～14的范围。
2.根据权利要求1所述的清洗液，其中，所述胺化合物(A)的含量为0.2～4.0质量％。
3.根据权利要求1或2所述的清洗液，其中，所述水的含量为28～59质量％。
4.根据权利要求1～3中任一项所述的清洗液，其中，所述水溶性有机溶剂(B)含有选自由二乙二醇单甲醚、二乙二醇单丁醚、三乙二醇单甲醚、二丙二醇单甲醚、及N,N-二甲基异丁酰胺组成的组中的1者以上。
5.根据权利要求1～4中任一项所述的清洗液，其中，所述胺化合物(A)含有选自由3-氨基-1-丙醇、N,N-二乙基-1,3-二氨基丙烷、及双(六亚甲基)三胺组成的组中的1者以上。
6.根据权利要求1～5中任一项所述的清洗液，其用于去除干蚀刻残渣。
7.一种半导体基板的制造方法，其包括使用权利要求1～6中任一项所述的清洗液对包含钴的半导体基板进行清洗的工序。
8.根据权利要求7所述的半导体基板的制造方法，其中，所述半导体基板包含：含有钴的金属布线层、层间绝缘膜、和含有氧化铝的干蚀刻阻挡层。
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