CN1665755A - 清除蚀刻残留物的组合物及其应用 - Google Patents
清除蚀刻残留物的组合物及其应用 Download PDFInfo
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- CN1665755A CN1665755A CN038162229A CN03816222A CN1665755A CN 1665755 A CN1665755 A CN 1665755A CN 038162229 A CN038162229 A CN 038162229A CN 03816222 A CN03816222 A CN 03816222A CN 1665755 A CN1665755 A CN 1665755A
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Abstract
包含水、有机二羧酸、缓冲剂和氟源物质或可还包含可与水混溶的有机溶剂的组合物，它们能清除蚀刻残留物。
Description
发明领域
本发明涉及从一个物体的显微结构上有选择地清除蚀刻残留物。本发明是有选择地清除残留物，不会侵蚀与用来清除残留物的组合物接触的金属和/或二氧化硅。此外，本发明涉及适合清除蚀刻残留物的某些清除组合物。
发明领域
在生产微电子结构的过程中涉及许多步骤。在生产集成电路的工艺中，有时要求选择性蚀刻半导体的表面。从历史上看，已有许多极为不同的蚀刻工艺在选择性清除材料方面获得了不同程度的成功。此外，选择性蚀刻微电子结构中的不同层，被认为是集成电路生产工艺中的一个关键步骤。
在形成通孔、金属线和沟槽的过程中，人们越来越多地选用反应活性离子蚀刻(RIE)工艺来转移图像。例如，需要多层互连线后端的复杂半导体器件，如高级DRAMS和微处理器，采用RIE产生通孔、金属线和沟槽结构。通孔用来通过中间层电介质使某一层硅、硅化物或金属布线与下一层布线发生接触。金属线是用于器件互连的导电结构。沟槽结构用于形成金属线结构。通孔、金属线和沟槽结构一般使得金属和合金，如Al、AlCu、Cu、Ti、TiN、Ta、TaN、W、TiW、硅和硅化物，如硅化钨、硅化钛或硅化钴裸露出来。RIE工艺一般会留下(复杂混合物的)残留物，包括再次溅射的氧化物以及可能来自光刻胶的有机物质、在平版印刷中用来形成通孔、金属线或沟槽结构的抗反射涂层物质。
因此，需要一种选择性清除材料和工艺，它能够清除一般使用等离子体，特别是使用RIE技术进行选择性蚀刻时留下的残留物。此外，还需要一种选择性清除材料和工艺，它能够清除蚀刻残留物，相对于金属、硅、硅化物和/或中间层介电材料(如同样可能与清除组合物接触的沉积氧化物)，它对残留物具有高度的选择性。
发明概述
本发明提供了能从基底上选择性清除蚀刻残留物的组合物，它不会侵蚀同样可能与该组合物接触的金属。此外，本发明提供的组合物对氧化硅的蚀刻速率最小，对电介质的蚀刻速率通常也较低。
更具体地，本发明涉及适合清除蚀刻残留物的组合物，它包含：
A.多达约80重量％的有机溶剂，它与水混溶；
B.约5-50重量％的水；
C.约1-20重量％的有机二羧酸；
D.约1-20重量％的碱；
E.约0.1-10重量％氟离子源物质。
碱D与二羧酸C形成缓冲剂。
本发明还涉及从基底上清除蚀刻残留物的方法，它是使基底与上述组合物接触。
从下面的详细描述中，本领域技术人员不难看出本发明的其他目标和优点。以下只是描述本发明的一些优选实施方式，只是实施本发明时考虑到的最佳方式。将会认识到，本发明还可有其他不同的实施方式，其若干细节可以从各种显而易见的方面进行修改，只要不偏离本发明。因此，所提供的图文应当看作是说明性的图文，不对本发明构成限制。
附图简述
图1所示为各种含二羧酸酸的配剂在不同pH下的掺磷未硬化TEOS蚀刻速率。
图2所示为各种含二羧酸酸的配剂在不同pH下的未掺杂未硬化TEOS蚀刻速率。
图3所示为马来酸缓冲氟化物剥离剂和氨基磺酸缓冲氟化物剥离剂的PTEOS蚀刻速率，两种剥离剂的pH均调节到7.0。
图4所示为三种产品的PTEOS蚀刻速率，这三种产品是乙酸缓冲的氟化物剥离剂、氨基磺酸缓冲的氟化物剥离剂和实施例8。
图5所示为对铝线的清除效果。
图6所示为对氧化物敏感通孔的清除效果。
本发明的最佳实施方式
本发明涉及选择性清除蚀刻残留物，特别是反应活性离子蚀刻带来的残留物。此外，蚀刻残留物还存在于一些制品中，这些制品也包含金属、硅、硅酸盐和/或中间层电介质，如沉积氧化硅和衍生氧化硅(如TEOS和旋涂玻璃)，其中残留物和金属、硅、硅化物和/或中间层电介质都会与清除组合物接触。本发明提供了选择性清除蚀刻后残留物的方法，该方法不会明显侵蚀金属、硅、二氧化硅和中间层电介质。金属通常是铜、铜合金、钛、氮化钛、钽、氮化钽、钨、钛/钨、铝和/或铝合金。本发明清除的残留物较好为反应活性离子蚀刻产生的残留物。
本发明组合物包含约5-50重量％、宜为约20-45重量％、最好约25-30重量％的水。所用水宜为去离子水。
此外，本发明组合物包含约1-20重量％、宜为约1-10重量％、最好约2-5重量％的有机二羧酸。
有机二羧酸可以是饱和酸或不饱和酸，可以是直链、支链或环状的。
合适的饱和酸的例子有乙二酸、丙二酸、丁二酸、戊二酸和己二酸。不饱和酸的例子有反丁烯二酸或顺丁烯二酸。环酸的例子有邻苯二甲酸和对苯二甲酸。优选丁二酸、丙二酸、顺丁烯二酸、己二酸和邻苯二甲酸。更为优选的酸是顺丁烯二酸和己二酸，最好是己二酸。
出人意料的是，根据本发明的研究，虽然本发明组合物中存在二羧酸，但并没有得到预料中的高氧化物蚀刻速率，原因是剥离剂溶液的pH值呈酸性。不仅如此，这些组合物的氧化物蚀刻速率极低，在某些情况下简直就不存在。据观察，抑制氧化物蚀刻需要二羧酸酸和/或其盐。因此，不含二羧酸酸或其盐的组合物不具有本发明的氧化物蚀刻抑制性。
此外，本发明组合物可包含有机或无机碱，它与有机二羧酸酸一起形成缓冲剂；碱的含量约为0.5-20重量％，较好约为1-10重量％，最好约为2-5重量％。
这些配剂的pH可以是1-7之间的任何值，较好约为5.5-6.0，具体取决于所选的二羧酸酸及其有效缓冲范围。具体地说，二羧酸酸可用两个pKa表征，缓冲剂通常是在溶液的pH在一指定pKa两边约0.75pH单位的范围内形成。例如，丙二酸的pKa值是pK1＝2.8和pK2＝5.7。那么，我们就可以用丙二酸作为缓冲剂，其pH保持在2.05-3.55和4.95-6.45之间。类似地，己二酸的pKa值为pK1＝4.5和pK2＝5.5。由于两个pH范围几乎重叠，己二酸的有效pH缓冲范围在3.75-6.25之间。缓冲非常重要，因为清除能力、介电性质和金属蚀刻性质都在某种程度上取决于pH。pH的变化会引起清除能力和基底蚀刻性的明显变化。例如，半水溶性氟化物剥离剂在pH＝4.75难以对铜明显，但当pH＝7.5或更高时，则会对铜严重侵蚀，使器件的关键尺寸发生无可挽回的损失。
合适的碱的例子包括(但不限于)氢氧化铵胺和氢氧化季铵。
碱不宜包含钠和钾等金属离子，因为它们容易污染基底。碱优选为氢氧化铵或单乙醇胺(MEA)。
本发明组合物还可包含氟离子化合物，其含量一般约为0.1-10重量％，宜为0.1-5重量％，最好约为0.5-3重量％。
提供氟离子的本发明化合物通常有氢氟酸、氟化铵、氟化季铵盐(如氟化四甲基铵和氟化四丁基铵)、氟硼酸盐、氟硼酸、四氟硼酸四丁基铵和六氟化铝。也可以采用脂族伯、仲或叔胺的氟盐，它们具有如下化学式：
R1N(R3)R2F
其中R1、R2和R3各自独立地取H或烷基。
R1、R2和R3基团中的碳原子总数一般不超过12。氟化物优选是氟化铵。
本发明组合物还包含0-80重量％可与水混溶的有机溶剂，宜包含约1-80重量％。可与水混溶的有机溶剂的优选含量约为30-65重量％，最好约为50-60重量％。
可与水混溶的有机溶剂的例子包括(但不限于)二甲基乙酰胺、N-甲基吡咯烷酮、二甲基砜、二甲基甲酰胺、N-甲基甲酰胺、甲酰胺、二甲基-2-哌啶酮(DMPD)、四氢糠醇、丙三醇、乙二醇和其他酰胺、醇或砜，或者多官能化合物，如羟胺或氨基醇。
如果采用溶剂，则优选的溶剂为二甲基乙酰胺、二甲基-2-哌啶酮和N-甲基吡咯烷酮。
如果需要，本发明组合物还可以包含防腐蚀剂。如果存在，防腐蚀剂的用量一般约为10重量％，较好约为0.5-5重量％，最好约为1-2重量％。
防腐蚀剂的例子包括(但不限于)儿茶酚、没食子酸、苯并***、雷锁酚、其他酚类、酸或***。
此外，当本发明组合物用在含铜的基底上时，它不宜包含苯并***，因为苯并***容易粘结在铜表面上。苯并***存在于原来本领域的各种组合物中。
本发明基底组合物的某些例子示于表1，优选组合物示于表2。
表1
| 组分 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 实施例6 | 实施例7 | 实施例8 | 实施例9 | 实施例10 | 实施例11 | 实施例12 |
| 二甲基乙酰胺 | 60 | 60 | 60 | 60 | 60 | 60 | 60 | 60 | 60 | 60 | 60 | 60 |
| 水 | 29.8 | 31.3 | 29.3 | 30.8 | 33.55 | 32.55 | 31.75 | 30.85 | 33.5 | 34.75 | 31.59 | 30.5 |
| 丁二酸 | 4 | 4 | 4 | 4 | 4 | |||||||
| 丙二酸 | 3.5 | 3.5 | ||||||||||
| 己二酸 | 3 | 3 | ||||||||||
| 邻苯二甲酸 | 4 | |||||||||||
| 顺丁烯二酸 | 4 | 4 | ||||||||||
| 28％NH4OH | 3.7 | 3.7 | 4.7 | 4.7 | 2.2 | 2.6 | 3 | 3.9 | 1.25 | 1 | 3.16 | 4.25 |
| 40％NH4F | 2.5 | 1 | 2.5 | 1 | 1.25 | 1.25 | 1.25 | 1.25 | 1.25 | 1.25 | 1.25 | 1.25 |
| PH(5％溶液) | 5.44 | 5.42 | 5.72 | 5.41 | 5.67 | 5.7 | 5.36 | 6.17 | 4.39 | 4.77 | 6.15 | 7 |
| PTEOS蚀刻速率 | 17.94 | 4.25 | 64 | 38.55 | 1.35 | 0.29 |
表2 优选配剂
| 组分 | 实施例7 | 实施例8 | 实施例9 | 实施例10 | 实施例11 | 实施例12 |
| 二甲基乙酰胺 | 60 | 60 | 60 | 60 | 60 | 60 |
| 去离子水 | 29.8 | 31.05 | 27.3 | 34.75 | 33.75 | 32.5 |
| 顺丁烯二酸 | 4 | 4 | 4 | 4 | ||
| 己二酸 | 3 | 3 | ||||
| 单乙醇胺 | 2 | 2 | ||||
| 28％氢氧化铵 | 3.7 | 3.7 | 3.7 | |||
| 40％氟化铵 | 2.5 | 1.25 | 5 | 1.25 | 1.25 | 2.5 |
| pH(5％溶液) | 6.48 | 6.59 | 6.55 | 2.37 | 5.6 | 5.5 |
表3 所示为选定的几种酸的pKa值和预期的有效缓冲范围。
表3酸的pKa值和有效缓冲范围
| 二酸 | 分子量 | pK1，pK2 | 缓冲范围 | |
| 乙二酸 | 90.04 | 1.27，4.27 | 0.52-2.02，3.52-5.02 | |
| 丙二酸 | 104.06 | 2.8，5.7 | 2.05-3.55，4.95-6.45 | |
| 丁二酸 | 118.09 | 4.2，5.63 | 3.45-6.38 | |
| 戊二酸 | 132.12 | 3.8，6.08 | 3.05-4.55，5.33-6.83 | |
| 己二酸 | 146.14 | 4.4，5.4 | 3.65-6.15 | |
| 顺丁烯二酸 | 116.07 | 1.9，6.3 | 1.15-2.65，5.55-7.05 | |
| 反丁烯二酸 | 116.07 | |||
| 邻苯二甲酸 | 166.13 | |||
| 乙酸 | 60.05 | 4.75 | 4.0-5.5 | |
| 丙烯酸 | 72.06 | |||
| HEPES | 238.31 | 7.6 | 6.85-8.35 | |
前面通过一些例子介绍了本发明。前面仅介绍了本发明的优选实施方式，但如上所述，应当理解本发明可以其他各种组合方式、改进形式和条件加以应用，并且可以根据上述介绍和/或相关技术或知识，在这里所阐述的发明思想范围内作出改变或改进。上述实施方式还可用来解释本发明的最佳实施方式，使得本领域的其他技术人员按这些实施方式或其他实施方式来利用本发明，并根据本发明的具体应用作出各种改进。因此，前面的说明并未将本发明限制在这里所介绍的形式上。同样，附属的权利要求应当理解为包括各种等价实施方式。
Claims (33)
1.一种适合清除蚀刻残留物的组合物，它包含：
A.多达约80重量％可水混溶的有机溶剂；
B.约5-50重量％的水；
C.约1-20重量％的有机二羧酸；
D.约0.5-20重量％的碱，它与上述二酸一起形成缓冲剂；
E.约0.1-10重量％的氟离子源物质。
2.权利要求1所述组合物，其特征在于，所述二羧酸选自乙二酸、丙二酸、丁二酸、戊二酸、己二酸、反丁烯二酸、顺丁烯二酸、邻苯二甲酸和对苯二甲酸。
3.权利要求1所述的组合物，其特征在于，所述有机二羧酸选自丁二酸、丙二酸、顺丁烯二酸、己二酸和邻苯二甲酸。
4.权利要求1所述的组合物，其特征在于，所述有机二羧酸选自顺丁烯二酸或己二酸。
5.权利要求1所述的组合物，其特征在于，所述有机二羧酸选自己二酸。
6.权利要求1所述的组合物，其特征在于，所述碱选自氢氧化铵、胺和氢氧化季铵。
7.权利要求1所述的组合物，其特征在于，所述碱是氢氧化铵或单乙醇胺。
8.权利要求1所述的组合物，其特征在于，所述氟离子源物质选自氢氟酸、氟化铵、氟化季铵、氟硼酸盐、氟硼酸、二氟化锡、氟化锑、四氟硼酸四丁基铵、六氟化铝，脂族伯、仲或叔胺的氟盐，它们具有如下化学式：
R1N(R3)R2
其中R1、R2和R3各自独立地取H或烷基。
9.权利要求1所述的组合物，其特征在于，所述氟离子源物质是氟化铵。
10.权利要求1所述的组合物，其特征在于，所述可与水混溶的有机溶剂的含量约为1-80重量％。
11.权利要求10所述的组合物，其特征在于，所述可与水混溶的有机溶剂选自二甲基乙酰胺、N-甲基吡咯烷酮、二甲基砜、二甲基甲酰胺、N-甲基甲酰胺、甲酰胺、DMPD、四氢糠醇、丙三醇和乙二醇。
12.权利要求10所述的组合物，其特征在于可与水混溶的有机溶剂选自二甲基乙酰胺、DMPD或NMP。
13.权利要求1所述的组合物，其特征在于，pH约为1-7。
14.权利要求1所述的组合物，其特征在于，pH约为5.5-6。
15.权利要求1所述的组合物，其特征在于，它不含苯并***。
16.从基底上清除蚀刻残留物的方法，它包括使所述基底与一种组合物接触，该组合物包含：
A.多达约80重量％可与水混溶的有机溶剂；
B.约5-50重量％的水；
C.约1-20重量％的有机二羧酸；
D.约0.5-20重量％的碱，它与上述二酸一起形成缓冲剂；
E.约0.1-10重量％氟离子源物质。
17.权利要求16所述的方法，其特征在于，所述有机二羧酸选自乙二酸、丙二酸、丁二酸、戊二酸、己二酸、反丁烯二酸、顺丁烯二酸、邻苯二甲酸和对苯二甲酸。
18.权利要求16所述的方法，其特征在于，所述有机二羧酸选自丁二酸、丙二酸、顺丁烯二酸、己二酸和邻苯二甲酸。
19.权利要求16所述的方法，其特征在于，所述有机二羧酸选自顺丁烯二酸或己二酸。
20.权利要求16所述的方法，其特征在于，所述有机二羧酸是己二酸。
21.权利要求16所述的方法，其特征在于，所述碱选自氢氧化铵、胺和氢氧化季铵。
22.权利要求16所述的方法，其特征在于，所述碱是氢氧化铵或单乙醇胺。
23.权利要求16所述的方法，其特征在于，所述氟离子源物质选自氢氟酸、氟化铵、氟化季铵、氟硼酸盐、氟硼酸、二氟化锡、氟化锑、四氟硼酸四丁基铵、六氟化铝，脂族伯、仲或叔胺的氟盐，它们具有如下化学式：
R1N(R3)R2
其中R1、R2和R3各自独立地取H或烷基。
24.权利要求16所述的方法，其特征在于，所述氟离子源物质是氟化铵。
25.权利要求16所述的方法，其特征在于，所述可与水混溶的有机溶剂的含量约为1-80重量％。
26.权利要求25所述的方法，其特征在于，所述可与水混溶的有机溶剂选自二甲基乙酰胺、N-甲基吡咯烷酮、二甲基砜、二甲基甲酰胺、N-甲基甲酰胺、甲酰胺、DMPD、四氢糠醇、丙三醇和乙二醇。
27.权利要求25所述的方法，其特征在于，所述可与水混溶的有机溶剂选自二甲基乙酰胺、DMPD或NMP。
28.权利要求16所述的方法，其特征在于，pH约为1-7。
29.权利要求16所述的方法，其特征在于，pH约为5.5-6。
30.权利要求16所述的方法，其特征在于，它不含苯并***。
31.权利要求16所述的方法，其特征在于，所述基底还包括选自金属、硅、硅化物和中间层介电材料的物质。
32.权利要求31所述的方法，其特征在于，所述中间层介电材料包括氧化硅或衍生的氧化硅。
33.权利要求31所述的方法，其特征在于，所述金属选自铜、铜合金、钛、氮化钛、钽、氮化钽、钨、钛/钨、铝和/或铝合金。
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- 2002-07-10 US US10/191,060 patent/US6677286B1/en not_active Expired - Lifetime
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- 2003-07-10 KR KR1020057000264A patent/KR20050025316A/ko not_active Application Discontinuation
- 2003-07-10 CN CNB038162229A patent/CN1278975C/zh not_active Expired - Fee Related
- 2003-07-10 AU AU2003251802A patent/AU2003251802A1/en not_active Abandoned
- 2003-07-10 EP EP03763377A patent/EP1534643A1/en not_active Withdrawn
- 2003-07-10 JP JP2004520050A patent/JP2005532691A/ja active Pending
- 2003-07-10 MY MYPI20032599A patent/MY130650A/en unknown
- 2003-07-10 WO PCT/US2003/021402 patent/WO2004005211A1/en active Application Filing
- 2003-11-26 US US10/723,737 patent/US6821352B2/en not_active Expired - Lifetime
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| WO2007056919A1 (fr) * | 2005-11-15 | 2007-05-24 | Anji Microelectronics (Shanghai) Co., Ltd | Composition detergente aqueuse |
| CN1966636B (zh) * | 2005-11-15 | 2011-08-03 | 安集微电子（上海）有限公司 | 清洗液组合物 |
| CN107217332A (zh) * | 2017-03-28 | 2017-09-29 | 深圳新宙邦科技股份有限公司 | 一种氮/硼/氟三元共掺杂碳纤维及其制备方法 |
| CN108103584A (zh) * | 2017-11-13 | 2018-06-01 | 德清丽晶能源科技有限公司 | 一种用于多晶金刚线切硅片表面处理的酸性制绒添加剂及其使用方法 |
| CN110540369A (zh) * | 2018-07-12 | 2019-12-06 | 蓝思科技（长沙）有限公司 | 一种用于褪镀fgar膜的褪镀液及其制备方法和应用 |
| CN114072488A (zh) * | 2019-05-01 | 2022-02-18 | 富士胶片电子材料美国有限公司 | 蚀刻组合物 |
| CN114008181A (zh) * | 2019-06-19 | 2022-02-01 | 弗萨姆材料美国有限责任公司 | 用于半导体衬底的清洁组合物 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP1534643A1 (en) | 2005-06-01 |
| TW200420755A (en) | 2004-10-16 |
| JP2005532691A (ja) | 2005-10-27 |
| US6677286B1 (en) | 2004-01-13 |
| MY130650A (en) | 2007-07-31 |
| KR20050025316A (ko) | 2005-03-14 |
| AU2003251802A1 (en) | 2004-01-23 |
| US20040171503A1 (en) | 2004-09-02 |
| CN1278975C (zh) | 2006-10-11 |
| WO2004005211A1 (en) | 2004-01-15 |
| US6821352B2 (en) | 2004-11-23 |
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