CN113667552A - 一种用于铜大马士革工艺的清洗液 - Google Patents
一种用于铜大马士革工艺的清洗液 Download PDFInfo
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- CN113667552A CN113667552A CN202010413065.4A CN202010413065A CN113667552A CN 113667552 A CN113667552 A CN 113667552A CN 202010413065 A CN202010413065 A CN 202010413065A CN 113667552 A CN113667552 A CN 113667552A
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- CN
- China
- Prior art keywords
- acid
- cleaning solution
- damascene process
- copper damascene
- ammonium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000004140 cleaning Methods 0.000 title claims abstract description 86
- 239000010949 copper Substances 0.000 title claims abstract description 51
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 48
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 45
- 230000008569 process Effects 0.000 title claims abstract description 41
- 229910052751 metal Inorganic materials 0.000 claims abstract description 43
- 239000002184 metal Substances 0.000 claims abstract description 43
- 230000007797 corrosion Effects 0.000 claims abstract description 20
- 238000005260 corrosion Methods 0.000 claims abstract description 20
- 239000003112 inhibitor Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- -1 organic acid ammonium salt Chemical class 0.000 claims abstract description 17
- 239000002738 chelating agent Substances 0.000 claims abstract description 10
- 239000007800 oxidant agent Substances 0.000 claims abstract description 10
- 150000007530 organic bases Chemical class 0.000 claims abstract description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- KPSSIOMAKSHJJG-UHFFFAOYSA-N neopentyl alcohol Chemical compound CC(C)(C)CO KPSSIOMAKSHJJG-UHFFFAOYSA-N 0.000 claims description 16
- 150000001412 amines Chemical group 0.000 claims description 9
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- KAESVJOAVNADME-UHFFFAOYSA-N 1H-pyrrole Natural products C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 6
- CMGDVUCDZOBDNL-UHFFFAOYSA-N 4-methyl-2h-benzotriazole Chemical compound CC1=CC=CC2=NNN=C12 CMGDVUCDZOBDNL-UHFFFAOYSA-N 0.000 claims description 6
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- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 claims description 6
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 6
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 claims description 4
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- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C—CHEMISTRY; METALLURGY
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- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11D3/2017—Monohydric alcohols branched
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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Abstract
一种用于铜大马士革工艺的清洗液,包括:氧化剂、螯合剂、有机碱、表面张力调节剂、金属缓蚀剂、有机酸铵盐、和水。本发明通过在清洗液中添加表面张力调节剂,在TiN硬掩模完全去除,金属材料、非金属材料以及低k介质材料得到很好的保护前提下,进一步降低了清洗液的表面张力,使金属缓蚀剂易于从晶圆表面脱附,进而使刻蚀残留物完全去除,进一步增强了清洗效果,提高了半导体器件的良率,且本申请的用于铜大马士革工艺的清洗液不含氟化物,操作窗口较大(适用于20℃~80℃),PH值适用范围广(pH值为5~14),在高端半导体清洗领域具有良好的应用前景。
Description
技术领域
本申请涉及半导体制造过程中的晶圆清洗领域,尤其涉及一种用于14nm及更小技术节点高端半导体清洗液领域。
背景技术
铜是一种稳定金属,在与刻蚀气体反应时不会产生挥发性的副产物,因而在互连工艺中不能像铝一样直接使用干法刻蚀工艺蚀刻铜,以形成金属互连线图形。IBM公司在1997年研发出大马士革工艺,该工艺通过光刻以及干法蚀刻工艺在介电材料层上形成金属互连线图形的凹槽,在淀积金属阻挡层,铜籽晶层和金属铜,再用CMP的方式去除多余的金属,形成所需的金属连线。多层铜互连工艺一般需用使用同时形成互连线沟槽与互连通孔的双大马士革工艺。
在集成电路(IC)制造中,铜双大马士革工艺应用越来越广泛,高速旋转单片机清洗也成为主流清洗方式。随着互连线特征尺寸进一步减小到14nm及以下技术节点,去胶等工艺中的等离子体损伤会对低k材料的机械与物化性能产生严重影响,使集成结构中k值局部增加,削弱低k介质材料的优势。此外,由于蚀刻残留物的低表面能和交联性质,以及残留物成分物理和化学性质的变化,加之清洗液与设备膜材料和结构之间的兼容性问题,使得寻找能够有效去除等离子体刻蚀残留物的同时又能保护低k介质材料、非金属材料和金属材料的低表面张力清洗液越来越具有挑战性。
目前,关于集成电路领域的半导体清洗液的报道主要以国外为主。美国高级技术材料公司在专利CN101366107B中公开了一种用于从微电子器件基底上除去刻蚀残留物,高选择性去除含钛(TiN)硬掩模材料的含水氧化组合物及其制备和使用方法。基板材料主要有低k介电材料如有机聚合物、有机硅酸盐玻璃OSG、掺碳氧化物(CDO)玻璃、正硅酸四乙酯(TEOS)、FSG等,金属材料主要是铜和钴。该清洗液组合物主要以H2O2作为氧化剂,以伯胺、仲胺、叔胺和胺-N-氧化物等胺类物质作为氧化剂稳定剂,任选至少一种有机酸作为金属螯合剂,任选至少一种唑类作为金属缓蚀剂,配合以缓冲剂和有机共溶剂以及水,在pH值3~9,30~50℃温度条件下,从微电子器件上选择性和有效地除去含钛等离子体刻蚀后残留物、侧壁聚合残留物、含铜通孔残留物和/或含钛硬掩模层。该清洗液可以稳定6~24h实现从微电子器件上高效清洗残余材料,同时不会损坏介电材料和金属互连材料。
最新报道中,美国Versum Material公司在专利US2020035485A1中公开了一种用于从电子电路器件除去TiN硬掩模的组合物。主要以双氧水作为氧化剂,大分子有机酸作为双氧水稳定剂,唑类和多元醇类作为金属腐蚀抑制剂,季铵氢氧化物和铵盐作为蚀刻剂,水作为溶剂,加之以任选氟化物来保证清洗力,在pH值大于5.5的环境下选择性地除去氮化钛和来自等离子体刻蚀过程中的残留物,同时使Cu、Co、低k介电材料等第二材料得到有效保护。在晶片或器件加工过程中通过稀氢氟酸去除后,铜损失受到氧化铜厚度的影响,该发明中提到含有氨基的腐蚀抑制剂可提供更好的氧化铜厚度性能。
发明内容
为解决现有技术中的用于铜大马士革工艺的清洗液无法完全去除金属孔道内的刻蚀残留物的问题,本申请提供一种用于铜大马士革工艺的清洗液,包括:氧化剂、螯合剂、有机碱、表面张力调节剂、金属缓蚀剂、有机酸铵盐、和水。
进一步地,所述氧化剂的含量为0.1wt%-30wt%。
进一步地,所述螯合剂的含量为0.05-1000ppm。
进一步地,所述螯合剂的含量为0.1-10ppm。
进一步地,所述有机碱的含量为0.1wt%-20wt%。
进一步地,所述表面张力调节剂的含量为10ppm-10wt%。
进一步地,所述表面张力调节剂的含量为10ppm-5wt%。
进一步地,所述表面张力调节剂的含量为10ppm-3%。
进一步地,所述金属缓蚀剂的含量为0.01wt%-20wt%。
进一步地,所述有机酸铵盐的含量为0.01wt%-50wt%。
进一步地,所述水的含量为35.1wt%-96.9wt%。
进一步地,所述氧化剂选自H2O2、N-甲基吗啉氧化物(NMMO或NMO)、过氧化苯甲酰、过乙酸(CH3(CO)OOH)、过氧化脲((CO(NH2)2)H2O2)、硝酸、过氧乙酸、过氧苯甲酸、或四氧嘧啶中的一种或多种。
进一步地,所述螯合剂选自甘氨酸、丝氨酸、脯氨酸、亮氨酸、丙氨酸、天冬氨酸、天冬酰胺、谷氨酰胺、缬氨酸、赖氨酸、胱氨酸、乙二胺四乙酸(EDTA)、反式-1,2环己二胺四乙酸(CDTA)、尿酸、吡啶甲酸、次氮基三乙酸(NTA)、羟基乙叉二膦酸(HEDP)、乙二胺-N,N’-二琥铂酸(EDDS)、谷氨酸、二乙烯三胺五乙酸(DTPA)、羟乙基乙二胺三乙酸(HEDTA)、亚氨基二乙酸(IDA)、氨三乙酸、水杨酸、葡萄糖酸、烟酸、酒石酸、柠檬酸、1,4,7,10-四氮杂环十二烷-1,4,7,10-四乙酸(DOTA)、乙二醇四乙酸(EGTA)、1,2-双(邻氨基苯氧基)乙烷-N,N,N’,N’-四乙酸、乙二胺-N,N’-双(2-羟基苯乙酸)(HDDHA)、或丙二胺四乙酸中的一种或多种。
进一步地,所述有机碱选自季胺氢氧化物、有机胺、或有机醇胺中的一种或多种。
进一步地,所述季胺氢氧化物选自四甲基氢氧化铵(TMAH)、四乙基氢氧化铵(TEAH)、三甲基苯基氢氧化铵(TMPAH)、四丙基氢氧化铵(TPAH)、四丁基氢氧化铵(TBAH)、苄基三甲基氢氧化铵(BTMAH)、苄基三乙基氢氧化铵(BTEAH)、胆碱氢氧化物、氢氧化铵、十二烷基三甲基氢氧化铵(DTAH)、或十六烷基三甲基氢氧化铵(CTOH)中的一种或多种。
进一步地,所述有机胺选自单乙胺、二乙胺、三乙胺、三丙胺、N'N-二乙基乙二胺、羟乙基乙二胺、环己胺、1,2-丙二胺、或五甲基二乙烯三胺中的一种或多种。
进一步地,所述有机醇胺选自单乙醇胺(MEA)、二乙醇胺(DEA)、三乙醇胺(TEA)、二甘醇胺(DGA)、异丙醇胺、或N-甲基乙醇胺中的一种或多种。
进一步地,所述有机碱的金属离子的含量<50ppb。
进一步地,所述表面张力调节剂为极性有机物一元醇和/或极性有机物醚类,所述极性有机物醚类的结构通式为R-O-R、R-O-R'、Ar-O-R、Ar-O-Ar或Ar-O-Ar',其中,R=烃基,R'=烃基,R和R'可以相同,也可以不同,相同为对称醚,不相同为混合醚,如果R、R'分别是一个有机基团两端的碳原子则称为环醚,Ar=芳烃基,Ar'=芳烃基,Ar和Ar'可以相同,也可以不同。
进一步地,所述极性有机物一元醇选自甲醇、乙醇、正丙醇、异丙醇、正丁醇、异丁醇、二级丁醇、三级丁醇、新戊醇、环己醇、辛醇、苯甲醇、香茅醇、或橙花醇中的一种或多种。
进一步地,所述极性有机物醚类选自乙醚、丙二醇甲醚、二丙二醇甲醚(DPM)、丙二醇苯醚、甲基叔丁醚、四氢呋喃(THF)、环氧乙烷、苯甲醚、1,2-环氧丙烷、1,4-二氧六环、甲基烯丙基醚、正丙醚、或丁基缩水甘油醚中的一种或多种。
进一步地,所述金属缓蚀剂为唑类杂环化合物。
进一步地,所述唑类杂环化合物选自苯并三氮唑(BTA)、1,2,4-三氮唑、5-甲基苯并三氮唑(TTA)、羟基苯并三唑、吡唑、甲苯三唑、3,5-二甲基吡唑、四氮唑、4-氨基-1,2,4-三唑、苯并噻唑、甲基-1H-苯并三唑(TTL)、2-氨基苯并噻唑、2-巯基苯并噻唑、3-氨基-5-羟基吡唑、1-苯基吡唑、巯基苯并咪唑、5-氨基四唑、3-巯基-1,2,4-三唑、3-异丙基-1,2,4-三唑、2-(5-氨基-戊基)-苯并三唑、5-苯硫醇-苯并三唑、甲基四唑、5-苯基-苯并三唑、5-硝基-苯并三唑、3-氨基-5-巯基-1,2,4-三唑、1-氨基-1,2,4三唑、羟苯并三唑、1-氨基-1,2,3-苯并三唑、或噻唑中的一种或多种。
进一步地,所述有机酸铵盐选自甲酸铵、草酸铵、乳酸铵、酒石酸铵、柠檬酸三铵、乙酸铵、氨基甲酸铵、碳酸铵、苯甲酸铵、乙二胺四乙酸四铵(EDTA四铵)、EDTA三铵、EDTA二铵、琥珀酸铵、1-H-吡唑-3-甲酸铵、丙二酸铵、己二酸铵、或亚氨基二乙酸铵中的一种或多种。优选地,所述有机酸铵盐为螯合能力强的有机酸铵盐。
本申请的所有材料和试剂均市售可得。
与现有技术相比较,本发明的优势在于:
本发明公开了一种用于铜大马士革工艺的清洗液,主要用于14nm及更小技术节点高端半导体清洗液领域。本发明通过在清洗液中添加表面张力调节剂,在TiN硬掩模完全去除,金属材料、非金属材料以及低k介质材料得到很好的保护前提下,进一步降低了清洗液的表面张力,使金属缓蚀剂易于从晶圆表面脱附,进而使清洗后晶圆的金属孔道内的刻蚀残留物能够被完全去除,进一步增强了清洗效果,提高了半导体器件的良率,且本申请的用于铜大马士革工艺的清洗液不含氟化物,操作窗口较大(适用于20℃~80℃),PH值适用范围广(pH值为5~14),在高端半导体清洗领域具有良好的应用前景。
具体实施方式
下面结合具体实施例,详细阐述本发明的优势。
制备方法:按照下述表1中各个实施例和对比例的配方(特定组分及其对应的特定含量)将各个组分进行简单混合。
表1.不同实施例及对比例的配方和清洗温度
效果实施例
用于测试蚀刻速率的测试对象及其来源:
TiN(氮化钛)空白晶片——Ramco Specialties Inc.(美国拉姆科专业有限公司)
Cu(铜)空白晶片——Ramco Specialties Inc.
Co(钴)空白晶片——Ramco Specialties Inc.
SiON(氮氧化硅)空白晶片——Ramco Specialties Inc.
TEOS(二氧化硅)空白晶片——Ramco Specialties Inc.
BDII(低介电常数氧化硅)空白晶片——Ramco Specialties Inc.
TiN、Cu、Co等金属蚀刻速率测试方法:
(1)利用Napson四点探针仪测试5*5cm金属空白晶片(TiN空白晶片、Cu空白晶片、Co空白晶片)的电阻初值(Rs1);
(2)将该5*5cm金属空白晶片在迷你单片机mini-SWT上400rpm,TiN空白晶片经清洗液处理5min,Cu空白晶片和Co空白晶片化学处理10min;
(3)取出该5*5cm金属空白晶片,用去离子水(DIW)清洗,高纯氮气吹干,再利用Napson四点探针仪测试5*5cm金属空白晶片的电阻值(Rs2);
(4)将上述电阻值和蚀刻时间输入到合适的程序可计算出金属的蚀刻速率。
SiON、TEOS、BDII等非金属蚀刻速率(Etch Rate)测试方法:
(1)按照标准开启Nanospec6100测厚仪,选用合适的测试程序,将5*5cm非金属空白晶片(SiON空白晶片、TEOS空白晶片、BDII空白晶片)放入Nanospec6100测厚仪上测试非金属空白晶片厚度,将非金属空白晶片旋转90°继续测试,连续测试4次,记录数值;
(2)若非金属空白晶片为BDII,需用水冲洗干净,马弗炉350℃处理20min,干燥器冷却至室温再测试前值;(其他晶片无需步骤2)
(3)将该5*5cm非金属空白晶片在mini-SWT上400rpm,清洗液处理10min;
(4)取出该5*5cm非金属空白晶片,用DIW清洗,高纯氮气吹干,在Nanospec6100测厚仪上按程序1测试晶片厚度,记录数值;
(5)若非金属空白晶片为BDII,需用水冲洗干净,马弗炉350℃处理20min,干燥器冷却至室温再测试后值;(其他晶片无需步骤5)
(6)将上述前后厚度值和蚀刻时间输入合适的程序中,蚀刻速率计算为厚度变化除以化学处理时间。
将按照表1的实施例与对比例制备得到的不同清洗液,利用克吕士K100型表面张力仪使用悬滴法测试不同溶液的表面张力。按照上述蚀刻速率测试方法测试不同空白晶片的蚀刻速率,并利用X射线光电子能谱分析仪(XPS)测试金属缓蚀剂在铜或钴空白晶片表面的吸附情况,因为金属缓蚀剂含有N元素,所以,以铜表面的N元素的含量判断金属缓蚀剂在铜表面的吸附量。同时在50℃、400rpm/min的条件下,使用mini-SWT单片机清洗图案晶圆90s,水漂洗干净,氮气吹干,Hitachi SU8220型扫描电镜(SEM)观察图形晶圆的清洗效果。不同空白晶片的蚀刻速率、表面吸附结果、表面张力及清洗效果见表2。
表2.不同实施例与对比例的蚀刻速率、表面吸附结果、表面张力及清洗结果
从表2中可以看出:本发明的清洗液在TiN硬掩模完全去除的情况下,对半导体制程中所用的金属(如Cu和Co)和非金属(SiON、TEOS、BDII)基本不会刻蚀,其腐蚀情况均满足半导体业界通常在高速旋转单片机清洗的要求。
对比例1与实施例30对照表明,不添加表面张力调节剂,溶液的表面张力较高,金属缓蚀剂在空白铜晶片表面的吸附(XPS)较多,晶圆清洗后金属孔道残留物较多;添加了表面张力调节剂新戊醇,溶液的表面张力得到一定程度的降低,金属缓蚀剂在空白铜晶片表面的吸附也比不添加时要少,进而在图形晶圆的清洗残留物更少。
实施例30与实施例31表明,添加不同浓度的新戊醇,溶液的表面张力达到可调控,随着新戊醇浓度的增加,溶液的表面张力下降,相应的清洗液在晶片表面的吸附量和清洗后的残留物也逐渐减少,有利于提高半导体器件的良率。
对比例3与实施例31对照表明,包含相同质量的丙二醇清洗液和包含相同质量的一元醇清洗液,包含丙二醇的清洗液的表面张力要比包含一元醇的清洗液大的多;对比例4与对比例3、实施例31对照表明,包含相同质量的山梨醇的清洗液的表面张力比包含相同质量的新戊醇(一元醇)的清洗液要大的多,同时,比包含相同质量的丙二醇(二元醇)清洗液的表面张力也要大一些,这会对清洗液在晶圆表面的吸附和脱附过程造成影响,进而影响清洗效果。由表2的实施例31、对比例3和对比例4可知,包含新戊醇的清洗液在晶片表面完全无吸附,金属孔道残留物被完全清洗干净,而包含丙二醇或山梨醇的清洗液在晶片表面存在轻微吸附,清洗后在金属孔道内仍然存在少量残留物。由此可知,清洗液的表面张力越小,清洗液在晶圆表面越容易脱附,清洗后的金属孔道内的残留物越少。
对比例2与实施例32对照表明,不添加表面张力调节剂,溶液的表面张力较高,在空白铜晶片表面的吸附较多,晶圆清洗后金属孔道残留物较多;添加了表面张力调节剂丙二醇苯醚的体系,可以降低溶液的表面张力,减少溶液在空白铜晶片表面的吸附,提高清洗能力。实施例32与实施例33表明,丙二醇苯醚浓度的增加,溶液的表面张力降低,清洗液在晶片表面的吸附量和残留物也进一步减少,清洗效果得到明显的提升。原理为:醇醚类极性有机物,分子内含有亲水基,在水溶液中,亲水基与水分子接触,受到水分子向下的吸引力。由于亲水基的极性弱于水分子,这种吸引力弱于水分子之间的吸引力,因此在有醇醚分子排列的水溶液表面,比没有醇醚等极性有机物的水溶液表面受力不平衡的状态要弱,分子向内部的运动减弱,表面分子密度增加,分子间的有效距离变短,分子间引力减弱,表面“绷紧”程度降低,表面张力下降。
综上,本发明的积极进步效果在于:本发明开发的一种用于铜大马士革工艺的清洗液,通过添加表面张力调节剂,在TiN硬掩模完全去除,金属材料、非金属材料以及低k介质材料得到很好的保护前提下,进一步降低了清洗液的表面张力,进而使金属缓蚀剂易于从晶圆表面脱附,使刻蚀残留物完全去除,进一步增强了清洗效果,提高了半导体器件的良率,操作窗口较大,在高端半导体清洗领域具有良好的应用前景。
以上对本发明的具体实施例进行了详细描述,但其只是作为范例,本发明并不限制于以上描述的具体实施例。对于本领域技术人员而言,任何对本发明进行的等同修改和替代也都在本发明的范畴之中。因此,在不脱离本发明的精神和范围下所作的均等变换和修改,都应涵盖在本发明的范围内。
Claims (24)
1.一种用于铜大马士革工艺的清洗液,其特征在于,包括:氧化剂、螯合剂、有机碱、表面张力调节剂、金属缓蚀剂、有机酸铵盐、和水。
2.如权利要求1所述的用于铜大马士革工艺的清洗液,其特征在于,所述氧化剂的含量为0.1wt%-30wt%。
3.如权利要求1所述的用于铜大马士革工艺的清洗液,其特征在于,所述螯合剂的含量为0.05-1000ppm。
4.如权利要求3所述的用于铜大马士革工艺的清洗液,其特征在于,所述螯合剂的含量为0.1-10ppm。
5.如权利要求1所述的用于铜大马士革工艺的清洗液,其特征在于,所述有机碱的含量为0.1wt%-20wt%。
6.如权利要求1所述的用于铜大马士革工艺的清洗液,其特征在于,所述表面张力调节剂的含量为10ppm-10wt%。
7.如权利要求6所述的用于铜大马士革工艺的清洗液,其特征在于,所述表面张力调节剂的含量为10ppm-5wt%。
8.如权利要求7所述的用于铜大马士革工艺的清洗液,其特征在于,所述表面张力调节剂的含量为10ppm-3%。
9.如权利要求1所述的用于铜大马士革工艺的清洗液,其特征在于,所述金属缓蚀剂的含量为0.01wt%-20wt%。
10.如权利要求1所述的用于铜大马士革工艺的清洗液,其特征在于,所述有机酸铵盐的含量为0.01wt%-50wt%。
11.如权利要求1所述的用于铜大马士革工艺的清洗液,其特征在于,所述水的含量为35.1wt%-96.9wt%。
12.如权利要求1所述的用于铜大马士革工艺的清洗液,其特征在于,所述氧化剂选自H2O2、N-甲基吗啉氧化物、过氧化苯甲酰、过乙酸、过氧化脲、硝酸、过氧乙酸、过氧苯甲酸、或四氧嘧啶中的一种或多种。
13.如权利要求1所述的用于铜大马士革工艺的清洗液,其特征在于,所述螯合剂选自甘氨酸、丝氨酸、脯氨酸、亮氨酸、丙氨酸、天冬氨酸、天冬酰胺、谷氨酰胺、缬氨酸、赖氨酸、胱氨酸、乙二胺四乙酸、反式-1,2环己二胺四乙酸、尿酸、吡啶甲酸、次氮基三乙酸、羟基乙叉二膦酸、乙二胺-N,N’-二琥铂酸、谷氨酸、二乙烯三胺五乙酸、羟乙基乙二胺三乙酸、亚氨基二乙酸、氨三乙酸、水杨酸、葡萄糖酸、烟酸、酒石酸、柠檬酸、1,4,7,10-四氮杂环十二烷-1,4,7,10-四乙酸、乙二醇四乙酸、1,2-双(邻氨基苯氧基)乙烷-N,N,N’,N’-四乙酸、乙二胺-N,N’-双(2-羟基苯乙酸)、或丙二胺四乙酸中的一种或多种。
14.如权利要求1所述的用于铜大马士革工艺的清洗液,其特征在于,所述有机碱选自季胺氢氧化物、有机胺、或有机醇胺中的一种或多种。
15.如权利要求14所述的用于铜大马士革工艺的清洗液,其特征在于,所述季胺氢氧化物选自四甲基氢氧化铵、四乙基氢氧化铵、三甲基苯基氢氧化铵、四丙基氢氧化铵、四丁基氢氧化铵、苄基三甲基氢氧化铵、苄基三乙基氢氧化铵、胆碱氢氧化物、氢氧化铵、十二烷基三甲基氢氧化铵、或十六烷基三甲基氢氧化铵中的一种或多种。
16.如权利要求14所述的用于铜大马士革工艺的清洗液,其特征在于,所述有机胺选自单乙胺、二乙胺、三乙胺、三丙胺、N'N-二乙基乙二胺、羟乙基乙二胺、环己胺、1,2-丙二胺、或五甲基二乙烯三胺中的一种或多种。
17.如权利要求14所述的用于铜大马士革工艺的清洗液,其特征在于,所述有机醇胺选自单乙醇胺、二乙醇胺、三乙醇胺、二甘醇胺、异丙醇胺、或N-甲基乙醇胺中的一种或多种。
18.如权利要求1所述的用于铜大马士革工艺的清洗液,其特征在于,所述有机碱的金属离子的含量<50ppb。
19.如权利要求1所述的用于铜大马士革工艺的清洗液,其特征在于,所述表面张力调节剂为极性有机物一元醇和/或极性有机物醚类,所述极性有机物醚类的结构通式为R-O-R、R-O-R'、Ar-O-R、Ar-O-Ar或Ar-O-Ar',其中,R=烃基,R'=烃基,Ar=芳烃基,Ar'=芳烃基。
20.如权利要求19所述的用于铜大马士革工艺的清洗液,其特征在于,所述极性有机物一元醇选自甲醇、乙醇、正丙醇、异丙醇、正丁醇、异丁醇、二级丁醇、三级丁醇、新戊醇、环己醇、辛醇、苯甲醇、香茅醇、或橙花醇中的一种或多种。
21.如权利要求19所述的用于铜大马士革工艺的清洗液,其特征在于,所述极性有机物醚类选自乙醚、丙二醇甲醚、二丙二醇甲醚、丙二醇苯醚、甲基叔丁醚、四氢呋喃、环氧乙烷、苯甲醚、1,2-环氧丙烷、1,4-二氧六环、甲基烯丙基醚、正丙醚、或丁基缩水甘油醚中的一种或多种。
22.如权利要求1所述的用于铜大马士革工艺的清洗液,其特征在于,所述金属缓蚀剂为唑类杂环化合物。
23.如权利要求22所述的用于铜大马士革工艺的清洗液,其特征在于,所述唑类杂环化合物选自苯并三氮唑、1,2,4-三氮唑、5-甲基苯并三氮唑、羟基苯并三唑、吡唑、甲苯三唑、3,5-二甲基吡唑、四氮唑、4-氨基-1,2,4-三唑、苯并噻唑、甲基-1H-苯并三唑、2-氨基苯并噻唑、2-巯基苯并噻唑、3-氨基-5-羟基吡唑、1-苯基吡唑、巯基苯并咪唑、5-氨基四唑、3-巯基-1,2,4-三唑、3-异丙基-1,2,4-三唑、2-(5-氨基-戊基)-苯并三唑、5-苯硫醇-苯并三唑、甲基四唑、5-苯基-苯并三唑、5-硝基-苯并三唑、3-氨基-5-巯基-1,2,4-三唑、1-氨基-1,2,4三唑、羟苯并三唑、1-氨基-1,2,3-苯并三唑、或噻唑中的一种或多种。
24.如权利要求1所述的用于铜大马士革工艺的清洗液,其特征在于,所述有机酸铵盐选自甲酸铵、草酸铵、乳酸铵、酒石酸铵、柠檬酸三铵、乙酸铵、氨基甲酸铵、碳酸铵、苯甲酸铵、乙二胺四乙酸四铵、乙二胺四乙酸三铵、乙二胺四乙酸二铵、琥珀酸铵、1-H-吡唑-3-甲酸铵、丙二酸铵、己二酸铵、或亚氨基二乙酸铵中的一种或多种。
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