CN111315859A - 基于氟化物的清洁组合物 - Google Patents
基于氟化物的清洁组合物 Download PDFInfo
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- CN111315859A CN111315859A CN201880071944.4A CN201880071944A CN111315859A CN 111315859 A CN111315859 A CN 111315859A CN 201880071944 A CN201880071944 A CN 201880071944A CN 111315859 A CN111315859 A CN 111315859A
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Images
Classifications
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- 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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- H—ELECTRICITY
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Abstract
本发明涉及一种清洁组合物,其包含:a)组合物总重量的1‑5重量%的氟化铵;b)组合物总重量的30‑70重量%的水溶性有机溶剂;c)组合物总重量的1.5‑20重量%的有机胺;和d)组合物总重量的31‑60重量%的去离子水。根据本发明的清洁组合物提供了良好的清洁功效,同时是温和的清洁组合物并且具有稳定的pH。
Description
技术领域
本发明涉及适用于半导体晶圆清洁的基于氟化物的清洁组合物。
背景技术
半导体器件诸如集成电路和大规模集成电路、以及液晶面板装置和其他显示面板装置的制造包括以下步骤:在金属层或绝缘层上形成均匀的光致抗蚀剂涂层;进行所需的曝光和显影以形成光致抗蚀剂图案;使用光致抗蚀剂图案作为掩模通过化学气相沉积来(选择性地)蚀刻具有金属层或绝缘层的衬底以形成微电路;和用液体剥离剂(stripper)从衬底上除去不需要的光致抗蚀剂层、蚀刻残留物、残留的光致抗蚀剂和光致抗蚀剂副产物中的一种或多种。已经使用各种有机液体光致抗蚀剂剥离溶液从衬底上去除不需要的光致抗蚀剂层、蚀刻残留物、残留的光致抗蚀剂和光致抗蚀剂副产物。现有技术经常在光致抗蚀剂剥离溶液中使用包含氟化合物诸如氢氟酸的组合物以去除不需要的光致抗蚀剂层。
现有技术中描述的一类光致抗蚀剂剥离溶液主要包含:(a)氢氟酸与不含金属的碱的盐、(b)水溶性有机溶剂、和(c)水,且pH为5至8。与这种溶液有关的问题通常是关于氢氟酸的盐的量,较低的量造成清洁效率差,而较高的量造成溶解性问题。
另一类光致抗蚀剂剥离溶液包含碱性物质以调节溶液的pH。这种类型的组合物的实例包含:(a)氢氟酸与不含金属离子的碱的盐:(b)水溶性有机溶剂;(c)碱性物质;和(d)水。通常,在这种类型的溶液中优选的pH值为8.5至10.0,并且现有技术表明,可以通过少量的0.1-0.3重量%的碱性物质来实现这样的pH值。这种溶液的问题是,用水稀释会显著降低pH值。此外,还存在因水冲洗引起的铝金属腐蚀的问题。
现有技术还公开了一种含有氢氟酸的盐的缓冲清洁组合物。通常,这些组合物的pH为7-11。该pH范围是优选的,因为对TEOS(通过原硅酸四乙酯的化学气相沉积制成的二氧化硅膜)的损害小。该缓冲***有助于pH值的稳定性,但是,当用水稀释清洁组合物时,pH值仍会波动。
因此,仍然需要一种清洁组合物,该清洁组合物提供高清洁效率,同时在用水稀释期间具有稳定的pH值,并且是温和的且不会对介电材料诸如SiO2和金属层诸如铝和铝合金造成损害。
附图说明
图1示出了水与AlCu蚀刻速率(ER)之间的关系。
发明内容
本发明涉及一种清洁组合物,其包含:a)组合物总重量的1-5重量%的氟化铵;b)组合物总重量的30-70重量%的水溶性有机溶剂;c)组合物总重量的1.5-20重量%的有机胺;和d)组合物总重量的31-60重量%的去离子水。
本发明涉及根据本发明的组合物在半导体清洁中的用途。
本发明还包括一种从衬底去除蚀刻残留物、残留光致抗蚀剂和光致抗蚀剂副产物中的一种或多种的方法,其包括以下步骤:使其上存在蚀刻残留物、残留光致抗蚀剂和光致抗蚀剂副产物中的一种或多种的衬底与根据本发明的组合物接触。
具体实施方式
在以下段落中将更详细地描述本发明。除非明确地指出相反,否则这样描述的每个方面可以与任何其他一个或多个方面组合。特别地,指明为优选或有利的任何特征可以与指明为优选或有利的任何其他一个或多个特征组合。
在本发明的上下文中,除非上下文另外指出,否则将根据以下定义来解释所使用的术语。
除非上下文另外明确指出,本文所用的单数形式“一个”、“一种”和“该”包括单数和复数指代物。
本文所用的术语“包含(comprising)”、“包含(comprise)”和“包含(comprisedof)”与“包括(including)”、“包括(include)”或“含有(containing)”、“含有(contain)”同义,并且是包括性的或开放式的且不排除其他未陈述的元件、要素或方法步骤。
数值端点的陈述包括相应范围内包含的所有数值和分数以及所陈述的端点。
除非另外指出,否则本文中提及的所有百分比、份数、比例以及类似物均基于重量。
当以范围、优选的范围、或优选的上限值和优选的下限值的形式表示量、浓度或其他值或参数时,应理解为具体公开了通过将任何上限值或优选值与任何下限值或优选值组合得到的任何范围,而不考虑所得到的范围是否在上下文中明确提及。
本说明书中引用的所有参考文献均通过引用全文并入本文。
除非另有定义,否则用于公开本发明的所有术语,包括技术和科学术语,均具有本发明所属领域的普通技术人员通常所理解的含义。作为进一步的指导,包括术语定义以更好地理解本发明的教导。
本发明涉及一种清洁组合物,其包含:a)组合物总重量的1-5重量%的氟化铵;b)组合物总重量的30-70重量%的水溶性有机溶剂;c)组合物总重量的1.5-20重量%的有机胺;和d)组合物总重量的31-60重量%的去离子水。
根据本发明的清洁组合物包含相对高含量的氟化铵以提供高清洁效率,然而,尽管含量高,氟化铵仍保持可溶。另外,当用水稀释时,根据本发明的清洁组合物具有稳定的pH值。此外,根据本发明的清洁组合物是温和的清洁溶液,并且不会损坏介电材料诸如SiO2以及金属层诸如铝和铝合金。
根据本发明,组合物中氟化铵大于1%被认为是高含量,而组合物中氟化铵小于0.1%被认为是低含量。通常,高氟化铵含量对清洁有好处,但是高含量的氟化铵可能会引起溶解性问题并会损坏金属表面(Al、AlCu、Cu)和介电材料(SiO2)。通常,低氟化铵含量不会造成损害,但是清洁功效受到不利影响。
根据本发明的清洁组合物包含大量的氟化铵。使用氟化铵是因为它有助于实现高浓度的氟阴离子,从而导致高的清洁效率。尽管组合物中氟化铵的含量高,但它不会对Al、AlCu、Cu和SiO2(TEOS)表面造成损害。
适用于本发明的市售氟化铵例如但不限于来自Morita Chemical IndustriesCO.,Ltd.的电子级40%氟化铵溶液和来自Kanto Chemical Co.,Inc.的氟化铵(40%)。
根据本发明的清洁组合物包含组合物总重量的1-5重量%,优选2-4重量%,更优选2.5-3.5重量%的氟化铵。
如果氟化铵的含量小于1%,则清洁效率降低,而当氟化铵的含量大于5%时,则氟化铵不溶于富溶剂溶液。
根据本发明的清洁组合物包含水溶性有机溶剂。合适的水溶性有机溶剂会促进其他成分在清洁组合物中的溶解性,此外,它还提供了良好的清洁效率。
适用于本发明的水溶性有机溶剂选自N-甲基吡咯烷酮(NMP)、二甲基亚砜(DMSO)、甲基二甘醇(MDG)、丁基二甘醇(buthyl diglycol,BDG)、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、γ-丁内酯、乙二醇、丙二醇及它们的混合物,优选所述溶剂选自N-甲基吡咯烷酮(NMP)、二甲基亚砜(DMSO)及它们的混合物。
DMSO是优选的水溶性有机溶剂,因为它促进氟化铵的优异溶解性。DMSO还促进待从表面去除的树脂的溶解性。
在一个实施方案中,根据本发明的清洁组合物包含一种或多种水溶性有机溶剂与DMSO的混合物。对其他水溶性有机溶剂没有特别限制,只要它可与水和DMSO混溶即可。这种水溶性有机溶剂的实例包括但不限于N-甲基吡咯烷酮(NMP)、甲基二甘醇(MDG)、丁基二甘醇(BDG)。优选将N-甲基吡咯烷酮(NMP)与DMSO组合使用,因为它提供良好的清洁效率。
适用于本发明的市售水溶性有机溶剂是例如但不限于来自Toray Fine ChemicalCo.,Ltd.的DMSO、来自Mitsubishi Chemical Corporation的N-甲基-2-吡咯烷酮(NMP)和来自BASF SE的N-甲基-2-吡咯烷酮(蒸馏)。
根据本发明的清洁组合物包含组合物总重量的30-70重量%,优选35-65重量%,更优选45-65重量%,甚至更优选50-61重量%的水溶性有机溶剂。
如果有机溶剂含量小于30%,则组合物相应地富含水,并且会在Al、Cu和AlCu表面上造成损害。而超过70%的过高有机溶剂含量会造成氟化铵的溶解性差。
当使用溶剂DMSO和NMP的组合时,DMSO:NMP的比率优选为99:1至10:90,更优选为50:50至20:80。
根据本发明的清洁组合物包含有机胺。当用水稀释时,有机胺为组合物提供pH稳定性。降低pH值会引起金属诸如铝和铝合金的腐蚀。有机胺促进减少对硅氧化物的损害。此外,有机胺促进氟化铵的溶解性。
适用于本发明的有机胺选自单乙醇胺、二乙醇胺、三乙醇胺、单异丙醇胺、2-(2-氨基乙基氨基)乙醇、2-氨基-2-甲基-1-丙醇、N-甲基乙醇胺、2-(二甲基氨基)乙醇、乙二胺、丙二胺及它们的混合物,优选地,所述有机胺为单乙醇胺、三乙醇胺。
三乙醇胺是优选的有机胺,因为它提供了pH稳定性,并且促进了待从表面除去的树脂的溶胀和溶解。
适用于本发明的市售有机胺为例如但不限于来自BASF SE的三乙醇胺(纯)和单乙醇胺(纯);和来自Dow Chemical Company的三乙醇胺DOWTM和单乙醇胺DOWTM。
根据本发明的清洁组合物包含组合物总重量的1.5-20重量%,优选2-15重量%,更优选2.5-12.5重量%,甚至更优选3.5-5重量%的有机胺。
当有机胺的含量小于1.5%时,当用水稀释该组合物时pH波动,并且TEOS被破坏,而当有机胺的含量大于20%时,组合物对Al和AlCu表面造成损害。
根据本发明的清洁组合物包含水。水提高氟化铵的溶解性和AlCu蚀刻速率。
在根据本发明的组合物中使用的水必须是去离子水,因为金属离子污染对半导体器件的电性能产生负面影响。去离子水的纯度以电阻率为特征。对于适合用于本发明的去离子水,电阻率优选大于15MΩ/cm,更优选大于17MΩ/cm,甚至更优选大于18MΩ/cm。电阻率可以通过使用得自HORIBA Ltd.的HE-480R和得自MyronCompany的Ultrameter IITM来测量。
根据本发明的清洁组合物包含组合物总重量的31-60重量%,优选32-50重量%,更优选32-45重量%,甚至更优选32-40重量%的水。
如果水量少于31%,则氟化铵的溶解度降低,而如果水量超过60%,则组合物将对Al、Cu和AlCu表面造成损害。
根据本发明的组合物可以进一步包含酸。适用于本发明的酸可以是有机酸或无机酸,优选有机酸。
可以将有机酸添加到根据本发明的组合物中以调节pH,以充当pH缓冲剂、腐蚀抑制剂或螯合剂。
适用于本发明的有机酸可以选自甲酸、乙酸、丙酸、丁酸、异丁酸、草酸、丙二酸、琥珀酸、戊二酸、马来酸、富马酸、苯甲酸、邻苯二甲酸、1,2,3-苯三甲酸、乙醇酸、乳酸、苹果酸、柠檬酸、酒石酸及它们的混合物。
根据本发明的组合物可以包含组合物总重量的0.1-10.0重量%,优选0.5-5.0重量%,并且更优选1.0-3.0重量%的有机酸。
适用于本发明的市售有机酸是例如但不限于来自Showa Kako Corporation的柠檬酸一水合物和无水柠檬酸。
根据本发明的清洁组合物可以进一步包含一种或多种另外的组分,所述另外的组分选自表面活性剂,所述表面活性剂选自阴离子表面活性剂、非离子表面活性剂及它们的混合物;腐蚀抑制剂,所述腐蚀抑制剂选自唑化合物、硫醇化合物、糖醇诸如木糖醇和山梨糖醇;和螯合剂。
根据本发明的清洁组合物通过将原料在共混罐中共混而制得。优选地,在共混时将温度控制在低于40℃以避免不希望的副反应和任何原料的蒸发。优选采用封闭***进行共混以避免任何原料的蒸发。
根据本发明的组合物具有8.0至11.0,优选8.5至10.5的pH。在室温下使用玻璃电极法由10%的水溶液和未稀释的溶液测量pH。使用由Horiba,Ltd.制造的pH计(型号:F-51)测量pH。
优选pH为8.0至11.0,因为其在清洁效率与对金属表面(Al、AlCu、Cu)和介电材料(SiO2)的损伤之间提供平衡。如果组合物的pH大于11.0,则清洁效率降低并且造成金属表面损坏。另一方面,如果组合物的pH低于8.0,则对电介质材料(SiO2)造成损害。
根据本发明的组合物可用于半导体清洁中,优选用于半导体批量清洁、半导体批量喷雾清洁、半导体刷洗清洁和半导体单晶圆(single wafer)清洁中,更优选用于半导体单晶圆清洁中。
本发明涉及一种从衬底去除蚀刻残留物、残留光致抗蚀剂和光致抗蚀剂副产物中的一种或多种的方法,其包括以下步骤:使其上存在蚀刻残余物、残余光致抗蚀剂和光致抗蚀剂副产物中的一种或多种的衬底与根据本发明的组合物接触。
实施例
在室温下使用玻璃电极法由10%的水溶液和未稀释的溶液测量pH。使用由Horiba,Ltd.制造的pH计(型号:F-51)测量pH。
由处理时间和在硅晶圆上形成的AlCu膜的厚度损失来确定AlCu蚀刻速率(ER)。通过使用由Napson Corporation制造的RT-70四点探针来测量AlCu膜的厚度。在确定初始AlCu厚度后,将测试晶圆浸入25℃的测试溶液中。30分钟后,从测试溶液中取出测试晶圆,用去离子水冲洗3分钟,并且在氮气下完全干燥。然后,测量AlCu厚度以确定由于浸入测试溶液中而造成的厚度损失。
由处理时间和在硅晶圆上形成的TEOS膜的厚度损失来确定TEOS蚀刻速率(ER)。通过使用由Otsuka electronics co.Ltd.制造的光学厚度监测仪(型号:FE-3000)来测量TEOS膜的厚度。在确定初始TEOS厚度后,将测试晶圆浸入25℃的测试溶液中。30分钟后,从测试溶液中取出测试晶圆,用去离子水冲洗3分钟,并且在氮气下完全干燥。然后,测量TEOS厚度以确定由于浸入测试溶液中而造成的厚度损失。
AlCu涂布的晶圆:向晶圆涂布300nm市售的气相沉积的AlCu合金(Al:99.5%,Cu:0.5%)膜。
TEOS涂布的晶圆:向晶圆涂布100nm通过市售的原硅酸四乙酯的化学气相沉积制得的二氧化硅膜。
将涂布的晶圆切成2.5cm×2.5cm的小块,并浸入25℃的测试溶液中。
表1举例说明了在实施例1-8中的根据本发明的清洁组合物。所有这些实施例均具有高浓度的氟化铵和稳定的pH值,此外,所有组合物均未损坏TEOS和AlCu表面。
图1示出了水与AlCu蚀刻速率(ER)之间的关系。图1包含对比例14和实施例1-5的组合物的AlCu ER数据。
如图1所示,对比例14的AlCu ER出乎意料地高。此外,AlCu ER随着水浓度的增加突然降低。表明本发明的水浓度非常重要。
表1
实施例 | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 |
氟化铵 | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 |
DMSO | 30 | 29 | 26.5 | 24 | 19 | 20 | 20 | 20 |
NMP | 30 | 29 | 26.5 | 24 | 19 | 40 | 38 | 32.5 |
TEA | 4.5 | 4.5 | 4.5 | 4.5 | 4.5 | 2.5 | 4.5 | 10 |
水 | 32.5 | 34.5 | 39.5 | 44.5 | 54.5 | 34.5 | 34.5 | 34.5 |
溶解性 | 可溶 | 可溶 | 可溶 | 可溶 | 可溶 | 可溶 | 可溶 | 可溶 |
pH | 8.9 | 8.9 | 8.9 | 8.8 | 8.8 | 8.8 | 8.9 | 9.1 |
pH 10% | 8.4 | 8.4 | 8.4 | 8.4 | 8.4 | 8.2 | 8.4 | 8.6 |
AlCu ER(A/min) | 8.3 | 3.7 | 2.2 | 1.9 | 3.7 | 6.8 | 4.8 | 3.7 |
TEOS ER(A/分钟) | 2.3 | 1.5 | 0.4 | 0.2 | 0.2 | 3 | 1.7 | 1.1 |
表2举例说明了清洁组合物的对比例(5-10)。这些实施例具有以下问题,诸如氟化铵的溶解性、pH稳定性、AlCu或TEOS(通过原硅酸四乙酯的化学气相沉积制成的二氧化硅膜)蚀刻速率。
表2
对比例 | 9 | 10 | 11 | 12 | 13 | 14 |
氟化铵 | 3 | 3 | 3 | 3 | 1 | 3 |
DMSO | 70 | 33.5 | 20 | 20 | 70 | 31.25 |
NMP | 33.5 | 42.5 | 42.4 | 31.25 | ||
TEA | 0 | 0.1 | 4.5 | |||
水 | 27 | 30 | 34.5 | 34.5 | 29 | 30 |
溶解性 | 不溶 | 不溶 | 可溶 | 可溶 | 可溶 | 可溶 |
pH | - | - | 8.3 | 8.4 | 9 | |
pH 10% | - | - | 6.0 | 7.1 | 8.5 | |
AlCu ER | 15.2 | 13.9 | ||||
TEOS ER | 8.8 | 9.9 | 9.2 | 3.9 |
Claims (11)
1.清洁组合物,其包含:
a)组合物总重量的1-5重量%的氟化铵;
b)组合物总重量的30-70重量%的水溶性有机溶剂;
c)组合物总重量的1.5-20重量%的有机胺;和
d)组合物总重量的31-60重量%的去离子水。
2.根据权利要求1所述的组合物,其中所述组合物包含组合物总重量的2-4重量%、优选2.5-3.5重量%的氟化铵。
3.根据权利要求1或2所述的组合物,其中所述水溶性有机溶剂选自N-甲基吡咯烷酮、二甲基亚砜、甲基二甘醇、丁基二甘醇、N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、γ-丁内酯、乙二醇、丙二醇及它们的混合物,优选所述溶剂选自N-甲基吡咯烷酮、二甲基亚砜及它们的混合物。
4.根据权利要求1至3中任一项所述的组合物,其中所述组合物包含组合物总重量的35-65重量%、优选45-65重量%、更优选50-61重量%的水溶性有机溶剂。
5.根据权利要求1至4中任一项所述的组合物,其中所述有机胺选自单乙醇胺、二乙醇胺、三乙醇胺、单异丙醇胺、2-(2-氨基乙基氨基)乙醇、2-氨基-2-甲基-1-丙醇、N-甲基乙醇胺、2-(二甲基氨基)乙醇、乙二胺、丙二胺及它们的混合物,优选所述有机胺是三乙醇胺。
6.根据权利要求1至5中任一项所述的组合物,其中所述组合物包含组合物总重量的2-15重量%、优选2.5-12.5重量%、更优选3.5至5重量%的有机胺。
7.根据权利要求1至6中任一项所述的组合物,其中所述组合物包含组合物总重量的32-50重量%、优选32-45重量%、更优选32-40重量%的去离子水。
8.根据权利要求1至7中任一项所述的组合物,其进一步包含选自以下的有机酸:甲酸、乙酸、丙酸、丁酸、异丁酸、草酸、丙二酸、琥珀酸、戊二酸、马来酸、富马酸、苯甲酸、邻苯二甲酸、1,2,3-苯三甲酸、乙醇酸、乳酸、苹果酸、柠檬酸、酒石酸、葡萄糖酸、乙醛酸、没食子酸及它们的混合物。
9.根据权利要求1至8中任一项所述的组合物,其pH为8.0至11.0,优选为8.5至10.5。
10.根据权利要求1至9中任一项所述的组合物的用途,其用于半导体清洁中,优选用于半导体批量清洁、半导体批量喷雾清洁、半导体刷洗清洁和半导体单晶圆清洁中,更优选用于半导体单晶圆清洁中。
11.从衬底去除蚀刻残留物、残留光致抗蚀剂和光致抗蚀剂副产物中的一种或多种的方法,其包括以下步骤:
使其上存在蚀刻残留物、残留光致抗蚀剂和光致抗蚀剂副产物中的一种或多种的衬底与根据权利要求1至9中任一项所述的组合物接触。
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