CN101171551B - 用于清除蚀刻后和灰化的光致抗蚀剂残余物及大部分光致抗蚀剂的组合物 - Google Patents
用于清除蚀刻后和灰化的光致抗蚀剂残余物及大部分光致抗蚀剂的组合物 Download PDFInfo
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
- H01L21/02068—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers
- H01L21/02071—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers the processing being a delineation, e.g. RIE, of conductive layers
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- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
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- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/34—Imagewise removal by selective transfer, e.g. peeling away
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K13/00—Etching, surface-brightening or pickling compositions
- C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
- C09K13/06—Etching, surface-brightening or pickling compositions containing an inorganic acid with organic material
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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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- C11D7/08—Acids
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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
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
- C11D7/5004—Organic solvents
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- G—PHYSICS
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- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/42—Stripping or agents therefor
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Abstract
本发明提供了用于清洁微电子基板的清洁组合物，所述清洁组合物基本上可以完全清洁这些基板并抑制金属的腐蚀或使这些基板的金属元素基本上无腐蚀，且与现有技术含碱性的清洁组合物相比需要相对短的清洁时间和相对低的温度。本发明还提供了使用此清洁组合物清洁微电子基板而不产生任何此微电子基板金属元素的明显腐蚀的方法。本发明的清洁组合物包括(a)至少一种有机溶剂，(b)至少一种未中和的含磷的无机酸，和(c)水。任选地本发明的清洁组合物可以含有其他成分，如表面活性剂、金属配合或螯合剂、腐蚀抑制剂等。本发明的清洁组合物的特征为不含有机胺、羟胺或其他会中和含磷的无机酸成分的强碱，如铵碱等。本发明清洁和去除残余物的组合物尤其适合于清洁含有铝、钛和钨的微电子基板。
Description
技术领域
本发明涉及清除蚀刻后(post-etch)和/或光致抗蚀剂灰化残余物的方法和用于清洁微电子基板(尤其是含有微电子成分的铝和钛)的清洁组合物。当用于清洁此微电子基板及随后的水洗时，本发明的组合物提高了的对金属的保护，即抑制腐蚀。
背景技术
在微电子领域，已经建议使用许多光致抗蚀剂剥离剂和残余物清洁剂作为生产线下游或后端的清洁剂。在生产过程中，光致抗蚀剂的薄膜沉积在基板物质上，然后在薄膜上成像电路图案。烘焙后，用光致抗蚀剂展开剂清除暴露的抗蚀剂。然后，经过等离子蚀刻气体或化学蚀刻溶液，将所得图案转印到下层物质，所述下层物质一般为电介质或金属。蚀刻气体或化学蚀刻溶液选择性地蚀刻基板未被光致抗蚀剂保护的区域。离子蚀刻方法的结果是，在基板和光致抗蚀剂的蚀刻口(通路)的边上和周围沉积了光致抗蚀剂和蚀刻材料副产物作为残余物。
另外，蚀刻步骤中止后，必须将抗蚀剂掩模从基板被保护的区域清除使下步操作能够进行。这可以通过使用合适的离子灰化气体或湿化学剥离剂在离子灰化步骤中完成。找到一种用于清除这些抗蚀剂掩模材料而对金属电路无不良影响(如腐蚀、蚀刻或钝化)的适合的组合物已经证实是有问题的。
随着微电子制造的集成水平提高，和图案化的微电子仪器的尺寸的降低，提供合适的光致抗蚀剂剥离剂和清洁组合物已经变得越来越困难，所述光致抗蚀剂剥离剂和清洁组合物提供合适的剥离和清洁性质而不产生其他不利影响。在半导体和平板显示器领域，在光致抗蚀剂剥离、残余物清除和水洗期间，金属腐蚀问题是严重的缺点，尤其是使用选自如铝、钛和钨的金属和合金时。
用于微电子应用的一般残余物清除剂可以是含碱性的组合物，所述组合物包括与有机胺或羟胺或其他一般在有机溶剂或其他溶剂化物中的强碱混合的极性有机溶剂，以减少对金属和电介质的攻击或腐蚀。已经表明胺、羟胺和其他强碱增加了去除溶剂混合物中的光致抗蚀剂和残余物的效力。然而，此碱性灰化残余物的去除制剂从空气中吸收二氧化碳，此吸收在大多数情况下缩短清洁剂溶液的有效洗涤时间。而且，这些碱性清洁剂组合物反应相对较慢，并要求基板在升高的温度下保持在清洁剂溶液中很长时间。而且，在去除剂之后的水漂洗可以产生强碱水溶液，且此强碱水溶液可以导致相当程度的金属从压花线上的损失，尤其是对碱性水溶液腐蚀非常敏感的铝。媒介洗涤(一般与异丙醇)增加了不希望的时间、安全因素、环境后果及操作步骤的成本。
因此，有了对用于光致抗蚀剂和残余物的剥离和清洁组合物的需要，使能够完全清除来自微电子基板的蚀刻和/或灰化残余物，以及大块光致抗蚀剂，尤其是对这样不产生任何明显的金属腐蚀的清洁剂和残余物清除组合物的需要。
发明概述
本发明提供了用于清洁微电子基板的清洁组合物，所述组合物能够基本上完全清洁此基板，并抑制金属腐蚀或使这些基板的金属元素基本上无腐蚀，且与现有技术含碱性的清洁组合物相比需要相对短的清洁时间和相对低的温度。本发明还提供了使用此清洁组合物清洁微电子基板而不产生任何此微电子基板金属元素的明显腐蚀的方法。本发明的清洁组合物包括(a)至少一种水溶性或可与水混合的有机溶剂，(b)至少一种未中和的含磷的无机酸，和(c)水。任选地本发明的清洁组合物可以含有其他成分，如表面活性剂、金属配合或螯合剂、腐蚀抑制剂等。本发明的清洁组合物的特征为不含有机胺、羟胺或其他会中和含磷的无机酸成分的强碱。本发明清洁和去除残余物的组合物尤其适合于清洁含有铝、钛和钨的微电子基板。
发明详述及优选实施方案
本发明提供了用于清洁微电子基板的清洁组合物，所述组合物能够基本上完全清洁此基板，并抑制金属腐蚀或使这些基板的金属元素基本上无腐蚀。本发明还提供了使用此清洁组合物清洁微电子基板而不产生任何此微电子基板金属元素的明显腐蚀的方法。本发明的清洁组合物包括(a)至少一种有机溶剂，(b)至少一种未中和的含磷的无机酸，和(c)水。
本发明的清洁组合物含有一种或多种适合的水溶性或可与水混合的有机溶剂。在多种有机溶剂中，适合的有醇、多羟基醇例如丙三醇、二醇例如丙二醇和二甘醇、乙二醇醚例如2-(2-乙氧基乙氧基)乙醇(卡必醇)、烷基吡咯烷酮例如N-甲基吡咯烷酮(NMP)、1-羟基烷基-2-吡咯烷酮例如1-(2-羟基乙基)-2-吡咯烷酮(HEP)、二甲基甲酰胺(DMF)、二甲基乙酰胺(DMAC)、砜例如环丁砜、及亚砜例如二甲基亚砜(DMSO)。有机溶剂优选为极性有机溶剂。优选的水溶性有机溶剂为二甘醇、丙二醇、N-甲基吡咯烷酮、环丁砜、DMSO和二甲基乙酰胺。基于组合物的重量，本发明的清洁组合物含有一种或多种有机溶剂的量一般为约35％到约95％，优选从约60％到约90％，更优选为约75％到约85％。
本发明的清洁组合物含有一种或多种未中和的含磷的无机酸。任何合适的未中和的含磷的无机酸均可用于本发明。这些未中和的含磷的无机酸的实例包括但不限于亚磷酸(H3PO3)、次磷酸(H3PO2)和磷酸(H3PO4)。清洁组合物中的未中和的含磷的无机酸以下述有机溶剂成分对未中和的含磷的无机酸成分的重量比例存在于清洁组合物中：从约3∶1到约40∶1，优选为从约3∶1到约20∶1，且更优选为从约4∶1到10∶1。
基于组合物的重量，本发明的清洁组合物的水成分可以以下述量存在：从约3％到约60％，优选为从5％到50％，且更优选为从约5％到约10％。一般而言，由于未中和的含磷的无机酸通常作为含水溶液使用，所以水成分将作为未中和的含磷的无机酸部分加入到清洁组合物中。然而，除酸成分外，水可以作为单独的成分加入。
本发明的组合物还可含有任何合适的水溶性两性，非离子型、阳离子型或阴离子型表面活性剂。加入表面活性剂将降低制剂的表面张力并改善被清洁表面的润湿性并因此提高了组合物的清洁作用。如果需要进一步抑制铝的腐蚀，还可以加入表面活性剂以降低铝的腐蚀速率。而且，表面活性剂的性质可以辅助粒子的分散，促进更好的清洁。本发明的组合物可以使用任何合适的两性，阳离子或非离子型表面活性剂中。具体合适的表面活性剂的实例包括，但不限于：3，5-二甲基-1-己炔-3-醇(Surfynol-61)、乙氧基化的2，4，7，9-四甲基-5-癸炔-4，7-二醇(Surfynol-465)、聚四氟乙烯十六烷氧基丙基甜菜碱(cetoxypropylbetaine)(Zonyl FSK)、Zonyl FSH、Triton X-100(即辛基苯氧聚乙氧基乙醇)等。一般根据对组合物的重量分数，加入的表面活性剂的量从0到约5wt％，优选为0.001到约3wt％。
本发明的清洁组合物还可以任选含有其他成分，包括但不限于在微电子清洁组合物中使用的腐蚀抑制剂和类似的非腐蚀成分。这些化合物还包括儿茶酚、间苯二酚、没食子酸、没食子酸丙酯、连苯三酚、氢醌、苯并三唑衍生物、和多官能团羧酸，例如柠檬酸、酒石酸、葡萄糖酸、葡糖二酸、甘油酸、草酸、邻苯二甲酸、马来酸、扁桃酸、丙二酸、乳酸和水杨酸。
不需要有机或无机螯合或金属络合剂，但是当将其加入到本发明的组合物中时，其可以提供重要的益处，例如提高产品的稳定性、清洁力和抗防腐蚀性。合适的螯合或络合剂的实例包括但不限于：反-1，2-环己二胺四乙酸(CyDTA)、乙二胺四乙酸(EDTA)、焦磷酸盐、亚烷基-二膦酸衍生物(如1-羟基乙烷-1，1-二膦酸盐(HEDPA))。基于组合物的重量，在组合物中存在的螯合剂的量为0到约5wt％，优选为从约0.1到约2wt％。
在一个本发明的优选实施方案中，清洁组合物含有次磷酸和水，以及N-甲基吡咯烷酮、环丁砜、二甘醇，和DMSO中的一种或多种。在另一个优选实施方案中，此清洁组合物含有亚磷酸和水，以及N-甲基吡咯烷酮、环丁砜、二甘醇，和DMSO中的一种或多种。
在本发明的另一方面，本发明包括清洁微电子基板的方法，此基板包含光致抗蚀剂聚合材料、残余物(如灰化或蚀刻残余物)、和金属组成的层，此方法包括将基板与清洁组合物接触足够时间以清洁基板，其中清洁组合物含有下述成分：
a.至少一种水溶性或可与水混合的有机溶剂，
b.至少一种未中和的含磷的无机酸，和
c.水，
其中所述组合物不含有机胺、羟胺和会中和含磷无机酸成分的强碱。所述方法尤其适合于清洁含有多金属层的微电子基板，特别是有铝、钛和钨金属存在的基板。
本发明的组合物，它们用于清洁微电子基板的用途和它们无金属腐蚀的性质通过下述实施例说明，但不限于下述实施例。
下述实施例和表格使用下述缩写。
NMP＝N-甲基吡咯烷酮
DEG＝二甘醇
DMSO＝二甲基亚砜
PG＝丙二醇
DMAC＝二甲基乙酰胺
HPA＝次磷酸
PA＝亚磷酸
HEDPA＝1-羟基乙烷-1，1-二膦酸
实施例1-7
通过将微电子设备浸入本发明的组合物中，检测本发明的组合物清洁微电子设备的能力，该基板中含有Al/TiN(铝/钛氮化物)层，所述Al/TiN层已经用光致抗蚀剂包被，暴露(exposed)、显像、硬蚀刻和灰化产生了富钛通道，这些通道一般非常难在低温下清洁。将样品基板在45℃下浸入到清洁组合物中10分钟，然后用DI水冲洗1分钟。表1中的结果证明了本发明组合物的清洁和相对无腐蚀的性质。
表1
| 组合物 | 溶剂 | ％ | 酸 | ％ | ％水 | ％清洁 | ％蚀刻 |
| 1 | NMP | 83.3 | HPA | 8.3 | 8.3 | 90 | 5 |
| 2 | NMP | 83.3 | PA | 8.3 | 8.3 | 70 | 20 |
| 3 | DMSO | 83.3 | HPA | 8.3 | 8.3 | 70 | 20 |
| 4 | 环丁砜 | 83.3 | HPA | 8.3 | 8.3 | 70 | 20 |
| 5 | 环丁砜 | 40 | HPA | 1 0 | 50 | 80 | 10 |
| 6 | DEG | 83.3 | HPA | 8.3 | 8.3 | 90 | 5 |
| 7 | DEG | 90 | HPA | 4.5 | 4.5 | 70 | 10 |
实施例8-17
通过将微电子设备浸入本发明的组合物中，检测本发明的组合物清洁微电子设备的能力，该基板中含有Al/TiN(铝/钛氮化物)层，所述Al/TiN层已经用光致抗蚀剂包被，暴露、显像、硬蚀刻和灰化产生了金属线，这些金属线一般比实施例1-7中的通道更容易清洁。将样品基板在65℃下浸入到清洁组合物中20分钟，然后用DI水冲洗1分钟。表2中的结果证明了本发明组合物的清洁和相对无腐蚀的性质，尤其在选择添加剂存在时。
表2
| 组合物 | 溶剂 | ％ | ％HPA | ％水 | ％HEDPA | 清洁 | 蚀刻 |
| 8 | DMSO | 77 | 3.8 | 10 | 9.2 | 100％ | 0％ |
| 9 | DMSO | 83 | 4.2 | 7.8 | 5 | 100％ | 10％ |
| 10 | NMP | 86 | 2.2 | 6.6 | 5.2 | 90％ | 0％ |
| 11 | NMP | 77 | 3.8 | 10 | 9.2 | 100％ | 10％ |
| 12 | NMP | 86 | 4.3 | 7.1 | 2.6 | 100％ | 50％ |
| 13 | NMP | 83 | 4.2 | 7.8 | 5 | 100％ | 20％ |
| 14 | PG | 83 | 4.2 | 7.8 | 5 | 100％ | 20％ |
| 15 | DMAC | 71.4 | 7.1 | 13 | 8.5 | 100％ | 20％ |
| 16 | DMAC | 90.1 | 2.3 | 4.9 | 2.7 | 70％ | 20％ |
| 17 | DMSO | 77 | 3.8(PA) | 10 | 9.2 | 100％ | 0％ |
虽然本发明在此描述参考其具体的实施例，但是在不背离在此公开的本发明的精神和范围内，可以对本发明进行改变、更改和变化。因此，本发明将包含落入要求保护的权利要求的精神和范围内的所有改变、更改和变化。
Claims (14)
1.用于清洁微电子基板的组合物，其基本上由下列成分组成：
(a)至少一种水溶性或可与水混合的有机溶剂，
(b)至少一种未中和的含磷的无机酸，和
(c)水，
且任选
(d)至少一种表面活性剂，
(e)至少一种腐蚀抑制剂，和
(f)至少一种金属络合剂；
其中所述组合物不含有机胺、羟胺和会中和含磷无机酸成分的强碱，其中水溶性或可与水混合的有机溶剂占组合物重量的35％到95％，且有机溶剂成分与未中和的含磷无机酸的重量比例范围为3∶1到40∶1。
2.如权利要求1的组合物，其中基于组合物的重量，组合物中含有的水的量为5％到10％。
3.如权利要求1的组合物，其中未中和的含磷的无机酸包括选自下列的酸：亚磷酸(H3PO3)、次磷酸(H3PO2)和磷酸(H3PO4)。
4.如权利要求3的组合物，其中水溶性或可与水混合的有机溶剂成分选自N-甲基吡咯烷酮、环丁砜、二甲亚砜、二甘醇、丙二醇和二甲基乙酰胺。
5.如权利要求3的组合物，其中未中和的含磷的无机酸包括亚磷酸(H3PO3)。
6.如权利要求3的组合物，其中未中和的含磷的无机酸包括次磷酸(H3PO2)。
7.如权利要求1的组合物，其中含有作为络合剂的1-羟基乙烷-1，1-二膦酸。
8.一种清洁微电子基板的方法，所述基板含有光致抗蚀剂聚合材料、残余物和金属，该方法包括使基板与清洁组合物接触足够的时间以清洁基板，其中所述清洁组合物基本上由下列成分组成：
(a)至少一种水溶性或可与水混合的有机溶剂，
(b)至少一种未中和的含磷的无机酸，和
(c)水，
且任选
(d)至少一种表面活性剂，
(e)至少一种腐蚀抑制剂，和
(f)至少一种金属络合剂；
其中所述组合物不含有机胺、羟胺和会中和含磷无机酸成分的强碱，其中水溶性或可与水混合的有机溶剂占组合物重量的35％到95％、且有机溶剂成分与未中和的含磷无机酸的重量比例范围为3∶1到40∶1。
9.如权利要求8的方法，其中基于组合物的重量，组合物中含有的水的量为5％到10％。
10.如权利要求8的方法，其中未中和的含磷的无机酸包括选自下列的酸：亚磷酸(H3PO3)、次磷酸(H3PO2)和磷酸(H3PO4)。
11.如权利要求10的方法，其中水溶性或可与水混合的有机溶剂成分选自N-甲基吡咯烷酮、环丁砜、二甲亚砜、二甘醇、丙二醇和二甲基乙酰胺。
12.如权利要求10的方法，其中未中和的含磷的无机酸包括亚磷酸(H3PO3)。
13.如权利要求10的方法，其中未中和的含磷的无机酸包括次磷酸(H3PO2)。
14.如权利要求8的方法，其中含有作为络合剂的1-羟基乙烷-1，1-二膦酸。
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| US20110056516A1 (en) * | 2007-02-28 | 2011-03-10 | Adair Richard E | Process for surface treatment of metals |
| US20090148335A1 (en) * | 2007-02-28 | 2009-06-11 | Adair Richard E | Process for surface treatment of metals |
| CN101373342B (zh) * | 2008-10-23 | 2011-03-02 | 江阴江化微电子材料股份有限公司 | 一种酸性剥离液及其制备方法 |
| US20110253171A1 (en) * | 2010-04-15 | 2011-10-20 | John Moore | Chemical Composition and Methods for Removing Epoxy-Based Photoimageable Coatings Utilized In Microelectronic Fabrication |
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- 2006-04-18 JP JP2008510018A patent/JP2008541426A/ja active Pending
- 2006-04-18 KR KR1020077025627A patent/KR20080005408A/ko not_active Application Discontinuation
- 2006-04-18 WO PCT/US2006/014466 patent/WO2006121580A2/en active Application Filing
- 2006-04-18 BR BRPI0611377-0A patent/BRPI0611377A2/pt not_active IP Right Cessation
- 2006-04-18 CN CN2006800155059A patent/CN101171551B/zh active Active
- 2006-04-18 CA CA002606849A patent/CA2606849A1/en not_active Abandoned
- 2006-04-18 EP EP06750494.4A patent/EP1883863B1/en not_active Not-in-force
- 2006-04-18 US US11/911,346 patent/US7754668B2/en not_active Expired - Fee Related
- 2006-05-03 TW TW095115752A patent/TWI425323B/zh active
- 2006-05-03 MY MYPI20062030A patent/MY144723A/en unknown
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2007
- 2007-08-16 ZA ZA200706853A patent/ZA200706853B/xx unknown
- 2007-11-01 IL IL187121A patent/IL187121A/en not_active IP Right Cessation
- 2007-11-06 NO NO20075670A patent/NO20075670L/no not_active Application Discontinuation
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| EP0827188A2 (en) * | 1996-08-09 | 1998-03-04 | Mitsubishi Gas Chemical Company, Inc. | Cleaning liquid for producing semiconductor device and process for producing semiconductor device using same |
| EP1035446A2 (en) * | 1999-03-08 | 2000-09-13 | Mitsubishi Gas Chemical Company, Inc. | Resist stripping composition and process for stripping resist |
| US6783695B1 (en) * | 1999-06-29 | 2004-08-31 | Micron Technology, Inc. | Acid blend for removing etch residue |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101171551A (zh) | 2008-04-30 |
| CA2606849A1 (en) | 2006-11-16 |
| TW200702942A (en) | 2007-01-16 |
| BRPI0611377A2 (pt) | 2010-08-31 |
| NO20075670L (no) | 2007-11-06 |
| IL187121A (en) | 2013-06-27 |
| US20080261846A1 (en) | 2008-10-23 |
| IL187121A0 (en) | 2008-02-09 |
| KR20080005408A (ko) | 2008-01-11 |
| JP2008541426A (ja) | 2008-11-20 |
| EP1883863B1 (en) | 2014-01-22 |
| ZA200706853B (en) | 2008-09-25 |
| US7754668B2 (en) | 2010-07-13 |
| TWI425323B (zh) | 2014-02-01 |
| WO2006121580A3 (en) | 2007-02-15 |
| EP1883863A2 (en) | 2008-02-06 |
| WO2006121580A2 (en) | 2006-11-16 |
| MY144723A (en) | 2011-10-31 |
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