CN101972755A - Ulsi铜材料抛光后表面清洗方法 - Google Patents
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000004140 cleaning Methods 0.000 title claims abstract description 38
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 38
- 239000010949 copper Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 title abstract description 5
- 230000010354 integration Effects 0.000 title abstract 2
- 238000005498 polishing Methods 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 239000003112 inhibitor Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 239000012530 fluid Substances 0.000 claims description 18
- 239000004094 surface-active agent Substances 0.000 claims description 13
- 239000002738 chelating agent Substances 0.000 claims description 12
- 230000007797 corrosion Effects 0.000 claims description 10
- 238000005260 corrosion Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- BYACHAOCSIPLCM-UHFFFAOYSA-N 2-[2-[bis(2-hydroxyethyl)amino]ethyl-(2-hydroxyethyl)amino]ethanol Chemical compound OCCN(CCO)CCN(CCO)CCO BYACHAOCSIPLCM-UHFFFAOYSA-N 0.000 claims description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 2
- 229960001484 edetic acid Drugs 0.000 claims description 2
- 239000013522 chelant Substances 0.000 abstract description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 1
- 239000002736 nonionic surfactant Substances 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 230000003628 erosive effect Effects 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 239000006061 abrasive grain Substances 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- DYUQAZSOFZSPHD-UHFFFAOYSA-N Phenylpropyl alcohol Natural products CCC(O)C1=CC=CC=C1 DYUQAZSOFZSPHD-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229960004011 methenamine Drugs 0.000 description 2
- -1 phenylpropyl alcohol triazole Chemical class 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 206010057040 Temperature intolerance Diseases 0.000 description 1
- AYSYSOQSKKDJJY-UHFFFAOYSA-N [1,2,4]triazolo[4,3-a]pyridine Chemical compound C1=CC=CN2C=NN=C21 AYSYSOQSKKDJJY-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- 238000010504 bond cleavage reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000008543 heat sensitivity Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Classifications
-
- 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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/72—Ethers of polyoxyalkylene glycols
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
-
- 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/0073—Anticorrosion compositions
-
- 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/33—Amino carboxylic acids
-
- 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
- H01L21/02074—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers the processing being a planarization of conductive layers
-
- C11D2111/22—
Abstract
本发明涉及一种ULSI铜材料抛光后表面清洗方法,具体步骤如下:制备清洗液,按重量%计:非离子型表面活性剂1-4%、FA/OII型螯合剂0.5-3%、FA/OII型阻蚀剂0.1-5%、余量去离子水;混合搅拌均匀后制备成pH值为7.4-8.2水溶性表面清洗液;使用步骤(1)制备的清洗液对碱性化学机械抛光后的铜材料在2000Pa-3000Pa的低压力、1000-5000ml/min的流量条件下进行抛光清洗,抛光清洗时间至少为0.5-2分钟,以使铜材料表面洁净。采用该清洗方法有益效果是:清洁分布不均的抛光液被迅速冲走,可获得洁净、完美的抛光表面。该方法操作简单,不需添加其它设备,成本低、效率高、无污染,可明显改善器件性能,提高成品率。
Description
技术领域
本发明涉及半导体材料的清洗方法,特别涉及一种ULSI铜材料抛光后表面清洗方法。
背景技术
集成电路密度的增加和器件尺寸的减小使线间电容及金属连线的电阻增大,由此引起的RC延迟也增大。金属铜具有低的电阻率、优越的抗电迁移特性和低的热敏感性,产生较小的RC延迟并能提高电路的可靠性,铜线取代传统的铝线成为互连线的理想材料。
铜CMP成为ULSI制备中倍受世界各国关注的核心技术之一,世界各国都在加紧对其进行封闭研究,以期优先占领国际市场。目前,铜批量抛光生产后,CMP工序中的抛光工艺完成后,铜材料表面原子刚刚断键,表面能很高,极易吸附小颗粒而降低自身表面能。因此,抛光液中的磨料颗粒容易吸附在铜表面,颗粒周围残留的抛光液表面张力大呈小球状分布在铜表面而继续与铜发生化学反应,极易造成腐蚀不均匀,表面一致性较差。从而造成后续加工中成本的提高及器件成品率的降低。
发明内容
本发明的目的在于克服上述不足之处,提供一种简便易行、无污染、洁净的铜材料抛光后表面清洗方法,解决了铜材料抛光后铜表面能量高、表面张力大、残留抛光液分布不均、沾污金属离子的问题。
为实现上述目的本发明所采用的实施方式如下:一种ULSI铜材料抛光后表面清洗方法,其特征在于:具体实施步骤如下,以下按重量%计:
(1)制备清洗液:
将表面活性剂1-4%、FA/OII型螯合剂0.5-3%、FA/OII型阻蚀剂0.1-5%、余量去离子水,混合搅拌均匀后制备成pH值为7.4-8.2的水溶性表面清洗液;
(2)使用步骤(1)中制备的清洗液对碱性化学机械抛光后的铜材料在2000Pa-3000Pa低压力下、1000-5000ml/min的大流量条件下进行抛光清洗,抛光清洗时间至少0.5-2分钟。
所述步骤(1)采用的表面活性剂为市售的FA/OI型表面活性剂、Oπ-7((C10H21-C6H4-O-CH2CH2O)7-H)、Oπ-10((C10H21-C6H4-O-CH2CH2O)10-H)、O-20(C12-18H25-37-C6H4-O-CH2CH2O)70-H)、JFC的一种。
所述步骤(1)采用的螯合剂为市售FA/OII型螯合剂:乙二胺四乙酸四(四羟乙基乙二胺)其结构式如下:
所述步骤(1)采用的阻蚀剂为天津晶岭微电子材料有限公司市售FA/OII型阻蚀(氧)剂,为乌洛托品(六亚甲基四胺)和苯丙三氮唑(连三氮杂茚)的复合物,其中所述乌洛托品分子式为C6H12N4,结构式为:
所述苯丙三氮唑分子式为C6H5N3,结构式为:
本发明的有益效果是:CMP工序中的抛光工艺后立即使用清洗液对铜材料进行大流量清洗,清洁分布不均的抛光液被迅速冲走,可获得洁净、完美的抛光表面。选用表面活性剂可使抛光后表面高的表面张力迅速降低,减少损伤层,提高表面质量的均匀性;选用的螯合剂可与对表面残留的金属离子发生反应,生成可溶性的大分子螯合物,在大流量水抛液作用下脱离表面;选用的阻蚀剂可在抛光后表面形成单分子钝化膜,阻止表面不均匀分布的抛光液继续与基体反应,提高抛光后表面的完美性。
该方法在抛光工艺后立即使用清洗液对铜材料进行大流量清洗,能有效解决现有技术存在问题:(1)低压、大流量水抛液清洗无滞后时间,既能有效优化、降低铜表面粗糙度,又能快速将铜表面吸附的磨料颗粒冲走;(2)清洗液中添加非离子表面活性剂能有效降低铜表面残留抛光液的表面张力的同时,优先吸附在铜表面形成活性剂单分子层,有效保护铜材料,避免磨料颗粒周围非均匀腐蚀产生的腐蚀圈;(3)清洗液可使铜材料表面分布不均的残留抛光液被迅速冲走,可获得洁净、完美的抛光表面。
总之,该方法操作简单,不需添加其它设备,成本低、效率高、无污染,可明显改善器件性能,提高成品率。
具体实施方式
以下结合较佳实施例,对依据本发明提供的具体实施方式详述如下:
实施例1:
在18MΩ超纯去离子水1912g中分别加入FA/O表面活性剂20g、FA/OII型螯合剂60g、FA/OII型阻蚀(氧)剂8g,边加入边搅拌均匀,搅拌均匀后制备成2000g pH值为7.4-8.2水溶性表面清洗液;利用制备好的清洗液对碱性化学机械抛光后的铜材料在3000Pa的低压力、5000ml/min的大流量条件下进行抛光清洗,抛光清洗时间2分钟,以使铜材料表面光泽,表面非均匀性可控制在0.07,表面粗糙度0.5nm。
所述的阻蚀剂为FA/OII型阻蚀(氧)剂;螯合剂为FA/OII型螯合剂;表面活性剂为FA/OI型表面活性剂、Oπ-7((C10H21-C6H4-O-CH2CH2O)7-H)、Oπ-10((C10H21-C6H4-O-CH2CH2O)10-H)、O-20(C12-18H25-37-C6H4-O-CH2CH2O)70-H)、JFC的一种;均为天津晶岭微电子材料有限公司的市售产品。
实施例2:
在18MΩ超纯去离子水2745g中分别加入FA/O表面活性剂110g、FA/OII型螯合剂15g、FA/OII型阻蚀(氧)剂130g,边加入边搅拌均匀,搅拌均匀后制备成3000g pH值为7.4-8.2水溶性表面清洗液;利用制备好的清洗液对碱性化学机械抛光后的铜材料在2000Pa的低压力、1000ml/min的大流量条件下进行抛光清洗,抛光清洗时间1分钟,以使铜材料表面光泽,表面非均匀性可控制在0.04,表面粗糙度0.2nm。
其它同实施例1。
实施例3:
在18MΩ超纯去离子水3320g中分别加入FA/O表面活性剂90g、FA/OII型螯合剂35g、FA/OII型阻蚀(氧)剂115g,边加入边搅拌均匀,搅拌均匀后制备成3560g pH值为7.4-8.2水溶性表面清洗液;利用制备好的清洗液对碱性化学机械抛光后的铜材料在2500Pa的低压力、3000ml/min的大流量条件下进行抛光清洗,抛光清洗时间1分钟,以使铜材料表面光泽,表面非均匀性可控制在0.05,表面粗糙度0.3nm。
其它同实施例1。
上述参照实施例对ULSI铜材料抛光后表面清洗方法进行的详细描述,是说明性的而不是限定性的,可按照所限定范围列举出若干个实施例,因此在不脱离本发明总体构思下的变化和修改,应属本发明的保护范围之内。
Claims (4)
1.一种ULSI铜材料抛光后表面清洗方法,其特征在于:具体实施步骤如下,以下按重量%计:
(1)制备清洗液:
将表面活性剂1-4%、FA/OII型螯合剂0.5-3%、FA/OII型阻蚀剂0.1-5%、余量去离子水,混合搅拌均匀后制备成pH值为7.4-8.2的水溶性表面清洗液;
(2)使用步骤(1)中制备的清洗液对碱性化学机械抛光后的铜材料在2000Pa-3000Pa低压力下、1000-5000ml/min的大流量条件下进行抛光清洗,抛光清洗时间0.5-2分钟。
2.按照权利要求1所述的ULSI铜材料抛光后表面清洗方法,其特征在于:所述步骤(1)采用的表面活性剂为市售的FA/OI型表面活性剂、Oπ-7((C10H21-C6H4-O-CH2CH2O)7-H)、Oπ-10((C10H21-C6H4-O-CH2CH2O)10-H)、O-20(C12-18H25-37-C6H4-O-CH2CH2O)70-H)、JFC的一种。
3.按照权利要求1所述的ULSI铜材料抛光后表面清洗方法,其特征在于:所述步骤(1)采用的螯合剂为市售FA/OII型螯合剂:乙二胺四乙酸四(四羟乙基乙二胺)。
4.按照权利要求1所述的ULSI铜材料抛光后表面清洗方法,其特征在于:所述步骤(1)采用的阻蚀剂为市售的FA/OII型阻蚀剂。
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PCT/CN2010/080474 WO2012009942A1 (zh) | 2010-07-21 | 2010-12-30 | Ulsi铜材料抛光后表面清洗方法 |
US13/738,965 US8912134B2 (en) | 2010-07-21 | 2013-01-10 | Method of cleaning copper material surfaces in ultra large scale integrated circuits after polishing the same |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2012009941A1 (zh) * | 2010-07-21 | 2012-01-26 | 河北工业大学 | 超大规模集成电路多层铜布线化学机械抛光后的洁净方法 |
CN105925389A (zh) * | 2016-05-23 | 2016-09-07 | 昆山金城试剂有限公司 | 稀土研磨液专用清洗剂 |
CN110813891A (zh) * | 2019-11-15 | 2020-02-21 | 河北工业大学 | 用于铜cmp后清洗磨料颗粒的清洗液及清洗方法 |
CN112175756A (zh) * | 2020-11-05 | 2021-01-05 | 河北工业大学 | 用于去除多层铜互连阻挡层cmp后表面残留物的清洗液 |
CN115261152A (zh) * | 2022-08-05 | 2022-11-01 | 长鑫存储技术有限公司 | 清洗剂及其应用 |
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Also Published As
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CN101972755B (zh) | 2012-02-01 |
US20130123158A1 (en) | 2013-05-16 |
US8912134B2 (en) | 2014-12-16 |
WO2012009942A1 (zh) | 2012-01-26 |
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