WO2012009942A1 - Ulsi铜材料抛光后表面清洗方法 - Google Patents

Ulsi铜材料抛光后表面清洗方法 Download PDF

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WO2012009942A1
WO2012009942A1 PCT/CN2010/080474 CN2010080474W WO2012009942A1 WO 2012009942 A1 WO2012009942 A1 WO 2012009942A1 CN 2010080474 W CN2010080474 W CN 2010080474W WO 2012009942 A1 WO2012009942 A1 WO 2012009942A1
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polishing
copper material
cleaning
cleaning solution
oii
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PCT/CN2010/080474
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French (fr)
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刘玉岭
刘效岩
刘钠
何彦刚
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河北工业大学
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Priority to US13/738,965 priority Critical patent/US8912134B2/en

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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
    • 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
    • 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
    • C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
    • C11D2111/10—Objects to be cleaned
    • C11D2111/14—Hard surfaces
    • C11D2111/22—Electronic devices, e.g. PCBs or semiconductors

Definitions

  • the present invention relates to a method of cleaning a semiconductor material, and more particularly to a method of surface cleaning of a ULSI copper material after polishing.
  • Copper CMP has become one of the core technologies in ULSI preparation that has received worldwide attention.
  • countries around the world are stepping up their closed research to give priority to the international market.
  • the surface of the copper material is just broken, the surface energy is high, and it is easy to adsorb small particles and reduce the surface energy. Therefore, the abrasive particles in the polishing liquid are easily adsorbed on the surface of the copper, and the surface tension of the polishing liquid remaining around the particles is distributed in a small spherical shape on the copper surface to continue chemical reaction with copper, which is liable to cause uneven etching and poor surface consistency. . This results in increased costs in subsequent processing and a reduction in device yield.
  • the object of the present invention is to overcome the above-mentioned deficiencies, and to provide a simple, easy-to-use, non-polluting and clean copper surface cleaning method after polishing, which solves the problem that the surface energy of the copper material after polishing is high, the surface tension is large, and the residual polishing liquid is distributed. Uneven, contaminated metal ions.
  • a ULSI copper material post-polishing surface cleaning method characterized in that the specific implementation steps are as follows, and the following are in terms of % by weight:
  • the polishing time is at least 0.5-2 minutes.
  • the surfactant used in the step (1) is a commercially available FA/OI type surfactant
  • the chelating agent used in the step (1) is a commercially available FA/OII type chelating agent: ethylenediaminetetraacetic acid tetrakis(tetrahydroxyethylethylenediamine) having the following structural formula:
  • the corrosion inhibitor for the step (1) meter is a commercially available FA/ ⁇ type corrosion inhibitor (oxygen) agent of Tianjin Jingling Microelectronics Material Co., Ltd., which is urotropine (hexamethylenetetramine) and styrene-acrylic acid.
  • the compound of the urotropine of triazole (triazoxide) is C 6 H 12 N 4 , and the structural formula is:
  • the benzotriazole has the formula C6H5N3 and the structural formula is
  • the beneficial effects of the invention are as follows: Immediately after the polishing process in the CMP process, the copper material is cleaned at a large flow rate by using the cleaning liquid, and the polishing liquid with uneven cleaning distribution is quickly washed away, and a clean and perfect polished surface can be obtained.
  • the surfactant can be used to rapidly reduce the surface tension of the polished surface, reduce the damage layer and improve the uniformity of the surface quality.
  • the chelating agent can react with the residual metal ions to form a soluble macromolecular chelate.
  • the surface is separated from the surface by a large flow of water; the selected corrosion inhibitor can form a single-molecular passivation film on the surface after polishing, preventing the polishing liquid whose surface is unevenly distributed from continuing to react with the substrate, thereby improving the perfection of the surface after polishing.
  • the method uses a cleaning liquid to clean the copper material at a large flow rate immediately after the polishing process, which can effectively solve the problems in the prior art: (1) Low-pressure, high-flow water-drip cleaning without lag time, which can effectively optimize and reduce the copper surface Roughness can quickly wash away the abrasive particles adsorbed on the copper surface; (2) Adding nonionic surfactant to the cleaning solution can effectively reduce the surface tension of the residual polishing liquid on the copper surface, and preferentially adsorb the active agent on the copper surface.
  • Monolayer effectively protect copper material, avoid corrosion ring caused by non-uniform corrosion around abrasive particles; (3)
  • the cleaning solution can make the residual polishing liquid with uneven distribution on the surface of copper material be washed away quickly, and obtain clean and perfect polishing. surface.
  • the method is simple in operation, does not need to add other equipment, has low cost, high efficiency, and no pollution, and can obviously improve device performance and improve yield.
  • the corrosion inhibitor is a FA/OII type corrosion inhibitor (oxygen) agent; the chelating agent is a FA/OII type chelating agent; the surfactant is a FA/OI type surfactant, ⁇ ⁇ -7 (( 0 ⁇ 21 - 6 ⁇ 4 - ⁇ - ⁇ 2 ⁇ 2 ⁇ ) 7 - ⁇ ), ⁇ ⁇ -10 ((C 10 H 21 -C 6 H 4 -O-CH 2 CH 2 O) 10 -H), O-20 ( C 12-18 H 25-37 -C 6 H 4 -O-CH 2 CH 2 O) 70 -H), One of JFC; all of which are commercially available products of Tianjin Jingling Microelectronics Materials Co., Ltd.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Physics & Mathematics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Detergent Compositions (AREA)
  • Cleaning Or Drying Semiconductors (AREA)

Description

ULSI铜材料抛光后表面清洗方法
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 说
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。 书
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 I 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、
O,-7((C10H21-C6H4-O-CH2CH2O)7-H), Οπ-10 ((C10H21-C6H4-O-CH2CH2O)10-H)、 O-20 (C12-18H25-37-C6H4-O-CH2CH2O)7。-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：
Figure imgf000003_0001
所述步骤（1 )米用的阻蚀剂为天津晶岭微电子材料有限公司市售 FA/ΟΠ 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 所述乌洛托品分子式为 C6H12N4， 结构式为：
Figure imgf000003_0002
所述苯丙三氮唑分子式为 C6H5N3 , 结构式为
Figure imgf000003_0003
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 18ΜΩ超纯去离子水 1912g中分别加入 FA/0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、 Οπ-7(( 0Η21- 6Η4-Ο- Η2 Η2Ο)7-Η)、 Οπ-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 18ΜΩ超纯去离子水 2745g中分别加入 FA/0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 18ΜΩ超纯去离子水 3320g中分别加入 FA/0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

权利要求书
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、 0 ^ -7((C10H21-C6H4-O-CH2CH2O)7-H)、 Ο,-ΙΟ ((C10H2rC6H4-O-CH2CH2O)10-H)、 O-20 (C12— 18H25— 37-C6H4-0-CH2CH20)7。-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。
PCT/CN2010/080474 2010-07-21 2010-12-30 Ulsi铜材料抛光后表面清洗方法 WO2012009942A1 (zh)

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CN101908503A (zh) * 2010-07-21 2010-12-08 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
CN110813891B (zh) * 2019-11-15 2022-02-18 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
CN115261152B (zh) * 2022-08-05 2024-03-29 长鑫存储技术有限公司 清洗剂及其应用

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