US20020025762A1 - Biocides for polishing slurries - Google Patents

Biocides for polishing slurries Download PDF

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Publication number
US20020025762A1
US20020025762A1 US09/775,865 US77586501A US2002025762A1 US 20020025762 A1 US20020025762 A1 US 20020025762A1 US 77586501 A US77586501 A US 77586501A US 2002025762 A1 US2002025762 A1 US 2002025762A1
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United States
Prior art keywords
biocide
methyl
isothiazolin
slurry
polishing
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.)
Abandoned
Application number
US09/775,865
Inventor
Qiuliang Luo
Wendy Goldberg
Qianqiu Ye
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RONDEL HOLDINGS Inc
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RONDEL HOLDINGS Inc
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Application filed by RONDEL HOLDINGS Inc filed Critical RONDEL HOLDINGS Inc
Priority to US09/775,865 priority Critical patent/US20020025762A1/en
Assigned to RONDEL HOLDINGS, INC. reassignment RONDEL HOLDINGS, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: GOLDBERG, WENDY B., YE, QIANQIU (CHRISTINE), LUO, QIULIANG
Publication of US20020025762A1 publication Critical patent/US20020025762A1/en
Abandoned legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions
    • C09G1/02Polishing compositions containing abrasives or grinding agents
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1454Abrasive powders, suspensions and pastes for polishing
    • C09K3/1463Aqueous liquid suspensions

Definitions

  • This invention relates to the protection of polishing slurries and silica dispersions from the proliferation of bacteria and/or fungi by means of biocides.
  • U.S. Pat. No. 3,377,275 discloses a synergistic blend of 3,5-di-methyl tetrahydro 1,3,5,2H-thiadiazine-2-thione in combination with formaldehyde as a microbiocide for aqueous colloidal silica sols.
  • biocides which do not significantly affect the polishing performance of both particle-free solutions for use with fixed abrasive pads and slurries comprising metal oxide abrasives such as alumina, ceria, zirconia, and silica. These biocides comprise a five-membered organic ring compound containing both a sulfur and a nitrogen in the ring.
  • a chemical polishing solution for use with a fixed abrasive pad was made up with the following components: ammonium hydrogen phosphate, iminodiacetic acid, 5-methyl-1H-benzotriazole, surfactant, and hydrogen peroxide. Removal rates were determined using a Strasbaugh 6DS-SP Planarizer and a 3M fixed abrasive matrix MRW64 pad. The process was fixed at 4 psi downforce, 60 rpm platen speed, and 40 rpm carrier speed.
  • Biocide 1 (Kathon CGICP II available from Rohn and Haas Company, Philadelphia, Pa.) and Biocide 2 (Neolone M50 available from Rohm and Haas Company, Philadelphia, Pa.) were added at a concentration of 0.15% by weight to solution batches.
  • the active ingredients in these biocides are 2-methyl-4-isothiazolin-3-one and 5-chloro-2-methyl-4-isothiazolin-3-one. Results of polishing patterned wafers are shown in Table 1.
  • a polishing slurry comprising as major components iodic acid, lactic acid, potassium hydrogen phthalate, and metal oxide abrasive (a mixture of alumina and titania) was made up as slurry A. To a portion of this slurry was added 0.10% by weight of Kathon® CGICP biocide (active ingredients 2-methyl-4-isothiazolin-3-one and 5-chloro-2-methyl-4-isothiazolin-3-one). This slurry was designated slurry B.
  • Wafers comprising tungsten (W), titanium (Ti), and silicon dioxide (Ox) were polished on a standard CMP polishing machine using slurry A and slurry B. Results of the polishing are shown in Table 3. TABLE 3 Avg. W RR Avg. Ti RR Avg. Ox RR Slurry Angstroms/min Angstroms/min Angstroms/min A 3392 545 65 B 3533 564 64 B 3565 889 105 A 3291 891 62
  • a CMP slurry was made up with the following major components: Klebosol 1498-50 (silica sol), citric acid (complexing agent), benzotriazol (corrosion inhibitor), and a surfactant. Addition of a small amount (about 0.1%) of Neolone® (available from Rohm and Haas Company) gave adequate biocide protection to the CMP slurry while the slurry provided slightly improved surface quality when the slurry was used as a second step slurry for polishing semiconductor wafers comprising copper.
  • biocide comprised of 2-methyl-4-isothiazolin-3-one and/or 5-chloro-2-methyl-4-isothiazolin-3-one in an amount sufficient to provide antibacterial and antifungal protection to the slurry does not adversely affect the polishing performance of a slurry. It performs particularly well on slurries which comprise Klebosol® silica sol as an ingredient.
  • a sufficient amount of biocide is in the range of 0.01% to 1% by weight of the CMP solution or slurry.

Abstract

Compounds containing both a sulfur and a nitrogen in a five-membered ring structure are used as biocides in polishing solutions and slurries.

Description

    CROSS REFERENCE TO RELATED APPLICATION
  • This application claims the benefit of U.S. Provisional Patent Application Ser. No. 60/182,960 filed Feb. 16, 2000.[0001]
  • FIELD OF THE INVENTION
  • This invention relates to the protection of polishing slurries and silica dispersions from the proliferation of bacteria and/or fungi by means of biocides. [0002]
  • DESCRIPTION OF RELATED ART
  • The problem of bacterial and fungal growth in silica polishing slurries is addressed in U.S. Pat. No. 5,230,833 (Romberger et al.). It includes a thorough summary of the early related art. Bactericides disclosed in '833 are tetramethylammonium chloride, tetraethylammonium chloride, tetrapropylammonium chloride, alkylbenzyldimethylammonium chloride, and alkylbenzyldimethylammonium hydroxide, wherein the alkyl chaim ranges from 1 to about 20 carbon atoms. Also, the preferred biocide is sodium chlorite or sodium hypochlorite. The preferred fungicide is sodium OMADINE® (pyrithone). [0003]
  • U.S. Pat. No. 3,377,275 discloses a synergistic blend of 3,5-di-methyl tetrahydro 1,3,5,2H-thiadiazine-2-thione in combination with formaldehyde as a microbiocide for aqueous colloidal silica sols. [0004]
  • It has been found in recent years that the above chemicals are not always compatible with abrasive slurries used for chemical-mechanical polishing (CMP) of semiconductor wafers and with abrasive free slurries used with fixed abrasive polishing pads for semiconductor wafer polishing. It is the object of this invention to provide biocides which are not detrimental to the polishing of semiconductor wafers. Embodiments of the invention will now be described by way of example, with reference to the following detailed description. [0005]
  • SUMMARY OF THE INVENTION
  • It has been found that a five membered organic ring compound containing both a sulfur and a nitrogen in the ring provide biocide protection of CMP slurries without affecting polishing performance. Examples of such compounds are 5-chloro-2-methyl-4-isothiazolin-3-one and 2-methyl-4-isothiazolin-3-one. [0006]
  • DETAILED DESCRIPTION
  • A class of biocides has been found which do not significantly affect the polishing performance of both particle-free solutions for use with fixed abrasive pads and slurries comprising metal oxide abrasives such as alumina, ceria, zirconia, and silica. These biocides comprise a five-membered organic ring compound containing both a sulfur and a nitrogen in the ring.[0007]
  • EXAMPLE 1
  • A chemical polishing solution for use with a fixed abrasive pad was made up with the following components: ammonium hydrogen phosphate, iminodiacetic acid, 5-methyl-1H-benzotriazole, surfactant, and hydrogen peroxide. Removal rates were determined using a Strasbaugh 6DS-SP Planarizer and a 3M fixed abrasive matrix MRW64 pad. The process was fixed at 4 psi downforce, 60 rpm platen speed, and 40 rpm carrier speed. Biocide 1 (Kathon CGICP II available from Rohn and Haas Company, Philadelphia, Pa.) and Biocide 2 (Neolone M50 available from Rohm and Haas Company, Philadelphia, Pa.) were added at a concentration of 0.15% by weight to solution batches. The active ingredients in these biocides are 2-methyl-4-isothiazolin-3-one and 5-chloro-2-methyl-4-isothiazolin-3-one. Results of polishing patterned wafers are shown in Table 1. [0008]
    TABLE 1
    Polishing Results
    10 um 25 um 100 um 90% BP 0.5 0.5
    Sample lines lines lines 4.5/.5 120 um Bpe 2.5/2.5 1.5/1.5
    Control #1 461 652 1126 908 515 23 159 167
    Biocide #1 503 751  922 692 472 40 212 221
    Biocide #2 510 658 1085 855 570 93 301 242
    Control #2 652 830 1052 1003  649 47 348 279
  • These results show little or no effect from adding the biocide to the particle-free solutions. Similar solutions were prepared and evaluated using a challenge test with the intentional additions of bacteria and fungi. [0009]
    TABLE 2
    Challenge Test Results
    Sample Days Testing Results*
    Control 14 4F
    Biocide #1 14 0
    Biocide #2 14 0
  • EXAMPLE 2
  • A polishing slurry comprising as major components iodic acid, lactic acid, potassium hydrogen phthalate, and metal oxide abrasive (a mixture of alumina and titania) was made up as slurry A. To a portion of this slurry was added 0.10% by weight of Kathon® CGICP biocide (active ingredients 2-methyl-4-isothiazolin-3-one and 5-chloro-2-methyl-4-isothiazolin-3-one). This slurry was designated slurry B. [0010]
  • Wafers comprising tungsten (W), titanium (Ti), and silicon dioxide (Ox) were polished on a standard CMP polishing machine using slurry A and slurry B. Results of the polishing are shown in Table 3. [0011]
    TABLE 3
    Avg. W RR Avg. Ti RR Avg. Ox RR
    Slurry Angstroms/min Angstroms/min Angstroms/min
    A 3392 545 65
    B 3533 564 64
    B 3565 889 105
    A 3291 891 62
  • EXAMPLE 3
  • A CMP slurry was made up with the following major components: Klebosol 1498-50 (silica sol), citric acid (complexing agent), benzotriazol (corrosion inhibitor), and a surfactant. Addition of a small amount (about 0.1%) of Neolone® (available from Rohm and Haas Company) gave adequate biocide protection to the CMP slurry while the slurry provided slightly improved surface quality when the slurry was used as a second step slurry for polishing semiconductor wafers comprising copper. [0012]
  • It is obvious from the above results that the addition of a biocide comprised of 2-methyl-4-isothiazolin-3-one and/or 5-chloro-2-methyl-4-isothiazolin-3-one in an amount sufficient to provide antibacterial and antifungal protection to the slurry does not adversely affect the polishing performance of a slurry. It performs particularly well on slurries which comprise Klebosol® silica sol as an ingredient. A sufficient amount of biocide is in the range of 0.01% to 1% by weight of the CMP solution or slurry. [0013]

Claims (12)

What is claimed is:
1. An aqueous solution, for use in CMP of semiconductor wafers wherein a fixed abrasive polishing pad is used, which contains essentially no abrasive particles and which is protected from bacterial and fungal activity by means of a biocide comprising an organic compound with a five membered ring containing both a sulfur and a nitrogen group in said ring.
2. An aqueous slurry, for use in CMP of semiconductor wafers, which contains abrasive particles and which is protected from bacterial and fungal activity by means of a biocide comprising an organic compound with a five membered ring containing both a sulfur and a nitrogen group in said ring.
3. The solution of claim 1 wherein said biocide is from the group comprising 2-methyl-4-isothiazolin-3-one and 5-chloro-2-methyl-4-isothiazolin-3-one.
4. The slurry of claim 2 wherein said biocide is from the group comprising 2-methyl-4-isothiazolin-3-one and 5-chloro-2-methyl-4-isothiazolin-3-one.
5. The solution of claim 1 wherein said biocide is present in the range of 0.01% to 1% by weight of said solution.
6. The slurry of claim 2 wherein said biocide is present in the range of 0.01% to 1% by weight of said slurry.
7. A method of polishing a semiconductor wafer comprising: applying a solution at a polishing interface between a fixed abrasive polishing pad and said wafer, said solution comprising essentially no abrasive particles and which is protected from bacterial and fungal activity by means of a biocide comprising an organic compound with a five membered ring containing both a sulfur and a nitrogen group in said ring.
8. A method of polishing a semiconductor wafer comprising: applying a slurry at a polishing interface between a polishing pad and said wafer, said solution comprising abrasive particles and which is protected from bacterial and fungal activity by means of a biocide comprising an organic compound with a five membered ring containing both a sulfur and a nitrogen group in said ring.
9. A method according to claim 5 wherein said biocide is from the group comprising 2-methyl-4-isothiazolin-3-one and 5-chloro-2-methyl-4-isothiazolin-3-one.
10. A method according to claim 6 wherein said biocide is from the group comprising 2-methyl-4-isothiazolin-3-one and 5-chloro-2-methyl-4-isothiazolin-3-one.
11. A method according to claim 5 wherein said biocide is present in the range of 0.01% to 1% by weight of said solution.
12. A method according to claim 6 wherein said biocide is present in the range of 0.01% to 1% by weight of said slurry.
US09/775,865 2000-02-16 2001-02-02 Biocides for polishing slurries Abandoned US20020025762A1 (en)

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Cited By (24)

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Publication number Priority date Publication date Assignee Title
US20030181345A1 (en) * 2002-03-25 2003-09-25 Jinru Bian Tantalum barrier removal solution
US20030196386A1 (en) * 2002-04-22 2003-10-23 Jsr Corporation Aqueous dispersion for chemical mechanical polishing
US6750257B2 (en) * 2000-08-04 2004-06-15 Fuso Chemical, Ltd. Colloidal silica slurry
US20050070211A1 (en) * 2003-09-25 2005-03-31 Jinru Bian Barrier polishing fluid
US7300480B2 (en) 2003-09-25 2007-11-27 Rohm And Haas Electronic Materials Cmp Holdings, Inc. High-rate barrier polishing composition
US20080020577A1 (en) * 2006-07-21 2008-01-24 Cabot Microelectronics Corporation Gallium and chromium ions for oxide rate enhancement
CN101437918A (en) * 2006-05-02 2009-05-20 卡伯特微电子公司 Compositions and methods for cmp of semiconductor materials
US20100101448A1 (en) * 2008-10-24 2010-04-29 Dupont Air Products Nanomaterials Llc Polishing Slurry for Copper Films
EP2977418A1 (en) 2014-07-25 2016-01-27 Air Products And Chemicals, Inc. Chemical mechanical polishing (cmp) of cobalt-containing substrate
EP3037511A1 (en) 2014-12-23 2016-06-29 Air Products And Chemicals, Inc. Semi-aqueous photoresist or semiconductor manufacturing residue stripping and cleaning composition with improved silicon passivation
WO2016115096A1 (en) 2015-01-12 2016-07-21 Air Products And Chemicals, Inc. Composite abrasive particles for chemical mechanical planarization composition and method of use thereof
EP3088486A1 (en) 2015-04-27 2016-11-02 Air Products And Chemicals, Inc. Low dishing copper chemical mechanical planarization
EP3101076A1 (en) 2015-06-05 2016-12-07 Air Products And Chemicals, Inc. Barrier chemical mechanical planarization slurries using ceria-coated silica abrasives
EP3153558A1 (en) 2015-09-25 2017-04-12 Air Products And Chemicals, Inc. Chemical mechanical polishing composition
EP3231848A1 (en) 2016-03-31 2017-10-18 Versum Materials US, LLC Composite particles, method of refining and use thereof
EP3257910A1 (en) 2016-06-16 2017-12-20 Versum Materials US, LLC Chemical mechanical polishing (cmp) composition, method and system for cobalt-containing substrate
EP3263667A1 (en) 2016-07-01 2018-01-03 Versum Materials US, LLC Additives for barrier chemical mechanical planarization
EP3366742A1 (en) 2017-02-28 2018-08-29 Versum Materials US, LLC Chemical mechanical planarization of films comprising elemental silicon
EP3476910A1 (en) 2017-10-27 2019-05-01 Versum Materials US, LLC Composite particles, method of refining and use thereof
EP3588535A1 (en) 2018-06-26 2020-01-01 Versum Materials US, LLC Post chemical mechanical planarization (cmp) cleaning
EP3604468A1 (en) 2018-07-31 2020-02-05 Versum Materials US, LLC Tungsten chemical mechanical planarization (cmp) with low dishing and low erosion topography
EP3608378A1 (en) 2018-08-09 2020-02-12 Versum Materials US, LLC Chemical mechanical planarization composition for polishing oxide materials and method of use thereof
JP2020065051A (en) * 2018-09-26 2020-04-23 バーサム マテリアルズ ユーエス,リミティド ライアビリティ カンパニー Method for increasing oxide/nitride selectivity and low oxide trench dishing uniformity in chemical mechanical planarization (cmp) for shallow trench isolation (sti)
CN111500197A (en) * 2019-01-30 2020-08-07 弗萨姆材料美国有限责任公司 Shallow trench isolation chemical mechanical planarization polishing with adjustable silicon oxide and silicon nitride removal rates

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US6750257B2 (en) * 2000-08-04 2004-06-15 Fuso Chemical, Ltd. Colloidal silica slurry
US7491252B2 (en) 2002-03-25 2009-02-17 Rohm And Haas Electronic Materials Cmp Holdings, Inc. Tantalum barrier removal solution
US20030181345A1 (en) * 2002-03-25 2003-09-25 Jinru Bian Tantalum barrier removal solution
US20030196386A1 (en) * 2002-04-22 2003-10-23 Jsr Corporation Aqueous dispersion for chemical mechanical polishing
EP1357161A2 (en) * 2002-04-22 2003-10-29 JSR Corporation Aqueous dispersion for chemical mechanical polishing
EP1357161A3 (en) * 2002-04-22 2003-12-03 JSR Corporation Aqueous dispersion for chemical mechanical polishing
US6786944B2 (en) 2002-04-22 2004-09-07 Jsr Corporation Aqueous dispersion for chemical mechanical polishing
US20050070211A1 (en) * 2003-09-25 2005-03-31 Jinru Bian Barrier polishing fluid
US7241725B2 (en) 2003-09-25 2007-07-10 Rohm And Haas Electronic Materials Cmp Holdings, Inc. Barrier polishing fluid
US7300480B2 (en) 2003-09-25 2007-11-27 Rohm And Haas Electronic Materials Cmp Holdings, Inc. High-rate barrier polishing composition
CN101437918A (en) * 2006-05-02 2009-05-20 卡伯特微电子公司 Compositions and methods for cmp of semiconductor materials
US20090156006A1 (en) * 2006-05-02 2009-06-18 Sriram Anjur Compositions and methods for cmp of semiconductor materials
US7501346B2 (en) * 2006-07-21 2009-03-10 Cabot Microelectronics Corporation Gallium and chromium ions for oxide rate enhancement
US20080020577A1 (en) * 2006-07-21 2008-01-24 Cabot Microelectronics Corporation Gallium and chromium ions for oxide rate enhancement
US20100101448A1 (en) * 2008-10-24 2010-04-29 Dupont Air Products Nanomaterials Llc Polishing Slurry for Copper Films
US8506661B2 (en) * 2008-10-24 2013-08-13 Air Products & Chemicals, Inc. Polishing slurry for copper films
EP2977418A1 (en) 2014-07-25 2016-01-27 Air Products And Chemicals, Inc. Chemical mechanical polishing (cmp) of cobalt-containing substrate
EP3037511A1 (en) 2014-12-23 2016-06-29 Air Products And Chemicals, Inc. Semi-aqueous photoresist or semiconductor manufacturing residue stripping and cleaning composition with improved silicon passivation
US10073351B2 (en) 2014-12-23 2018-09-11 Versum Materials Us, Llc Semi-aqueous photoresist or semiconductor manufacturing residue stripping and cleaning composition with improved silicon passivation
WO2016115096A1 (en) 2015-01-12 2016-07-21 Air Products And Chemicals, Inc. Composite abrasive particles for chemical mechanical planarization composition and method of use thereof
US10418247B2 (en) 2015-01-12 2019-09-17 Versum Materials Us, Llc Composite abrasive particles for chemical mechanical planarization composition and method of use thereof
US10109493B2 (en) 2015-01-12 2018-10-23 Versum Materials Us, Llc Composite abrasive particles for chemical mechanical planarization composition and method of use thereof
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US9978609B2 (en) 2015-04-27 2018-05-22 Versum Materials Us, Llc Low dishing copper chemical mechanical planarization
EP3101076A1 (en) 2015-06-05 2016-12-07 Air Products And Chemicals, Inc. Barrier chemical mechanical planarization slurries using ceria-coated silica abrasives
US10144850B2 (en) 2015-09-25 2018-12-04 Versum Materials Us, Llc Stop-on silicon containing layer additive
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EP3257910A1 (en) 2016-06-16 2017-12-20 Versum Materials US, LLC Chemical mechanical polishing (cmp) composition, method and system for cobalt-containing substrate
EP3263667A1 (en) 2016-07-01 2018-01-03 Versum Materials US, LLC Additives for barrier chemical mechanical planarization
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EP3588535A1 (en) 2018-06-26 2020-01-01 Versum Materials US, LLC Post chemical mechanical planarization (cmp) cleaning
EP3604468A1 (en) 2018-07-31 2020-02-05 Versum Materials US, LLC Tungsten chemical mechanical planarization (cmp) with low dishing and low erosion topography
EP3608378A1 (en) 2018-08-09 2020-02-12 Versum Materials US, LLC Chemical mechanical planarization composition for polishing oxide materials and method of use thereof
JP2020065051A (en) * 2018-09-26 2020-04-23 バーサム マテリアルズ ユーエス,リミティド ライアビリティ カンパニー Method for increasing oxide/nitride selectivity and low oxide trench dishing uniformity in chemical mechanical planarization (cmp) for shallow trench isolation (sti)
CN111500197A (en) * 2019-01-30 2020-08-07 弗萨姆材料美国有限责任公司 Shallow trench isolation chemical mechanical planarization polishing with adjustable silicon oxide and silicon nitride removal rates
US11608451B2 (en) * 2019-01-30 2023-03-21 Versum Materials Us, Llc Shallow trench isolation (STI) chemical mechanical planarization (CMP) polishing with tunable silicon oxide and silicon nitride removal rates

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