US3817727A - Abrasive polishing suspensions and method for making same - Google Patents

Abrasive polishing suspensions and method for making same Download PDF

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Publication number
US3817727A
US3817727A US00235651A US23565172A US3817727A US 3817727 A US3817727 A US 3817727A US 00235651 A US00235651 A US 00235651A US 23565172 A US23565172 A US 23565172A US 3817727 A US3817727 A US 3817727A
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US
United States
Prior art keywords
glycol
carbopol
linde
suspensions
water
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Expired - Lifetime
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US00235651A
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English (en)
Inventor
P Yancey
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Praxair ST Technology Inc
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Union Carbide Corp
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Publication date
Application filed by Union Carbide Corp filed Critical Union Carbide Corp
Priority to US00235651A priority Critical patent/US3817727A/en
Priority to DE19732312372 priority patent/DE2312372C3/de
Priority to CA166,932A priority patent/CA972167A/en
Priority to JP3016773A priority patent/JPS536755B2/ja
Priority to FR7309511A priority patent/FR2176798B1/fr
Application granted granted Critical
Publication of US3817727A publication Critical patent/US3817727A/en
Assigned to MORGAN GUARANTY TRUST COMPANY OF NEW YORK, AND MORGAN BANK ( DELAWARE ) AS COLLATERAL ( AGENTS ) SEE RECORD FOR THE REMAINING ASSIGNEES. reassignment MORGAN GUARANTY TRUST COMPANY OF NEW YORK, AND MORGAN BANK ( DELAWARE ) AS COLLATERAL ( AGENTS ) SEE RECORD FOR THE REMAINING ASSIGNEES. MORTGAGE (SEE DOCUMENT FOR DETAILS). Assignors: STP CORPORATION, A CORP. OF DE.,, UNION CARBIDE AGRICULTURAL PRODUCTS CO., INC., A CORP. OF PA.,, UNION CARBIDE CORPORATION, A CORP.,, UNION CARBIDE EUROPE S.A., A SWISS CORP.
Assigned to UNION CARBIDE CORPORATION, reassignment UNION CARBIDE CORPORATION, RELEASED BY SECURED PARTY (SEE DOCUMENT FOR DETAILS). Assignors: MORGAN BANK (DELAWARE) AS COLLATERAL AGENT
Assigned to UNION CARBIDE COATINGS SERVICE TECHNOLOGY CORPORATION reassignment UNION CARBIDE COATINGS SERVICE TECHNOLOGY CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: UNION CARBIDE COATINGS SERVICE CORPORATION
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • 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
    • H01L21/02002—Preparing wafers
    • H01L21/02005—Preparing bulk and homogeneous wafers
    • H01L21/02008—Multistep processes
    • H01L21/0201—Specific process step
    • H01L21/02024—Mirror polishing
    • 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
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives
    • C09K3/1454—Abrasive powders, suspensions and pastes for polishing
    • C09K3/1463—Aqueous liquid suspensions

Definitions

  • the suspension media consists essentially of a glycol base thickened by a neutralized carboxy polymethylene polymer.
  • This invention relates to abrasive polishing suspensions and, more particularly, to permanent suspensions of powdered abrasive materials in a nonaqueous or partially aqueous glycol base.
  • the glycol base suspension media can be made to permanently suspend abrasive powdered particles so that they will not settle out or cake at the bottom of the container as is the case with presently available metallographic and semi-conductor polishing formulations.
  • the suspending media has anti-drying properties due to the low vapor pressure of the glycol base. The evaporamm rate is minimized and periodic additions of fluid are not required to maintain the properties of the polishing compound While on the lap.
  • Another factor contributing to the anti-drying properties, of the suspensions of the present invention is the high hygroscopicity of the glycol family of compounds. For example, at 80 F. and 60% relatively humidity a 50% aqueous solution of ethylene glycol would lose through evaporation a maximum of of its water.
  • glycol base suspensions are completely soluble in water and are soluble in many organic materials normally insoluble in Water. This is an advantage over oil based lapping compounds. Further, suspensions made from glycol based formulations have a much broader useful temperature range. A' pure ethylene glycol base would be liquid from 12 C. to 200 C., over twice the range of pure water. Also, since glycols reduce surface tension in aqueous systems, they provide superior wetting properties by their presence in the polishing suspensions.
  • the present invention is predicated on the use of various glycols such as ethylene glycol, diethylene glycol and triethylene glycol, but preferably ethylene glycol alone or in combination with each other and/or water.
  • glycols such as ethylene glycol, diethylene glycol and triethylene glycol, but preferably ethylene glycol alone or in combination with each other and/or water.
  • a carboxy polymethylene polymer of high molecular weight to thicken the suspension and produce a permanent suspension of abrasive particles in the glycol or glycol water base.
  • Suspensions made according to the invention have a shelf life exceeding one yearwithout settling of abrasive powder particles.
  • Typical powders are aluminum oxide powders having an unagglomerated average of particle size in the range of from about .05 to 1.0 microns, sold by Union Carbide Corporation under the trade name'Linde Type A, B or C.
  • Other powders could be, for example,
  • the suspensions are made by blending a carboxy polymethylene polymer of high molecular weight, such as the type sold by B. F. Goodrich Chemical Co. under the trade name Carbopol 941 into ethylene glycol.
  • the Carbopol 941 is supplied as dry, fluflz'y powders in acid form requiring neutralization to develop optimum properties.
  • Carbopol 941 as described in Service Bulletin GC36 (Revised) of The B. F.
  • Goodrich Chemical Company is a commercially available water-soluble carboxy vinyl polymer resin having the following properties Physical properties Appearance: Flufly, white acid powder Bulk density: 13 pounds per cubic foot (approximate) Specific gravity: 1.41 Moisture content as shipped: 2% maximum Equilibrium moisture content, room temperature, at
  • EXAMPLE I 1.0 gram of Carbopol 941 resin was blended into 400 cc. ethylene glycol. After allowing the mixture to soak for several minutes, 10 cc. of a 25% aqueous solution of diisopropanolamine was blended with the Carbopol/ glycol mixture to neutralize the Carbopol and form a thick mucilage. In another blender 150 grams of Linde A (0.3a) alumina polishing powder was dispersed in another 400 cc. of ethylene glycol. Twenty drops ofred dye were added for coloring. This alumina dispersion was quickly poured into the previously prepared Carbopol mucilage in the first blender and thoroughly blended into the mucilage. A permanent pink suspension of Linde A in ethylene glycol resulted. The composition of the suspension was as follows:
  • EXAMPLE III 1.0 gram of Carbopol 941 resin was blended with 400 cc. of ethylene glycol- After allowing mixture to soak for several .minutes, 10 cc. of 25 aqueous solutionof diisopropanolamine was blended into the Carbopol/ glycol mixture to neutralize the Carbopol and form a thick mucilage. In another blender 150 grams of Linde A alumina powder were dispersed in 400 cc. of water. Twenty drops of red dye were added to this dispersion. The alumina/water mixture was quickly transferred to the Carbopol mucilage in the first blender and thoroughly blended with the mucilage. A permanent pink suspension of Linde A'in a water/glycol base resulted. The composition of the suspension was'as follows:
  • EXAMPLE IV Identical procedure to Example II I except Linde C alumina powder and yellow dye were used in place of Linde A and red dye. A permanent yellow suspension of Linde C resulted.
  • EXAMPLE V Identical procedure to Example III, except l QOgrams of Linde B (0.05m alumina polishing powder and blue dye were used inplace of Linde A and red dye. A per-- manent blue suspension of Linde B resulted.
  • the ethylene glycol/carbopol mixture in the large tank was then neutralized with 200 cc. of aqueous diisopropanolamine.
  • the Linde C dispersion was then added quickly to the large tank containing the mucilage and the entire mixture was blended to 10-15 minutes using the Model 8A Eastern mixer previously mentioned.
  • Corundum 1600 abrasive powder was suspended in place of the Linde A.
  • Corundum 1600 is manufactured by Bausch & Lombe and has a mean particle size of approximately 10 microns. It is used extensively in the manufacture of ophthalmic lens.
  • Example EIII is w d awasusedinplace Same procedure and ingredients as used in Example EIII, except TAM Zirox B'abrasi-ve (Zirconium oxide) was suspended in place of Linde A. This polishing abrasive ha ,amai mum. P5 iz micrq sap is used'in precision glass and mineral-polishing EXAMPLE XI- q Same procedure andingredients as usedin #Example III, except Norton No. 320 SiCabrasive 'was suspended in p1ace of Linde A. This material has;a mean particle size of 32 microns.
  • EXAMPLEXV- 1 Same procedure and ingredients as used in Example III, except jewelers-rouge polishing compound used in place of Linde A. 1 v I EXAMPLE XVI Ethylene glycol 54.64 Powder 27.70 Water 17.23 Carbopol 0.12 e 25% aqueous solution of diis'opropanolamine 0.30
  • the alumina/water mixture was quickly transferred to the Carbopol mucilage in the first blender and thoroughly blended with the mucilage.
  • a permanent yellow suspension of- Linde C in awater/propylene glycol base resulted.
  • EXAMPLE XXIII 1.0 gram of Carbopol 941 resin blended into 400 cc. propylene glycol. After allowing the mixture to soak for several minutes, cc. of a 25% aqueous solution of diisopropanolamine was blended with the Carbopol/ glycol mixture to neutralize the Carbopol and form a thick mucilage. In another blender 150 grams of Linde C (1.0a) alumina polishing powder was dispersed in another 400 cc. of propylene glycol. Twenty drops of yellow dye were added for coloring. This alumina dispersion was quickly poured into the previously prepared Carbopol mucilage in the first blender and thoroughly blended into the mucilage. A permanent yellow suspension of Linde C in propylene glycol resulted.
  • Example I and XXIII illustrate the use of two nonaqueous glycol formulations using the lowest molecular weight members of two families of glycols, the ethylene glycols and propylene glycols.
  • Examples XIX through XXI illustrate the use of higher order ethylene glycols in a water/ glycol formulation. It is a reasonable assumption that the higher molecular weight polyethylene glycols of the form HOCH (CH -O-CH ),,CI-I -OH would form successful suspensions, both aqueous and non-aqueous, for higher values of n than have been attempted in the examples listed. This would especially be true for n up to 7, which glycols are still liquid at ambient conditions.
  • All of the previous examples have utilized only a slight excess of neutralizing agent leaving the suspensions in a neutral or slightly alkaline invironment with pH lower than 10.
  • All of the neutralizing agents for Car-bopol resins are bases, either organic such as diisopropanolamine used throughout most of the examples, or inorganic such as NaOH in Example VI.
  • Other bases which will neutralize Carbopol resins in the ethylene glycol/water system are ammonium hydroxide, triethanolamine, monoethanolamine, triethylamine, and Ethomeen C-25.
  • Diisopropanolamine has been found to be the most eflicient neutralizing agent in the present systems and is the preferred agent.
  • An advantage of the suspensions made using this preferred organic base is that there are no inorganic ions, such as Na, present to any extent. Ions such as sodium are very deleterious to polished semi-conductor substrates.
  • the Carbopol 941 is preferred in these formulations over the other Carbopol resins due to its ability to form relatively low viscosities in ionic systems.
  • the other Carbopol resins are used to provide much thicker emulsions and suspensions.
  • these alumina suspensions are as widespread as the powders from which they are formed. They can be used in essentially all polishing operations which now use the alumina powders, with the new advantage of being easier to handle than the powder counterpart. Being viscous, they remain on the laps longer than a similar water slurry, and they are much less susceptible to drying on the lap. Since they are chemically neutral, they will not corrode laps as will some of the other formulations on the market.
  • a polishing composition consisting essentially of an abrasive polishing powder having an unagglomerated particle size of from about .01 to about microns suspended in a media consisting essentially of a glycol thickened by a neutralized carboxy polymethylene polymer.
  • composition according to claim 1 wherein said media consists essentially of ethylene glycol thickened by a neutralized carboxy polymethylene polymer and up to 50% by weight water.
  • a polishing composition consisting essentially of alumina powder having an unagglomerated average particle size of from .05 to 1.0 micron suspended in a media consisting essentially of ethylene glycol thickened by a neutralized carboxy polymethylene polymer and up to 50% by weight water.
  • a permanent polishing composition suspension consisting essentially of about 84.6 percent wt.-percent ethylene glycol, about 14.3 wt.-percent alumina polishing powder, about 0.1 wt.-percent carboxy polymethylene polymer of high molecular weight and about 1.0 wt.-percent of a 25 aqueous solution of diisopropanolamine.
  • a permanent polishing composition suspension consisting essentially of about 44.1 wt.-percent ethylene glycol, 40 wt.-percent water, 14.8 wt.-percent alumina powder, about 0.10 wt.-percent carboxy polymethylene polymer and about 1.0 wt.-percent of a 25% aqueous solution of diisopropanolamine.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Physics & Mathematics (AREA)
  • Power Engineering (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Paints Or Removers (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
US00235651A 1972-03-17 1972-03-17 Abrasive polishing suspensions and method for making same Expired - Lifetime US3817727A (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
US00235651A US3817727A (en) 1972-03-17 1972-03-17 Abrasive polishing suspensions and method for making same
DE19732312372 DE2312372C3 (de) 1972-03-17 1973-03-13 Schleif- und Poliermittelsuspensionen
CA166,932A CA972167A (en) 1972-03-17 1973-03-14 Abrasive polishing suspensions and method for making same
FR7309511A FR2176798B1 (en, 2012) 1972-03-17 1973-03-16
JP3016773A JPS536755B2 (en, 2012) 1972-03-17 1973-03-16

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US00235651A US3817727A (en) 1972-03-17 1972-03-17 Abrasive polishing suspensions and method for making same

Publications (1)

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US3817727A true US3817727A (en) 1974-06-18

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Country Status (4)

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US (1) US3817727A (en, 2012)
JP (1) JPS536755B2 (en, 2012)
CA (1) CA972167A (en, 2012)
FR (1) FR2176798B1 (en, 2012)

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4038048A (en) * 1975-02-14 1977-07-26 Thrower Jr Herbert T Lapping composition containing a carboxy vinyl polymer
FR2414387A1 (fr) * 1978-01-16 1979-08-10 Grace W R Ltd Compositions pour le polissage du silicium et du germanium et leur procede d'utilisation
US4222747A (en) * 1978-01-05 1980-09-16 Essilor International, Cie Generale D'optique Polishing material for ophthalmic lenses
US4242842A (en) * 1979-08-08 1981-01-06 La Pierre Synthetique Baikowski, S.A. Precision polishing suspension and method for making same
US4358295A (en) * 1980-03-27 1982-11-09 Matsushita Electric Industrial Co., Ltd. Polishing method
WO1996016436A1 (en) * 1994-11-18 1996-05-30 Advanced Micro Devices, Inc. Method of making a chemical-mechanical polishing slurry and the polishing slurry
EP0837115A1 (de) * 1996-10-17 1998-04-22 Wacker Siltronic Gesellschaft für Halbleitermaterialien Aktiengesellschaft Sägesuspension und Verfahren zum Abtrennen von Scheiben von einem Kristall
US5855633A (en) * 1997-06-06 1999-01-05 Lockheed Martin Energy Systems, Inc. Lapping slurry
US5916855A (en) * 1997-03-26 1999-06-29 Advanced Micro Devices, Inc. Chemical-mechanical polishing slurry formulation and method for tungsten and titanium thin films
US20070060479A1 (en) * 2000-09-18 2007-03-15 Highsmith Ronald E Agricultural chemical suspensions
CN113718328A (zh) * 2021-11-04 2021-11-30 山东裕航特种合金装备有限公司 一种船用铝合金铸件的表面处理方法

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS50144989A (en, 2012) * 1974-05-13 1975-11-21
JPS5131793A (ja) * 1974-09-13 1976-03-18 Hitachi Chemical Co Ltd Yuyoseifuenooruhokozokuhorumuarudehitojushi no seiho
RU2034889C1 (ru) * 1993-04-02 1995-05-10 Научно-производственное объединение "Алтай" Композиция для суперфинишной доводки поверхности материала

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2783137A (en) * 1951-06-08 1957-02-26 Dow Chemical Co Grinding compositions and making of same
US3053646A (en) * 1960-07-15 1962-09-11 Dow Chemical Co Grinding and polishing compositions and method of making same
NL263408A (en, 2012) * 1962-04-10

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4038048A (en) * 1975-02-14 1977-07-26 Thrower Jr Herbert T Lapping composition containing a carboxy vinyl polymer
US4222747A (en) * 1978-01-05 1980-09-16 Essilor International, Cie Generale D'optique Polishing material for ophthalmic lenses
FR2414387A1 (fr) * 1978-01-16 1979-08-10 Grace W R Ltd Compositions pour le polissage du silicium et du germanium et leur procede d'utilisation
US4260396A (en) * 1978-01-16 1981-04-07 W. R. Grace & Co. Compositions for polishing silicon and germanium
US4242842A (en) * 1979-08-08 1981-01-06 La Pierre Synthetique Baikowski, S.A. Precision polishing suspension and method for making same
US4358295A (en) * 1980-03-27 1982-11-09 Matsushita Electric Industrial Co., Ltd. Polishing method
WO1996016436A1 (en) * 1994-11-18 1996-05-30 Advanced Micro Devices, Inc. Method of making a chemical-mechanical polishing slurry and the polishing slurry
EP0837115A1 (de) * 1996-10-17 1998-04-22 Wacker Siltronic Gesellschaft für Halbleitermaterialien Aktiengesellschaft Sägesuspension und Verfahren zum Abtrennen von Scheiben von einem Kristall
US5947102A (en) * 1996-10-17 1999-09-07 Wacker Siltronic Gesellschaft Fur Halbleitermaterialien Ag Method for cutting wafers from a crystal
US5916855A (en) * 1997-03-26 1999-06-29 Advanced Micro Devices, Inc. Chemical-mechanical polishing slurry formulation and method for tungsten and titanium thin films
US5855633A (en) * 1997-06-06 1999-01-05 Lockheed Martin Energy Systems, Inc. Lapping slurry
US20070060479A1 (en) * 2000-09-18 2007-03-15 Highsmith Ronald E Agricultural chemical suspensions
US7332457B2 (en) 2000-09-18 2008-02-19 Honeywell International Inc. Agricultural chemical suspensions
CN113718328A (zh) * 2021-11-04 2021-11-30 山东裕航特种合金装备有限公司 一种船用铝合金铸件的表面处理方法

Also Published As

Publication number Publication date
JPS4913232A (en, 2012) 1974-02-05
DE2312372A1 (de) 1973-09-20
CA972167A (en) 1975-08-05
FR2176798B1 (en, 2012) 1976-05-21
FR2176798A1 (en, 2012) 1973-11-02
JPS536755B2 (en, 2012) 1978-03-10
DE2312372B2 (de) 1976-02-12

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Owner name: MORGAN GUARANTY TRUST COMPANY OF NEW YORK, AND MOR

Free format text: MORTGAGE;ASSIGNORS:UNION CARBIDE CORPORATION, A CORP.,;STP CORPORATION, A CORP. OF DE.,;UNION CARBIDE AGRICULTURAL PRODUCTS CO., INC., A CORP. OF PA.,;AND OTHERS;REEL/FRAME:004547/0001

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Free format text: RELEASED BY SECURED PARTY;ASSIGNOR:MORGAN BANK (DELAWARE) AS COLLATERAL AGENT;REEL/FRAME:004665/0131

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Free format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNOR:UNION CARBIDE COATINGS SERVICE CORPORATION;REEL/FRAME:005240/0883

Effective date: 19900102