WO2020071576A1 - Graisse contenant du fluor pour équipement à semi-conducteur - Google Patents

Graisse contenant du fluor pour équipement à semi-conducteur

Info

Publication number
WO2020071576A1
WO2020071576A1 PCT/KR2018/012693 KR2018012693W WO2020071576A1 WO 2020071576 A1 WO2020071576 A1 WO 2020071576A1 KR 2018012693 W KR2018012693 W KR 2018012693W WO 2020071576 A1 WO2020071576 A1 WO 2020071576A1
Authority
WO
WIPO (PCT)
Prior art keywords
mass
fluorine
grease
semiconductor equipment
pfpe
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.)
Ceased
Application number
PCT/KR2018/012693
Other languages
English (en)
Korean (ko)
Inventor
최인석
김광식
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Publication of WO2020071576A1 publication Critical patent/WO2020071576A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/06—Mixtures of thickeners and additives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M107/00—Lubricating compositions characterised by the base-material being a macromolecular compound
    • C10M107/38—Lubricating compositions characterised by the base-material being a macromolecular compound containing halogen
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M119/00—Lubricating compositions characterised by the thickener being a macromolecular compound
    • C10M119/02—Hydrocarbon polymers; Hydrocarbon polymers modified by oxidation
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M119/00—Lubricating compositions characterised by the thickener being a macromolecular compound
    • C10M119/22—Lubricating compositions characterised by the thickener being a macromolecular compound containing halogen
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M151/00—Lubricating compositions characterised by the additive being a macromolecular compound containing sulfur, selenium or tellurium
    • C10M151/04—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Form in which the lubricant is applied to the material being lubricated semi-solid; greasy

Definitions

  • the present invention relates to a fluorine-containing grease for semiconductor equipment. More specifically, fluorine-containing grease, an lubricant optimized for the characteristics of semiconductor equipment, has a short stroke distance due to the characteristics of semiconductor equipment and takes into account that the temperature rises rapidly when the equipment is loaded in a short time. It relates to a fluorine-containing grease for semiconductor equipment that can reduce and increase the central pumping performance in the case of mold equipment.
  • Fluorine-containing greases have been conventionally known. Fluorine-containing greases have been prepared by suspending polytetrafluoroethylene (PTFE) polymers in perfluorinated liquids such as perfluoropolyether (PFPE) (see USP 4472290).
  • PTFE polytetrafluoroethylene
  • PFPE perfluoropolyether
  • the disclosed invention comprises: 15-50% by weight of a polytetrafluoroethylene or tetrafluoroethylene (hereinafter referred to as TFE) copolymer having predominantly or partially fluorine and other ethylenically unsaturated monomers; 30 to 84.5% by weight of a perfluoroether oil having a viscosity comprised between 20 and 4000 cst at 20 ° C; 0.5 to 10% by weight of a surfactant or dispersant having a perfluoropolyether or perfluoroalkyl chain; And 0 to 10% by weight of anti-corrosion and / or antiwear additives, wherein the (per) fluoropolymer particles based on the TFE or their totals have an average size smaller than microns, and are the same as above. It relates to a fluorine grease having a composition having a wear diameter value of at least 25% lower than that of a conventional fluorine grease having the same component of the product.
  • TFE polyt
  • the disclosed invention may exhibit performance as a lubricant used in a general machine or the like, but when additives are used in semiconductor equipment using fatty acid oil, there are problems such as particle generation.
  • the present invention is to solve the problems of the prior art, the object of the present invention is to meet the characteristics of the temperature rise in a short time and short stroke distance of the semiconductor equipment, it is possible to improve the prevention of particle contamination of the equipment and equipment prevention It provides a fluorine-containing grease for semiconductor equipment.
  • perfluoropolyether perfluoropolyether: PFPE
  • polytetrafluoroethylene polytetrafluoroethylene: PTFE
  • sulfurized bis dibutylcarmabodithioate
  • di- ⁇ -oxodioxodiol-diol sulfurized bis (dibutylcarbamodithioato) di- ⁇ -oxodioxodimolybdenum)
  • a fluorine-containing grease for semiconductor equipment comprising at least%.
  • perfluoropolyether perfluoropolyether: PFPE
  • PFPE perfluoropolyether
  • polytetrafluoroethylene polytetrafluoroethylene
  • organic sulfurized bis Di- ⁇ -oxodioxodiol didenum
  • sulfurized bis dibutylcarbamodithioato
  • di- ⁇ -oxodioxodimolybdenum 0.1% by mass to 10% by mass of fluorine-containing grease for semiconductor equipment
  • PFPE perfluoropolyether
  • PTFE polytetrafluoroethylene
  • sulfurized bis dibutyl carmathiothio
  • PFPE perfluoropolyether
  • PTFE polytetrafluoroethylene
  • organic sulfurized bis dibutyl carmathiothioate
  • Di- ⁇ -oxodioxodiol fluorine-containing grease for semiconductor equipment which contains at least 2% by mass of sulfurized bis (dibutylcarbamodithioato) di- ⁇ -oxodioxodimolybdenum).
  • the present invention it is possible to meet the characteristics of the temperature rise in a short time and a short stroke distance of the semiconductor equipment, improve the prevention of particle contamination of the equipment and the equipment, and consequently the life of the semiconductor equipment. It works.
  • perfluoropolyether perfluoropolyether: PFPE
  • PFPE perfluoropolyether
  • polytetrafluoroethylene polytetrafluoroethylene
  • sulfurized bis A fluorine-containing grease for semiconductor equipment comprising at least 0.1% to 10% by mass of dibutyl-carmabothiothio) di- ⁇ -oxodioxodioldiobium (sulfurized bis (dibutylcarbamodithioato) di- ⁇ -oxodioxodimolybdenum)
  • dibutyl-carmabothiothio di- ⁇ -oxodioxodioldiobium
  • sulfurized bis dibutylcarbamodithioato di- ⁇ -oxodioxodimolybdenum
  • Semiconductor equipment is sensitive to the problem of particle and contamination due to the characteristics of the target product and the long service life of expensive equipment. It is the key to effectively reduce the wear caused by friction between parts of the equipment during operation, and it shows a lot of difference in the life of the equipment according to the performance of the grease, which is a lubricant for this.
  • Grease is composed of thickeners (solid powder), base oil (liquid) and additives (powder), and the degree of hardness or softness is adjusted according to the mixing ratio. Since grease is a mixture of the above three materials, it is indicated as a national grade (National Lubricants Grease Institute_Grade: NLGI_Grade) rather than a viscosity grade.
  • the lead grade is determined by the depth at which the iron mass enters the grease for 1 minute by placing the grease in the container at room temperature (25 ° C) and placing the specified iron mass on the grease. Hard grease has a low level of depth into which the iron mass has entered the grease and soft grease has a high level of depth with which the iron mass has entered the grease.
  • the leading grade is represented by 9 grades of "000, 00, 0, 1, 2, 3, 4, 5, 6", and the lower the grade, the softer the grease.
  • the leading class "2" is known as the most commonly used grease.
  • the existing grease used in semiconductor equipment has also used the leading grade "2". However, it has been found that the temperature of the equipment rises sharply due to the short stroke time and the load applied in a short time in semiconductor equipment using the leading grade "2" grease.
  • the grease yields wear resistance through a four-ball test. It has been found through experiments that the wear resistance of grease influences the life of the semiconductor equipment, and the wear resistance of the grease used in the semiconductor equipment greatly depends on the lead grade, the type of base oil PFPE and the selection of additives.
  • the grease as a lubricant may be liquid wet grease and gel or solid dry grease.
  • the fluorine-containing grease for semiconductor equipment of the present invention is dry grease due to the characteristics of the semiconductor equipment used. More specifically, it is a wet type lubrication, but the thickener contains the base oil PFPE, and it represents the intermediate form of the liquid and solid phases of a mechanism that repeats discharge and absorption. This state of property is called a non-Newtonian viscous fluid.
  • the thickener of the fluorine-containing grease for semiconductor equipment of the present invention uses polytetrafluoroethylene (PTFE).
  • polytetrafluoroethylene polytetrafluoroethylene: PTFE
  • PTFE polytetrafluoroethylene
  • the base oil of the fluorine-containing grease for semiconductor equipment of the present invention uses perfluoropolyether (PFFPE).
  • the perfluoropolyether has excellent fluidity, little oxidation degradation and evaporation, maintains stable performance for a long time, and has low surface friction.
  • the additive of the fluorine-containing grease for semiconductor equipment of the present invention uses sulfurized bis (dibutylcarbamodithioato) di- ⁇ -oxodioxodimolybdenum (dibutylcarbamodithioato) di- ⁇ -oxodioxodimolybdenum).
  • Sulfurized bis di- ⁇ -oxodioxodioldinum (sulfurized bis (dibutylcarbamodithioato) di- ⁇ -oxodioxodimolybdenum)) is a dry grease for semiconductor equipment and mixed with fluorine-based materials. This is a stable material.
  • the fluorine-containing grease for semiconductor equipment of the present invention is 60% by mass to 90% by mass of perfluoropolyether (PFPE) as a base oil, and 10% by mass to 40% by mass of polytetrafluoroethylene (PTFE) as a thickener.
  • PFPE perfluoropolyether
  • PTFE polytetrafluoroethylene
  • Sulfurized bis (dibutylcarbamodithioato) di- ⁇ -oxodioxodimolybdenum sulfurized bis (dibutylcarbamodithioato) di- ⁇ -oxodioxodimolybdenum)
  • Sulfurized bis (dibutylcarbamodithioato) di- ⁇ -oxodioxodimolybdenum)) as an additive at least 0.1% to 10% by mass It is a composition.
  • the fluorine-containing grease for semiconductor equipment 73% by mass of perfluoropolyether (PFPE) as a base oil, 25% by mass of polytetrafluoroethylene (PTFE) as a thickener, additive It is a composition comprising at least 2% by mass of sulfurized bis (sulfurized bis (dibutylcarbamodithioato) di- ⁇ -oxodioxodimolybdenum) di- ⁇ -oxodioxodimolybdenum.
  • PFPE perfluoropolyether
  • PTFE polytetrafluoroethylene
  • the fluorine-containing grease for semiconductor equipment is 60% by mass to 90% by mass of perfluoropolyether (PFPE) as a base oil, and polytetrafluoroethylene (PTFE) as a thickener. 10% by mass to 40% by mass, 0.1% by mass of organic sulfurized bis (dibutylcarbamodithioato) di- ⁇ -oxodioxodimolybdenum (di-carbodithioato) di- ⁇ -oxodioxodimolybdenum) It is a structure containing at least 10% by mass.
  • PFPE perfluoropolyether
  • PTFE polytetrafluoroethylene
  • the fluorine-containing grease for semiconductor equipment 73% by mass of perfluoropolyether (PFPE) as a base oil, 25% by mass of polytetrafluoroethylene (PTFE) as a thickener, It is a composition containing at least 2% by mass of organic sulfide bis (dibutylcarmabodithioate) di- ⁇ -oxodioxodioldinum (sulfurized bis (dibutylcarbamodithioato) di- ⁇ -oxodioxodimolybdenum) as an additive.
  • PFPE perfluoropolyether
  • PTFE polytetrafluoroethylene
  • the base oil of the existing fluorine-containing grease uses Fomblin R PFPE from Solvay, but among the "Y, M, W, and Z" types of Solvay Fomblin R PFPE, the medium and low-priced "Y" type is used.
  • the "Y” type which has a relatively low viscosity index (visibility index: an index of stable properties that does not spread at high temperatures and has good fluidity at low temperatures), is known to exhibit many disadvantages in terms of high temperature stability due to the characteristics of semiconductor devices when used in semiconductor equipment. , It is known to exhibit many disadvantages in the life of the lubricant, that is, durability.
  • the perfluoropolyether which is the base of the embodiments of the present invention, uses Fomblin R PFPE of Solvay, but of Fomblin R PFPE "Y, M, W, Z” type of Solvay " By using M "type, the high temperature stability of semiconductor equipment has been improved.
  • viscosity index viscosity index: ASTM D2270
  • surface friction ASTM D1331, 20 ° C (dynes / cm)
  • 4 ball test ASTM D4172 B 75, 1hr, 1200RPM 40kg, average diameter (mm) It was found that the lower the value of), the better the performance as a lubricant.
  • PFPE perfluoropolyether
  • the additive of the embodiments of the present invention has a direct relationship with the abrasion resistance of the semiconductor equipment as described above, so it can influence the life of the expensive semiconductor equipment.
  • the base oil and thickener fluorine-based material of the present invention is a stable material that is not mixed unless it is a fluorine-based system, sulfurized bis (dibutylcarmabothiothio) di- ⁇ -oxodioxodiololidenum (sulfurized bis (dibutylcarbamodithioato) di- ⁇ -oxodioxodimolybdenum).
  • the sulfurized bis (dibutylcarmabodithioate) di- ⁇ -oxodioxodiol-diol (sulfurized bis (dibutylcarbamodithioato) di- ⁇ -oxodioxodimolybdenum)) is known as molybdenum disulfide in Korean and is an inorganic lubricant. Molybdenum disulfide is used, and it shows simplicity as a dry lubricant, but inorganic molybdenum disulfide has the disadvantage of causing contamination of semiconductor equipment due to its black color and dusting problem.
  • the fluorine-containing grease for semiconductor equipment of the present invention was found to be optimized for semiconductor equipment when an organic molybdenum disulfide (yellow) was used as an additive.
  • the organic-based molybdenum disulfide was confirmed through several experiments as being excellent in lubrication, as well as in a fluorine-based material with little heterogeneity, little equipment contamination, and optimized for wear resistance and extreme pressure environments.
  • the fluorine-containing grease for semiconductor equipment of the present invention is a base oil of M type perfluoropolyether (PFPE) first in a mixing container in a clean room manufacturing environment of 10,000 classes or less due to the characteristics used in semiconductor equipment.
  • PFPE perfluoropolyether
  • Liquid Liquid
  • an organic molybdenum disulfide additive (powder) are added based on the composition ratios of the above-described examples, and then mixed for a period of time to pass through a gel state.
  • It is manufactured to be manufactured by minimizing the oil separation between the thickener and the base oil by distributing the thickener at a constant rate through the first 3 mill rolling process and the second 3 mill rolling process.
  • the manufacturing process is very simple and satisfies the requirements of ultra-low dust generation, which is the most important in the semiconductor manufacturing environment.
  • the fluorine-containing grease for semiconductor equipment of the present invention manufactured by the above process when used in semiconductor equipment, forms a semi-permanent lubricating form that has a thin lubricating film thickness and strong lubricating strength through ion bonding with a metal surface.
  • Test Items unit standard Test result Test Methods Admixture degree (25 °C) 1 / 10mm 310-340 330 KS M 2032 NLGI rating - One One - Thickener - - PTFE - Base oil viscosity (VG 40 °C, 100 °C) cSt - 161, 44.8 KS M 2014 Dropping point °C 220 or more none KS M 2033 Copper plate corrosion (100 °C / 24h) - No color change 1a KS M 2088 Evaporation amount (99 °C / 22h) % 1.8 or less 0.11 KS M 2037 Stability (25 °C) 1 / 10mm 340 or less 328 KS M 2051 Weaning degree (100 °C / 24h) % 5.0 or less 0.08 KS M 2050 4 ball wear mm - 0.48 ASTM D2266
  • the reason for the fluorine-containing grease for semiconductor equipment of the present invention was 0.08 to 0.13, and it is preferable to keep it below 0.9.
  • the 4-ball wear test value of the fluorine-containing grease for semiconductor equipment of the present invention was found to be 0.48 mm-0.56 mm, and preferably maintained at 0.8 mm or less.
  • the present invention is a lubricant grease for semiconductor manufacturing equipment, which has a very high industrial application.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

La présente invention concerne une graisse contenant du fluor pour un équipement à semi-conducteur, et l'invention concerne une graisse contenant du fluor pour un équipement à semi-conducteur, comprenant au moins : de 60 à 90 % en poids de perfluoropolyéther (PFPE)-M en tant qu'huile de base; de 10 à 40 % en poids de polytétrafluoroéthylène (PTFE) en tant qu'épaississant; et de 0,1 à 10 % en poids de bis(dibutylcarbamodithioato)di-μ-oxodioxodimolybdène) sulfuré en tant qu'additif.
PCT/KR2018/012693 2018-10-01 2018-10-25 Graisse contenant du fluor pour équipement à semi-conducteur Ceased WO2020071576A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR1020180116732A KR102021703B1 (ko) 2018-10-01 2018-10-01 반도체장비용 불소 함유 그리스
KR10-2018-0116732 2018-10-01

Publications (1)

Publication Number Publication Date
WO2020071576A1 true WO2020071576A1 (fr) 2020-04-09

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PCT/KR2018/012693 Ceased WO2020071576A1 (fr) 2018-10-01 2018-10-25 Graisse contenant du fluor pour équipement à semi-conducteur

Country Status (2)

Country Link
KR (1) KR102021703B1 (fr)
WO (1) WO2020071576A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102023122435A1 (de) * 2023-08-22 2025-02-27 Tdk Electronics Ag Mischung zur Beschichtung einer elektrischen Vorrichtung, Verfahren zur Herstellung einer Überzugsschicht auf einer elektrischen Vorrichtung und elektrische Vorrichtung

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102732428B1 (ko) * 2022-07-08 2024-11-20 주식회사 한국타우 클린룸 내 반도체 생산장비 적용 불소 함유 그리스
KR102732429B1 (ko) * 2022-07-08 2024-11-20 주식회사 한국타우 클린룸 내 디스플레이 생산장비 적용 불소 함유 그리스
KR102558260B1 (ko) * 2023-03-06 2023-07-24 (주)루브텍시스템 카메라 모듈 액추에이터용 불소 함유 윤활제 및 이의 제조방법.

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JP4505954B2 (ja) * 2000-06-12 2010-07-21 Ｎｏｋクリューバー株式会社 潤滑グリース組成物
US20100222244A1 (en) * 2006-01-17 2010-09-02 Patrizia Maccone Lubricating compositions based on perfluoropolyethers
JP5073986B2 (ja) * 2006-08-01 2012-11-14 協同油脂株式会社 グリース組成物及び軸受
KR20140018369A (ko) * 2011-06-17 2014-02-12 클뢰버 루브리케이션 뮌헨 에스이 운트 코.카게 퍼플루오로폴리에테르계 윤활그리스
JP2018505250A (ja) * 2014-12-15 2018-02-22 ソルベイ スペシャルティ ポリマーズ イタリー エス．ピー．エー． フッ素化ポリマーを含む水性組成物

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IT1290428B1 (it) 1997-03-21 1998-12-03 Ausimont Spa Grassi fluorurati

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JP4505954B2 (ja) * 2000-06-12 2010-07-21 Ｎｏｋクリューバー株式会社 潤滑グリース組成物
US20100222244A1 (en) * 2006-01-17 2010-09-02 Patrizia Maccone Lubricating compositions based on perfluoropolyethers
JP5073986B2 (ja) * 2006-08-01 2012-11-14 協同油脂株式会社 グリース組成物及び軸受
KR20140018369A (ko) * 2011-06-17 2014-02-12 클뢰버 루브리케이션 뮌헨 에스이 운트 코.카게 퍼플루오로폴리에테르계 윤활그리스
JP2018505250A (ja) * 2014-12-15 2018-02-22 ソルベイ スペシャルティ ポリマーズ イタリー エス．ピー．エー． フッ素化ポリマーを含む水性組成物

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102023122435A1 (de) * 2023-08-22 2025-02-27 Tdk Electronics Ag Mischung zur Beschichtung einer elektrischen Vorrichtung, Verfahren zur Herstellung einer Überzugsschicht auf einer elektrischen Vorrichtung und elektrische Vorrichtung

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