US20190276763A1 - Grease composition and rolling bearing - Google Patents

Grease composition and rolling bearing Download PDF

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Publication number
US20190276763A1
US20190276763A1 US16/425,508 US201916425508A US2019276763A1 US 20190276763 A1 US20190276763 A1 US 20190276763A1 US 201916425508 A US201916425508 A US 201916425508A US 2019276763 A1 US2019276763 A1 US 2019276763A1
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Prior art keywords
mass
thickener
soap
fluorine
grease composition
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US16/425,508
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Inventor
Yusuke Asai
Yusuke Enomoto
Shintaro TAKATA
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MinebeaMitsumi Inc
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MinebeaMitsumi Inc
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Priority claimed from PCT/JP2017/043140 external-priority patent/WO2018101432A1/ja
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Assigned to MINEBEA MITSUMI INC. reassignment MINEBEA MITSUMI INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: ASAI, YUSUKE, Takata, Shintaro, ENOMOTO, YUSUKE
Publication of US20190276763A1 publication Critical patent/US20190276763A1/en
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    • 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
    • C10M169/02—Mixtures of base-materials and thickeners
    • 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
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/028—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms
    • C10M2205/0285—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms used as base material
    • 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
    • C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/16—Paraffin waxes; Petrolatum, e.g. slack wax
    • C10M2205/163—Paraffin waxes; Petrolatum, e.g. slack wax used as base material
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
    • C10M2207/123—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic
    • C10M2207/1236—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic used as thickening agent
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/127—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids polycarboxylic
    • C10M2207/1276—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids polycarboxylic used as thickening agent
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/128—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
    • C10M2207/1285—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof used as thickening agents
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28—Esters
    • C10M2207/2805—Esters used as base material
    • 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
    • C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2213/06—Perfluoro polymers
    • C10M2213/0606—Perfluoro polymers used as base material
    • 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
    • C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2213/06—Perfluoro polymers
    • C10M2213/062—Polytetrafluoroethylene [PTFE]
    • C10M2213/0626—Polytetrafluoroethylene [PTFE] used as thickening agents
    • 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
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/08—Amides
    • C10M2215/0813—Amides used as thickening agents
    • 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
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/10—Amides of carbonic or haloformic acids
    • C10M2215/102—Ureas; Semicarbazides; Allophanates
    • C10M2215/1026—Ureas; Semicarbazides; Allophanates used as thickening material
    • 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
    • C10M2290/00—Mixtures of base materials or thickeners or additives
    • C10M2290/10—Thickener
    • 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
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/02—Groups 1 or 11
    • 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
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/04—Groups 2 or 12
    • 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
    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
    • C10N2020/01—Physico-chemical properties
    • C10N2020/055—Particles related characteristics
    • C10N2020/06—Particles of special shape or size
    • 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
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • 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
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/08—Resistance to extreme temperature
    • 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
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/76—Reduction of noise, shudder, or vibrations
    • 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
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/02—Bearings
    • 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—Semi-solids; greasy
    • C10N2210/01—
    • C10N2210/02—
    • C10N2230/08—
    • C10N2230/76—
    • C10N2240/02—

Definitions

  • the present disclosure relates to a grease composition and a rolling bearing, and particularly to a grease composition realizing excellent acoustic characteristics not only under a high temperature and high speed environment but also under a high load environment, and a rolling bearing suitable for a small motor.
  • small diameter ball bearing As a rolling bearing used for small motors such as a fan motor and a high speed motor used for automobiles, there is for example, so-called small diameter ball bearing having an outer diameter of 22 mm or less. Since such a small diameter ball bearing is required to have durability under a high temperature environment, a fluorine-based grease excellent in heat resistance and oxidation resistance, a hybrid grease of a fluorine-based grease and a urea-based grease excellent in heat resistance, and the like are conventionally used as lubricants.
  • Patent Document 1 discloses a rolling bearing filled with a grease containing fluororesin particles as a thickener, a specific aspartic acid ester-based rust inhibitor and an oiliness agent in a fluorine-based base oil (perfluoropolyether oil), in order to realize high temperature durability and low temperature torque property.
  • the above fluorine-based grease particularly a fluorine-based grease using perfluoropolyether as a base oil
  • the fluorine oil (perfluoropolyether) which is a base oil decomposes to generate hydrofluoric acid, whereby corrosion on a metal surface such as a raceway surface of the bearing is caused.
  • the metal corrosion on the raceway surface may become a cause of deterioration of acoustic characteristic and occurrence of rotation failure.
  • the present disclosure has been conceived in view of such a situation, and an object of the present disclosure is to provide a grease composition capable of preventing noise increase under high temperature and high speed condition as well as under a high load condition, and also a rolling bearing excellent in heat-resistant acoustic characteristic and load-bearing acoustic characteristic by applying the grease composition of the present disclosure.
  • the inventors of the present application have conducted intensive studies to achieve the above object and, as a result, found that by blending in base oil specific amounts of three types of thickeners, i.e., a fluorine-based thickener, a urea-based thickener and a soap-based thickener such as a calcium complex soap thickener, a grease composition excellent in heat resistance and load resistance and capable of preventing noise increase in a high temperature and high speed test and a high load test can be obtained.
  • a fluorine-based thickener i.e., a fluorine-based thickener, a urea-based thickener and a soap-based thickener such as a calcium complex soap thickener
  • one aspect according to the present disclosure relates to a grease composition, containing a fluorine-based base oil and a non-fluorine-based base oil as base oils; and a fluorine-based thickener, a urea-based thickener and at least one soap-based thickener selected from the group consisting of a calcium complex soap thickener, a calcium soap thickener, a barium soap thickener, a magnesium soap thickener and a sodium soap thickener as thickeners.
  • the urea-based thickener contains at least one of an aliphatic-aromatic urea, an alicyclic-aliphatic urea and an aliphatic urea.
  • the urea-based thickener contains a diurea compound represented by the following General Formula (1):
  • R 1 and R 3 each independently represent a monovalent aliphatic hydrocarbon group, a monovalent alicyclic hydrocarbon group or a monovalent aromatic hydrocarbon group, and at least one of R 1 and R 3 represents a monovalent aliphatic hydrocarbon group or a monovalent alicyclic hydrocarbon group, and
  • R 2 represents a divalent aromatic hydrocarbon group
  • the grease composition contains 70 mass % to 90 mass % of a total amount of the fluorine-based base oil and the non-fluorine-based base oil, 9 mass % to 18 mass % of the fluorine-based thickener, 0.5 mass % to 7 mass % of the urea-based thickener, and 0.3 mass % to 3 mass % of the calcium complex soap thickener, based on a total amount (100 mass %) of the grease composition.
  • the calcium complex soap thickener is a calcium complex soap of an aliphatic dicarboxylic acid and a monoamide monocarboxylic acid.
  • the grease composition contains 70 mass % to 90 mass % of a total amount of the fluorine-based base oil and the non-fluorine-based base oil, 9 mass % to 18 mass % of the fluorine-based thickener, 0.5 mass % to 7 mass % of the urea-based thickener, and 0.3 mass % to 3 mass % of the calcium soap thickener, based on a total amount of the grease composition.
  • the grease composition contains 70 mass % to 90 mass % of a total amount of the fluorine-based base oil and the non-fluorine-based base oil, 9 mass % to 18 mass % of the fluorine-based thickener, 0.5 mass % to 7 mass % of the urea-based thickener, and 0.6 mass % to 3.6 mass % of the barium soap thickener, based on a total amount of the grease composition.
  • the grease composition contains 70 mass % to 90 mass % of a total amount of the fluorine-based base oil and the non-fluorine-based base oil, 9 mass % to 18 mass % of the fluorine-based thickener, 0.5 mass % to 7 mass % of the urea-based thickener, and 0.6 mass % to 3.6 mass % of the magnesium soap thickener, based on a total amount of the grease composition.
  • the grease composition contains 70 mass % to 90 mass % of a total amount of the fluorine-based base oil and the non-fluorine-based base oil, 9 mass % to 18 mass % of the fluorine-based thickener, 0.5 mass % to 7 mass % of the urea-based thickener, and 0.6 mass % to 3.6 mass % of the sodium soap thickener, based on a total amount of the grease composition.
  • non-fluorine-based base oil is one or more selected from the group consisting of a hydrocarbon-based synthetic oil, an ether-based synthetic oil, an ester-based synthetic oil, and a silicone-based synthetic oil.
  • the present disclosure also relates to a rolling bearing in which the grease composition is filled.
  • FIG. 1 is a schematic view for explaining a structure of a rolling bearing according to the present disclosure.
  • FIG. 2 is a graph showing results (Anderon values of M band) of a heat resistance test and a load resistance test by an Anderon meter when the content of calcium complex soap thickener is changed in a mixed grease of three types of greases, i.e., a fluorine-based grease, a urea-based grease and a calcium complex soap grease.
  • FIG. 3 is a graph showing results (Anderon values of M band) of the heat resistance test and load resistance test by the Anderon meter when the content of calcium soap thickener is changed in a mixed grease of three types of greases, i.e., a fluorine-based grease, a urea-based grease and a calcium soap grease.
  • FIG. 4 is a graph showing results (Anderon values of M band) of the heat resistance test and load resistance test by the Anderon meter when the content of barium soap thickener is changed in a mixed grease of three types of greases, i.e., a fluorine-based grease, a urea-based grease and a barium soap grease.
  • FIG. 5 is a graph showing results (Anderon values of M band) of the heat resistance test and load resistance test by the Anderon meter when the content of magnesium soap thickener is changed in a mixed grease of three types of greases, i.e., a fluorine-based grease, a urea-based grease and a magnesium soap grease.
  • FIG. 6 is a graph showing results (Anderon values of M band) of the heat resistance test and load resistance test by the Anderon meter when the content of sodium soap thickener is changed in a mixed grease of three types of greases, i.e., a fluorine-based grease, a urea-based grease and a sodium soap grease.
  • FIG. 7 is a graph showing results (Anderon values of M band) of the heat resistance test and load resistance test by the Anderon meter when the content of lithium soap thickener is changed in a mixed grease of three types of greases, i.e., a fluorine-based grease, a urea-based grease and a lithium soap grease.
  • the fluorine-based grease has a problem that fluorine oils (base oils) decompose during use under a high load and corrosion of the metal surface occurs due to generation of hydrofluoric acid, and among the fluorine oils, this problem particularly easily occurs in a grease using perfluoropolyether having a straight chain structure as a base oil.
  • the inventors of the present application have investigated a preferred constitution of a grease composition having heat resistance and load resistance, and it is found that blending a hybrid grease of a fluorine-based grease and a urea-based grease which has good heat resistance, with a soap-based grease containing a soap-based thickener such as a calcium complex soap thickener, as a thickener, can lead to solution against corrosion on the raceway surface in a high load condition.
  • a soap-based grease containing a soap-based thickener such as a calcium complex soap thickener
  • the inventors of the present application first compared and examined the influence of the changes in the blending amounts of the urea-based grease and the calcium complex soap grease on the heat resistance and load resistance of a mixed grease by changing their blending amounts while maintaining constant the blending amount of the fluorine-based grease to eliminate the influence of the fluorine-based grease in the mixed grease of the three types of greases (the fluorine-based grease, the urea-based grease, and the calcium complex soap grease as an example of the soap-based grease).
  • a bearing using the mixed grease was rotated under a high temperature and high speed condition or a high load condition, then the acoustic performance was measured using an Anderon meter, and the obtained Anderon value was used as an indicator of heat resistance and load resistance. Therefore, as described later, in the present disclosure, a load resistance test (load resistance evaluation) means an acoustic evaluation test after rotating the bearing under a high load condition, and a heat resistance test (heat resistance evaluation) means an acoustic evaluation test after rotating the bearing under a high temperature environment.
  • FIG. 2 shows results obtained by an Anderon meter in a heat resistance test (preload: 39 N, test temperature: 180° C., rotation speed: 21,000 rpm, 200 hours) and in a load resistance test (preload: 500 N, test temperature: room temperature, rotation speed: 3,000 rpm, 100 hours) when the blending amounts of the fluorine-based grease, the urea-based grease and the calcium complex soap grease are changed in a mixed grease (grease composition) of three types of grease (the fluorine-based grease, the urea-based grease and the calcium complex soap grease).
  • a mixed grease grey composition
  • FIG. 2 shows the content (mass %) of the calcium complex soap thickener based on the total amount of the mixed grease indicated by the horizontal axis, and the Anderon value of M band after each test indicated by the vertical axis, when in mixed greases of three types of grease, the blending amount of the fluorine-based grease is changed from 90 mass % to 49 mass % (the content of the fluorine-based thickener being in the range of 17.8 mass % to 9.8 mass % based on 100 mass % of the mixed grease), the blending amount of the urea-based grease is changed from 0 mass % to 48 mass % (the content of the urea-based thickener being in the range of 0 mass % to 7.2 mass % based on 100 mass % of the mixed grease), and the blending amount of the calcium complex soap grease is changed from 0 mass % to 29 mass % (the content of the calcium complex soap thickener being in the range of 0 mass % to 4.3 mass % based
  • the broken line parallel to the horizontal axis indicates the Anderon value of 15.
  • the Anderon value In the test conditions of the Examples, significant wear was observed when the Anderon value was 15 or more. Therefore, it was evaluated that the Anderon value less than 15 is preferable.
  • the content of the calcium complex soap thickener based on the total amount of the mixed grease is in the range of 0.3 mass % to 3 mass %, particularly 0.5 mass % to 3 mass % (the blending amount of the calcium complex soap grease based on the total amount of the mixed grease being in the range of 2 mass % to 20 mass %, particularly 4 mass % to 20 mass %) in the mixed grease of three types of greases, i.e., the fluorine-based grease, the urea-based grease and the calcium complex soap grease, good acoustic characteristic can be obtained in both the load resistance test and the heat resistance test.
  • the range indicated by the arrow parallel to the horizontal axis indicates the content range of the calcium complex soap thickener which can provide good acoustic characteristic (Anderon value: less than 15) in both the load resistance test and the heat resistance test.
  • a grease composition to be filled in a rolling bearing according to the present disclosure (hereinafter simply referred to as “grease composition”) is characterized by combining specific thickeners as described below in detail.
  • FIG. 1 is a cross-sectional view of a rolling bearing (ball bearing) 10 according to a preferred embodiment of the present disclosure.
  • the rolling bearing 10 has a basic structure similar to that of the conventional rolling bearing and includes an annular inner ring 11 , an annular outer ring 12 , a plurality of rolling elements 13 , a cage 14 , and annular sealing members 15 ( 15 a , 15 b ).
  • the inner ring 11 is a cylindrical structure to be disposed coaxially with a central axis of a shaft.
  • the outer ring 12 is a cylindrical structure disposed coaxially with the inner ring 11 on an outer circumferential side of the inner ring 11 .
  • Each of the plurality of rolling elements 13 is a sphere (ball) disposed on a raceway in a bearing space (annular space) 16 formed between the inner ring 11 and the outer ring 12 . That is, the rolling bearing 10 in the present embodiment is a ball bearing.
  • a grease composition G is filled as a lubricant.
  • the annular sealing members 15 are formed of, for example, a steel plate extending from an inner circumferential surface of the outer ring 12 toward the inner ring 11 side, and seal the bearing space 16 from the outside.
  • the amount of the grease composition G filled in the bearing space 16 is, for example, 5% to 50% of the volume of the bearing space 16 . An amount of about 25% to 35% is preferred in order to achieve both the torque performance and the life performance.
  • a raceway 12 a being a concave portion having an arc-shaped cross section is formed in a circumferential direction of the outer ring 12 .
  • a raceway 11 a being a concave portion having an arc-shaped section is formed in a circumferential direction of the inner ring 11 .
  • the plurality of rolling elements 13 are guided in the circumferential direction by the raceway 11 a and the raceway 12 a.
  • the cage 14 is disposed in the track and is configured to retain the plurality of rolling elements 13 .
  • the cage 14 is an annular member installed coaxially with the central axis of the shaft, and includes a plurality of concave portions (ball pockets) for retaining the rolling elements 13 around the central axis.
  • the shape (such as crown shape or ribbon type) and the material (such as steel plate or resin) of the cage 14 can be selected appropriately and are not limited to specific shapes and materials.
  • the grease composition G acts to reduce the friction between the rolling elements 13 and the cage 14 and the friction between the rolling elements 13 and the inner ring 11 or the outer ring 12 .
  • the grease composition G filled in the rolling bearing 10 enters between the rolling element 13 and the inner ring 11 or the outer ring 12 when the rolling bearing 10 rotates.
  • a fluorine-based base oil and a non-fluorine-based base oil are used as base oils.
  • fluorine-based base oil examples include those containing perfluoropolyether (PFPE) as a main component.
  • PFPE perfluoropolyether
  • PFPE is a compound represented by the general formula: RfO(CF 2 O) p (C 2 F 4 O) q (C 3 F 6 O) r Rf (Rf: perfluoro lower alkyl group; p, q, and r: integer).
  • Perfluoropolyether is broadly classified into a linear perfluoropolyether and a side-chain perfluoropolyether, and the linear perfluoropolyether has a smaller temperature dependency of kinetic viscosity than the side-chain perfluoropolyether. This means that the linear perfluoropolyether has a lower viscosity than the side-chain perfluoropolyether in a low temperature environment and has a higher viscosity than the side-chain perfluoropolyether in a high temperature environment.
  • the viscosity in a high temperature environment be high, that is, it is preferable to use a linear perfluoropolyether.
  • the non-fluorine-based base oil is not particularly limited, and hydrocarbon-based synthetic oils, ether-based synthetic oils such as alkyl ether oils and alkyl diphenyl ether oils, ester-based synthetic oils, and silicone-based synthetic oils, which are generally used as a grease base oil, can be used alone or in combination as the non-fluorine-based base oil.
  • hydrocarbon-based synthetic oils examples include polyalphaolefins (PAO) such as normal paraffin, isoparaffin, polybutene, polyisobutylene, a 1-decene oligomer, a 1-decenethylene oligomer or the like.
  • PAO polyalphaolefins
  • ester-based synthetic oils examples include: diester oils such as dibutyl sebacate, di-2-ethylhexyl sebacate, dioctyl sebacate, dioctyl adipate, diisodecyl adipate, ditridecyl adipate, ditridecyl phthalate, and methyl acetylcinolate; aromatic ester oils such as trioctyl trimellitate, tri-2-ethylhexyl trimellitate, tridecyl trimellitate, tetraoctyl pyromellitate and tetra-2-ethylhexyl pyromellitate; polyol ester oils such as trimethylolpropane caprylate, trimethylolpropane pelargonate, pentaerythritol-2-ethylhexanoate and pentaerythritol pelargonate; and carbonate ester oils.
  • alkyl diphenyl ether oils examples include monoalkyl diphenyl, dialkyl diphenyl, polyalkyl diphenyl, or the like.
  • aromatic ester oils are preferred, and can be used alone or in combination.
  • the blending proportion of the fluorine-based base oil and the non-fluorine-based base oil is not particularly limited, and for example, the ratio (fluorine-based base oil: non-fluorine-based base oil) based on the total amount (100 mass %) of the base oils can be (95 mass % to 5 mass %: 5 mass % to 95 mass %), or more preferably, (95 mass % to 40 mass %: 5 mass % to 60 mass %),
  • the total amount of the fluorine-based base oil and the non-fluorine-based base oil in the total amount of the grease composition according to the present disclosure can be 70 mass % to 90 mass %, preferably 75 mass % to 95 mass % and more preferably 75 mass % to 85 mass %.
  • a fluorine-based thickener, a urea-based thickener and at least one soap-based thickener selected from the group consisting of a calcium complex soap thickener, a calcium soap thickener, a barium soap thickener, a magnesium soap thickener and a sodium soap thickener are added as thickeners to the grease composition according to an embodiment of the present invention.
  • the total amount of the fluorine-based thickener, the urea-based thickener and at least one soap-based thickener selected from the group consisting of a calcium complex soap thickener, a calcium soap thickener, a barium soap thickener, a magnesium soap thickener and a sodium soap thickener is 10 mass % to 30 mass %, particularly 10 mass % to 20 mass %, based on the total amount of the grease composition.
  • fluororesin particles are preferred, and for example, particles of polytetrafluoroethylene (PTFE) are preferably used.
  • PTFE is a polymer of tetrafluoroethylene and is represented by the general formula: [C 2 F 4 ] n (n: degree of polymerization).
  • fluorine-based thickener examples include a perfluoroethylene propylene copolymer (FEP), an ethylene tetrafluoroethylene copolymer (ETFE), and a tetrafluoroethylene perfluoroalkyl vinyl ether copolymer (PFA).
  • FEP perfluoroethylene propylene copolymer
  • ETFE ethylene tetrafluoroethylene copolymer
  • PFA tetrafluoroethylene perfluoroalkyl vinyl ether copolymer
  • the size of the PTFE particles is not particularly limited, and for example, polytetrafluoroethylene having an average particle size of 0.5 ⁇ m to 100 ⁇ m can be used.
  • the shape of the PTFE particles is not particularly limited, and may be spherical, polyhedral, needle-like, or other shapes.
  • the fluorine-based thickener is preferably used in an amount of 9 mass % to 18 mass % based on the total amount of the grease composition.
  • the urea compound is excellent in both heat resistance and water resistance, and is particularly excellent in stability at a high temperature, it is suitably used as a thickener for the parts subjected to a high temperature environment.
  • a urea compound such as a diurea compound, a triurea compound, and a polyurea compound can be used as the urea-based thickener. Particularly, from the viewpoint of heat resistance and acoustic characteristic (quietness), it is preferable to use a diurea compound.
  • the type of the urea compound preferably includes at least one of an aliphatic-aromatic urea, an alicyclic-aliphatic urea and an aliphatic urea.
  • Urea compounds conventionally known can be used as the above mentioned urea-based thickeners.
  • the diurea compound represented by the following General Formula (1) is a urea-based thickener suitable for an embodiment according to the present invention.
  • R 2 represents a divalent aromatic hydrocarbon group.
  • Examples of the monovalent aliphatic hydrocarbon group include a linear or branched, saturated or unsaturated alkyl group having 6 to 26 carbon atoms.
  • Examples of the monovalent alicyclic hydrocarbon group include a cycloalkyl group having 5 to 12 carbon atoms.
  • examples of the aromatic hydrocarbon group include a monovalent or divalent aromatic hydrocarbon group having 6 to 20 carbon atoms.
  • the urea compound used as the urea-based thickener can be synthesized using an amine compound and an isocyanate compound.
  • Examples of the amine compound to be used here include: aliphatic amines represented by hexylamine, octylamine, dodecylamine, hexadecylamine, octadecylamine, stearylamine, oleylamine or the like; cycloaliphatic amines represented by cyclohexylamine or the like; and aromatic amines represented by aniline, p-toluidine, ethoxyphenylamine or the like.
  • isocyanate compound examples include: aromatic diisocyanates such as phenylene diisocyanate, tolylene diisocyanate, diphenyl diisocyanate, and diphenylmethane diisocyanate; and aliphatic diisocyanates such as octadecane diisocyanate, decane diisocyanate, and hexane diisocyanate.
  • aromatic diisocyanates such as phenylene diisocyanate, tolylene diisocyanate, diphenyl diisocyanate, and diphenylmethane diisocyanate
  • aliphatic diisocyanates such as octadecane diisocyanate, decane diisocyanate, and hexane diisocyanate.
  • an aliphatic-aromatic diurea compound obtained by using an aliphatic amine and an aromatic amine as an amine raw material and an aromatic diisocyanate it is preferable to use an aliphatic-aromatic diurea compound obtained by using an aliphatic amine and an aromatic amine as an amine raw material and an aromatic diisocyanate to carry out the synthesis.
  • the urea-based thickener is preferably used in an amount of 0.5 mass % to 7 mass % based on the total amount of the grease composition.
  • a soap-based thickener is used in an embodiment according to the present invention, in addition to the above fluorine-based thickener and urea-based thickener.
  • a calcium complex soap thickener a calcium soap thickener, a barium soap thickener, a magnesium soap thickener, and a sodium soap thickener can be used as the soap-based thickener.
  • a calcium complex soap having improved heat resistance it is preferable to use a calcium complex soap having improved heat resistance in an embodiment according to the present invention.
  • a calcium complex soap of a higher fatty acid and a lower fatty acid a calcium complex soap containing a calcium salt of a dibasic acid and a fatty acid, or the like can be used.
  • a calcium complex soap of an aliphatic dicarboxylic acid and a monoamide monocarboxylic acid is preferable to use as the calcium complex soap thickener to be used in the grease composition according to an embodiment of the present invention.
  • a saturated or unsaturated dicarboxylic acid having 2 to 20 carbon atoms is used as the aliphatic dicarboxylic acid.
  • saturated dicarboxylic acid examples include an oxalic acid, a malonic acid, a succinic acid, a methylsuccinic acid, a glutaric acid, an adipic acid, a pimelic acid, a suberic acid, an azelaic acid, a sebacic acid, a nonamethylenedicarboxylic acid, a decamethylene dicarboxylic acid, an undecane dicarboxylic acid, a dodecane dicarboxylic acid, a tridecane dicarboxylic acid, a tetradecane dicarboxylic acid, a pentadecane dicarboxylic acid, a hexadecane dicarboxylic acid, a heptadecane dicarboxylic acid, and an octadecane dicarboxylic acid.
  • adipic acid Preferably used are an adipic acid, a pimelic acid, a suberic acid, an azelaic acid, a sebacic acid, a nonamethylenedicarboxylic acid, a decamethylene dicarboxylic acid, an undecane dicarboxylic acid, a dodecane dicarboxylic acid, a tridecane dicarboxylic acid, a tetradecane dicarboxylic acid, a pentadecane dicarboxylic acid, a hexadecane dicarboxylic acid, a heptadecane dicarboxylic acid, and an octadecane dicarboxylic acid.
  • unsaturated dicarboxylic acid for example, a maleic acid, a fumaric acid, alkenyl succinic acids such as a 2-methylene succinic acid, a 2-ethylene succinic acid, and a 2-methylene glutaric acid are used.
  • saturated or unsaturated dicarboxylic acids may be used alone or in combination of two or more.
  • Examples of the monoamide monocarboxylic acid include those in which one carboxyl group in the aliphatic dicarboxylic acid is amidated.
  • examples of the amine for amidating the carboxyl group include: aliphatic primary amines such as butylamine, amylamine, hexylamine, heptylamine, octylamine, nonylamine, decylamine, laurylamine, myristylamine, palmitylamine, stearylamine, and behenylamine; aliphatic secondary amines such as dipropylamine, diisopropylamine, dibutylamine, diamylamine, dilaurylamine, monomethyllaurylamine, distearylamine, monomethylstearylamine, dimyristylamine, and dipalmitylamine; aliphatic unsaturated amines such as allylamine, diallylamine, oleylamine, and dioleylamine; alicyclic amines such as cyclopropylamine, cyclobutylamine, cyclopentylamine, and cyclohex
  • hexylamine, heptylamine, octylamine, nonylamine, decylamine, laurylamine, myristylamine, palmitylamine, stearylamine, behenylamine, dibutylamine, diamylamine, monomethyllaurylamine, monomethylstearylamine, and oleylamine are preferably used.
  • a commercially available product can suitably be used as the calcium complex soap thickener.
  • a calcium complex soap obtained by adding an aliphatic dicarboxylic acid and a monoamide monocarboxylic acid to a non-fluorine-based base oil, performing heating and stirring under a temperature at which stirring is possible, the reaction proceeds efficiently, and the base oil does not deteriorate (for example, about 80° C. to 180° C.), and adding calcium hydroxide thereto, may also be used.
  • the calcium complex soap thickener is preferably used in an amount of 0.3 mass % to 3 mass % based on the total amount of the grease composition.
  • a metal salt of an aliphatic monocarboxylic acid that is, a calcium salt, a barium salt, a magnesium salt or a sodium salt of an aliphatic monocarboxylic acid, can be used as the calcium soap thickener, the barium soap thickener, the magnesium soap thickener and the sodium soap thickener.
  • the aliphatic carboxylic acid may be any of linear, branched, saturated and unsaturated, and generally fatty acids having about 2 to 30 carbon atoms, for example, 12 to 24 carbon atoms can be used. Specific example thereof include: saturated fatty acids such as a butyric acid, a caproic acid, a caprylic acid, a pelargonic acid, a capric acid, a lauric acid, a myristic acid, a palmitic acid, a stearic acid, and a behenic acid; and unsaturated fatty acids such as an oleic acid, a linoleic acid, a lysic acid, and a ricinoleic acid (ricinoleic acid).
  • saturated fatty acids such as a butyric acid, a caproic acid, a caprylic acid, a pelargonic acid, a capric acid, a lauric acid, a myristic acid, a palmitic acid,
  • a calcium salt, a barium salt, a magnesium salt, a sodium salt of the stearic acid, the lauric acid and the ricinoleic acid can be used as representative examples of the calcium soap thickener, the barium soap thickener, the magnesium soap thickener and the sodium soap thickener.
  • the calcium soap thickener is preferably used in an amount of 0.3 mass % to 3 mass % based on the total amount of the grease composition.
  • the barium soap thickener is preferably used in an amount of 0.6 mass % to 3.6 mass % based on the total amount of the grease composition; the magnesium soap thickener is preferably used in an amount of 0.6 mass % to 3.6 mass % based on the total amount of the grease composition; and the sodium soap thickener is preferably used in an amount of 0.6 mass % to 3.6 mass % based on the total amount of the grease composition.
  • the grease composition may contain additives usually used in the grease composition, if necessary, within a range not hindering the effects of the present invention.
  • additives examples include an antioxidant, an extreme pressure agent, a metal deactivator, a friction inhibitor (anti-wear agent), a rust inhibitor, an oiliness improver, a viscosity index improver, and a viscosifier.
  • the total amount of the additives is generally 0.1 mass % to 10 mass % based on the total amount of the grease composition.
  • antioxidants examples include: hindered phenol-based antioxidants such as octadecyl-3-(3,5-di-t-butyl-4-hydroxyphenyl) propionate, pentaerythritol tetrakis[3-(3,5-di-t-butyl-4-hydroxyphenyl) propionate], 2,4-bis-(n-octylthio)-6-(4-hydroxy-3,5-di-t-butylanilino)-1,3,5-triazine, 1,3,5-trimethyl-2,4,6-tris(3,5-di-t-butyl-4-hydroxybenzyl) benzene, triethylene glycol bis[3-(3-t-butyl-5-methyl-4-hydroxyphenyl) propionate], 1,6-hexanediol-bis[3-(3,5-di-t-butyl-4-hydroxyphenyl) propionate], 2,2-thio-diethylene bis
  • extreme pressure agent examples include: phosphorus compounds such as phosphate ester, phosphite ester, and phosphate ester amine salt; sulfur compounds such as sulfides and disulfides; chlorinated compounds such as chlorinated paraffin and chlorinated diphenyl; and metal salts of a sulfur compound such as zinc dialkyldithiophosphate and molybdenum dialkyldithiocarbamate.
  • phosphorus compounds such as phosphate ester, phosphite ester, and phosphate ester amine salt
  • sulfur compounds such as sulfides and disulfides
  • chlorinated compounds such as chlorinated paraffin and chlorinated diphenyl
  • metal salts of a sulfur compound such as zinc dialkyldithiophosphate and molybdenum dialkyldithiocarbamate.
  • metal deactivator examples include benzotriazole and sodium nitrite.
  • anti-wear agent examples include tricresyl phosphate and polymer esters.
  • polymer esters examples include esters of aliphatic monovalent carboxylic acids and divalent carboxylic acids with polyhydric alcohols. Specific examples of the polymer esters include, but are not limited to, PRIOLUBE (registered trademark) series manufactured by Croda Japan KK.
  • the grease composition according to an embodiment of the present invention can be obtained by mixing the above various base oils and various thickeners at a predetermined proportion and optionally adding other additives.
  • the grease composition may also be produced by blending three types of greases, i.e., a fluorine-based grease containing a fluorine-based base oil and a fluorine-based thickener, a urea-based grease containing a non-fluorine-based base oil and a urea-based thickener, and a soap-based grease (a calcium complex soap grease, a calcium soap grease, a barium soap grease, a magnesium soap grease, or a sodium soap grease) containing a non-fluorine-based base oil and a soap-based thickener (a calcium complex soap thickener, a calcium soap thickener, a barium soap thickener, a magnesium soap thickener, or a sodium soap thickener), with other additives if desired.
  • the grease composition may also be produced by blending one or two of the above base greases with the remaining base oil and thickener and, if desired, other additives.
  • the content of the thickener based on the base grease is about 10 mass % to 30 mass %.
  • the content of each thickener based on the respective base grease is as follows: fluorine-based thickener: 15 mass % to 30 mass %; urea-based thickener: 10 mass % to 20 mass %; and soap-based thickener (calcium complex soap thickener, calcium soap thickener, barium soap thickener, magnesium soap thickener, or sodium soap thickener): 10 mass % to 20 mass %.
  • the rolling bearing of the present embodiment is particularly preferably used as a rolling bearing of small motors (e.g., brushless motors and fan motors) of automobiles, household electric appliances, information equipment and the like.
  • small motors e.g., brushless motors and fan motors
  • rolling bearing is cited as a ball bearing in the above embodiment, the present invention is not limited to this but can be applied to other rolling bearings, for example, roller bearings.
  • non-fluorine-based base oil synthetic oil 1, mixed oil of polyalphaolefin oil and ester oil
  • non-fluorine-based base oil synthetic oil 2, polyalphaolefin oil
  • fluorine-based thickener PTFE (polytetrafluoroethylene, particle size 10 ⁇ m to 25 ⁇ m
  • urea-based thickener urea compound containing aliphatic-aromatic urea
  • urea-based thickener urea compound containing alicyclic-aliphatic urea
  • urea-based thickener urea compound containing aliphatic urea
  • Ca complex soap thickener calcium complex soap of aliphatic dicarboxylic acid and monoamide monocarboxylic acid
  • Ba soap thickener 12OHBa soap (barium 12-hydroxystearate)
  • Li soap thickener 12OHLi soap (lithium 12-hydroxystearate)
  • the urea-based thickeners (b2-1 to b2-3) are added in an amount of 10 mass % to 20 mass % based on the total amount of the base grease containing the urea-based thickener and the non-fluorine-based base oil: synthetic oil 1 (a2).
  • the Ca complex soap thickener (b3-1), the Ca soap thickener (b3-2), the Ba soap thickener (b3-3), the Mg soap thickener (b3-4), the Na soap thickener (b3-5), or the Li soap thickener (b3-6) is added in an amount of 10 mass % to 20 mass % based on the total amount of the base grease containing the complex soap thickener, the Ca soap thickener, the Ba soap thickener, the Mg soap thickener, the Na soap thickener, or the Li soap thickener and the non-fluorine-based base oil: synthetic oil 2 (a3).
  • the other additives were added such that the total amount of the above antioxidant and extreme pressure agent was 3 mass % based on the grease composition (total mass) of Examples and Comparative Example.
  • the test grease composition was filled in a steel shielded ball bearing (inner diameter 8 mm, outer diameter 22 mm, width 7 mm) at 25% to 35% of the bearing volume.
  • the ball bearing was set in a housing and a preload of 39 N was applied to the outer ring from the axial direction. Then a shaft was inserted into the inner diameter of the bearing and the shaft was connected to a rotation shaft of a test motor, so that the inner ring of the ball bearing was arranged to be rotated.
  • the housing was heated to 180° C.
  • the ball bearing was rotated at a test temperature of 180° C. and a rotation speed of 21,000 rpm for 200 hours, and then subjected to an acoustic evaluation test according to the following procedures.
  • Each test grease of examples and comparative example was tested three times to obtain the average value.
  • the test grease composition was filled in a steel shielded ball bearing (inner diameter 8 mm, outer diameter 22 mm, width 7 mm) at 25% to 35% of the bearing volume.
  • the ball bearing was set in a housing and a preload of 500 N was applied to the outer ring from the axial direction. Then a shaft was inserted into the inner diameter of the bearing and the shaft was connected to a rotation shaft of a test motor, so that the inner ring of the ball bearing was arranged to be rotated.
  • the ball bearing was rotated at room temperature at a rotation speed of 3,000 rpm for 100 hours, and then subjected to an acoustic evaluation test according to the following procedures.
  • Each test grease of examples and comparative example was tested three times to obtain the average value.
  • the acoustic performance of the ball bearing using the test grease composition was evaluated by measuring the Anderon value of M band (300 Hz to 1800 Hz) using an Anderon meter.
  • Blending amount in the table in terms of mass % is a value based on the total mass of the grease composition.
  • FIG. 2 shows the results of the respective Anderon values of the M band after the heat resistance test and load resistance test for grease compositions (Examples 1 to 15, Comparative Examples 11 to 13, Comparative Example 15, Comparative Example 17, and Comparative Example 18) in which the content of a fluorine-based thickener is 17.8 mass % to 9.8 mass % (blending amount of the fluorine-based grease based on the total amount of the grease composition: 90 mass % to 49 mass %), the content of the urea-based thickener is 0 mass % to 7.2 mass % (blending amount of the urea-based grease: 0 mass % to 48 mass %), and the content of the calcium complex soap thickener is 0 mass % to 4.3 mass % (blending amount of the calcium complex soap grease: 0 mass % to 29 mass %).
  • a fluorine-based thickener is 17.8 mass % to 9.8 mass % (blending amount of the fluorine-based grease based on the total amount of the grease composition:
  • the horizontal axis represents the content (mass %) of the calcium complex soap thickener based on the total amount of grease composition
  • the vertical axis represents the Anderon value of M band after the tests.
  • the broken line parallel to the horizontal axis indicates an Anderon value of 15, and the range indicated by the arrow parallel to the horizontal axis indicates the content range of the calcium complex soap thickener which can obtain good acoustic characteristic in both the load resistance test and the heat resistance test.
  • the Anderon value For the acoustic characteristic after the load resistance test, as the content of the calcium complex soap thickener becomes smaller than 0.3 mass %, the Anderon value rapidly increases; on the other hand, when the content of the calcium complex soap thickener is larger than 0.3 mass %, the Anderon value is less than 15 and the acoustic characteristics are stable in a good state.
  • the Anderon value For the acoustic characteristics after the heat resistance test, as the content of the calcium complex soap thickener becomes larger than 3 mass %, the Anderon value rapidly increases; on the other hand, when the content of the calcium complex soap thickener is smaller than 3 mass %, the Anderon value is less than 15 and the acoustic characteristics are stable in a good state.
  • FIG. 3 shows the results of the respective Anderon values of the M band after the heat resistance test and load resistance test for grease compositions (Examples 16 to 30, Comparative Examples 11 to 13, Comparative Example 20, Comparative Example 22, and Comparative Example 23) in which the content of the calcium soap thickener based on the total amount of the grease composition is 0 mass % to 4.3 mass % (blending amount of the calcium soap grease based on the total amount of the grease composition: 0 mass % to 29 mass %).
  • the horizontal axis represents the content (mass %) of the calcium soap thickener based on the total amount of grease composition
  • the vertical axis represents the Anderon value of M band after the tests.
  • the broken line attached parallel to the horizontal axis indicates an Anderon value of 15
  • the range indicated by the arrows provided parallel to the horizontal axis indicates the content range of the calcium soap thickener which can obtain good acoustic characteristic in both the load resistance test and the heat resistance test.
  • FIG. 4 shows the results of the respective Anderon values of the M band after the heat resistance test and load resistance test for grease compositions (Examples 31 to 42, Comparative Examples 11 to 13, Comparative Example 24, and Comparative Examples 26 to 30) in which the content of the barium soap thickener based on the total amount of the grease composition is in the range of 0 mass % to 5.4 mass % (blending amount of the barium soap grease based on the total amount of the grease composition: 0 mass % to 36 mass %).
  • the horizontal axis represents the content (mass %) of the barium soap thickener based on the total amount of grease composition
  • the vertical axis represents the Anderon value of M band after the tests.
  • the broken line parallel to the horizontal axis indicates an Anderon value of 15
  • the range indicated by the arrow parallel to the horizontal axis indicates the content range of the barium soap thickener which can obtain good acoustic characteristic in both the load resistance test and the heat resistance test.
  • FIG. 5 shows the results of the respective Anderon values of the M band after the heat resistance test and load resistance test for grease compositions (Examples 43 to 54, Comparative Examples 11 to 13, Comparative Example 31, and Comparative Examples 33 to 37) in which the content of the magnesium soap thickener based on the total amount of the grease composition is in the range of 0 mass % to 5.4 mass % (blending amount of the magnesium soap grease based on the total amount of the grease composition: 0 mass % to 36 mass %).
  • the horizontal axis represents the content (mass %) of the magnesium soap thickener based on the total amount of grease composition
  • the vertical axis represents the Anderon value of M band after the tests.
  • the broken line parallel to the horizontal axis indicates an Anderon value of 15
  • the range indicated by the arrow parallel to the horizontal axis indicates the content range of the magnesium soap thickener which can obtain good acoustic characteristics in both the load resistance test and the heat resistance test.
  • FIG. 6 shows the results of the respective Anderon values of the M band after the heat resistance test and load resistance test for grease compositions (Examples 55 to 66, Comparative Examples 11 to 13, Comparative Example 38, and Comparative
  • the horizontal axis represents the content (mass %) of the sodium soap thickener based on the total amount of grease composition, and the vertical axis represents the Anderon value of M band after the tests.
  • the broken line parallel to the horizontal axis indicates an Anderon value of 15
  • the range indicated by the arrow parallel to the horizontal axis indicates the content range of the sodium soap thickener which can obtain good acoustic characteristics in both the load resistance test and the heat resistance test.
  • the content of the calcium soap thickener is between 0.3 mass % and 3 mass %
  • the content of the barium soap thickener is between 0.6 mass % and 3.6 mass %
  • the content of the magnesium soap thickener is between 0.6 mass % and 3.6 mass %
  • the content of the sodium soap thickener is between 0.6 mass % and 3.6 mass %.
  • the acoustic characteristic shows the same tendency as the acoustic characteristic of the grease composition using the calcium complex soap thickener in FIG. 2 .
  • FIG. 7 shows the results of the respective Anderon values of the M band after the heat resistance test and load resistance test for grease compositions (Comparative Example 11 to Comparative Example 13, and Comparative Example 45 to Comparative Example 51) in which the content of the lithium soap thickener based on the total amount of the grease composition is in the range of 0 mass % to 4.3 mass % (blending amount of the lithium soap grease based on the total amount of the grease composition: 0 mass % to 29 mass %).
  • the horizontal axis represents the content (mass %) of the lithium soap thickener based on the total amount of grease composition
  • the vertical axis represents the Anderon value of M band after the tests.
  • the broken line parallel to the horizontal axis indicates an Anderon value of 15.
  • the Anderon value remains higher than 15, regardless of the content of the lithium soap thickener.
  • the Anderon value is less than 15, but when the content of the lithium soap thickener is larger than 0.6 mass %, the Anderon value is higher than 15. Accordingly, it is confirmed that when the fluorine-based thickener and the urea-based thickener are used in combination with the lithium soap thickener, good acoustic characteristic cannot be obtained in neither the load resistance test nor the heat resistance test.
  • a grease composition containing the fluorine-based thickener, the urea-based thickener and the calcium complex soap thickener in a specific proportion that is, a grease composition containing 9 mass % to 18 mass % of the fluorine-based thickener, 0.5 mass % to 7 mass % of the urea-based thickener, and 0.3 mass % to 3 mass % of the calcium complex soap thickener based on the total amount of the grease composition as shown in Table 1, the average Anderon value is less than 15 and the acoustic performance is good in both the heat resistance test (180° C., 21,000 rpm, preload: 39 N, 200 hours rotation) and the load resistance test (room temperature, 3,000 rpm, preload: 500 N, 100 hours rotation).
  • the grease composition of the present invention to which a fluorine-based thickener, a urea-based thickener, and a soap-based thickener selected from the group consisting of a calcium complex soap thickener, a calcium soap thickener, a barium soap thickener, a magnesium soap thickener and a sodium soap thickener are added, can prevent noise increase and have good heat resistance (high temperature high speed characteristic) and load resistance (high load characteristic) even in use under a high temperature environment (for example, 180° C. or higher) and under a high load condition (for example, 500 N).
  • the acoustic characteristic is evaluated using a standard small diameter ball bearing having an outer diameter of 22 mm.
  • the rolling bearing to which the present disclosure is directed is not limited to this size, and the size of the rolling bearing according to the embodiment of the present disclosure can be suitably selected, and also the type of the rolling bearing can be suitably selected.

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US16/425,508 2016-11-30 2019-05-29 Grease composition and rolling bearing Abandoned US20190276763A1 (en)

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