JP2019089924A - Thermal conductive oil composition, heat release agent and electronic device - Google Patents

Abstract

To provide a thermal conductive oil composition and a heat release agent, excellent in dripping resistance, and an electronic device in which a thermal conductive oil composition held in a gap between a heat generation member and a cooling member, and a heat release agent are excellent in dripping resistance.SOLUTION: There are provided a thermal conductive oil composition consisting of (A) a heat resistant organic oil, (B) a nonionic surfactant, and (C) a thermal conductive fine particles with content of (A) of 20 to 57 vol.%, content of (C) of 80 to 43 vol.% (total 100 vol.%) and the content of (B) of 0.02 wt.% or more and less than 0.2 wt.% of the content of (C), in which (B) is (B-1) polyoxyethylene-polyoxypropylene glycol having HLB value of more than 1.8 and 18 or less, or (B-2) a nonionic surfactant having HLB value of more than 9.5 and 19 or less and containing a polyoxyethylene unit and a hydrophobic group, and a heat release agent. There is provided an electronic device in which the heat release agent is held in a gap between a heat generation member and a cooling member.SELECTED DRAWING: Figure 1

Description

The present invention relates to a thermally conductive oil composition excellent in thermal conductivity and sag resistance, a heat dissipation agent excellent in thermal conductivity and sag resistance, and an electronic device including the heat dissipation agent.

The non-hardening thermally conductive oil composition mainly composed of a heat resistant oil and thermally conductive fine particles is heat generated from electronic components and chips such as a capacitor, a resistor, a diode, a memory, and a computing element (CPU), Alternatively, it is used as a so-called heat dissipating agent, which is a medium for efficiently transmitting heat generated from a semiconductor package having these electronic components and chips and heat generated from an electronic device such as a circuit board to a heat dissipating member.

Patent Document 1 (Japanese Patent Application Laid-Open No. 2002-201483) discloses a high thermal conductivity grease composition containing an inorganic powder and a base oil containing a mineral oil or a synthetic oil, wherein the inorganic powder contains two types of inorganic materials having different average particle sizes. The base oil contains 0.2 to 2.0% by weight of a surfactant based on the weight of the inorganic powder, 10 to 30% by volume of the base oil, and 70% of the inorganic powder. A high thermal conductivity grease composition has been proposed which is characterized by containing ~ 90 vol%, and it is aimed to be compatible with the high thermal conductivity and the good dispensability.
As the surfactant, a nonionic surfactant having an HLB of 9 or less is preferred in order to obtain good dispensability even at room temperature.

However, the gap between the heat generating member and the cooling member of the electronic component / electronic device or the gap between the high temperature member and the heat radiating member is held, and the holding portion is held vertically or substantially vertically There is a problem that the high thermal conductivity grease composition can not be said to be excellent in sag resistance, as it is unconscious to the usage where it is exposed to a high temperature thermal cycle.

Patent Document 2 (Japanese Patent No. 4899137) has a thermal conductivity comprising (A) heat resistant organic oil, (B) thermally conductive fine particles, and (C) a polyvalent metal salt of a higher fatty acid having 12 or more carbon atoms. Oil composition, in particular, the content of component (A) is 20 to 50% by volume, the content of component (B) is 80 to 50% by volume (total amount 100% by volume), component (C) The said heat conductive oil composition whose content of B is 0.05-5.0 weight% of content of a component (B) is disclosed.

However, even when a large amount of thermally conductive particles is contained, the viscosity is not so large, and the coating workability, the injectability and other workability are excellent, and the object is to have excellent thermal conductivity and heat resistance. And the gap between the heat generating member and the cooling member of the electronic component / electronic device or the gap between the high temperature member and the heat radiating member, and the holding portion is held vertically or substantially vertically for a long time at low temperature and high temperature There is a problem that the heat conductive oil composition can not be said to be excellent in sag resistance because it is unconscious to the usage to which it is exposed to the thermal cycle of the above.

Japanese Patent Laid-Open No. 2002-201483 Patent 4899137 gazette

The inventors of the present invention have conducted intensive studies to develop a thermally conductive oil composition and a heat dissipating agent free from the above problems, and the gap between the heat generating member and the cooling member of the electronic component / electronic device or the high temperature member A thermally conductive oil composition which is sandwiched in a gap between members, and the sandwiching portion is held in the vertical direction or the substantially vertical direction and does not substantially drop even if exposed to low temperature and high temperature cold cycles for a long period of time A heat dissipating agent could be invented.
It is an object of the present invention to be held in a gap between a heat generating member and a cooling member of an electronic component / electronic device, or in a gap between a high temperature member and a heat radiating member, with the sandwiching portion held vertically or substantially vertically. It is an object of the present invention to provide a thermally conductive oil composition and a heat dissipating agent which do not substantially sag even when exposed to low temperature and high temperature cold heat cycles for a long time. An object of the present invention is to provide an electronic device including such a heat dissipating agent.

The means for achieving this purpose is
"The claim 1 of
A heat conductive oil composition comprising (A) heat resistant organic oil, (B) nonionic surfactant and (C) heat conductive fine particles, wherein the content of (A) heat resistant organic oil is 20 to 20. 57% by volume, the content of (C) thermally conductive fine particles is 80 to 43% by volume (total amount 100% by volume), the content of (B) nonionic surfactant is (C) heat conduction Wt% or more and less than 0.2 wt% of the content of the organic fine particles, (B) the nonionic surfactant has (B-1) HLB value of 1.8 or more and 18 or less Polyoxyethylene-polyoxypropylene glycol, or (B-2) a nonionic surfactant having a HLB value of greater than 9.5 and not more than 19 and containing a polyoxyethylene unit and a hydrophobic group Heat conductive oil composition characterized by the above.
Claim 2
The thermally conductive oil composition according to claim 1, wherein the nonionic surfactant (B-2) containing a polyoxyethylene unit and a hydrophobic group further contains a hydroxyl group.
Claim 3
The thermal conductivity according to claim 1 or 2, wherein [the viscosity at 150 ° C] / [the viscosity at 25 ° C] of the thermally conductive oil composition is 0.31 to 20. Oil composition. It consists of

The means for achieving this purpose is
"The claim 4 of
A heat conductive oil composition comprising (A) heat resistant organic oil, (B) nonionic surfactant and (C) heat conductive fine particles, wherein the content of (A) heat resistant organic oil is 20 to 20. 57% by volume, the content of (C) thermally conductive fine particles is 80 to 43% by volume (total amount 100% by volume), the content of (B) nonionic surfactant is (C) heat conduction Wt% or more and less than 0.2 wt% of the content of the organic fine particles, (B) the nonionic surfactant has (B-1) HLB value of 1.8 or more and 18 or less Polyoxyethylene-polyoxypropylene glycol, or (B-2) a nonionic surfactant having a HLB value of greater than 9.5 and not more than 19 and containing a polyoxyethylene unit and a hydrophobic group Characteristic, heat dissipation agent.
Claim 5
The heat dissipating agent according to claim 4, wherein the nonionic surfactant (B-2) containing a polyoxyethylene unit and a hydrophobic group further contains a hydroxyl group.
Claim 6
The heat sink according to claim 4 or 5, wherein the viscosity of the heat sink at 150 ° C / the viscosity at 25 ° C is 0.31 to 20. It consists of

The means for achieving this purpose is
"The claim 7 of
(A) heat resistant organic oil, (B) non-ionic surfactant and (C) heat conduction in the gap between the heat generating member and the cooling member of the electronic component / electronic device or the gap between the high temperature member and the heat radiating member Conductive oil composition comprising fine particles, wherein the content of (A) heat resistant organic oil is 20 to 57% by volume, and the content of (C) heat conductive particles is 80 to 43% by volume ( The total amount is 100% by volume, and the content of (B) the nonionic surfactant is 0.02% by weight or more and less than 0.2% by weight of the content of the (C) thermally conductive fine particles, B) The nonionic surfactant has a (B-1) polyoxyethylene-polyoxypropylene glycol having an HLB value of 1.8 or more and 18 or less, or (B-2) an HLB value of 9.5 or more A heat sink, which is a non-ionic surfactant having a size of 19 or less and containing a polyoxyethylene unit and a hydrophobic group, is sandwiched. An electronic device characterized by
Claim 8
The electronic device according to claim 7, wherein the nonionic surfactant (B-2) containing the polyoxyethylene unit and the hydrophobic group further contains a hydroxyl group. It consists of

The thermally conductive oil composition of the present invention is excellent in thermal conductivity and is held in the gap between the heat generating member and the cooling member of the electronic component / electronic device or in the gap between the high temperature member and the heat radiating member. Even when exposed to a low temperature and high temperature cold cycle for a long period while being held in a direction or substantially vertical direction, the thermally conductive oil composition does not substantially drop.

The heat dissipating agent of the present invention is excellent in thermal conductivity, and is sandwiched between the heat generating member of the electronic component / electronic device and the cooling member, or between the high temperature member and the heat dissipating member. Even when exposed to a low temperature and a high temperature thermal cycle for a long time while being held in a direction, the heat dissipating agent does not substantially drop.

In the electronic device according to the present invention, the heat dissipation agent is held in the gap between the heat generating member and the cooling member of the electronic component / electronic device or the gap between the high temperature member and the heat radiating member, and the holding portion is held vertically or substantially vertically Even when exposed to low-temperature and high-temperature cold cycles for a long period of time, the heat-dissipating agent does not substantially drip down, so that excellent electronic device performance can be exhibited for a long period of time, and the reliability is excellent. effective.

The heat conductive oil composition of the present invention is a heat conductive oil composition comprising (A) heat resistant organic oil, (B) nonionic surfactant and (C) heat conductive fine particles, ) The content of the heat-resistant organic oil is 20 to 57% by volume, and the content of the (C) thermally conductive fine particles is 80 to 43% by volume (total amount 100% by volume); (B) non-ionic interface The content of the active agent is 0.02% by weight or more and less than 0.2% by weight of the content of the (C) heat conductive fine particles, and (B) the nonionic surfactant is (B-1) HLB Polyoxyethylene-polyoxypropylene glycol having a value of 1.8 or more and 18 or less, or (B-2) an HLB value of more than 9.5 and 19 or less, and the polyoxyethylene unit and the hydrophobic group It is characterized by including a nonionic surfactant.

The heat resistant organic oil (A) is a dispersion medium for the (C) thermally conductive fine particles, and has the effect of making the fine particle component (C) into a viscous paste.

(A) The heat resistant organic oil is exemplified by aromatic hydrocarbon oil, phenyl ether oil, aromatic carboxylic acid ester oil, poly α-olefin, and in particular, phenyl ether oil, aromatic carboxylic acid ester oil Or poly alpha-olefins are desirable. Since the heat conductive oil composition is used in contact with the heat source for a long time, the organic oil needs to be heat resistant. When the heat resistant organic oil has an aromatic hydrocarbon group, the aromatic hydrocarbon group, particularly a phenyl group, usually has 5% by mole or more of all organic groups, preferably 10% by mole or more, and is more desirable. Is 40 mol% or more.

Phenyl ether-based oils include phenyl ether oils and alkyl phenyl ether oils in which an alkyl group is bonded to a phenyl group. Specific examples thereof include diphenyl ether, tetraphenyl ether, pentaphenyl ether, alkyl diphenyl ether, monoalkyl triphenyl ether, monoalkyl tetraphenyl ether and dialkyl tetraphenyl ether. Examples of the alkyl group include methyl group, ethyl group, butyl group, hexyl group, octyl group, decyl group, dodecyl group, tetradecyl group, hexadecyl group and octadecyl group.

The phenyl ether-based oil is preferably liquid at normal temperature, and its kinematic viscosity is usually 15 to 450 mm ² / s at 25 to 40 ° C.

The aromatic carboxylic acid ester-based oil includes alcohol ester of aromatic carboxylic acid, aralkyl alcohol ester of aromatic carboxylic acid, phenol ester of aromatic carboxylic acid, alkylphenol ester of aromatic carboxylic acid and the like. As the aromatic carboxylic acid for that purpose, there are benzoic acid, alkyl benzene carboxylic acid, terephthalic acid, trimellitic acid, naphthenic acid and the like. Examples of the alkyl group include a methyl group, an ethyl group, a butyl group, a hexyl group and an octyl group. Examples of alcohols for the alkyl ester include ethyl alcohol, butyl alcohol, cyclohexanol and octyl alcohol. Benzyl alcohol is exemplified as the aralkyl alcohol for the aralkyl ester. Examples of alkylphenols for alkylphenyl esters include p-methylphenol and p-octylphenol.
The aromatic carboxylic acid ester-based oil is desirably liquid at normal temperature, and its kinematic viscosity is usually 15 to 450 mm ² / s at 25 to 40 ° C.

The poly α-olefin is an oil obtained by polymerizing an α-olefin and having a carbon-carbon double bond at the α position, and may have an alkyl group as a branched structure.
The poly α-olefin is desirably liquid at normal temperature, and its kinematic viscosity is usually 15 to 450 mm ² / s at 25 to 40 ° C.

The heat resistant organic oil may be used in combination of two or more.

When the content of (A) heat resistant organic oil in the heat conductive oil composition is too large, the heat conductivity of the heat conductive oil composition decreases, and when it is too small, the heat conductive oil composition is viscous paste (A) The heat resistant organic oil is 20 to 57% by volume of the heat conductive oil composition, preferably 28 to 55% by volume, more preferably 29 to 53% by volume. desirable.

(C) The thermally conductive fine particles have the function of imparting thermal conductivity or heat dissipation to the thermally conductive oil composition of the present invention. Typical examples thereof are inorganic fine particles and metal fine particles excellent in thermal conductivity. Examples of the inorganic fine particles include fine particulate alumina, zinc oxide, silicon nitride, boron nitride, aluminum nitride, silicon carbide, calcium carbonate, zinc carbonate, silica, magnesium oxide, titanium oxide, iron oxide, iron oxide, carbon black, graphite and diamond. Be done. Examples of metal-based fine particles include fine-grained platinum, gold, silver, copper, palladium, indium, aluminum, nickel, tin, lead, zinc, bismuth, iron, cobalt, and alloys of these metals. Alumina, zinc oxide, silicon nitride, boron nitride, aluminum nitride and silicon carbide are preferred in view of high thermal conductivity.
Two or more types of these inorganic fine particles and metal fine particles may be used in combination.
The (C) thermally conductive particles may be those in which a part or the whole of the surface of the organic fine particles is coated with a thermally conductive material. The surface of these thermally conductive particles may be subjected to water repellent treatment, hydrophilic treatment or addition treatment of functional groups.

The shape of the thermally conductive fine particles (C) is not particularly limited, and examples thereof include spheres, oval spheres, prisms, polyhedrons, flakes, needles, and amorphous. The particle size is not particularly limited as long as single particles are hardly visible to the naked eye, but in order to have appropriate thermal conductivity, the average particle size is preferably in the range of 0.1 μm to 50 μm, More preferably, it is in the range of 0.2 μm to 30 μm. In order to obtain high thermal conductivity, thermally conductive particles having two or more different average particle sizes may be used in combination.
The average particle diameter is preferably a median diameter D50, and the median diameter D50 is a volume distribution of the thermally conductive particles by means of a laser diffraction type particle size distribution measuring device (for example, "LA-300" manufactured by Horiba, Ltd.). It is a particle size value when the integrated value becomes 50% in the volume based particle size distribution curve measured on the basis of the standard.

If the amount of (C) thermally conductive particles is too large, the thermally conductive oil composition can not be formed into a viscous paste, and if too small, the thermal conductivity of the thermally conductive oil composition decreases. 80 to 43% by volume of the conductive oil composition (total amount with (A) heat resistant organic oil is 100% by volume), preferably 72 to 45% by volume, 71 to 47% by volume More desirable.

(B) The nonionic surfactant includes (B-1) polyoxyethylene-polyoxypropylene glycol having an HLB value of 1.8 or more and 18 or less, and (B-2) an HLB value of 9.5. It is selected from non-ionic surfactants which are greater than or equal to 19 and contain polyoxyethylene units and hydrophobic groups.

(B-1) Polyoxyethylene-polyoxypropylene glycol is a copolymer of ethylene oxide and propylene oxide, is composed of a polyoxyethylene unit and a polyoxypropylene unit, and both molecular chain terminals are hydroxyl groups. It is usually liquid at normal temperature, but may be solid.
The hydroxyl group and the polyoxyethylene unit are hydrophilic, and the polyoxypropylene unit is hydrophobic so as to have surface activity.
The molar ratio and number of units of the polyoxyethylene unit and the polyoxypropylene unit are not particularly limited as long as the HLB value is 1.8 or more and 18 or less.
The lower limit of the HLB value is 1.8 or more in terms of the availability of the nonionic surfactant.

(B-1) As polyoxyethylene-polyoxypropylene glycol,
Polyoxyethylene polyoxypropylene glycol (5E.O.) (30 P.O.) (HLB value 1.9),
Polyoxyethylene polyoxypropylene glycol (10E.O.) (30P.O.) (HLB value 4.9),
Polyoxyethylene polyoxypropylene glycol (25E.O.) (35P.O.) (HLB value 8.1),
Polyoxyethylene polyoxypropylene glycol (48 E. O.) (35 P. O.) (HLB value 10.1),
Polyoxyethylene polyoxypropylene glycol (200 E.O.) (70 P.O.),
Polyoxyethylene polyoxypropylene glycol (300 E.O.) (55 P.O.) (HLB value 15.5) is illustrated. Here, E. O. Means oxyethylene unit, P.I. O. Means an oxypropylene unit.

These HLB values are greater than 9.5 and less than or equal to 18 in terms of sag resistance. The lower limit of the HLB value is greater than 9.5, preferably 9.6 or more, in terms of sag resistance. The upper limit of the HLB value is 18 or less, preferably 17 or less, in terms of the availability of nonionic surfactants.

(B-2) It is preferable that the nonionic surfactant containing a polyoxyethylene unit and a hydrophobic group further contains a hydroxyl group. The hydroxyl group is preferably located at the end of the polyoxyethylene unit.
As a hydrophobic group here, an alkyl group having 5 to 22 carbon atoms, an alkylene group, an oxyalkyl group, an oxyalkylene group, an alkylphenyl group, an oxy (alkylphenyl) group, an aralkyl group and an oxyaralkyl group are exemplified. However, polyoxypropylene units are not the only ones.

Polyoxyethylene as a nonionic surfactant containing a polyoxyethylene unit and a hydrophobic group which is the component (B-2), and a nonionic surfactant containing a hydroxyl group, a polyoxyethylene unit and a hydrophobic group Monoalkyl ether, polyoxyethylene monoalkyl phenyl ether, polyoxyethylene monoalkyl naphthyl ether, polyoxyethylene hydrogenated castor oil, polyoxyethylene hydrogenated castor oil, polyoxyethylene alkylamide, polyoxyethylene mono fatty acid ester, polyoxyethylene Di-fatty acid ester, polyoxyethylene propylene glycol fatty acid ester, polyoxyethylene sorbitan mono-fatty acid ester, polyoxyethylene sorbitan tri-fatty acid ester, polyoxyethylene bisphenol A ether, polyoxyethylene Lene bisphenol F ether, polyoxy polycyclic phenyl ether, polyoxyethylene phenyl ether, polyoxyethylene styrenated phenyl ether, polyoxyethylene alkyl diether, polyoxyethylene di-styrenated phenyl ether, polyoxyethylene cumyl phenyl ether, poly Examples include oxyethylene tribenzyl phenyl ether and polyoxyethylene benzyl ether.

Among these, the component (B-2) is one having an HLB value of more than 9.5 and 19 or less.
The lower limit of the HLB value is greater than 9.5, preferably 9.6 or more, in terms of sag resistance. The upper limit of the HLB value is 19 or less, preferably 18 or less, in terms of the availability of nonionic surfactants.

The content of the (B) nonionic surfactant is 0.02% by weight or more and less than 0.2% by weight of the content of the (C) thermally conductive particles, and preferably the (C) thermally conductive particles 0.05% by weight or more and 0.19% by weight or less of the content of
If it is less than 0.02% by weight, it has no effect on the sagging resistance of the heat conductive oil composition, and if it is 0.2% by weight or more, the mixture has a very high viscosity and the hard and non-uniform dumplings Because it is likely to
For example, in the case of 0.21% by weight, the viscosity may be very high (450 Pa · s or more), and in the case of 0.3% by weight, it may be in the form of non-uniform dumpling.

The heat conductive oil composition of the present invention is in the form of a viscous paste at normal temperature, and can also be referred to as a "heat conductive viscous paste composition".
Viscous pastes include creams and oil compounds.
Usually, in many cases, it is thixotropic, and as shear stress continues, the viscosity gradually decreases and becomes fluid, and when it stops, the viscosity gradually increases to its original state.
The thermal conductivity of the thermally conductive oil composition of the present invention is preferably 0.5 W / m · K or more at the time of measurement under the measurement conditions defined in the examples, and is 0.9 W / m · K or more. Is more desirable.

The heat conductive oil composition of the present invention contains a pigment, a coloring agent, a thixo agent, a heat resistant stabilizer, an antioxidant, an ultraviolet light absorber, a solvent and the like as long as the effect of the present invention is not impaired. May be

The thixotropic agent is a component for reducing the bleeding out of the base oil from the heat conductive oil composition of the present invention. Examples of such thixotropic agents include sorbitol-based thixotropic agents and amide-based thixotropic agents.

As a sorbitol type thixotropic agent, benzylidene sorbitols are preferable, and bis (p-methylbenzylidene) sorbitol, bis (p-ethylbenzylidene) sorbitol, dibenzylidene sorbitol, tribenzylidene sorbitol, alkyl-substituted dibenzylidene sorbitol having 3 or more carbon atoms Is illustrated.

Amide-based thixotropic agents include saturated fatty acid monoamides such as lauric acid amide and stearic acid amide, unsaturated fatty acid monoamides such as oleic acid amide, substituted amides such as N-lauryl lauric acid amide and N-stearyl stearic acid amide, methylol stearin Saturated fatty acid bisamides such as methylolamides such as acid amides, methylenebisstearic acid amides, ethylenebislauric acid amides, ethylenebishydroxystearic acid amides, unsaturated fatty acid bisamides such as methylenebis oleic acid amides, m-xylylene bisstearic acid Aromatic bisamides such as amides, ethylene oxide adducts of fatty acid amides, fatty acid ester amides, fatty acid ethanolamides, N-butyl-N'-ste And substituted ureas such as Lil urea is exemplified. Two or more types of thixotropic agents may be used in combination.

The blending amount of the sorbitol-based thixotropic agent or the amide-based thixotropic agent is an amount sufficient to reduce the bleeding out of the heat-resistant organic oil which is the base oil from the heat-conductive oil composition of the present invention over time. (A) 0.01 to 10 parts by weight per 100 parts by weight of the heat resistant organic oil is desirable, and 0.1 to 5.0 parts by weight is more desirable.

When the sorbitol-based thixotropic agent or the amide-based thixotropic agent is solid at normal temperature, it is desirable to add it in advance together with the whole or a part of the heat-resistant organic oil and dissolve it at a temperature above its melting point.

The heat conductive oil composition of the present invention is excellent in heat resistance and oxidation resistance, but may further contain a heat resistance stabilizer, an antioxidant and the like in order to further improve the heat resistance and oxidation resistance. The type of heat resistant stabilizer or antioxidant is not particularly limited, and metal salts of aromatic carboxylic acid, alkyl phenolate, maleic acid, monoester metal salt of maleic acid, alkyl mercaptan, mercapto acid, ester metal salt of mercapto acid, Inorganic acid metal salt, metal hydroxide, 2,6-differential butyl-4-methylphenol, n-octadecyl-3- (3 ′, 5′-differential butyl-4′-hydroxyphenyl) propionate, 4,4, Examples thereof include hindered phenols such as 4'-butylidenebis (3-methyl-6-tertiary butylphenol) and amines.

The blending amount of these heat stabilizers and antioxidants is preferably 0.01 to 20 parts by weight per 100 parts by weight of (A) heat resistant organic oil, and more preferably 0.05 to 10 parts by weight. Preferably, it is 0.10 to 7.5 parts by weight.

In the mixer, the heat conductive oil composition of the present invention is mixed with predetermined amounts of (A) heat resistant organic oil (B) nonionic surfactant and (C) heat conductive fine particles until uniform. It can be easily manufactured by doing. It may be any of normal temperature mixing and heating mixing under the atmosphere, or may be mixed under reduced pressure. In that case, when the (B) nonionic surfactant is solid or waxy, it is preferable that the temperature at the time of heating is 40 ° C to 100 ° C.
Commercial products and purchased products may be used as they are for component (A), component (B) and component (C), but component (A) may be heat-treated in advance, and component (C) may be Pulverization, classification, degassing, dehydration, heat treatment, etc. may be performed in advance.

The total amount of each predetermined amount of (A) heat resistant organic oil, (B) non-ionic surfactant, and (C) thermally conductive fine particles may be introduced into a mixer and mixed, but (B) non-ionic The surfactant and (C) thermally conductive fine particles may be mixed, and then the mixture and (A) heat resistant organic oil may be mixed. In addition, (B) a nonionic surfactant is dissolved in an organic solvent, the solution and (C) heat conductive fine particles are mixed, then the organic solvent is removed, and (A) mixed with a heat resistant organic oil. It is good. In addition, (B) a nonionic surfactant is dissolved in an organic solvent and mixed with (C) heat conductive fine particles, and the mixture and (A) heat resistant organic oil are mixed, and then the organic solvent is removed. It is good. Further, (A) heat resistant organic oil and (B) non-ionic surfactant may be mixed under normal temperature or by heating, and the mixture and (C) heat conductive fine particles may be mixed.
In any case, degassing after mixing is preferred.
After mixing, three rolls may be applied to improve uniformity.

The mixer used for mixing and stirring is not particularly limited as long as it can uniformly mix and stir the (A) component, the (B) component and the (C) component, but a stirring tank and a uniaxial or multi-axial stirring blade can be used. What is equipped is preferable. The number of stirring blades is not particularly limited, but two or more are preferable in order to obtain high kneading action.
Above all, planetary mixers and planetary stirrers are preferred in terms of the uniformity of the mixture.
The planetary mixer has a structure in which the kneaded material in the stirring tank is stirred and kneaded using a 2-shaft stirring blade that rotates and revolves each other, and a dead space in which the stirring blade does not reach the stirring tank Less is. The rotational speed and rotational speed of the stirring blade may be selected appropriately.
The planetary stirring device performs uniform stirring of the material by rotating the container containing the material at high speed while rotating on a revolving track at the same time.

The thermally conductive oil composition of the present invention is in the form of a viscous paste at normal temperature. The viscosity (25 ° C.) is preferably 50 Pa · s to 450 Pa · s, more preferably 100 Pa · s to 350 Pa · s, when measured under the measurement conditions defined in the examples.

The viscosity of the thermally conductive oil composition of the present invention is temperature-dependent, and [viscosity at 150 ° C] / [viscosity at 25 ° C] is 0.31 to 20, preferably 0.32 to 10. When [Viscosity at 150 ° C.] / [Viscosity at 25 ° C.] is less than 0.31, the sag resistance is poor.

The thermally conductive oil composition of the present invention may be either electrically insulating, semiconductive or conductive. (C) By selecting the type and the blending amount of the thermally conductive fine particles, any of the electric insulating property, the semiconductive property, and the conductive property can be obtained. In the case of electrical insulation, it is desirable that the volume resistivity be 1 × 10 ¹⁰ Ω · cm or more. When semiconductive, it is desirable to be in the range of 1 × 10 ⁰ Ω · cm to 1 × 10 ¹⁰ Ω · cm. In the case of electrical conductivity, that is, electrical conductivity, it is desirable that the volume resistivity be 1 × 10 ⁰ Ω · cm or less.

The thermally conductive oil composition of the present invention is preferably stored in a plastic container, a metal can, a glass bottle, a tube, a cartridge or the like. Refrigerated storage may be carried out for the purpose of improving storage stability, and a storage temperature of -5 ° C or less is exemplified.

The heat conductive oil composition of the present invention is suitable for heat radiation of heat generating members, heat generating devices, high temperature members, and high temperature devices. In particular, it is held in the gap or gap between the heat generating member and the cooling member of the electronic component / electronic device, or in the gap or gap between the high temperature member (for example, semiconductor package, circuit board) and the heat dissipation member (for example, heat dissipation fin) It is used in the form of another or in the form of an intervening form. The heat generating member and the cooling member, and the high temperature member and the heat radiating member do not repeatedly shift and move as in the sliding portion.
The method for applying the thermally conductive oil composition of the present invention to the above-mentioned member, gap or space is not particularly limited, and examples include injection, dispense application, print application, spray application, roller application and brush application.

The heat dissipating agent of the present invention is a heat conductive oil composition comprising (A) heat resistant organic oil, (B) non-ionic surfactant and (C) heat conductive fine particles, wherein (A) heat resistant organic composition The content of oil is 20 to 57% by volume, the content of (C) heat conductive fine particles is 80 to 43% by volume (total amount 100% by volume), the content of (B) nonionic surfactant The amount of (C) the content of the thermally conductive fine particles is 0.02% by weight or more and less than 0.2% by weight, and the (B) nonionic surfactant has a (B-1) HLB value of 1. Polyoxyethylene-polyoxypropylene glycol having 8 or more and 18 or less, or (B-2) non-ionic containing a polyoxyethylene unit and a hydrophobic group, having an HLB value of more than 9.5 and 19 or less It is characterized by being a surfactant.
The respective components, their blending ratios, contents and additives are as already described for the heat conductive oil composition. The properties, characteristics, manufacturing method, storage method, method of use, places of use, etc. of the heat dissipating agent are the same as those of the heat conductive oil composition.

The electronic device according to the present invention comprises (A) heat resistant organic oil, (B) in the gap or gap between the heat generating member and the cooling member of the electronic component / electronic device or in the gap or gap between the high temperature member and the heat dissipation member. A thermally conductive oil composition comprising an ionic surfactant and (C) thermally conductive fine particles, wherein the content of (A) heat resistant organic oil is 20 to 57% by volume, (C) thermal conductivity The content of fine particles is 80 to 43% by volume (total volume 100% by volume), and the content of (B) nonionic surfactant is 0.02% by weight or more of the content of (C) thermally conductive fine particles Or less than 0.2% by weight, and (B) the nonionic surfactant is (B-1) polyoxyethylene-polyoxypropylene glycol having an HLB value of 1.8 or more and 18 or less, or B-2) A HLB value of greater than 9.5 but not greater than 19 and containing a polyoxyethylene unit and a hydrophobic group It is characterized in that a heat dissipating agent which is an on-state surfactant is sandwiched or interposed. The nonionic surfactant (B-2) containing a polyoxyethylene unit and a hydrophobic group preferably further contains a hydroxyl group.

Thermal conductive oil composition held in the gap or gap between the heat generating member and the cooling member of the electronic component / electronic device, or the gap or gap between the high temperature member and the heat radiating member, the thickness of the heat radiating agent is less than 50 μm There is a possibility that a gap may be generated between the heated electronic component and the heat dissipation member due to a slight displacement of the pressure and the pressure, and if it is larger than 500 μm, the heat resistance increases due to its thickness and the heat dissipation effect deteriorates. The range of 50 to 500 μm is preferable, and 100 to 200 μm is more preferable.

Capacitors, resistors, diodes, memories, arithmetic elements (CPUs) as electronic parts, driver ICs for LCD TVs and plasma TVs, MPU chip sets, semiconductor power modules, control modules for industrial equipment and robots, switching power supplies, automotive electrical components , An audio amplifier is illustrated.
As electronic devices, LCD TVs, plasma TVs, organic EL TVs, projectors, personal computers, game machines, DVDs, hard disks, refrigerators, air conditioners, IH heaters, heat pumps, hybrid cars, hybrid computers, supercomputers, trains, aerospace devices, robots, and others Current and voltage control devices and their components are illustrated.

注：モレスコハイルーブは商標である。 The components used in Examples and Comparative Examples are as follows.
(A) Heat resistant organic oil

Note: Moresco High Lube is a trademark.

注：ニューポール、EMALEX、NIKKOL、DECAGLYN、エマルゲン、エヌジェボン、イオネットは商標である。 (B) Nonionic surfactant

Note: New Pole, EMALEX, NIKKOL, DECAGLYN, Emulgen, Enjebon, Ionet are trademarks.

注：D50（メジアン径）は、レーザ回折式粒度分布測定装置（例えば、堀場製作所製「ＬＡ−３００」）により、アルミナ粒子または酸化亜鉛粒子の粒度分布を体積基準で測定し、得られた体積基準粒度分布曲線において積算値が５０％となるときの粒径値である。
アドマファインとLPZINCは商標である。 (C) Thermally conductive fine particles

Note: D50 (median diameter) is the volume obtained by measuring the particle size distribution of alumina particles or zinc oxide particles on a volume basis with a laser diffraction particle size distribution analyzer (for example, "LA-300" manufactured by Horiba, Ltd.) The particle size value at which the integrated value is 50% in the standard particle size distribution curve.
Adma Fine and LPZINC are trademarks.

The properties of the thermally conductive oil composition and the heat radiating agent in the examples and comparative examples were measured by the following test methods. The measurement temperature is 25 ° C. unless otherwise specified. The term "parts" refers to "parts by weight". The temperature at the time of mixing under heating is a temperature in the range of approximately 40 ° C. to 100 ° C. The mixing time under heating is not limited as long as the mixture is uniform, and is, for example, 10 minutes to 60 minutes.

[Measurement of viscosity of composition]
Viscometer: E-type viscometer (cone plate type) manufactured by Toki Sangyo Co., Ltd., TV-20
Rotor: 3 ° x R 9.7 mounted Rotor speed: 3 rpm

[Viscosity-temperature dependence]
Viscometer: B-type viscometer (single cylinder type) manufactured by Toki Sangyo Co., Ltd., RB-80 U
Rotor: Mount the ST rotor for a small amount.
Rotor speed: 0.5 rpm
The viscosities were measured at 25 ° C. and 150 ° C., and [viscosity at 150 ° C./viscosity at 25 ° C.] was calculated to obtain viscosity-temperature dependence.

[Drop test]
The dripping property is prepared by preparing a test piece in which a predetermined amount of a heat conductive oil composition (heat dissipation agent) is filled between a flat 50 mm square aluminum plate and a flat 50 mm square glass plate (gap 0.1 mm). It is installed in a thermal shock tester with one cycle of −40 ° C./30 minutes to + 150 ° C./30 minutes while standing vertically, the test piece is taken out after 100 cycles, and the heat remaining in the gap The weight of the conductive oil composition (heat radiating agent) was measured, and the weight reduction rate was calculated.

[Thermal conductivity]
A thermally conductive oil composition was sandwiched between silicon wafers of 10 mm × 10 mm square and 0.8 mm thickness so as to have a thickness of 40 μm or 80 μm, to obtain a test body. The thermal resistance (unit; ° C / W) was measured for each test body, the relationship between each thickness (unit; m) and the thermal resistance was plotted on a graph to draw a straight line, and the slope was taken as the thermal conductivity (unit; W Calculated as / mK).

Example 1
As component (A) (a-1) 15.85 parts of Moresco hylobe LB-100 (alkyl diphenyl ether, liquid) manufactured by MORESCO, Inc., as component (B) (b-1) manufactured by Sanyo Chemical Industries, Ltd. 0.15 part of Pall PE-61 (polyoxyethylene polyoxypropylene glycol (5E.O.) (30 P.O.), liquid, HLB 1.9), component (C) as (c-1) ADMATEX CORPORATION Adma fine alumina (true spherical shape, D50: 5.5 μm alumina powder) and (c-2) Admafine Co., Ltd. Adma fine AO-502 (spherical shape, D50: 0.7 μm alumina powder) A mixture of 25 parts and 84.00 parts was charged into a commercially available planetary mixer (hereinafter referred to as "planetary mixer") and mixed until uniform. The resulting viscous paste-like thermally conductive oil composition (hereinafter referred to as "viscous paste-like composition") is degassed to measure its viscosity at 25 ° C and its viscosity at 150 ° C, and it drips off. The test was done. The measurement results and the test results are shown in Table 4.

Example 2
In Example 1, instead of (b-1) Neupol PE-61 (polyoxyethylene polyoxypropylene glycol (5E.O.) (30 P.O., liquid, HLB 1.9), (b-2) ) Viscous under the same conditions except using Sanyo Chemical Industries, Ltd. new pole PE-62 (polyoxyethylene polyoxypropylene glycol (10E.O.) (30 P.O.), liquid, HLB 4.9) A paste-like composition was prepared, the viscosity at 25 ° C. and the viscosity at 150 ° C. were measured, and a sag test was conducted. The measurement results and the test results are shown in Table 4.

[Example 3]
In Example 1, instead of (b-1) Neupol PE-61 (polyoxyethylene polyoxypropylene glycol (5E.O.) (30P.O., liquid, HLB 1.9), (b-3) ) Viscous under the same conditions except using Sanyo Kasei Kogyo's Nypol PE-64 (polyoxyethylene polyoxypropylene glycol (25E.O.) (30P.O.), liquid, HLB 8.1) A paste-like composition was prepared, the viscosity at 25 ° C. and the viscosity at 150 ° C. were measured, and a sag test was conducted. The measurement results and the test results are shown in Table 4.

Example 4
In Example 1, instead of (b-1) Neupol PE-61 (polyoxyethylene polyoxypropylene glycol (5E.O.) (30P.O., liquid, HLB 1.9), (b-3) ) New pole PE-64 (polyoxyethylene polyoxypropylene glycol (25E.O.) (30P.O.), liquid, HLB 8.1) and (b-4) Sanyo Chemical Industries, Ltd. manufactured by Sanyo Chemical Industries, Ltd. A mixture of 22 parts to 78 parts (liquid, HLB 9.7) of Newpol PE-75 (polyoxyethylene polyoxypropylene glycol (48 E.O.) (35 P. O.), liquid, HLB 10.1) manufactured by C.N. A viscous paste-like composition was prepared under the same conditions except for the above, and the viscosity at 25 ° C and the viscosity at 150 ° C were measured, and a sag test was conducted. The measurement results and the test results are shown in Table 4.

[Example 5]
In Example 1, instead of (b-1) Neupol PE-61 (polyoxyethylene polyoxypropylene glycol (5E.O.) (30 P.O., liquid, HLB 1.9), (b-4) ) Viscous under the same conditions except using Sanyo Kasei Kogyo's Nypol PE-75 (polyoxyethylene polyoxypropylene glycol (48E.O.) (35P.O.), liquid, HLB10.1) A paste-like composition was prepared, the viscosity at 25 ° C. and the viscosity at 150 ° C. were measured, and a sag test was conducted. The measurement results and the test results are shown in Table 5.

[Example 6]
As component (A) (a-1) 15.95 parts of Moresco highlobe LB-100 (alkyl diphenyl ether, liquid) manufactured by MORESCO Co., Ltd., as component (B) (b-4) manufactured by Sanyo Chemical Industries, Ltd. Paul PE-108 (polyoxyethylene polyoxypropylene glycol (300E.O.) (55P.O.), solid, HLB 15.5) 0.05 parts, as component (C) (c-1) Admatex Co., Ltd. Adma fine alumina (true spherical shape, D50: 5.5 μm alumina powder) and (c-2) Admafine Co., Ltd. Adma fine AO-502 (spherical shape, D50: 0.7 μm alumina powder) 25 parts of the mixture 84.00 parts were charged into a planetary mixer and mixed under heat until uniform. The resulting viscous paste-like composition was defoamed, the viscosity at 25 ° C. and the viscosity at 150 ° C. were measured, and a sag test was performed. The measurement results and the test results are shown in Table 5.

[Example 7]
In Example 6, 15.85 parts are used in place of 15.95 parts of (a-1) Morescohylobe LB- 100 (alkyl diphenyl ether), (b-4) Newpol PE-108 (polyoxyethylene) A paste-like composition which is viscous under the same conditions except that 0.15 part is used instead of polyoxypropylene glycol (300 E. O.) (55 P. O.), solid, HLB 15.5). Were prepared to measure the viscosity at 25.degree. C. and the viscosity at 150.degree. C., and a sag test was conducted. The measurement results and the test results are shown in Table 5.

[Example 8]
In Example 1, instead of (b-1) Neupol PE-61 (polyoxyethylene polyoxypropylene glycol (5E.O.) (30 P.O., liquid, HLB 1.9), (b-8) ) A viscous paste-like composition was prepared under the same conditions except using Sanyo Chemical Industries, Ltd. New Pole BPE-100 (polyoxyethylene bisphenol A ether, liquid, HLB 13.2) manufactured by Sanyo Chemical Industries, Ltd., and its viscosity at 25 ° C. The viscosity at 150 ° C. was measured, and a drip test was performed. The measurement results and the test results are shown in Table 5.

[Example 9]
In Example 1, instead of (b-1) Neupol PE-61 (polyoxyethylene polyoxypropylene glycol (5E.O.) (30P.O., liquid, HLB 1.9), manufactured by Kao Corp. A viscous paste-like composition was prepared under the same conditions except using EMULGEN 103 (polyoxyethylene lauryl ether (3.8 EO) (liquid, HLB 9.7), and the viscosity at 25 ° C and the viscosity at 150 ° C were measured. The results of the measurement and the test results are shown in Table 6.

[Example 10]
In Example 7, instead of (b-4) Neupol PE-108 (polyoxyethylene polyoxypropylene glycol (300 E.O.) (55 P.O., solid, HLB 15.5), (b-11) ) A viscous paste-like composition was prepared under the same conditions except using Nippon Emulsion Co., Ltd. EMALEX-750 (polyoxyethylene lauryl ether (50 E.O.) (wax-like, HLB 18.4), 25 The viscosity at 150 ° C. and the viscosity at 150 ° C. were measured and a sag test was conducted, and the measurement results and the test results are shown in Table 6.

[Example 11]
In Example 7, instead of (b-4) Neupol PE-108 (polyoxyethylene polyoxypropylene glycol (300 E.O.) (55 P.O., solid, HLB 15.5), (b-12) ) A viscous paste-like composition was prepared under the same conditions except using Enjebon ECS-600 (polyoxyethylene cetyl stearyl diether (60 E. O.), solid, HLB 16.8) manufactured by Shin Nippon Rika Co., Ltd. The viscosity at 25 ° C. and the viscosity at 150 ° C. were measured, and a sag test was performed. The measurement results and the test results are shown in Table 6.

[Example 12]
In Example 1, instead of (b-1) Neupol PE-61 (polyoxyethylene polyoxypropylene glycol (5E.O.) (30 P.O., liquid, HLB 1.9), (b-13) ) A viscous paste-like composition was prepared under the same conditions except using Saneto Chemical Industries, Ltd. Ionetto T-20C (polyoxyethylene sorbitan monolaurate (20E.O., liquid, HLB 16.7)). The viscosity at 25 ° C. and the viscosity at 150 ° C. were measured, and a sag test was performed. The measurement results and the test results are shown in Table 6.

[Example 13]
In Example 1, (a-2) PA05010 (poly α-olefin, liquid) manufactured by Idemitsu Kosan Co., Ltd. is used in place of (a-1) Morescohylobe LB-100 (alkyl diphenyl ether, liquid), (b-1) Instead of Newpol PE-61 (polyoxyethylene polyoxypropylene glycol (5E.O.) (30P.O., liquid, HLB 1.9), (b-8) Sanyo Chemical Industries, Ltd. stock A viscous paste-like composition was prepared under the same conditions, except using company-made Newpol BPE-100 (polyoxyethylene bisphenol A ether, liquid, HLB 13.2), and the viscosity at 25 ° C. and the viscosity at 150 ° C. Was measured and a drip test was performed. The measurement results and the test results are shown in Table 7.

Example 14
As component (A) (a-1) 17.85 parts of Morescohylobe LB-100 (alkyl diphenyl ether, liquid) manufactured by MORESCO Co., Ltd., as component (B) (b-5) manufactured by Sanyo Chemical Industries, Ltd. 0.15 part of Pall PE-108 (polyoxyethylene polyoxypropylene glycol (300E.O.) (55P.O.), solid, HLB 15.5), as component (C) (c-2) ADMATEX CORPORATION 82.00 parts of Admafine AO-502 (a spherical shape, D50: 0.7 μm alumina powder) manufactured by Adma Fine were charged into a planetary mixer and mixed until uniform under heating. The resulting viscous paste-like composition was defoamed, the viscosity at 25 ° C. and the viscosity at 150 ° C. were measured, and a sag test was performed. The measurement results and the test results are shown in Table 7.

[Example 15]
As component (A) (a-1) 11.69 parts of Moresco Highlobe LB-100 (alkyl diphenyl ether, liquid) manufactured by MORE CO., LTD., As component (B) (b-5) manufactured by Sanyo Chemical Industries, Ltd. Paul PE-108 (polyoxyethylene polyoxypropylene glycol (300E.O.) (55P.O.), solid, HLB 15.5) 0.11 parts, as component (C) (c-3) Sakai Chemical Industry Co., Ltd. LPZINC-5 (polyhedral, D50: 5 μm zinc oxide powder) and (c-4) Zinc oxide powder (JIS Class 1) manufactured by Sakai Chemical Industry Co., Ltd. (polyhedral, D50: 0.7 μm zinc oxide powder) The mixture was charged into a planetary mixer and mixed under heat until uniform. The resulting viscous paste-like composition was defoamed, the viscosity at 25 ° C. and the viscosity at 150 ° C. were measured, and a sag test was performed. The measurement results and the test results are shown in Table 7.

[Example 16]
As component (A), 1.80 parts of olescohylobe LB-100 (alkyl diphenyl ether, liquid) manufactured by MORESCO, Inc. (alkyl diphenyl ether, liquid) and 0.10 parts of zinc oleate (solid) are added to a planetary mixer The solution was mixed under heating to dissolve zinc oleate in Morescohylobe LB-100. Next, as component (B) (b-5) Newpol PE-108 (polyoxyethylene polyoxypropylene glycol (300 E. O.) (55 P. O.), solid, HLB 15.5) manufactured by Sanyo Chemical Industries, Ltd. 0.10 parts, as component (C) (c-1) Admafine alumina manufactured by Admatex Co., Ltd. (true spherical shape, D50: 5.5 μm alumina powder) and (c-2) Admafines Corporation Admafine AO 90.00 parts of a mixture of 75 parts to 25 parts of -502 (true spherical shape, D50: 0.7 μm alumina powder) was charged into the planetary mixer and mixed until uniform under heating. The resulting viscous paste-like composition was defoamed, the viscosity at 25 ° C. and the viscosity at 150 ° C. were measured, and a sag test was performed. The measurement results and the test results are shown in Table 7.

Comparative Example 1
Component (A): 16.00 parts of Morescohylobe LB-100 (alkyl diphenyl ether, liquid) manufactured by MORSCO, Inc. (a-1), component (C) (c-1) Admafine manufactured by Admatex Co., Ltd. Alumina (true spherical shape, D50: 5.5 μm alumina powder) and (c-2) Admafines Co., Ltd. Admafine AO-502 (true spherical shape, D50: 0.7 μm alumina powder) vs. 25 parts of 75 parts 84.00 parts of the mixture were charged into a planetary mixer and mixed until uniform. The resulting viscous paste-like composition was defoamed, the viscosity at 25 ° C. and the viscosity at 150 ° C. were measured, and a sag test was performed. The measurement results and the test results are shown in Table 8.

Comparative Example 2
Component (A): 15.99 parts of Morescohylobe LB-100 (alkyl diphenyl ether, liquid) manufactured by MORSCO, Inc. (a-1), component (B) (b-5): manufactured by Sanyo Chemical Industries, Ltd. Paul PE-108 (polyoxyethylene polyoxypropylene glycol (300E.O.) (55P.O.), solid, HLB 15.5) 0.01 part, as component (C) (c-1) ADMATEX CORPORATION Adma fine alumina (true spherical shape, D50: 5.5 μm alumina powder) and (c-2) Admafine Co., Ltd. Adma fine AO-502 (spherical shape, D50: 0.7 μm alumina powder) 25 parts of the mixture 84.00 parts were charged into a planetary mixer and mixed until uniform. The resulting viscous paste-like composition was defoamed, the viscosity at 25 ° C. and the viscosity at 150 ° C. were measured, and a sag test was performed. The measurement results and the test results are shown in Table 8.

Comparative Example 3
Component (A): (a-1) Moresco High Lube LB-100 (alkyl diphenyl ether, liquid) manufactured by MORESCO, Inc. 15.60 parts, component (B) (b-5) manufactured by Sanyo Chemical Industries, Ltd. Paul PE-108 (polyoxyethylene polyoxypropylene glycol (300E.O.) (55P.O.), solid, HLB 15.5) 0.40 part, as component (C) (c-1) ADMATEX CO., LTD. Adma fine alumina (true spherical shape, D50: 5.5 μm alumina powder) and (c-2) Admafine Co., Ltd. Adma fine AO-502 (spherical shape, D50: 0.7 μm alumina powder) 25 parts of the mixture, 84.00 parts, was put into a planetary mixer and it was tried to mix until it became uniform, but because the mixture was hard and nonuniform in the form of lumps, measurement of thermal conductivity, viscosity measurement and dripping Test was impossible. The experimental results are shown in Table 8.

Comparative Example 4
Component (A) (a-1) 24.85 parts of Moresco High Lube LB-100 (alkyl diphenyl ether, liquid) manufactured by MORESCO, Inc. Component (B) (b-5) manufactured by Sanyo Chemical Industries, Ltd. 0.15 part of Pall PE-108 (polyoxyethylene polyoxypropylene glycol (300E.O.) (55P.O.), solid, HLB 15.5), component (C) as (c-1) Admatex Co., Ltd. Adma fine alumina (true spherical shape, D50: 5.5 μm alumina powder) and (c-2) Admafine Co., Ltd. Adma fine AO-502 (spherical shape, D50: 0.7 μm alumina powder) 25 parts of the mixture 75.00 parts were charged into a planetary mixer and mixed under heat until uniform. The resulting viscous paste-like composition was defoamed, the viscosity at 25 ° C. and the viscosity at 150 ° C. were measured, and a sag test was performed. The measurement results and the test results are shown in Table 8.

Comparative Example 5
Component (A): (a-1) Morescohillobe LB-100 (alkyl diphenyl ether, liquid) made by MORESCO Ltd. (alkyl diphenyl ether, liquid) 4.90 parts, as component (B) (b-5) made by Sanyo Chemical Industries, Ltd. Paul PE-108 (polyoxyethylene polyoxypropylene glycol (300E.O.) (55P.O.), solid, HLB 15.5) 0.10 parts, component (C) as (c-1) ADMATEX CORPORATION Adma fine alumina (true spherical shape, D50: 5.5 μm alumina powder) and (c-2) Admafine Co., Ltd. Adma fine AO-502 (spherical shape, D50: 0.7 μm alumina powder) 25 parts of the mixture 95.00 parts of the mixture was put into a planetary mixer and it was tried to mix until it became uniform under heating, but since the mixture was hard and nonuniform in the form of lumps, measurement of thermal conductivity and viscosity measurement Drooping Fall test was impossible. The experimental results are shown in Table 9.

Comparative Example 6
As component (A) (a-1) 15.85 parts of Morescohylobe LB-100 (alkyl diphenyl ether, liquid) manufactured by MORESCO, Inc., as component (B) (b-5) EMALEX manufactured by Nippon Emulsion Co., Ltd. DEG-di-O (polyethylene glycol dioleate type PEG-2 (2E.O), liquid, HLB 2.0) 0.15 parts, as component (C) (c-1) Admafine alumina manufactured by Admatex Co., Ltd. Spherical sphere, D50: Alumina powder of 5.5 μm) and (c-2) Admafine AO-502 (a spherical surface, D50: alumina powder of D50: 0.7 μm) manufactured by Admatex Co., Ltd. Mixture 84 of 25 parts .00 parts were charged into the planetary mixer and mixed until uniform. The resulting viscous paste-like composition was defoamed, the viscosity at 25 ° C. and the viscosity at 150 ° C. were measured, and a sag test was performed. The measurement results and the test results are shown in Table 9.

Comparative Example 7
Component (A): (a-1) Morescohillobe LB-100 (alkyl diphenyl ether, liquid) manufactured by MORESCO, Inc. 15.85 parts, as component (B): (b-7) NIKKOL manufactured by Nikko Chemicals Co., Ltd. DECAGLYN 2-SV (decaglyceryl distearate, solid, HLB 9.5) 0.15 part, as component (C) (c-1) Admatex Co., Ltd. Adma fine alumina Adma fine alumina (true spherical, D50: 5.5 μm Alumina powder) and (c-2) 84.00 parts of a mixture of 75 parts of admafine AO-502 (true spherical shape, D50: 0.7 μm alumina powder) manufactured by Admatechs Co., Ltd. and 25 parts are charged into a planetary mixer Then, they were mixed until uniform under heating. The resulting viscous paste-like composition was defoamed, the viscosity at 25 ° C. and the viscosity at 150 ° C. were measured, and a sag test was performed. The measurement results and the test results are shown in Table 9.

Comparative Example 8
As component (A) (a-1) 15.85 parts of Morescohilobe LB-100 (alkyl diphenyl ether, liquid) manufactured by MORESCO, Inc., as component (B) (b-9) Emulgen 103 manufactured by Kao Corporation (Polyoxyethylene lauryl ether (2.9 EO), liquid, HLB 8.1) 0.15 parts, as component (C) (c-1) Admatex Co., Ltd. Adma Fine Alumina (true spherical, D50: 5.5 μm Alumina powder) and (c-2) 84.00 parts of a mixture of 75 parts of admafine AO-502 (true spherical shape, D50: 0.7 μm alumina powder) manufactured by Admatechs Co., Ltd. and 25 parts are charged into a planetary mixer And mixed until uniform. The resulting viscous paste-like composition was defoamed, the viscosity at 25 ° C. and the viscosity at 150 ° C. were measured, and a sag test was performed. The measurement results and the test results are shown in Table 9.

Comparative Example 9
As component (A) (a-2) 16.00 parts of PA05010 (poly α-olefin, liquid) manufactured by Idemitsu Kosan Co., Ltd., as component (C) (c-1) Adma fine alumina manufactured by Admatex Co., Ltd. D50: Alumina powder of 5.5 μm) and (c-2) Admafine AO-502 (a spherical shape, D50: Alumina powder of D50: 0.7 μm) manufactured by Admatex Co., Ltd. A mixture 84.00 of 25 parts to 25 parts The parts were charged into a planetary mixer and mixed until uniform. The resulting viscous paste-like composition was defoamed, the viscosity at 25 ° C. and the viscosity at 150 ° C. were measured, and a sag test was performed. The measurement results and the test results are shown in Table 10.

Comparative Example 10
As component (A), (a-1) Morescohylobe LB-100 (alkyl diphenyl ether, liquid) 9.80 parts and 0.20 parts of zinc oleate (solid) manufactured by MORESCO, Inc. are introduced into a planetary mixer The solution was mixed under heating to dissolve zinc oleate in Morescohylobe LB-100. Next, as component (C) (c-1) Adma fine alumina manufactured by Admatex Co., Ltd. (true spherical shape, D50: 5.5 μm alumina powder) and (c-2) Adma fine manufactured Admafine AO-502 (c 90.00 parts of a mixture of 75 parts of a spherical sphere, D50: 0.7 μm alumina powder) to 25 parts was charged into the planetary mixer and mixed until uniform. The resulting viscous paste-like composition was defoamed, the viscosity at 25 ° C. and the viscosity at 150 ° C. were measured, and a sag test was performed. The measurement results and the test results are shown in Table 10.

注：比較例３は、混合物が固くて不均一な団子状のため、熱伝導率の測定と粘度測定と垂れ落ち試験が不可能であった。

Note: Comparative Example 3 was unable to measure the thermal conductivity, measure the viscosity, and measure the sag because the mixture was hard and inhomogeneous dumpling-like.

注：比較例５は、組成物が固くて不均一な団子状のため、熱伝導率測定と粘度測定と垂れ落ち試験が不可能であった。

Note: Comparative Example 5 could not be subjected to thermal conductivity measurement, viscosity measurement, and sag test because the composition was hard and uneven in the form of dumplings.

The thermally conductive oil composition of the present invention has excellent thermal conductivity and sag resistance, and therefore, electronic components such as heated capacitors, resistors, diodes, memories, arithmetic elements (CPUs), etc., these electronic components It is useful as a medium that efficiently transfers the heat of the electronic device such as a semiconductor package having a chip, a circuit board, etc. to a heat dissipation member, so-called heat dissipation agent. The heat dissipating agent according to the present invention is a heat dissipating member for heat of electronic devices such as heated capacitors, resistors, diodes, memories, electronic components such as arithmetic elements (CPUs), semiconductor components having these electronic components and chips, and circuit boards. It is useful as a medium to communicate efficiently.

In the electronic device according to the present invention, the heat dissipation agent is held or interposed in the gap between the heat generating member and the cooling member of the electronic component / electronic device or the gap between the high temperature member and the heat radiating member. Even when exposed to a low temperature and high temperature cold cycle for a long time while being held in the vertical direction, the heat dissipation agent does not substantially drip down, so long-term excellent electronic device performance can be exhibited, and reliability Useful as an excellent electronic device.

It is a sectional view of one example of electronic equipment of the present invention. The circuit of the circuit board 1 is not shown.

Reference Signs List 1 circuit board 2 solder 3 heat-generating electronic component 4 heat conductive oil composition or heat dissipating agent 5 heat dissipation member A electronic device

The means for achieving this purpose is
"The claim 1 of
A heat conductive oil composition comprising (A) heat resistant organic oil, (B) nonionic surfactant and (C) heat conductive alumina fine particles, wherein the content of (A) heat resistant organic oil is 20 ~ 57% by volume, the content of (C) thermally conductive alumina fine particles is 80 to 43% by volume (total amount 100% by volume), the content of (B) non-ionic surfactant is (C) The content of the thermally conductive alumina fine particles is 0.02% by weight or more and less than 0.2% by weight, and the (B) nonionic surfactant has a (B-1) HLB value of 1.8 or more, 18 (Ii) polyoxyethylene-polyoxypropylene glycol or (B-2) a nonionic surfactant having a HLB value of more than 9.5 and 19 or less and containing a polyoxyethylene unit and a hydrophobic group Oh Ri, (C) a thermally conductive alumina fine average particle size is characterized 0.1μm~50μm der Rukoto, 25 ° C. Thermal-conductive oil composition whose viscosity in 50 is more than 50 Pa.s and less than 450 Pa.s.
The thermally conductive oil composition according to claim 1, wherein the nonionic surfactant (B-2) containing a polyoxyethylene unit and a hydrophobic group according to claim 2 further contains a hydroxyl group. .
[Viscosity at 150 ° C.] / [Viscosity at 25 ° C.] of the thermally conductive oil composition according to claim 3 is 0.31 to 20, according to claim 1 or 2, Heat conductive oil composition.

The means for achieving this purpose is
"The claim 4 of
A heat conductive oil composition comprising (A) heat resistant organic oil, (B) nonionic surfactant and (C) heat conductive alumina fine particles, wherein the content of (A) heat resistant organic oil is 20 ~ 57% by volume, the content of (C) thermally conductive alumina fine particles is 80 to 43% by volume (total amount 100% by volume), the content of (B) non-ionic surfactant is (C) The content of the thermally conductive alumina fine particles is 0.02% by weight or more and less than 0.2% by weight, and the (B) nonionic surfactant has a (B-1) HLB value of 1.8 or more, 18 (Ii) polyoxyethylene-polyoxypropylene glycol or (B-2) a nonionic surfactant having a HLB value of more than 9.5 and 19 or less and containing a polyoxyethylene unit and a hydrophobic group Oh Ri, (C) a thermally conductive alumina fine average particle size is characterized 0.1μm~50μm der Rukoto, 25 ° C. The heat dissipation agent having a viscosity of 50 Pa · s or more and less than 450 Pa · s .
The heat dissipating agent according to claim 4, wherein the nonionic surfactant (B-2) containing a polyoxyethylene unit and a hydrophobic group according to claim 5 further contains a hydroxyl group.
Claim 6
The heat sink according to claim 4 or 5, wherein the viscosity of the heat sink at 150 ° C / the viscosity at 25 ° C is 0.31 to 20. It consists of

The means for achieving this purpose is
“(A) heat resistant organic oil, (B) nonionic surfactant in the gap between the heat generating member and the cooling member of the electronic component / electronic device according to claim 7 or the gap between the high temperature member and the heat radiating member And (C) a heat conductive oil composition comprising heat conductive alumina fine particles, wherein the content of the (A) heat resistant organic oil is 20 to 57% by volume, and the content of the (C) heat conductive fine particles Is 80 to 43% by volume (total volume 100% by volume), and the content of (B) the nonionic surfactant is 0.02% by weight or more of the content of the (C) thermally conductive alumina fine particles, 0. It is less than 2% by weight, and (B-1) a nonionic surfactant is a polyoxyethylene-polyoxypropylene glycol having an HLB value of 1.8 or more and 18 or less, or (B-2) ) Nonionic surfactants having a HLB value of greater than 9.5 and not more than 19 and containing polyoxyethylene units and hydrophobic groups Ri sex agent der, (C) a thermally conductive alumina particles has an average particle diameter of 0.1Myuemu～50myuemu, viscosity at 25 ° C. is 50 Pa · s or more, the heat dissipation material is sandwiched is less than 450 Pa · s An electronic device characterized by
The electronic device according to claim 7, wherein the nonionic surfactant (B-2) containing a polyoxyethylene unit and a hydrophobic group according to claim 8 further contains a hydroxyl group. It consists of

The heat conductive oil composition of the present invention is a heat conductive oil composition comprising (A) heat resistant organic oil, (B) nonionic surfactant and (C) heat conductive alumina fine particles, A) The content of the heat resistant organic oil is 20 to 57% by volume, and the content of the (C) thermally conductive alumina fine particles is 80 to 43% by volume (total amount 100% by volume), (B) non-ionic The content of the anionic surfactant is 0.02% by weight or more and less than 0.2% by weight of the content of the (C) thermally conductive alumina fine particles, and the (B) nonionic surfactant is (B- 1) polyoxyethylene-polyoxypropylene glycol having an HLB value of 1.8 or more and 18 or less, or (B-2) an HLB value of more than 9.5 and 19 or less, and having a polyoxyethylene unit and a hydrophobicity Ri nonionic surfactants der including sex groups, (C) a thermally conductive alumina particles have an average particle size 0.1μm~50μ And characterized in that a viscosity at 25 ° C. is 50 Pa · s or more, Ru der less than 450 Pa · s.

The heat-resistant organic oil (A) is a dispersion medium for the (C) thermally conductive alumina fine particles, and has the effect of forming the fine particle component (C) into a viscous paste.

The (C) thermally conductive alumina fine particles have the function of imparting thermal conductivity or heat dissipation to the thermally conductive oil composition of the present invention. Representative examples of generally thermally conductive fine particles, thermal conductivity is excellent inorganic fine particles or metallic particles. Examples of the inorganic fine particles include fine particulate alumina, zinc oxide, silicon nitride, boron nitride, aluminum nitride, silicon carbide, calcium carbonate, zinc carbonate, silica, magnesium oxide, titanium oxide, iron oxide, iron oxide, carbon black, graphite and diamond. Be done. Examples of metal-based fine particles include fine-grained platinum, gold, silver, copper, palladium, indium, aluminum, nickel, tin, lead, zinc, bismuth, iron, cobalt, and alloys of these metals. Alumina, zinc oxide, silicon nitride, boron nitride, aluminum nitride and silicon carbide are preferable in view of high thermal conductivity and heat dissipation , and alumina fine particles are particularly preferable .

The shape of the (C) thermally conductive alumina fine particle is not particularly limited, and examples thereof include a sphere, an oval sphere, a prism, a polyhedron, a flake, a needle and an amorphous. The particle size is not particularly limited as long as single particles are hardly visible to the naked eye, but in order to have appropriate thermal conductivity, the average particle size is preferably in the range of 0.1 μm to 50 μm, More preferably, it is in the range of 0.2 μm to 30 μm. In order to obtain high thermal conductivity, thermally conductive alumina fine particles having two or more different average particle sizes may be used in combination.
The average particle diameter is preferably a median diameter D50, and the median diameter D50 is a volume distribution of the thermally conductive particles by means of a laser diffraction type particle size distribution measuring device (for example, "LA-300" manufactured by Horiba, Ltd.). It is a particle size value when the integrated value becomes 50% in the volume based particle size distribution curve measured on the basis of the standard.

The content of the (B) nonionic surfactant is 0.02% by weight or more and less than 0.2% by weight of the content of the (C) thermally conductive alumina fine particles, and preferably the (C) thermal conductivity The content is 0.05% by weight or more and 0.19% by weight or less of the content of alumina fine particles.
If it is less than 0.02% by weight, it has no effect on the sagging resistance of the heat conductive oil composition, and if it is 0.2% by weight or more, the mixture has a very high viscosity and the hard and non-uniform dumplings Because it is likely to
For example, in the case of 0.21% by weight, the viscosity may be very high (450 Pa · s or more), and in the case of 0.3% by weight, it may be in the form of non-uniform dumpling.

The heat conductive oil composition of the present invention is prepared by mixing predetermined amounts of (A) heat resistant organic oil (B) nonionic surfactant and (C) heat conductive alumina fine particles in a mixer. It can be easily manufactured by mixing. It may be any of normal temperature mixing and heating mixing under the atmosphere, or may be mixed under reduced pressure. In that case, when the (B) nonionic surfactant is solid or waxy, it is preferable that the temperature at the time of heating is 40 ° C to 100 ° C.
Commercial products and purchased products may be used as they are for component (A), component (B) and component (C), but component (A) may be heat-treated in advance, and component (C) may be Pulverization, classification, degassing, dehydration, heat treatment, etc. may be performed in advance.

The total amount of each predetermined amount of (A) heat resistant organic oil, (B) non-ionic surfactant, and (C) thermally conductive alumina fine particles may be introduced into a mixer and mixed, but The ionic surfactant and (C) thermally conductive alumina fine particles may be mixed, and then the mixture and (A) heat resistant organic oil may be mixed. In addition, (B) a nonionic surfactant is dissolved in an organic solvent, the solution and (C) thermally conductive alumina fine particles are mixed, then the organic solvent is removed, and (A) mixed with a heat resistant organic oil. You may. In addition, (B) a nonionic surfactant is dissolved in an organic solvent and mixed with (C) heat conductive alumina fine particles, and the mixture and (A) heat resistant organic oil are mixed and then the organic solvent is removed You may. In addition, (A) heat resistant organic oil and (B) nonionic surfactant may be mixed under normal temperature or by heating, and the mixture and (C) heat conductive alumina fine particles may be mixed.
In any case, degassing after mixing is preferred.
After mixing, three rolls may be applied to improve uniformity.

The thermally conductive oil composition of the present invention is electrically insulating . It is desirable body volume resistivity is 1 × ¹⁰ 10 Ω · cm or more.

The heat dissipating agent of the present invention is a heat conductive oil composition comprising (A) heat resistant organic oil, (B) non-ionic surfactant and (C) heat conductive alumina fine particles, and (A) heat resistance The content of the organic oil is 20 to 57% by volume, and the content of the (C) thermally conductive alumina fine particles is 80 to 43% by volume (total amount 100% by volume), (B) nonionic surfactant The content of (C) the content of the thermally conductive alumina fine particles is 0.02% by weight or more and less than 0.2% by weight, and (B) the nonionic surfactant has a (B-1) HLB value Or polyoxyethylene-polyoxypropylene glycol having a molecular weight of at least 1.8 and at most 18 or (B-2) an HLB value of greater than 9.5 and at most 19 and containing a polyoxyethylene unit and a hydrophobic group It is characterized in that it is a nonionic surfactant.
The respective components, their blending ratios, contents and additives are as already described for the heat conductive oil composition. The properties, characteristics, manufacturing method, storage method, method of use, places of use, etc. of the heat dissipating agent are the same as those of the heat conductive oil composition.

The electronic device according to the present invention comprises (A) heat resistant organic oil, (B) in the gap or gap between the heat generating member and the cooling member of the electronic component / electronic device or in the gap or gap between the high temperature member and the heat dissipation member. A thermally conductive oil composition comprising an ionic surfactant and (C) thermally conductive alumina fine particles, wherein the content of the (A) heat resistant organic oil is from 20 to 57% by volume, and (C) the thermal conductivity The content of the reactive alumina fine particles is 80 to 43% by volume (total amount 100% by volume), and the content of the (B) nonionic surfactant is 0.02 of the content of the (C) thermally conductive alumina fine particles (B-1) polyoxyethylene-polyoxypropylene glycol having a HLB value of 1.8 or more and 18 or less, wherein the (B) nonionic surfactant has a weight percent or more and less than 0.2 percent by weight. Or (B-2) HLB value is greater than 9.5 and is 19 or less, and polyoxyethylene It is characterized in that a heat dissipating agent, which is a nonionic surfactant containing a unit and a hydrophobic group, is sandwiched or interposed. The nonionic surfactant (B-2) containing a polyoxyethylene unit and a hydrophobic group preferably further contains a hydroxyl group.

[Reference example]
As component (A) (a-1) 11.69 parts of Moresco Highlobe LB-100 (alkyl diphenyl ether, liquid) manufactured by MORE CO., LTD., As component (B) (b-5) manufactured by Sanyo Chemical Industries, Ltd. Paul PE-108 (polyoxyethylene polyoxypropylene glycol (300E.O.) (55P.O.), solid, HLB 15.5) 0.11 parts, as component (C) (c-3) Sakai Chemical Industry Co., Ltd. LPZINC-5 (polyhedral, D50: 5 μm zinc oxide powder) and (c-4) Zinc oxide powder (JIS Class 1) manufactured by Sakai Chemical Industry Co., Ltd. (polyhedral, D50: 0.7 μm zinc oxide powder) The mixture was charged into a planetary mixer and mixed under heat until uniform. The resulting viscous paste-like composition was defoamed, the viscosity at 25 ° C. and the viscosity at 150 ° C. were measured, and a sag test was performed. The measurement results and the test results are shown in Table 7.

The means for achieving this purpose is
"The claim 1 of
A heat conductive oil composition comprising (A) heat resistant organic oil, (B) nonionic surfactant and (C) heat conductive alumina fine particles, wherein the content of (A) heat resistant organic oil is 20 ~ 57% by volume, the content of (C) thermally conductive alumina fine particles is 80 to 43% by volume (total amount of (A) heat resistant organic oil and (C) thermally conductive alumina fine particles 100% by volume) And (B) the content of the nonionic surfactant is 0.02% by weight or more and less than 0.2% by weight of the content of the (C) thermally conductive alumina fine particles, and (B) the nonionic surfactant agent, (B-1) HLB value of 1.8 or more, 18 or less is polyoxyethylene - and polyoxypropylene glycol, the average particle size of (C) a thermally conductive alumina particles 0.1μm~50μm der is, viscosity of 50 Pa · s or higher at 25 ° C., Ri der less than 450 Pa · s, the thermal-conductive oil composition The [viscosity at 25 ° C.] / [viscosity at 0.99 ° C.], characterized in that it is a 0.31 to 20, thermally conductive oil composition. It consists of

The means for achieving this purpose is
"The claim 2 of
A heat conductive oil composition comprising (A) heat resistant organic oil, (B) nonionic surfactant and (C) heat conductive alumina fine particles, wherein the content of (A) heat resistant organic oil is 20 ~ 57% by volume, the content of (C) thermally conductive alumina fine particles is 80 to 43% by volume (total amount of (A) heat resistant organic oil and (C) thermally conductive alumina fine particles 100% by volume) And (B) the content of the nonionic surfactant is 0.02% by weight or more and less than 0.2% by weight of the content of the (C) thermally conductive alumina fine particles, and (B) the nonionic surfactant agent, (B-1) HLB value of 1.8 or more, 18 or less is polyoxyethylene - and polyoxypropylene glycol, the average particle size of (C) a thermally conductive alumina particles 0.1μm~50μm der is, viscosity of 50 Pa · s or higher at 25 ° C., Ri der less than 450 Pa · s, the thermal-conductive oil composition [Viscosity at 0.99 ° C.] / [viscosity at 25 ° C.] is characterized in that it is a 0.31 to 20, the heat dissipation material. It consists of

The means for achieving this purpose is
"The claim 3 of
(A) heat resistant organic oil, (B) non-ionic surfactant and (C) heat conduction in the gap between the heat generating member and the cooling member of the electronic component / electronic device or the gap between the high temperature member and the heat radiating member Conductive oil composition comprising fine alumina particles, wherein the content of (A) heat resistant organic oil is 20 to 57% by volume, and the content of (C) heat conductive alumina particles is 80 to 43 volume % (Total amount of (A) heat resistant organic oil and (C) heat conductive alumina fine particles ), and the content of (B) non-ionic surfactant is (C) heat conductive alumina fine particles Polyoxyethylene having a content of 0.02% by weight or more and less than 0.2% by weight, and (B) a nonionic surfactant having a (B-1) HLB value of 1.8 or more and 18 or less - a polyoxypropylene glycol, (C) a thermally conductive alumina particles had an average particle diameter of 0.1μm~50μm, 2 5 Viscosity at ° C. is 50 Pa · s or more, 450 Pa · s less than der is, emissivity agent is from 0.31 to 20 [Viscosity at 25 ° C.] / [viscosity at 0.99 ° C.] of the thermally conductive oil composition An electronic device characterized in that it is held.
Claim 4
A heat conductive oil composition comprising (A) heat resistant organic oil, (B) nonionic surfactant and (C) heat conductive alumina fine particles, wherein the content of (A) heat resistant organic oil is 20 ~ 57% by volume, and the content of (C) thermally conductive alumina fine particles is 80 to 43% by volume (the total amount of (A) heat resistant organic oil and (C) thermally conductive alumina fine particles 100% by volume) And (B) the content of the nonionic surfactant is 0.02% by weight or more and less than 0.2% by weight of the content of the (C) thermally conductive alumina fine particles, and (B) the nonionic surfactant The agent is a nonionic surfactant having (B-2) HLB value of greater than 9.5 and 19 or less and containing a polyoxyethylene unit and a hydrophobic group, and (C) thermally conductive alumina fine particles Having an average particle size of 0.1 μm to 50 μm and a viscosity at 25 ° C. of 50 Pa · s or more and less than 450 Pa · s, [150 ° C. Thermally conductive oil composition characterized in that the viscosity in a viscosity] / [the viscosity at 25 ° C.] is 0.31 to 20.
Claim 5
The nonionic surfactant (B-2) containing a polyoxyethylene unit and a hydrophobic group is polyoxyethylene monoalkyl ether, polyoxyethylene sorbitan mono fatty acid ester, polyoxyethylene bisphenol A ether, polyoxyethylene bisphenol F Ether, polyoxyethylene alkyl diether, polyoxyethylene polycyclic phenyl ether, polyoxyethylene phenyl ether, polyoxyethylene cumyl phenyl ether, polyoxyethylene tribenzyl phenyl ether, or polyoxyethylene benzyl ether The thermally conductive oil composition according to claim 4, wherein
Claim 6
A heat conductive oil composition comprising (A) heat resistant organic oil, (B) nonionic surfactant and (C) heat conductive alumina fine particles, wherein the content of (A) heat resistant organic oil is 20 ~ 57% by volume, and the content of (C) thermally conductive alumina fine particles is 80 to 43% by volume (the total amount of (A) heat resistant organic oil and (C) thermally conductive alumina fine particles 100% by volume) And (B) the content of the nonionic surfactant is 0.02% by weight or more and less than 0.2% by weight of the content of the (C) thermally conductive alumina fine particles, and (B) the nonionic surfactant The agent is a nonionic surfactant having (B-2) HLB value of greater than 9.5 and 19 or less and containing a polyoxyethylene unit and a hydrophobic group, and (C) thermally conductive alumina fine particles Having an average particle size of 0.1 μm to 50 μm and a viscosity at 25 ° C. of 50 Pa · s or more and less than 450 Pa · s, [150 ° C. The heat dissipation agent is characterized in that the viscosity in a viscosity] / [the viscosity at 25 ° C.] is 0.31 to 20.
According to claim 7,
The nonionic surfactant (B-2) containing a polyoxyethylene unit and a hydrophobic group is polyoxyethylene monoalkyl ether, polyoxyethylene sorbitan mono fatty acid ester, polyoxyethylene bisphenol A ether, polyoxyethylene bisphenol F Ether, polyoxyethylene alkyl diether, polyoxyethylene polycyclic phenyl ether, polyoxyethylene phenyl ether, polyoxyethylene cumyl phenyl ether, polyoxyethylene tribenzyl phenyl ether, or polyoxyethylene benzyl ether The heat dissipating agent according to claim 6, which is assumed to be.
Claim 8
(A) heat resistant organic oil, (B) non-ionic surfactant and (C) heat conduction in the gap between the heat generating member and the cooling member of the electronic component / electronic device or the gap between the high temperature member and the heat radiating member Conductive oil composition comprising fine alumina particles, wherein the content of (A) heat resistant organic oil is 20 to 57% by volume, and the content of (C) heat conductive alumina particles is 80 to 43 volume % (Total amount of (A) heat resistant organic oil and (C) heat conductive alumina fine particles), and the content of (B) non-ionic surfactant is (C) heat conductive alumina fine particles 0.02% by weight or more and less than 0.2% by weight of the content; (B) the nonionic surfactant has a (B-2) HLB value of more than 9.5 and 19 or less; Nonionic surfactant containing oxyethylene unit and hydrophobic group, (C) thermally conductive alumina fine particles have an average particle size of 0.1 μm to 5 μm A heat dissipating agent which is 0 μm, has a viscosity of 50 Pa · s or more and less than 450 Pa · s at 25 ° C. and a viscosity of 150 ° C./a viscosity at 25 ° C. of 0.31 to 20 is held. An electronic device characterized by
The method according to claim 9,
The nonionic surfactant (B-2) containing a polyoxyethylene unit and a hydrophobic group is polyoxyethylene monoalkyl ether, polyoxyethylene sorbitan mono fatty acid ester, polyoxyethylene bisphenol A ether, polyoxyethylene bisphenol F Ether, polyoxyethylene alkyl diether, polyoxyethylene polycyclic phenyl ether, polyoxyethylene phenyl ether, polyoxyethylene cumyl phenyl ether, polyoxyethylene tribenzyl phenyl ether, or polyoxyethylene benzyl ether The electronic device according to claim 8. It consists of

Polyoxyethylene as a nonionic surfactant containing a polyoxyethylene unit and a hydrophobic group which is the component (B-2), and a nonionic surfactant containing a hydroxyl group, a polyoxyethylene unit and a hydrophobic group Monoalkyl ether, polyoxyethylene monoalkyl phenyl ether, polyoxyethylene monoalkyl naphthyl ether, polyoxyethylene hydrogenated castor oil, polyoxyethylene hydrogenated castor oil, polyoxyethylene alkylamide, polyoxyethylene mono fatty acid ester, polyoxyethylene Di-fatty acid ester, polyoxyethylene propylene glycol fatty acid ester, polyoxyethylene sorbitan mono-fatty acid ester, polyoxyethylene sorbitan tri-fatty acid ester, polyoxyethylene bisphenol A ether, polyoxyethylene Ren bisphenol F ether, polyoxyethylene polycyclic phenyl ether, polyoxyethylene phenyl ether, polyoxyethylene styrenated phenyl ether, polyoxyethylene alkyl diethers, polyoxyethylene distyrenated phenyl ether, polyoxyethylene cumyl phenyl ether, Examples thereof include polyoxyethylene tribenzyl phenyl ether and polyoxyethylene benzyl ether.

[Example 9]
In Example 1, instead of (b-1) Neupol PE-61 (polyoxyethylene polyoxypropylene glycol (5E.O.) (30 P.O., liquid, HLB 1.9), (b-10) ) A viscous paste-like composition was prepared under the same conditions except using Kao Corporation Emalgen 10 5 (polyoxyethylene lauryl ether (3.8 EO) (liquid, HLB 9.7), and its viscosity at 25 ° C. The viscosity at 150 ° C. was measured, and a drip test was performed, and the measurement results and the test results are shown in Table 6.

Claims (8)

A heat conductive oil composition comprising (A) heat resistant organic oil, (B) nonionic surfactant and (C) heat conductive fine particles, wherein the content of (A) heat resistant organic oil is 20 to 20. 57% by volume, the content of (C) thermally conductive fine particles is 80 to 43% by volume (total amount 100% by volume), the content of (B) nonionic surfactant is (C) heat conduction Wt% or more and less than 0.2 wt% of the content of the organic fine particles, (B) the nonionic surfactant has (B-1) HLB value of 1.8 or more and 18 or less Polyoxyethylene-polyoxypropylene glycol, or (B-2) a nonionic surfactant having a HLB value of greater than 9.5 and not more than 19 and containing a polyoxyethylene unit and a hydrophobic group Heat conductive oil composition characterized by the above. The thermally conductive oil composition according to claim 1, wherein the nonionic surfactant (B-2) containing a polyoxyethylene unit and a hydrophobic group further contains a hydroxyl group. The thermally conductive oil according to claim 1 or 2, wherein [the viscosity at 150 ° C] / [the viscosity at 25 ° C] of the thermally conductive oil composition is 0.31 to 20. Composition. A heat conductive oil composition comprising (A) heat resistant organic oil, (B) nonionic surfactant and (C) heat conductive fine particles, wherein the content of (A) heat resistant organic oil is 20 to 20. 57% by volume, the content of (C) thermally conductive fine particles is 80 to 43% by volume (total amount 100% by volume), the content of (B) nonionic surfactant is (C) heat conduction Wt% or more and less than 0.2 wt% of the content of the organic fine particles, (B) the nonionic surfactant has (B-1) HLB value of 1.8 or more and 18 or less Polyoxyethylene-polyoxypropylene glycol, or (B-2) a nonionic surfactant having a HLB value of greater than 9.5 and not more than 19 and containing a polyoxyethylene unit and a hydrophobic group Characteristic, heat dissipation agent. The heat dissipating agent according to claim 4, wherein the nonionic surfactant (B-2) containing a polyoxyethylene unit and a hydrophobic group further contains a hydroxyl group. The heat sink according to claim 4 or 5, wherein the viscosity of the heat sink at 150 ° C / the viscosity at 25 ° C is 0.31 to 20. (A) heat resistant organic oil, (B) non-ionic surfactant and (C) heat conduction in the gap between the heat generating member and the cooling member of the electronic component / electronic device or the gap between the high temperature member and the heat radiating member Conductive oil composition comprising fine particles, wherein the content of (A) heat resistant organic oil is 20 to 57% by volume, and the content of (C) heat conductive particles is 80 to 43% by volume ( The total amount is 100% by volume, and the content of (B) the nonionic surfactant is 0.02% by weight or more and less than 0.2% by weight of the content of the (C) thermally conductive fine particles, B) The nonionic surfactant has a (B-1) polyoxyethylene-polyoxypropylene glycol having an HLB value of 1.8 or more and 18 or less, or (B-2) an HLB value of 9.5 or more A heat sink, which is a non-ionic surfactant having a size of 19 or less and containing a polyoxyethylene unit and a hydrophobic group, is sandwiched. An electronic device characterized by The electronic device according to claim 7, wherein the nonionic surfactant (B-2) containing the polyoxyethylene unit and the hydrophobic group further contains a hydroxyl group.

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