Measurement device for estimating thermal characteristics, and measurement method for estimating thermal characteristics by using same
11327034 · 2022-05-10
Assignee
Inventors
Cpc classification
International classification
Abstract
A measurement device for estimating thermal characteristics includes a heat generating source unit that has heat sensors for detecting heat radiating toward a measurement sample unit, and that heats the measurement sample unit, the measurement sample unit, and a heat cooling source unit that has heat sensors for detecting heat radiating from the measurement sample unit, and that cools the measurement sample unit, wherein those units are sequentially stacked, the measurement sample unit has a three-layer structure consisting of an object to be measured for estimating thermal characteristics, and heat conducting materials that sandwich the object, the heat conducting materials are adhered to the heat generating source unit and the heat cooling source unit one another through a heat-transfer promoting agent therebetween, the object to be measured for estimating thermal characteristics and the heat conducting materials are adhered to one another through physical contact, chemical contact, and/or chemical bond contact.
Claims
1. A measurement device for estimating thermal characteristics comprising: a measurement sample unit; a heat generating source unit that has heat sensors for detecting heat radiating toward the measurement sample unit, and that heats the measurement sample unit; a heat cooling source unit that has heat sensors for detecting heat radiating from the measurement sample unit, and that cools the measurement sample unit; and a support unit provided for the heat generating source unit, the measurement sample unit, and the heat cooling source unit, wherein the heat generating source unit, the measurement sample unit, the heat cooling source unit, and the support unit are sequentially stacked, the measurement sample unit has a three-layer structure consisting of an object to be measured for estimating thermal characteristics, and heat conducting materials that sandwich the object, the heat conducting materials are adhered to the heat generating source unit and the heat cooling source unit through a reducing agent for a value of interfacial contact thermal resistance comprising a heat-transfer promoting agent therebetween, the object to be measured for estimating the thermal characteristics has a sample embedded in a hardened material from an un-crosslinked liquid-silicone liquiform rubber composition, and the object to be measured for estimating the thermal characteristics and the heat conducting materials are adhered to one another through at least one of physical contact, chemical contact, and chemical bond contact, and are contacted in the measurement sample unit, and the heat-transfer promoting agent includes: high purity water selected from the group consisting of heavy water, distilled water, and ion-exchanged water, and at least one selected from the group consisting of: (i) a surface active agent selected from the group consisting of a cationic surfactant, a nonionic surfactant, an anionic surfactant, and an ampholytic surfactant, (ii) a water-soluble polymer selected from the group consisting of carboxy methyl cellulose, polyethylene glycol, and polyvinyl alcohol, (iii) a builder selected from the group consisting of sodium sulfate, sodium sulfite, sodium carbonate, ammonium sulfite, ammonium carbonate, sodium phosphate, sodium silicate, ammonium silicate, ammonium phosphate, sodium phosphite, ammonium phosphite, sodium nitrate, sodium nitrite, ethylenediaminetetraacetic acid, ethylenediamine, and ammonium ethylenediaminetetraacetate, and (iv) a metallic surface stabilizer selected from the group consisting of triazine trithiol metallic salt, benzotriazole hydrochloride, ethylenediaminetetraacetic acid, ethylenediaminetetraacetic acid-lactic acid, resorcin, t-butylphenol, and aminophenyl aniline.
2. The measurement device for estimating the thermal characteristics according to claim 1, further comprising a length measuring device which measures at least one of a thickness of the measurement sample unit and the object to be measured for estimating the thermal characteristics.
3. The measurement device for estimating the thermal characteristics according to claim 1, wherein the heat generating source unit consists of a heat insulation material, a heat generating source that indwells with joining to an insulating resin which contacts the heat insulation material, and a metallic block which contacts the insulating resin at a side of the measurement sample unit, and the heat insulation material, the heat generating source and the metallic block are sequentially stacked, and contacting thereof is bonding by a molecular adhesive agent.
4. The measurement device for estimating the thermal characteristics according to claim 1, wherein the measurement sample unit is the three-layer structure consisting of the heat conducting materials of two metallic plates, and the object to be measured for estimating the thermal characteristics sandwiched therebetween, and the heat conducting materials of the two metallic plates and the object to be measured are adhered through at least one of the physical contact, the chemical contact, and the chemical bond contact.
5. The measurement device for estimating the thermal characteristics according to claim 1, wherein at least one of thermal spaces, which have a permissible value of thermal resistance, a permissible affectedness of volatility, independence of pressurization, and independence of distance of a gap, are provided between the measurement sample unit and a metallic block in the heat generating source unit which contacts thereto, and between the measurement sample unit and a metallic block in the heat cooling source unit which contacts thereto.
6. The measurement device for estimating the thermal characteristics according to claim 1, wherein at least one of thermal spaces, which have a permissible value of thermal resistance, a permissible affectedness of volatility, independence of pressurization, and independence of distance of a gap, are provided between the heat conducting material in the measurement sample unit and a metallic block in the heat generating source unit which contacts thereto, and between the heat conducting material in the measurement sample unit and a metallic block in the heat cooling source unit which contacts thereto, and the thermal spaces are filled with the heat-transfer promoting agent.
7. The measurement device for estimating the thermal characteristics according to claim 1, wherein the heat conducting materials and the object to be measured for estimating the thermal characteristics are adhered through at least one of the chemical contact through a heat-transfer promoting agent and the chemical bond contact through a molecular adhesive agent.
8. The measurement device for estimating the thermal characteristics according to claim 1, wherein the measurement sample unit is the three-layer structure, and the object to be measured for estimating the thermal characteristics is a piece or plural pieces of measuring sheets having a thickness in a range of 0.001 mm to 20 mm per piece.
9. The measurement device for estimating the thermal characteristics according to claim 1, wherein the measurement sample unit has a single set or stacked plural sets of the three-layer structure in which the object to be measured for estimating the thermal characteristics is sandwiched between the heat conducting materials.
10. The measurement device for estimating the thermal characteristics according to claim 1, wherein the measurement sample unit has a single set or stacked plural sets of the three-layer structure.
11. The measurement device for estimating the thermal characteristics according to claim 1, wherein the measurement device measures a value of a contact thermal resistance between the object to be measured for estimating the thermal characteristics and the heat conducting materials in the three-layer structure, and a value of a thermal resistance and a thermal conductivity of the object to be measured for estimating the thermal characteristics, as standard average values of an identical object to be measured for estimating the thermal characteristics, the object to be measured for estimating the thermal characteristics is a piece or plural pieces of measuring sheets having in a range of 0.001 mm to 10 mm per piece, the values of the contact thermal resistance and the thermal resistance of the object to be measured for estimating the thermal characteristics are in a range of 0.001*10.sup.−3 m.sup.2K/W to 1 m.sup.2K/W, and the thermal conductivity of the object to be measured for estimating the thermal characteristics is in a range of 0.01 W/mK to 20 W/mK.
12. The measurement device for estimating the thermal characteristics according to claim 1, wherein the measurement device is used for measuring a value of a contact thermal resistance between the object to be measured for estimating the thermal characteristics and the heat conducting materials in the three-layer structure, and a value of a thermal resistance and a thermal conductivity of the object to be measured for estimating the thermal characteristics, as standard average values of an identical object to be measured for estimating the thermal characteristics, stacked plural sets of the three-layer structure are stacked at most 5 units, and an applied layer of the heat-transfer promoting agent having in a range of 5 mg/4.84 cm.sup.3 to 20 mg/4.84 cm.sup.3 is provided between the object to be measured for estimating the thermal characteristics and the heat conducting materials, and between the plural units of the three-layer structure, and the value of the thermal resistance is a total value of a thermal resistance of the objects to be measured for estimating the thermal characteristics within a range of 0.01 MPa to 3 MPa of pressure of a contacted surface on the stacked plural sets of the three-layer structure.
13. The measurement device for estimating the thermal characteristics according to claim 1, further comprising a load unit which is provided with a load measurement device, and which applies a load onto the measurement sample unit.
14. The measurement device for estimating the thermal characteristics according to claim 13, wherein the load unit has a load cell that conducts the load onto the object to be measured for estimating the thermal characteristics, and a circuit that converts deformation which is detected in the load cell by the load measurement device into a voltage.
15. A measurement method for estimating thermal characteristics comprising: measuring the thermal characteristics of a value of a contact thermal resistance, a value of a thermal resistance, and a thermal conductivity of an object to be measured for estimating the thermal characteristics using a measurement device for estimating the thermal characteristics comprising: a measurement sample unit; a heat generating source unit that has heat sensors for detecting heat radiating toward the measurement sample unit, and that heats the measurement sample unit; a heat cooling source unit that has heat sensors for detecting heat radiating from the measurement sample unit, and that cools the measurement sample unit; and a support unit provided for the heat generating source unit, the measurement sample unit, and the heat cooling source unit, wherein the heat generating source unit, the measurement sample unit, the heat cooling source unit, and the support unit are sequentially stacked; adhering the heat conducting materials to the heat generating source unit and the heat cooling source unit through a reducing agent for a value of interfacial contact thermal resistance comprising a heat-transfer promoting agent therebetween, preparing a three-layer structure consisting of an object to be measured for estimating the thermal characteristics, and the heat conducting materials that sandwich the object so that the measurement sample unit has the three-layer structure, adhering the object to be measured for estimating the thermal characteristics to the heat conducting materials through at least one of physical contact, chemical contact, and chemical bond contact, and then, measuring the thermal characteristics, wherein the heat-transfer promoting agent includes: high purity water selected from the group consisting of heavy water, distilled water, and ion-exchanged water, and at least one selected from the group consisting of: (i) a surface active agent selected from the group consisting of a cationic surfactant, a nonionic surfactant, an anionic surfactant, and an ampholytic surfactant, (ii) a water-soluble polymer selected from the group consisting of carboxy methyl cellulose, polyethylene glycol, and polyvinyl alcohol, (iii) a builder selected from the group consisting of sodium sulfate, sodium sulfite, sodium carbonate, ammonium sulfite, ammonium carbonate, sodium phosphate, sodium silicate, ammonium silicate, ammonium phosphate, sodium phosphite, ammonium phosphite, sodium nitrate, sodium nitrite, ethylenediaminetetraacetic acid, ethylenediamine, and ammonium ethylenediaminetetraacetate, and (iv) a metallic surface stabilizer selected from the group consisting of triazine trithiol metallic salt, benzotriazole hydrochloride, ethylenediaminetetraacetic acid, ethylenediaminetetraacetic acid-lactic acid, resorcin, t-butylphenol, and aminophenyl aniline.
16. A heat radiation method on the measurement method for estimating thermal characteristics according to claim 15, further comprising radiating heat in the three-layer structure, which is extracted from a cohort of manufacturing lots thereof or any one of the cohort of manufacturing lots, and which consists of an object to be measured for estimating the thermal characteristics, and heat conducting materials that sandwich and adhere the object through the at least one of the physical contact, the chemical contact, and the chemical bond contact, wherein the three-layer structure is sandwiched between a heat generating source material and a heat cooling source material, and is used for a portion in any one selected from an electric material, an electronic material, a printed-wiring assembly for a semiconductor component, a motor, a lighting equipment, an automobile supply, and a radiating material.
17. A reducing agent for a value of interfacial contact thermal resistance comprising a heat-transfer promoting agent, the heat-transfer promoting agent including: high purity water selected from the group consisting of heavy water, distilled water, and ion-exchanged water; and at least one selected from the group consisting of: (i) a surface active agent selected from the group consisting of a cationic surfactant, a nonionic surfactant, an anionic surfactant, and an ampholytic surfactant; (ii) a water-soluble polymer selected from the group consisting of a carboxy methyl cellulose, polyethylene glycol, and polyvinyl alcohol; (iii) a builder selected from the group consisting of sodium sulfate, sodium sulfite, sodium carbonate, ammonium sulfite, ammonium carbonate, sodium phosphate, sodium silicate, ammonium silicate, ammonium phosphate, sodium phosphite, ammonium phosphite, sodium nitrate, sodium nitrite, ethylenediaminetetraacetic acid, ethylenediamine, and ammonium ethylenediaminetetraacetate; and (iv) a metallic surface stabilizer selected from the group consisting of triazine trithiol metallic salt, benzotriazole hydrochloride, ethylenediaminetetraacetic acid, ethylenediaminetetraacetic acid-lactic acid, resorcin, t-butylphenol, and aminophenyl aniline, wherein the reducing agent is suitable for use in a measurement device for estimating thermal characteristics comprising: a measurement sample unit, a heat generating source unit that has heat sensors for detecting heat radiating toward the measurement sample unit, and that heats the measurement sample unit, a heat cooling source unit that has heat sensors for detecting heat radiating from the measurement sample unit, and that cools the measurement sample unit, the measurement sample unit has a three-layer structure consisting of an object to be measured for estimating thermal characteristics, and heat conducting materials that sandwich the object, the heat conducting materials are adhered to the heat generating source unit and the heat cooling source unit through a reducing agent for a value of interfacial contact thermal resistance comprising a heat-transfer promoting agent therebetween, and the object to be measured for estimating the thermal characteristics has a sample embedded in a hardened material from an un-crosslinked liquid-silicone liquiform rubber composition, and the object to be measured for estimating the thermal characteristics and heat conducting materials are adhered to one another through at least one of physical contact, chemical contact, and chemical bond contact, and are contacted in the measurement sample unit.
Description
BRIEF DESCRIPTION OF DRAWINGS
(1)
(2)
(3)
(4)
(5)
(6)
(7)
(8)
(9)
(10)
(11)
(12)
MODE FOR CARRYING OUT THE INVENTION
(13) Hereunder, the embodiments for carrying out the present invention are explained according to figures.
(14) First of all, outline of the overall features is explained.
(15) (Overall Features)
(16)
(17) Next, individual features of the load unit 3 which is connected to a data acquisition and control system (see
(18) (Feature of the Load Unit)
(19) The load unit 3 has a load screw rod 3a which loads pressure to the measurement sample unit 5, a SUS screw-cut plate 3b which screws the load screw rod 3a and constringes it by overspin, a guide 3g which makes the SUS screw-cut plate 3b move up and down without rotation during the overspin for constringing or back spin for easing, a load cell 3d which detects a load applied onto the measurement sample unit 5 by the load screw rod 3a, and a heat insulation plate 3e as a heat insulation block which connects to the load cell 3d and prevents heat radiation from the heat generating source unit 4. Although it is preferable to use reducing gears so as to apply the regular load in this case, thus contraption is not restricted. Distortion gauges 3f.sub.1 and 3f.sub.2, which detects the applied load by the load cell 3d as a strain voltage, are connected to a distortion measuring unit 9a (see
(20) (Feature of the Heat Generating Source Unit)
(21) The heat generating source unit 4 comprises a heat insulation plate 4a as a heat insulation block for addressing unidirectionally a heat flow from the heat generating source 4b, plural pieces of a heat generating source plate consisting of polyimide/stainless steel wire/polyimide (PI/SUS/PI) as insulating resin of polyimide films 4d.sub.1 and 4d.sub.2 and an electrothermal heater 4e for a heat generating source unit 4b, a wire 4f which supplies a stable direct current electricity and connects from a stabilized power supply 9c (see
(22) (Feature of the Measurement Sample Unit)
(23) The measurement sample unit 5 comprises one of the three-layer structure as a metallic plate/a sample to be measured/a metallic plate that consists of an object 5b to be measured for estimating thermal characteristics (the sample to be measured) and heat conducting materials (metallic plates) 5a and 5c which sandwich it. The three-layer structure has layers 5a.sub.1 and 5c.sub.1 (see
(24) As shown in
(25) The object 5b to be measured for estimating thermal characteristics not only can be appropriately selected as the sample to be measured whose thickness may be varied at any time, but also can be voluntarily selected as the sample to be measured having complex shapes and may be a three-layer structure having the complex shapes (see
(26) The measurement sample unit 5 consisting of the three-layer structure as shown in
(27) A length measuring device 8 (see
(28) The length measuring device 8 is used for correcting thickness of the sample, by measuring the thickness of the sample to be measured thereby after applying the load pressure on the surface to the object 5b to be measured for estimating thermal characteristics and then coming up to the steady state of temperature difference between both of the metallic blocks.
(29) The length measuring device 8 consist of an upper-side gauge head 8a.sub.1 of the length measuring device and a down-side gauge head 8a.sub.2 of the length measuring device. The gauge heads 8a.sub.1 and 8a.sub.2 of the length measuring device are respectively connected via wires 8b.sub.1 and 8b.sub.2 for a length measuring unit to a length measurement unit 9g in a data acquisition and control system 9 (see
(30) (Feature of the Heat Cooling Source Unit)
(31) The heat cooling source unit 6 comprises a down-side heat-collection metallic block 6a made of Al which contacts to the measurement sample unit 5, and thermocouples 6c.sub.1 and 6c.sub.2 as two thermosensors which connect to the down-side heat-collection metallic block 6a. The thermocouples 6c.sub.1 and 6c.sub.2 connect via wires 6d.sub.1 and 6d.sub.2 for a high-precision temperature-voltage measuring unit to the high-precision temperature-voltage measuring unit 9b in a data acquisition and control system 9 (see
(32) (Feature of the Support Unit)
(33) In the support unit 7, a heat insulation material 7a and a stillage 7b, which mounts the load unit 3, the heat generating source unit 4, the measurement sample unit 5 and the heat cooling source unit 6, are supported by pedestals 7c.sub.1 and 7c.sub.2 having a cone shape so as to be hard to be affected by external environment.
(34) (Features of the Data Acquisition and Control System and the Data-Indicating System)
(35) In the data acquisition and control system 9, a pair of thermocouples 4g.sub.1 and 4g.sub.2 connected to the upper-side heat-collection metallic block 4c of the heat generating source unit 4 and a pair of thermocouples 6c.sub.1 and 6c.sub.2 connected to the down-side heat-collection metallic block 6a of the heat cooling source unit 6, both which are used for detecting heat-transfer to the measurement sample unit 5 of the three-layer structure, are connected to the high-precision temperature-voltage measuring unit 9b for measuring and controlling the respective temperature. And a stabilized power supply of direct current electricity 9c and an electric shunt 9d, which are connected to the heat generating source 4b of the heat generating source unit 4, are connected to the high-precision temperature-voltage measuring unit 9b. Additionally, the distortion gauges 3f.sub.1 and 3f.sub.2 of a load cell 3d are connected to a distortion measuring unit 9a. The gauge heads 8a.sub.1 and 8a.sub.2 of the length measuring device are connected to the length measurement unit 9g in order to accurately measure the thickness of the object 5b to be measured for estimating thermal characteristics. The high-precision temperature-voltage measuring unit 9b, the distortion measuring unit 9a and the length measurement unit 9g are connected to a measurement and calculation unit 9e for estimating thermal characteristics. The measurement and calculation unit 9e for estimating thermal characteristics is connected to an external output interface unit 9f. Those are controlled by a central processing unit (CPU) of a computer which information-processes an electrical signal from a body of the measurement device 1 for estimating thermal characteristics via the data acquisition and control system.
(36) As shown in
(37) (Features Between of Respective Component Materials and Parts)
(38) As regards features between respective component materials and parts in the measurement device for estimating thermal characteristics, binding surfaces between different materials except for attachment of the measurement sample unit between the metallic blocks put into a bonding state which is mixed with the chemical bonds and the molecular forces by a molecular binding technology with using a molecular adhesive agent. Binding methods are employed so as to take into account of transmittance of stress or heat quantity.
(39) (Load to the Object to be Measured)
(40) As regards arrangement of the functional parts of the measurement device 1 for estimating thermal characteristics, the load unit 3 is stayed away from the object 5b to be measured for estimating thermal characteristics. There is a problem whether the measured pressure differs from a pressure at a portion of the sample to be measured or not. However, when both pressures are compared, there is little difference between both pressures below 0.4 MPa of pressure. There is difference within ±2% at approximately 1 MPa, while there is little difference between the measured thermal resistances. Therefore it is thought that there are few problems, because the commonsensical loaded pressure applied during the usage thereof is 1 MPa or less.
(41) (Bonding of the Heat Generating Source Unit)
(42) The heat generating source unit 4 of the measurement device 1 for estimating thermal characteristics is prepared as follows, in order to accurately measure the change of the temperature of the measurement sample unit 5 as the three-layer structure. The respective interfaces between the heat insulation plate 4a as the heat insulation material and the upper-side polyimide film 4d.sub.1 as insulation resin of the heat generating source 4b, between the upper-side polyimide film 4d.sub.1 and the circuit wiring 4e made of stemless as the electrothermal heater, between the circuit wiring 4e made of stemless and the down-side polyimide film 4d.sub.2, and between the down-side polyimide film 4d.sub.2 and the upper-side heat-collection metallic block 4c, are prepared through the molecular adhesive agent technique for bonding of non-fluent materials by soaking them into an aqueous solution (0.01 wt. %) of the molecular adhesive agent and then drying them, and contacting and heating them (at 120° C. for 10 min.) without using adhesive.
(43) (The Three-Layer Structure of the Measurement Sample Unit)
(44) When using the measurement device 1 for estimating thermal characteristics, there are interface layers of two portions (the heat conducting materials 5a and 5c as the metallic plates) of the contact interfaces 5ab and 5bc of the object to be measured. They are located between the down-side surface of the upper-side heat-collection metallic block 4c in the heat generating source unit 4 or the upper-side surface of the down-side heat-collection metallic block 6a of the heat cooling source unit 6 and the three-layer structure. Specifically low-volatile, pressure-independent and gap-length-independent heat spaces with extremely low value of thermal resistance are provided in any contact gap between metal/metal among the metallic plates, for example, Al/Al, Cu/Al, Al/Cu or Cu/Cu or alloy combination thereof. In the case, it is important that the value of thermal resistance of the contact gap layer between the materials is always kept as a constant value of contact thermal resistance in spite of the measurement conditions.
(45) As shown in
(46) (The Steady State in Measuring Thermal Resistance by the Measurement Device for Estimating Thermal Characteristics)
(47) An expeditious measurement is desired in the measurement of the thermal resistance. Therefore, an expeditious property was investigated by temporally measuring temperatures (T.sub.1 and T.sub.7) on the surfaces of both metallic blocks of the upper-side heat-collection metallic block 4c and the down-side heat-collection metallic block 6a as shown in
(48) Hereunder, the total value of thermal resistance of the three-layer structure as shown in
(49) R=the value of thermal resistance between (1)-(7)=R.sub.(1)+R.sub.(2)+R.sub.(3)+R.sub.(4)+R.sub.(5)+R.sub.(6)+R.sub.(7)
(50) And values of thermal resistance of components as the contact interface, the metal and the object to be measured are respectively illustrated as below;
(51) the value of contact thermal resistance between Al/Al=R.sub.(1)+R.sub.(7)=0.015 (10.sup.−3 m.sup.2 K/W)
(52) the value of contact thermal resistance between Al/the object to be measured=R.sub.(3)+R.sub.(5)=Rc (10.sup.−3 m.sup.2 K/W)
(53) the value of thermal resistance of Al=R.sub.(3)+R.sub.(6)=0.00417 (10.sup.−3 m.sup.2 K/W)
(54) the value of thermal resistance of the object to be measured=R.sub.(4)=Rs
(55) the total value of thermal resistance: Rt=R+Rc−0.015−2*0.00417 ΔT=T.sub.1−T.sub.7.
(56) (The Composition of the Heat-Transfer Promoting Agent)
(57) The thermal spaces, which are generated between the upper-side surface and the down-side surface of the heat conducting materials (the metallic plates) 5a and 5c of the three-layer structure as the measurement sample unit 5 in the measurement device 1 for estimating thermal characteristics, are filled up with a vehicle of the heat-transfer promoting agent. Thereby, the value of contact thermal resistance in the thermal spaces may be an extremely low value of thermal resistance, and low-volatile, pressure-independent and gap-length-independent.
(58) The heat-transfer promoting agent is coated onto the upper-side surface and down-side surface of two metallic plates such as Al plates on the top and bottom of the three-layer structure of the measurement sample unit 5 in the measurement device 1 for estimating thermal characteristics. The components of the heat-transfer promoting agent comprise high purity water selected from heavy water, distilled water and ion-exchanged water; a surface active agent selected from a cationic surfactant, a nonionic surfactant, an anionic surfactant, an ampholytic surfactant; carboxy methyl cellulose, polyethylene glycol, and polyvinyl alcohol; a builder selected from sodium sulfate, sodium sulfite, sodium carbonate, ammonium sulfite, ammonium carbonate, sodium phosphate, sodium silicate, ammonium silicate, ammonium phosphate, sodium phosphite, ammonium phosphite, sodium nitrate, sodium nitrite, ethylenediaminetetraacetic acid, ethylenediamine, and ammonium ethylenediaminetetraacetate; and/or a metallic surface stabilizer selected from triazine trithiol metallic salt, benzotriazole hydrochloride, EDTA (ethylenediaminetetraacetic acid), EDTA-lactic acid salt, resorcin, t-butylphenol, and aminophenyl aniline. In the case, the thermal spaces may have the extremely low value of thermal resistance, and become low-volatile, pressure-independent and gap-length-independent.
(59) The cationic surfactant for the present invention means trimethyl single-chained=higher-saturated-alkyl ammonium halogenide, trimethyl single-chained=higher-unsaturated-alkyl ammonium halogenide, dimethyl double-chained=higher-saturated-alkyl ammonium halogenide, trimethyl single-chained=higher-saturated-alkyl ammonium halogenide, trimethyl single-chained=higher-unsaturated-alkyl ammonium hydroxide, dimethyl double-chained=higher-saturated-alkyl ammonium hydroxide, dimethyl double-chained=higher-unsaturated-alkyl ammonium halogenide, methyl triple-chained=higher-saturated-alkyl ammonium halogenide, methyl triple-chained=higher-unsaturated-alkyl ammonium halogenide, quadruple-chained tetramethyl ammonium chloride, quadruple-chained tetraethyl ammonium chloride, quadruple-chained tetrapropyl ammonium chloride, quadruple-chained tetrabutyl ammonium chloride, triphenyl single-chained=higher-alkyl phosphonium halogenide, triphenyl single-chained=higher-alkyl phosphonium hydroxide, alkyl benzyl dimethyl ammonium salt, phosphatidyl inositol (PI), phosphatidyl serine (PS), phosphatidyl ethanol amine, tetrabutyl phosphonium bromide, tetraoctyl phosphonium bromide, tetrabutyl ammonium bromide, tetraoctyl ammonium bromide, and so on.
(60) The anionic surfactant is exemplified with steareth-6, sodium laureth sulfate, alkyl ether sulfate ester sodium salt, alkyl sulfonic acid sodium salt, linear-alkyl benzene sulfonic acid salt, alkyl ether sulfate sodium ester, alkyl ether sulfate sodium ester, reactant of tris(2-aminoethylamino) amine and organic acid, reactant of tris(2-aminoethylamino) amine and organic acid anhydride, 6-octylamino-1,3,5-triazine-4-thiol-2-thiosodium salt, 6-octylamino-1,3,5-triazine-4-thiol-2-thiopotassium salt, 6-triethoxysilyl propylamino-1,3,5-triazine-2-thiol-2-thiopotassium salt, 6-triethoxysilyl propylamino-1,3,5-triazine-2,4-diamino ethyl amine, 6-triethoxysilyl propylamino-1,3,5-triazine-2,4-diamino ethyl amine, 6-triethoxysilyl propylamino-1,3,5-triazine-2,4-diamino ethyl amine, 6-triethoxysilyl propylamino-1,3,5-triazine-2,4-dihydrazine, 6-di(trihydroxysilyl propyl)amino-1,3,5-triazine-2,4-diaminoethyl amine, 6-trihydroxysilyl propyl amino-1,3,5-triazine-2,4-diaminoethyl amine, saturated-alkyl benzene sulfonic acid salt, dialkyl sodium sulfosuccinate, saturated alkyl, monoalkyl acid salt, alkyl polyoxyethylene sulfonic acid salt, cocoyl glutamic acid TEA, cocamidemethyl MEA, cocamide MEA, ammonium laureth sulfate and so on.
(61) As ampholytic surfactant, alkyl amine oxide, fatty acid alkanolamide, alkyl amido propyl betaine, palm kernel fatty acid amido propyl betaine, alkyl amine oxide, alkyl amine oxide, alkyl betaine, lauryl hydroxy sultaine, laureth-16, lauramido propyl betaine, alkyl hydroxy sulfobetaine, alkyl amine oxide, alkyl glycoside, alkyl hydroxyl sulfobetaine, alkyl dimethyl amine oxide R(CH.sub.3).sub.2NO, alkyl carboxy betaine R(CH.sub.3).sub.2N.sup.+CH.sub.2COO.sup.−, 2-trihydroxysilyl propyl amino-3,5-diaminoethylamino-1,3,5-triazine, 2-(di-trihydroxysilyl propyl amino)-3,5-diaminoethylamino-1,3,5-triazine, 2-(di-trihydroxysilyl propyl)amino-4,6-diaminoethylamino-1,3,5-triazine, 2-(trihydroxysilyl propyl)amino-4,6-diaminoethylamino-1,3,5-triazine, 2-di(trihydroxysilyl propyl amino)-4,6-aminoethyl(diaminoethyl)amino-1,3,5-triazine, and 2-(di-trihydroxysilyl propyl) amino-4.6-di(diethylene triamino)amino-1,3,5-triazine etc. are effective.
(62) The nonionic surfactant falls into compounds such as distearic acid glycol, polyoxyethylene alkyl ether, polyoxyethylene alkyl ether RO(CH.sub.2CH.sub.2O).sub.mH (R is for example an alkyl group having 1-30 carbons, m is a number of additional mole of ethylene oxide for example 2-1000), fatty acid sorbitan ester, alkyl polyglycoside, fatty acid diethanol amide RCON(CH.sub.2CH.sub.2OH).sub.2 (R is as same as above), alkyl monoglyceryl ether ROCH.sub.2CH(OH)CH.sub.2OH (R is as same as above), coconut oil fatty acid PEG-7 glyceryl ester, polyoxyethylene alkyl ether and so on.
(63) The heat-transfer promoting agent may include other additives such as citric acid, EDTA tetrasodium salt, ethylene diamine disuccinic acid trisodium salt, panthenol, panthenyl ethyl HCl salt, methyl chloroisothiazolinone, sodium citrate, sodium xylenesulfonate, polyquaternium-10, tocopherol acetate, PPG-7, citric acid, lactic acid, potassium sorbate, glycerin, sodium hydroxide, sodium sulfite, EDTA, sodium benzoate, fragrance rice bran extract, rice extract, peony extract, lachancea, hydrolyzed rice ferment liquid, rice germ oil, cherry leaf extract, camellia seed extract, belamcanda chinensis extract, sapindus mukurossi extract, sodium chloride, citric acid, guar hydroxy propyl trimonium chloride, polyquaternium-10, polyquaternium-7, BG, ethanol, EDTA disodium salt, fragrance, caramel lemon fruit extract, kiwi extract, raspberry extract, glycyrrhizinic acid dipotassium salt, polyquaternium-10, cocamide MEA, laureth-3, sodium chloride, phosphoric acid, potassium hydroxide, benzyl alcohol, a stabilizing agent, metal sequestrant, disinfectant.
(64) Examples of the composition of the heat-transfer promoting agent or the dispersion fluent are ingredients of water of 49.7-99.88 wt. %, preferably 50-99.88 wt. %, more preferably 70-99.88 wt. %; the surface active agent of 0.1-50 wt. %, preferably 0.1-30 wt. %; the builder of 0.1-10 wt. %; and the metallic surface stabilizer of 0.1-5 wt. %. The indispensable principal ingredients are water and the surface active agent, and others take a subservient role. The surface active agent reduces viscosity of water, and coinstantaneously prevents surface vaporization. The builder increases an inhibitive effect on water vaporization by the surface active agent, and enhances contact to the metal surface and suppresses aggregation of bubbles.
(65) The foregoing indicates the examples, in which the heat conducting materials 5a and 5c as two metallic plates of the upper-side surface and down-side surface of the three-layer structure of the measurement sample unit 5 and the object 5b to be measured for estimating thermal characteristics in the measurement device 1 for estimating thermal characteristics, are tightly adhered through the chemical contact through the heat-transfer promoting agent. However, they may be tightly adhered through the chemical bond contact through the molecular adhesive agent. It is preferable that the bonding surfaces between the different materials such as the heat insulation plate 4a and the heat generating source 4b, the insulating resin 4d.sub.1 and 4d.sub.2 in the heat generating source 4b and the electrothermal heater 4e, the heat generating source 4b and the upper-side heat-collection metallic block 4c, and/or the down-side heat-collection metallic block 6a and the heat cooling source unit 6 except the bonding of the measurement sample unit in the measurement device 1 for estimating thermal characteristics, are tightly adhered to be bonded by the molecular bonding technology using the molecular adhesive agent through bonding figuration which mixes the chemical bond by more stronger covalent bonding than mere physical contact or chemical contact and the intermolecular force. Single molecule or plural molecules of the molecular adhesive agent molecules makes them bond chemically at both bonding sites thereof at once. They can be strongly bonded by the chemical bonding at many bonding sites each other.
(66) (Molecular Bonding Technology)
(67) According to the molecular bonding technology, various members of the same or different kind materials such as metal-metal, resin-resin or metal-resin, can be bonded through the chemical bonding by using the molecular adhesive agent. The molecular adhesive agent is reacted to the bonding sites such as active functions of hydroxyl groups which originally exist on the surface of the materials to be adhered, or the bonding sites such as amplified active functions which is prospectively generated on the surface of the materials to be adhered through reformulation by using acid or base etc. or by using heat, light, electricity or electromagnetic wave etc. Thereby, the molecular adhesive agent can adhere with them by the chemical bonding. Therefore, much stronger binding strength by the molecular adhesive agent is shown than one of binding by molecular force after curing a resin such as an agglutinant.
(68) Examples of the molecular adhesive agent are silane derivatives or triazine thiol derivatives having a silyl group and/or an amino group and a mercapto group which may have a substituent. The substituent is selected from the group consisting of an alkyl group, an alkoxy group, an ether group, a carbonyl group, a carboxyl group, a mercapto group an amino group, and a thioether group. The molecular adhesive agent is exemplified with the triazine thiol derivatives such as triethoxysilyl propyl triazine dithiol, tritrimethoxysilane propyl mercaptan, 6-trimethoxysilane decyl amino-1,3,5-triazine-2,4-dithiol, 6-dimethyl methoxysilane propyl amino-1,3,5-triazine-2,4-dithiol, 6-di(triethoxysilane propyl)amino-1,3,5-triazine-2,4-dithiol, 6-trimethoxysilyl propyl amino-1,3,5-triazine-2,4-di(amino ethyl)amine, and 6-6-trimethoxy silyl propyl amino-1,3,5-triazine-2,4-diazide; or the silane derivatives such as a silane coupling agent having active silyl group for forming a siloxane bond which is at least one selected from the group consisting of a hydrosilyl-containing silyl group, a vinyl-containing silyl group, an alkoxysilyl-containing silyl group, and a hydrolyzable group-containing silyl group.
(69) The molecular adhesive agent makes molecular-bonding generate after preparing solution or suspension thereof and applying it onto the surface of the materials to be adhered through coating, spraying or dipping. It is preferable that the concentration of the solution or suspension is 0.01-10 wt. %, the dipping time is 0.1-10 minutes, and the dipping temperature is 20-60° C.
(70) The molecular adhesive agent may be applied onto either surface to be bonded among the materials to be adhered, or onto both surfaces to be bonded among the materials to be adhered. At least one of the materials is applied with the molecular adhesive agent, and both materials are stuck on the surfaces to be adhered, and are exposed at room temperature or heat condition under optionally reduced or increased pressure to be adhered through the molecular bonding.
(71) (Use Method of the Three-Layer Structure)
(72) The object 5b to be measured for estimating thermal characteristics of the three-layer structure of the measurement sample unit 5 in the measurement device 1 for estimating thermal characteristics, is provided as 1 piece or plural pieces of 2 pieces or more. The relationship between the total thermal resistance and thickness thereof is determined through preferable measurement at 3 points or more by using the three-layer structure which comprises the object 5b to be measured for estimating thermal characteristics having 0.0001 mm-20 mm thickness per one piece.
(73) In the measurement device 1 for estimating thermal characteristics, when the object 5b to be measured for estimating thermal characteristics of the three-layer structure of the measurement sample unit 5 is measured by using one set (see 5 in
(74) As shown in
(75) After the objective measurement sample unit 5b.sub.1 having complex shapes as the object 5b to be measured for estimating thermal characteristics of the three-layer structure of the measurement sample unit 5 in the measurement device 1 for estimating thermal characteristics is embedded into a silicone liquid rubber 5b.sub.2, one set or plural set of 2 sets or more of the three-layer structures in which Al plates are physically contacted or chemically contacted at the upper side and the down side are stacked. Thereby, heat conducting mechanism between the metallic plates as the heat conducting materials 5a and 5c and the measurement sample or processing methods for advantageous heat conducting are enable to be developed.
(76) According to the measurement device 1 for estimating thermal characteristics, all of the value of contact thermal resistance, the value of thermal resistance and the thermal conductivity can be respectively measured as each average value by using the same measurement sample. The measurement device 1 for estimating thermal characteristics is suitable to estimate or measure the thickness of the object 5b to be measured for estimating thermal characteristics within 0.001-10 mm per 1 piece, the value of contact thermal resistance and the value of thermal resistance of the object to be measured within 0.001*10.sup.−3 m.sup.2 K/W-1 m.sup.2 K/W, and the thermal conductivity of the object 5b to be measured for estimating thermal characteristics within 0.1 W/mK-15 W/mK.
(77) (Determining Method for the Thermal Characteristics of the Three-Layer Structure)
(78) For the thermal characteristics (the contact thermal resistance, the thermal resistance and the thermal conductivity) of the object 5b to be measured for estimating thermal characteristics, at the beginning, two pieces of metallic plates as the heat conducting materials 5a and 5c having 1*22*22 mm cubic and the object 5b to be measured for estimating thermal characteristics having arbitrary thickness (Lx, 10.sup.−3 m) are used as total of three pieces having different thickness to prepare 3 sets of the three-layer structures by using 20 as previous mentioned (see
(79) The thermal characteristics (the contact thermal resistance, the thermal resistance and the thermal conductivity) of the object 5b to be measured for estimating thermal characteristics are calculated according to the following expression 1 by using the total value of thermal resistance (Rt, mK/W) as sum of the value of contact thermal resistance (Rc, mK/W) between the heat conducting materials 5a and 5c as the metallic plates of the three-layer structure and the object 5b having a constant thickness (Lx, 10.sup.−3 m) to be measured for estimating thermal characteristics and the value of thermal resistance (Rs, mK/W) of the object to be measured, the cross-section area (A) of the object 5b to be measured for estimating thermal characteristics, the temperature difference (ΔT) between the surface temperature T.sub.1 and T.sub.7 of the heat conducting materials 5a and 5c as the metallic plates of the three-layer structure, and the electricity (Φ), W).
[Expression 1]
Rt=A*ΔT/Φ expression 1
In the above expression 1, Φ is calculated from voltage E1 of the electric source of the heater and current i ((voltage E2 of the electric shunt)/(value of resistance Ro). The results thereof are shown in Table 1.
(80) TABLE-US-00001 TABLE 1 Thickness, electricity, surface area, temperature difference, and total value of thermal resistance of object to be measured of three-layer structure Thickness of Total Value Object to be Surface Temperature of Thermal Measured Electricity Area: A Difference: ΔT Resistance: Rt (mm) (W) (10.sup.−3 m.sup.2) (k) (10.sup.−3 m.sup.2K/W) 1.0 20.1 0.484 2.22 0.243 3.0 20.1 0.484 3.44 0.528 5.0 20.1 0.484 4.86 0.724
(81) In the antecedent, when the thickness (1.0, 2.0, 3.0 mm) of the object 5b to be measured for estimating thermal characteristics are fluctuated and then the thicknesses are plotted on the horizontal axis and the total value of thermal resistances are plotted on the vertical axis, the following linear relational expression 2 is obtained.
[Expression 2]
Rt=a Lx+b expression 2
The value of contact thermal resistance (Rc) is obtained from the intercept (b) thereof. The value of thermal resistance (Rs) of the object to be measured is obtained by subtracting the value of contact thermal resistance from the total value of thermal resistance. And the thermal conductivity (λ, W/m×K) of the object to be measured is obtained by dividing the thickness of the object to be measured by the value of thermal resistance. The results are shown in Table 2 as the measurement method for estimating thermal characteristics.
(82) TABLE-US-00002 TABLE 2 Total value of thermal resistance (Rt) of object to be measured of three-layer structure, value of contact thermal resistance (Rc), and value of thermal resistance (Rs) and thermal conductivity (λs) of object to be measured Value Total Value of Contact Value Total Value of Thermal Thermal of Thermal of Thermal Thermal Thickness Resistance: Rt Resistance: 2Rc Resistance: Rs Resistance Rto Conductivity: λs (mm) (10.sup.−3m.sup.2K/W) (10.sup.−3m.sup.2K/W) (10.sup.−3m.sup.2K/W) (10.sup.−3m.sup.2K/W) (W/mK) 1.0 0.243 0.128 0.115 0.007 8.69 8.19 3.0 0.528 0.128 0.400 0.007 7.50 (Average) 5.0 0.724 0.128 0.596 0.007 8.39
Embodiments
(83) Hereunder, embodiments of a measurement method for estimating thermal characteristics using a measurement device for estimating thermal characteristics of the present invention will be explained in detail. However, the scope of the present invention is not restricted by those embodiments.
Example 1
Embodiment Indicating Reasons for Occasion of Using Measurement Device for Estimating Accurate Thermal Characteristics
(84) As shown above, the thermal conductivity has been focused as an evaluation criterion of the heat conducting material. Thereby, reputations, in which the heat conducting materials having high thermal conductivity are excellent, are dominated in the industry world. Thus reputations may shake bases for manufacturing, those consequently cause to loss confidences of Japanese industries. Accordingly, the results of measurement of the value of thermal resistance and the thermal conductivity of the object 5b to be measured for estimating thermal characteristics by using the measurement device 1 for estimating thermal characteristics are indicated in Table 3.
(85) TABLE-US-00003 TABLE 3 Thermal conductivity of heat conducting material sheet having 0.2 mm as values in catalogs and results of measurement by using the present device Thermal Characteristics in Catalog Value Total Value Thermal of Contact Value of Thermal Conductivity Thermal Thermal of Thermal Resistance by using Conductivity Resistance Resistance (0.2 mm) Present Device Examples Company W/mK 10.sup.−3m.sup.2K/W 10.sup.−3m.sup.2K/W 10.sup.−3m.sup.2K/W W/mK Comparative A 9-11 0.0283 0.0132 .sup. 0.041 *.sup.2 14.5 Example 1 Comparative B 3.8 0.128 0.0230 0.151 8.19 Example 2 Comparative C 4.0 0.0195 0.0390 .sup. 0.048 *.sup.3 5.11 Example 3 Comparative D 6.2 0.228 0.0052 0.232 7.99 Example 4 Comparative E 1.5 0.215 0.0544 0.269 3.85 Example 5 Comparative F 2.8 0.0971 0.0629 0.160 4.0 Example 5 Example 1 SCL Inc. — 0.009 0.0242 .sup. 0.025 *.sup.1 4.18 Heat-transfer Promoting Agent 1 (Pure Water 95 g + Liquid Kitchen Detergent 5 g): 10 mg/4.84 cm.sup.2 Al Plate (Surface Roughness; 0.02 μm, Thermal Conductivity; 240 W/mK) Measurement Pressure: 0.3 MPa *.sup.1 to *.sup.3 indicate top 3 of the total Value of Thermal Resistance
(86) Products as the heat conducting material (the object to be measured for estimating thermal characteristics), which is manufactured and sold by Companies of A, B, C, D, E and F, were formed into the three-layer structures. Results of the three-layer structures, and results of a development article of Sulfur Chemical Laboratory Inc. (SCL Inc.), both which were measured by using the measurement device for estimating thermal characteristics, were obtained as Table 3. The results were indicated in Table 3, all which were converted into values of thermal characteristics of the object to be measured as 0.2 mm (pressure 0.3 MPa). The reason of limitation of 0.2 mm is that there are a lot of products having thickness of about 0.2 mm or less under practical, experimental or inspectional occasions. The values of the thermal conductivity in the catalogs of every company are generally smaller than the values obtained by the measurement device for estimating thermal characteristics. The sum of the value of the contact thermal resistance and the value of thermal resistance of the object to be measured means the total value of thermal resistance. Top 3 of the total value of thermal resistance and top 3 of the thermal conductivity are different each other. The development article (Example 1) of SLC Inc. was the heat conducting material having 4.18 W/mK. However, it indicates 0.025*10.sup.−3 m.sup.2 K/W of the total value of thermal resistance which was extremely smaller than the value of the product of company A having 14.5 W/mK. Nevertheless, the article of SCL Inc. was more superior than the product of company A practically, because the specific difference from the products is the low value of contact thermal resistance. The value of contact thermal resistance of the heat conducting materials having 0.2 mm or less in use affects the heat-transfer rather than the thermal conductivity.
Examples 2-6
Embodiments Using Stacked Plural Sets of the Three-Layer Structure
(87) As above mentioned in previous paragraphs, the three-layer structures were prepared by using the jig 20 for forming thereof (see
(88) TABLE-US-00004 TABLE 4 Measurement examples of one set to five sets of the three-layer structure of Cu (175 μm)/object to be measured (120 μm)/Cu (175 μm) Thermal Characteristics Value of Thermal Sample Resistance λ Object of Sets of Value of (W/mK) Nos. Whole to be Three-layer Volume Object of Thickness Measured Structure Intercept Rtc Resistance Rs Three-layer to be Example Piece (μm) (μm) (10.sup.−3m.sup.2K/W) (10.sup.−3m.sup.2K/W) (10.sup.−3m.sup.2K/W) Structure measured Example 2 1 0.470 0.120 0.039 0.0113 0.0277 12.05 4.33 Example 3 2 0.939 0.240 0.065 0.0537 14.45 4.55 Example 4 3 1.408 0.360 0.090 0.0787 15.64 4.57 Example 5 4 1.875 0.480 0.122 0.1107 15.36 4.34 Example 6 5 2.345 0.600 0.140 0.1287 16.75 4.66 Load: 0.5 MPa, Electricity: 20 W, ΔT: 1.38-4.97° C., Cu175/Rs120/Cu175 μm Rt = Rs + 2Rtc, λ = L/Rs Heat-transfer Promoting Agent 1 (Pure water 95 g + Liquid Kitchen Detergent 5 g): 10 mg/4.84 cm.sup.2, Al Plate (Surface Roughness; 0.02 μm, Thermal Conductivity; 240 W/mK), Measurement Pressure: 0.3 MPa
(89) The numbers of piece means the numbers of stacked sets of the three-layer structure. Total thickness means the thickness in which the three-layer structures were stacked under the load of 0.5 MPa. The thickness of one set of the three-layer structure of the object 5b to be measured for estimating thermal characteristics was within 0.120 mm±0.001 mm. The value of thermal resistance of the stacked plural sets of the three-layer structure means the total value of thermal resistance of the stacked plural sets of the three-layer structure, which consisted of Cu (0.175 mm)/the object to be measured (0.120 mm)/Cu (0.175 mm). Rtc was obtained by plotting relationships of the total thickness and the value of thermal resistance of the stacked plural sets of the three-layer structure, and then calculating a value of an intercept: Rtc (namely, the value of thermal resistance when thickness was 0; it means the value of contact thermal resistance). When subtracting Rtc from the value of thermal resistance of the stacked plural sets of the three-layer structure, the value of thermal resistance of the object to be measured having different thickness was obtained. Each of while values of thermal resistance was obtained by dividing by the total thickness the value of thermal resistance of the stacked plural sets of the three-layer structure. The thermal conductivity of the stacked plural sets of the object to be measured was obtained by dividing the thickness of the object to be measured by the value of the volume resistance (Rs) of the object to be measured.
(90) Although the three-layer substrate, in which thick copper plates were put in at both side, indicated high thermal conductivity altogether, that of the object to be measured was ca. 4 W/mK. For one set of the three-layer structure, a rate of the value of contact thermal resistance was large as 29%. This value was obtained under compression of 0.5 MPa. In a case when the condition is ca. 0.10 MPa as a usual usage, it is expected that the value increases double or more of 29%.
Examples 7-9, Comparative Examples 7-8, and Reference Example 1
Embodiments by Using Various Heat-Transfer Promoting Agents
(91) 20 mg/4.84 cm.sup.2 of various heat-transfer promoting agents were dropped by a dropper on the surface of the down-side heat-collection metallic block 6a (Al alloy, the thermal conductivity: 139 W/mk, Ra: 0.025 μm) arranged under the measurement sample unit 5 in the measurement device 1 for estimating thermal characteristics. They were smoothened with a glass rod, and then the overflowed agents were wiped up. Thereby, the heat-transfer promoting agents were applied within 10 mg±2 mg. Next, the upper-side heat-collection metallic block 4c (Al alloy, the thermal conductivity: 139 W/mk, Ra: 0.025 μm) was mounted onto the measurement sample unit 5 to be positioned. And then the load of 0.2 MPa was applied thereto, and the thin layer of the heat-transfer promoting agent was formed in the gap between the metallic blocks 4c and 6a. The results thereof are shown in Table 5. Incidentally, Comparative Example 7 in Table 5 indicates the case when water under atmospheric pressure was replaced instead of the heat-transfer promoting agent for the above-mentioned Examples. Comparative Example 8 in Table 5 indicates the case when a commercial item of a gel compound for heat radiation (G746 which is available from Shin-Etsu Chemical Co. Ltd., the thermal conductivity: 1.9 W/mK) was used. And Reference Example 1 in Table 5 indicates the case when air of atmospheric pressure was replaced instead of the heat-transfer promoting agent for the above-mentioned Examples.
(92) TABLE-US-00005 TABLE 5 Comparison of values of contact thermal resistance Value of Contact Thermal Resistance (10.sup.−3m.sup.2K/W) Average 10 min 20 min 30 min 40 min 50 min 60 min Value Example 7 Heat-transfer 0.0140 0.0140 0.0141 0.0147 0.0150 0.0155 0.0145 ± Promoting 0.0005 Agent 1 Example 8 Heat-transfer 0.0120 0.0125 0.0126 0.0124 0.0123 0.0122 0.0123 ± Promoting 0.0003 Agent 2 Example 9 Heat-transfer 0.0086 0.0089 0.0086 0.0088 0.0087 0.0088 0.0087 ± Promoting 0.0002 Agent 3 Comparative Pure Water 0.0190 0.0330 0.0393 0.0439 0.0475 0.0487 0.0081 ± Example 7 0.011 Comparative G746 0.0382 0.0379 0.0376 0.0374 0.0372 0.0370 0.0376 ± Example 8 (Compound) 0.0006 Reference Air 0.297 0.2992 0.3000 0.2986 0.29991 0.2985 0.298 ± Example 1 0.011 Heat-transfer Promoting Agent 1: Pure Water 95 g + Liquid Kitchen Detergent 5 g Heat-transfer Promoting Agent 2: Water 96.69 g + Isostearyl Sulfonic Acid Sodium Ester 2.1 g + Sodium Lactate 1.2 g, Triazine Trithiol monosodium 0.001 g Heat-transfer Promoting Agent 3: Pure Water 99 g + Oleyl Sulfonic Acid Ester Triethanolamine 0.8 g + Sodium Phosphite 0.1 g + Resorcin 0.1 g Heat-transfer Promoting Agent: 10 mg/4.84 cm.sup.2 Al Plate (Surface Roughness; 0.02 μm, Thermal Conductivity; 240 W/mK), Measurement Pressur: 0.3 MPa
(93) There was the physical contact between metals obtained by contact pressure on the interface gap between the metallic blocks. The distance between thus physical contacts was within 0.5 nm or less, and the heat thereof conducted by phonon oscillation. In the air space (Reference Example 1), the energy was exchanged by not only physical oscillation but also collision of molecules of oxygen and nitrogen to the interface wall of the metallic blocks. Although the pure water (Comparative Example 7) was an efficient substance (hydrogen bond molecules as water molecules) which received the energy from the wall having higher temperature (the wall of Al alloy block: the upper-side heat-collection metallic block 4c) and released (radiated) the energy to the wall having lower temperature (the wall of Al alloy block: the down-side heat-collection metallic block 6a) in the gap of contact interface of the metallic blocks, the value of contact thermal resistance between the metallic blocks increased with time because the water vaporized with time. Although the heat conductivity of the commercially available radiation material (Comparative Example 8) was higher at initial than that of water because the material comprised silicone oil and inorganic radiation materials (Al.sub.2O.sub.3 particles, 1 μm or less), change with time was small.
(94) The values of thermal resistance in the gap between the metallic blocks in the embodiments using the heat-transfer promoting agent of Examples 7-9 were kept as small and constant values for 60 min. compared to above-mentioned Comparative Examples 7-8 and Reference Example 1. It is expected that the vaporization of water and the transform between single molecule and cluster from water cluster with hydrogen bond are smoothly occurred, and then the energy transfers in the gap between the metallic blocks by minor addition of the surface active agent and the builder.
Examples 10-12, Comparative Example 9, and Reference Example 2
Embodiments for Indicating Relationship Between the Heat-Transfer Promoting Agent and Contact Pressure
(95) It was important whether the values of thermal resistance of the heat-transfer promoting agent were influenced or not by contact pressure which was loaded to the metallic blocks when the heat-transfer promoting agent was filled into the gap between the measurement sample unit 5 and the down-side heat-collection metallic block 6a (Al alloy, thermal conductivity: 139 W/mk, Ra: 0.025 μm) arranged thereunder in the measurement device 1 for estimating thermal characteristics, because the pressure onto the object to be measured predominated over the value of contact thermal resistance. The results under the contact pressure of 0.01-0.30 MPa are shown in Table 6.
(96) TABLE-US-00006 TABLE 6 Relationship between heat-transfer promoting agent in contact gap of Al/Al and contact pressure Contact Value of Contact Thermal Resistance (10.sup.−3m.sup.2K/W) Pressure Average Examples (MPa) 0.01 0.05 0.10 0.15 0.20 0.25 0.30 Value Example 10 Heat-transfer 0.0150 0.0150 0.0150 0.0144 0.0146 0.0143 0.0140 0.0145 ± Promoting 0.0002 Agent 1 Example 11 Heat-transfer 0.0126 0.0125 0.0124 0.0123 0.0123 0.0122 0.0121 0.0123 ± Promoting 0.0003 Agent 2 Example 12 Heat-transfer 0.0078 0.0077 0.0076 0.0076 0.0077 0.0078 0.0078 0.0077 ± Promoting 0.0001 Agent 3 Comparative G746 0.0481 0.0399 0.0372 0.0352 0.0329 0.0299 0.0282 0.0390 ± Example 9 (Compound) 0.0199 Reference Air 0.1977 0.1787 0.1660 0.1589 0.10505 0.1440 0.1380 0.1678 ± Example 2 0.0298 Heat-transfer Promoting Agent 1: Pure Water 95 g + Liquid Kitchen Detergent 5 g Heat-transfer Promoting Agent 2: Water 96.69 g + Isostearyl Sulfonic Acid Ammonium 2.1 g + Sodium Lactate 1.2 g, Triazine Trithiol monosodium 0.001 g Heat-transfer Promoting Agent 3: Pure Water 99.0 g + Oleyl Sulfonic Acid Ester Triethanolamine 0.8 g + Sodium Phosphite 0.1 g + Resorcin 0.1 g Heat-transfer Promoting Agent: 10 mg/4.84 cm.sup.2 Al Plate (Surface Roughness; 0.02 μm, Thermal Conductivity; 240 W/mK), Measurement Pressur: 0.3 MPa
(97) Although the value of contact thermal resistances in Comparative Example 9 and Reference Example 2 were affected by the contact pressure, those of Examples 10, 11 and 12 were hardly affected thereby. A pressure ratio of Comparative Example 9 was 0.3 MPa/0.01 MPa=0.58 and a pressure ratio of Reference Example 2 was 0.7, while pressure ratios of Examples 10-12 are 93-97. Therefore, the heat-transfer promoting agents of Examples were considerably excellent rather than the commercial items.
Examples 13-15, Comparative Example 10, and Reference Example 3
Embodiments for Indicating Relationship Between Surface Roughness and Contact Pressure
(98) It was important whether the values of thermal resistance of the heat-transfer promoting agent were influenced or not by the surface roughness of the metallic blocks when the heat-transfer promoting agent was filled into the gap between the measurement sample unit 5 and the down-side heat-collection metallic block 6a (Al alloy, thermal conductivity: 139 W/mk, Ra: 0.025 μm) arranged thereunder in the measurement device 1 for estimating thermal characteristics. The results under the surface roughness from 0.020±0.01 to 0.30±0.02 are shown in Table 7.
(99) TABLE-US-00007 TABLE 7 Relationship between mediums in contact gap of Al/Al and surface roughness Surface Roughness Value of Contact Thermal Resistance (10.sup.−3m.sup.2K/W) Examples (μm) 0.020 ± 0.01 0.020 ± 0.01 0.05 ± 0.01 0.10 ± 0.01 0.30 ± 0.02 Example 13 Heat-transfer 0.0146 0.0143 0.0146 0.0150 0.0151 Promoting Agent 1 Example 14 Heat-transfer 0.0123 0.0123 0.0124 0.0123 0.0123 Promoting Agent 2 Example 15 Heat-transfer 0.0066 0.0066 0.0067 0.0068 0.0068 Promoting Agent 3 Comparative G746 0.0372 0.0386 0.0401 0.0523 0.0882 Example 10 (Compound) Reference Air 0.1980 0.2010 0.5205 0.8120 1.2800 Example 3 Heat-transfer Promoting Agent 1: Pure Water 95 g + Liquid Kitchen Detergent 5 g Heat-transfer Promoting Agent 2: Ion-exchanged Water 97.5 g + Decyl Triethylene Glycol 2.0 g, EDTA 0.2 g + Triazine Trithiol monosodium 0.3 g Heat-transfer Promoting Agent 3: Pure Water 98.2 g, Diphenyl Dioctyl Phoshoroyl Bromide 1.5 g, Triethanolamine 0.3 g, Sodium Hyposulfite 0.2 g Contact Pressure: 0.2 MPa
(100) Although the roughness influence against the value of thermal resistance of Comparative Example 10 was 1.37 times and that of Reference Example 3 was 5.46 times, those of Examples 13, 14 and 15 were 0.1 or less in any cases. Therefore, it was obvious that the roughness influence is small, because of the characteristic of the surface active agent. Thus results mean new academic achievement as regards heat conduction on the interfaces.
Examples 16-17, Comparative Example 11
Embodiments for Indicating Influence of Physical Contact and Chemical Contact on Interface of Crosslinking Silicone Rubber of Three-Layer Structure
(101) Contact interfaces of the three-layer structure comprising 2 pieces of Al plate and crosslinking silicone rubber was investigated. And the results thereof are shown in
(102) As shown in
Examples 18-19, Comparative Example 12
Embodiments for Indicating Relationship of Medium on Contact Gap and Contact Pressure
(103) Various objects to be measured were investigated, and the results thereof are shown in Table 8. In the measurement for estimating thermal characteristics (Example 18) by using a heat-conductive complexed silicone rubber sheet (from the composition: 100 phr of SH851 silicone rubber which is available from Dow Corning Toray Co. Ltd., 200 phr of Al.sub.2O.sub.3-AS30 (30 μm) which is available from Showa Denko K.K., and 0.6 phr of RC-4; and under the condition: at 160° C., for 30 min., at 3 MPa) having 0.175 mm, the values of thermal resistance were 0.215-0.216*10.sup.−3 m.sup.2 K/W and almost constant as regards relationship of the total values of thermal resistance and contact pressure onto the object to be measured. Therefore, it is obvious that the total values of thermal resistance indicate the independent property on the contact interface pressure by using the heat-transfer promoting agent. And the total values of thermal resistance when using a heat-conductive complexed silicone rubber sheet with adhered PI (Example 19; 0.2 mm), which was prepared by molecular bonding of the above-mentioned heat-conductive complexed silicone rubber sheet onto polyimide (PI, 25 μm, Kapton 250EN), were marginally decreased within 0.341*10.sup.−3 m.sup.2 K/W to 0.333*10.sup.−3 m.sup.2 K/W under 0.01-0.60 MPa of interface pressure and were affected by the contact interface pressure. However, the rate of change (2.4%) was very small. While the values of Comparative Example 12 without using the heat-transfer promoting agent were decreased within 0.421*10.sup.−3 m.sup.2 K/W to 0.360*10.sup.−3 m.sup.2 K/W, whose rate of change was 14.5%, and the values were strongly affected by the contact interface pressure. The results indicate that the heat-transfer promoting agent significantly promotes the contact heat-transfer between the Al plate of the three-layer structure and the object to be measured.
(104) TABLE-US-00008 TABLE 8 Relationship between mediums in contact gap of Al/Al and contact interface pressure Total Value of Thermal Resistance (10.sup.−3m.sup.2K/W) Object Heat-transfer Contact Interface Pressure on Object to be Measured (MPa) to be Promoting Agent 0.01 0.05 0.1 0.2 0.3 0.4 0.5 0.6 Examples Measured 10 mg/4.84 cm.sup.2 MPa MPa MPa MPa MPa MPa MPa MPa Example 18 0.8 W With 0.216 0.216 0.215 0.215 0.215 0.215 0.215 0.215 Silicone Complexed Substrate Example 19 PI/Silicone With 0.341 0.340 0.338 0.336 0.335 0.334 0.333 0.333 Rubber Complexed Substrate Comparative PI/Silicone Without 0.421 0.405 0.392 0.381 0.378 0.373 0.367 0.360 Example 12 Rubber Complexed Substrate Heat-transfer Promoting Agent: Ion-exchanged Water 97.5 g + Decyl Triethylene Glycol 2.0 g, EDTA 0.2 g + Triazine Trithiol monosodium 0.3 g
Examples 20-22, Comparative Examples 13-15
Embodiments for Indicating Relationship of Number of Stacked Pieces of Sheets of the Object to be Measured with or without Using Heat-Transfer Promoting Agent and Contact Interface Pressure
(105) When performing the measurements for estimating thermal characteristics (Examples 18, 19 and 20) by using heat-conductive complexed silicone rubber sheets (from the composition: 100 phr of SH851 silicone rubber which is available from Dow Corning Toray Co. Ltd., 600 phr of Al.sub.2O.sub.3-AS30 (30 μm) which is available from Showa Denko K.K., and 0.6 phr of PC-4; and under the condition: at 160° C., for 30 min., at 3 MPa) having 0.180 to 0.225 mm, the heat-transfer promoting agent of 10 mg/4.84 cm.sup.3 was applied (Examples 20-22) onto 2 portions of the contact interface between the Al plate and the complexed sheet and onto 1 portion or 2 portions of the contact interface between the complexed sheets and the heat-transfer promoting agent was not applied (Comparative Examples 13-15). And 1-3 pieces of the complexed sheet were stacked, and then the relationship between the total value of thermal resistance and the object to be measured was measured. The results thereof are shown in Table 9.
(106) TABLE-US-00009 TABLE 9 Influence for value of thermal resistance of object to be measured according to number of stacked sheets of object to be measured with or without using heat-transfer promoting agent and contact interface pressure Number of Heat-transfer Stacked Sheet Total Value of Thermal Resistance (10.sup.−3m.sup.2K/W) Promoting Thickness Contact Interface Pressure (MPa) Examples Agent of Sheet 0.01 0.05 0.1 0.2 0.3 0.4 0.5 0.6 Example 20 With Agent of 1 Piece 0.138 0.090 0.086 0.086 0.086 0.086 0.086 0.086 10 mg/4.84 cm.sup.2 Comparative Without 0.200 mm 0.550 0.160 0.110 0.092 0.091 0.090 0.090 0.090 Example 13 Agent Example 21 With Agent of 2 Pieces 0.206 0.176 0.174 0.174 0.174 0.174 0.174 0.174 10 mg/4.84 cm.sup.2 Comparative Without 0.200 mm 0.750 0.280 0.220 0.197 0.191 0.188 0.185 0.182 Example 14 Agent Example 22 With Agent of 3 Pieces 0.315 0.258 0.255 0.255 0.255 0.255 0.255 0.255 10 mg/4.84 cm.sup.2 Comparative Without 0.200 mm 0.830 0.370 0.325 0.276 0.271 0.268 0.265 0.263 Example 15 Agent Heat-transfer Promoting Agent: Ion-exchanged Water 97.5 g + Decyl Triethylene Glycol 2.0 g, EDTA 0.2 g + Triazine Trithiol monosodium 0.3 g Heat-transfer Promoting Agent 3: Pure Water 98.2 g, Diphenyl Dioctyl Phoshoroyl Bromide 1.5 g, Triethanolamine 0.3 g, Sodium Hyposulfite 0.02 g Range of Thickness of Sheet: 0.220-0.240 mm Value of Thermal Resistance corrected as thickness of sheet of 0.200 mm
(107) It was obvious that the application of the heat-transfer promoting agent achieves the effects of obtaining the constant total value of thermal resistance at the extremely low contact interface pressure (ca. 0.05 MPa) or more, of attaining the independent property on the contact interface pressure, and of obtaining the accurate values of measurement for the value of thermal resistance as well as under the usage state thereof. On the other hand, it was obvious that the case (Comparative Examples) without using the heat-transfer promoting agent causes the adverse effects of decreasing the total values of thermal resistance with increasing the contact interface pressure, of obtaining the significantly different value from the actually-used contact interface pressure, of attaining the dependent property on the contact interface. Therefore the measured values of thermal resistance of the complexed materials were not exerted unless the interface pressure for the measurement is loaded. When they are used for small parts such as an inverter and LED, the increase of the contact interface pressure causes the difficult usage of larger and heavier components.
Examples 20-22, Comparative Examples 13-15
Embodiments for Indicating Relationship of Thickness and the Total Value of Thermal Resistance of the Object to be Measured
(108) A laser reflecting type short range sensor head GT2-S1 as a pencil type, which is available from Keyence Corporation and is a trade name, was used for the length measuring device 8 attached into the measurement device 1 for estimating thermal characteristics. The length measuring device 8 was a displacement gauge with high-sensitivity within 1 μm±0.1 μm or more. The length measuring device 8 was mounted onto the heat conducting material 5a as the upper-side supporting plate, and can measure the displacement distance from the heat conducting material 5c as the down-side supporting plate by the mechanism thereof. After the interface pressure (0.2 MPa) was loaded, the displacement distance was changed. In this time, the thickness of the object 5b to be measured for estimating thermal characteristics as the sample changed with the loaded interface pressure. The value of thermal resistance was simultaneously expressed as the value according to the thickness with change of the present interface pressure. In Examples 20-22 and Comparative Examples 13-15, for example, the objects 5b to be measured for estimating thermal characteristics having thickness of 0.2004 mm, 0.4040 mm and 0.6015 mm, which were measured as previously mentioned, were used. The heat conducting material 5a, the object 5b to be measured for estimating thermal characteristics, and the heat conducting material 5c in the measurement device 1 for estimating thermal characteristics were sandwiched and kept between the upper-side heat-collection metallic block 4c and the down-side heat-collection metallic block 6a, and then the values of thermal resistance were obtained by three-point plotting according to the total value of thermal resistance and the thickness of the samples.
(109) In Comparative Examples 13-15, the thickness of the sample to be measured was not corrected. And the value of contact thermal resistance on the contact interface which was calculated by using the same thickness of the sample to be measured even if the interface pressure was varied, the value of thermal resistance of the sample to be measured, and the thermal conductivity were obtained. In Examples 20-22, the thickness of the object 5b to be measured for estimating thermal characteristics as the sample after loading the interface pressure was measured by the length measuring device 8, and then the value of contact thermal resistance on the contact interface, the value of thermal resistance of the sample to be measured, and the thermal conductivity were obtained. The results are shown in Table 10 and
(110) TABLE-US-00010 TABLE 10 Influence for relationship of total value of thermal resistance and thickness of object to be measured, according to value of thermal resistance of object to be measured, value of contact thermal resistance on contact interface, and thermal conductivity with or without using length measuring device Value of Value of Contact Thermal Thermal Before/After Thickness of Total Value Resistance of Resistance Using Length Object to be of Thermal Object to be on Contact Thermal Measuring Measured Resistance Measured Interface Conductivity Device (mm) (10.sup.−3m.sup.2K/W) (10.sup.−3m.sup.2K/W) (10.sup.−3m.sup.2K/W) (W/mK) Example 20 After 0.1882 0.04820 0.04297 0.00523 4.38 Measurement Comparative Before 0.2004 0.04582 −0.0150 4.36 Example 13 Measurement Example 21 After 0.3836 0.90101 0.08584 0.00523 4.49 Measurement Comparative Before 0.4040 0.11210 −0.0150 3.60 Example 14 Measurement Example 22 After 0.57761 0.13404 0.12881 0.00523 4.48 Measurement Comparative Before 0.6015 0.17519 −0.0150 3.43 Example 15 Measurement
(111) As shown in Table 10 and
INDUSTRIAL APPLICABILITY
(112) The measurement device for estimating thermal characteristics and the measurement method for estimating thermal characteristics using the same of the present invention can apply the thermal measurement and analysis technology of the parts for usage of the various electric or electronic products such as the light emitting elements, the photoelectric conversion elements, the thermoelectric conversion elements, the wind turbine generation elements, the printed circuit boards, the semiconductor chips, a wide variety of the electric control elements or parts of the motors or the engines of the automobiles etc. The measured materials thereby can be used to be installed into the products.
EXPLANATIONS OF LETTERS OR NUMERALS
(113) Numerals mean as follows. 1: measurement device for estimating thermal characteristics, 2: transparent plastic case having window for taking in and out, 3: load unit, 3a: load screw rod, 3b: SUS screw-cut plate, 3c: SUS load plate, 3d: load cell, 3e: heat insulation plate, 3f.sub.1, 3f.sub.2: distortion gauge, 3g: guide, 3h.sub.1, 3h.sub.2: wirings for distortion gauge measurement, 4: heat generating source unit, 4a: heat insulation plate, 4b: heat generating source, 4c: upper-side heat-collection metallic block, 4d.sub.1, 4d.sub.2: insulating resin, 4e: electrothermal heater, 4f: wire, 4g.sub.1, 4g.sub.2: thermocouples, 4h.sub.1, 4h.sub.2: wire for a high-precision temperature-voltage measuring unit, 5, 5.sub.1, 5.sub.2, 5.sub.3: a measurement sample unit, 5a.sub.1: layer of heat-transfer promoting agent, 5a: heat conducting material, 5ab: contact interface of heat conducting material/object to be measured, 5b, 5b.sub.1: object to be measured for estimating thermal characteristics, 5b.sub.2: silicone liquid rubber, 5bc: contact interface of object to be measured/heat conducting material, 5c: heat conducting material, 5c.sub.1: layer of heat-transfer promoting agent, 6: heat cooling source unit, 6a: down-side heat-collection metallic block, 6b: thermal exchange cooling device, 6c.sub.1, 6c.sub.2: thermocouple, 6d.sub.1, 6d.sub.2: wire for high-precision temperature-voltage measuring unit, 6e.sub.1: inflow hole of cooling water, 6e.sub.2: outflow hole of cooling water, 7: a support unit, 7a: heat insulation material, 7b: stillage, 7c.sub.1, 7c.sub.2: pedestal having a cone shape, 8: length measuring device, 8a.sub.1, 8a.sub.2: gauge head of length measuring device, 8b.sub.1, 8b.sub.2: wire for length measuring unit, 9: data acquisition and control system, 9a: distortion measuring unit, 9b: high-precision temperature-voltage measuring unit, 9c: a stabilized power supply of direct current electricity, 9d: electric shunt, 9e: measurement and calculation unit for estimating thermal characteristics, 9f: external output interface unit, 9g: length measurement unit, 10: cooling-water circulating system, 10a: tank of stored cooling water for circulation, 10b: cooling-water circulating equipment, 11: data-indicating system, 11a: memory, 11b: display, 20: jig for building, 21a, 21b: right and left outer frame, 22: bolt, 23: upper-side spacer, 24: nut, 25: down-side spacer, T.sub.1: surface temperature of upper-side heat-collection metallic block, T.sub.7: surface temperature of down-side heat-collection metallic block