CN107163547A - A kind of solid-solid phase change thermal interfacial material and preparation method thereof - Google Patents
A kind of solid-solid phase change thermal interfacial material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/664—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6674—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
- C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K7/00—Constructional details common to different types of electric apparatus
- H05K7/20—Modifications to facilitate cooling, ventilating, or heating
- H05K7/2039—Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
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Abstract
The invention discloses a kind of solid-solid phase change thermal interfacial material and preparation method thereof.The phase-change thermal interface material includes at least one block polymers of polyurethane as matrix material, and is dispersed at least one of matrix material heat conductive filler；The block polymers of polyurethane includes soft segment strand and hard section strand, and after temperature exceedes phase transition temperature, soft segment strand is changed into amorphous state from crystalline state, and the thermal interfacial material occurs from a kind of solid-state phase to the transformation of another solid-state phase.The phase-change thermal interface material of the present invention no liquid and gas in phase transition process are produced, have the advantages that pliability is good, effect of impregnation is strong, heat transference efficiency is high, storing heat is big, suitable phase transition temperature, convenient formation, Volume Changes are small, performance is stable and service life is long, for the heat transference efficiency of device can be improved in heater members, the normal work of heater members is ensured, extends device lifetime.
Description
Technical field
The present invention relates to phase-change thermal interface material, more particularly to a kind of solid-solid phase-change thermal interfacial material and preparation method thereof.
Background technology
Information technology, the development of microelectric technique make electronic device show miniaturization, high-performance, high integration and many
The development trend of function, device size develops from micron order to nanoscale, and power is sent out from the small scale integration of hundreds of milliwatts
The large scale integrated circuit of hectowatt is opened up, causes the caloric value on unit volume/area to steeply rise.With stacking number
Lifting, the raising of device integration, space is become extremely difficult by huge limitation, heat transfer, and issue of ASIC thermal failure is more protruded.
Thermal interfacial material is that one kind can bond two interfaces, the high heat conduction material with good heat conductive ability and wetability
Material, it is most important during solving issue of ASIC thermal failure, accelerating heat transfer.Due between heater members surface and radiator
There is imperceptible rough space, when two Studies On Contacts of Rough Surfaces, actual contact area is less than 1%, and remaining is equal
For air void.The thermal conductivity of air is very low, causes the thermal contact resistance between heater members and radiator very big, heat without
Method is rapidly delivered to radiator from heater members, and the refrigerating function of radiator can not be played completely, and heater members are due to warm
Amount accumulation, temperature are too high, and hydraulic performance decline, service life will be caused to shorten, failure is even damaged.Use the hot interface of high thermal conductivity
Hole between material filling interface, excludes air therein, sets up fast and effectively hot between electronic component and radiator
Conduction pathway, can be greatly lowered thermal contact resistance, the effect of radiator is fully played, and ensure heater members just
Often work.
Being currently being widely used thermal interfacial material mainly has heat-conducting silicone grease, phase-change material etc..Heat-conducting silicone grease is a kind of paste
Thermal interfacial material, only need to apply last layer, it is not necessary to solidify when using in interface, but use after certain time, due to silicone grease
Occur to degenerate, suction out or parch and solvent the reason such as volatilization aging, heat conductivility will decline to a great extent.Phase-change material is a kind of
Heat transfer efficiency very high hot interface, usually solid-state, heat absorption is melt into liquid during more than certain temperature, prevents from continuing to heat up, and
Fully wetting heat transfer interface, reaches the effect of augmentation of heat transfer.But traditional phase-change thermal interface is located under chip operating temperature
In liquid phase, due to the mobility of liquid, cause the stability of faying face to decline, easily occur flowing spillover.
The content of the invention
It is an object of the invention to provide a kind of solid-solid phase-change thermal interfacial material, in heater members, to improve device
Heat transference efficiency, ensures the normal work of heater members, extends device lifetime.
The phase-change thermal interface material that the present invention is provided includes：At least one block polymers of polyurethane as matrix material,
Be dispersed at least one of matrix material heat conductive filler；The block polymers of polyurethane includes soft segment strand and hard
Segment molecule chain, after temperature exceedes phase transition temperature, soft segment strand is changed into amorphous state from crystalline state, and the thermal interfacial material occurs
From a kind of solid-state phase to the transformation of another solid-state phase.
In the solid-solid phase-change thermal interfacial material of the present invention, the block polymers of polyurethane accounts for the hot boundary by weight
The 5%-99.99% of facestock material；The heat conductive filler accounts for the 0.01%-95% of the thermal interfacial material by weight.
The solid-solid phase-change temperature range of thermal interfacial material of the present invention is big, is 30-120 DEG C, between soft segment melt temperature and firmly
Between section melt temperature, hard section ratio is higher, and phase transition temperature is higher.Less than soft segment melt temperature, the thermal interfacial material is solid-state；
After hard section melt temperature, the thermal interfacial material is liquid.
Phase transformation is adjusted by the control of the species of soft segment in block polymers of polyurethane and hard section, molecular weight and its ratio
Temperature：Soft segment part is made up of submissive regular strand, is easier to crystallize in temperature change and is melted, phase transition temperature is relatively low；
Hard section is made up of the stronger strand of polarity, hydrogen bond is easily formed between the moieties group, cohesive energy is larger, crystallization temperature compared with
Height, is difficult to melt, phase transition temperature is higher in temperature change；After the phase transition temperature for reaching soft segment, soft segment changes from crystalline solid state
For amorphous state, locally there is mobility, surface wettability obtains essential lifting, thermal conductivity can be greatly enhanced and connect
Contacting surface is accumulated, and now hard section remains as crystalline state, limits the flowing of soft segment, material is occurred without macroscopical flowing, keeps on the whole
Solid forms, so as to realize the solid-solid phase-change at hot interface.
It is preferred that, the soft segment of the block polymers of polyurethane is poly-dihydric alcohol and/or polyvalent alcohol strand, described hard
The strand that section obtains for isocyanates and chain extender reaction.According to soft and hard segments ratio demand, it polymerize isocyanates used and poly-
The molar ratio of two (many) first alcohol is 5:95 to 95:Within the scope of 5.Wherein described chain extender is alcohols chain extender, for example Isosorbide-5-Nitrae one
Butanediol, neopentyl glycol, 1,6-HD, glycerine, trimethylolpropane, diethylene glycol (DEG), triethylene glycol etc..
The heat conductive filler is the material of the forms such as the particle, fiber, thin slice of high heat conductance, preferably thermal conductivity be more than etc.
Can be ceramics, such as zinc oxide, aluminum oxide, boron nitride, aluminium nitride, magnesia ceramic material in 10W/ (mK) material；
Can also be metal, such as aluminium, copper, silver；Can also be carbon materials, such as graphene, CNT, carbon black, graphite flakes, carbon
Fiber etc.；And their compositions.
Present invention also offers the preparation method of the solid-solid phase-change thermal interfacial material, referring to Fig. 1, comprise the following steps：
1) by the poly-dihydric alcohol and/or polyvalent alcohol organic solvent diluting of one or more molecular weight 100~100000,
Obtain mixed solution；
2) in step 1) binary isocyanates and/or multicomponent isocyanate are added in obtained mixed solution, reaction is formed
Performed polymer；
3) alcohols chain extender is added in performed polymer, chain extending reaction is carried out；
4) one or more heat conductive fillers are added in the reactant solution that chain extending reaction is completed, and add corresponding phase
Hold agent, make solution dispersed；
5) by step 4) heating of obtained solution carries out polymerization curing reaction, while being dried in vacuo, until becoming completely
For solid-state, block polymers of polyurethane based composites are obtained；
6) by step 5) obtained block polymers of polyurethane based composites heating and melting, hot pressing film forming obtains solid-solid
Phase-change thermal interface material.
Above-mentioned steps 1) in, poly- two (many) first alcohol used are for example：Polyethylene glycol, polytetramethylene glycol, polypropylene glycol, polyethylene
Alcohol, PTMG, polyester-diol etc..It is preferred that first that (many) the first alcohol of one or more poly- two are dry in 60-120 DEG C of vacuum
It is blended after dry, is then added in organic solvent and dilutes, mechanical agitation is uniform, until poly- two (many) first alcohol are completely dissolved, is mixed
Close solution.The organic solvent is preferably dimethylformamide, acetone, tetrahydrofuran etc., and its consumption by mass is poly- two
10~20 times of (many) member alcohol.
Above-mentioned steps 2) in, used two (many) first isocyanates are for example：Methyl diphenylene diisocyanate, toluene diisocyanate
Acid esters, dimethyl diphenyl diisocyanate, hexamethylene diisocyanate, isoflurane chalcone diisocyanate, phenylene diisocyanate,
Naphthalene diisocyanate etc..Added in mixed solution after two (many) first isocyanates, the sustained response preferably at a temperature of 50-100 DEG C
1-2 hours, form performed polymer.Isocyanates provides hard section strand, poly- two with chain extender reaction for block polymers of polyurethane
(many) member alcohol provide soft segment strand for block polymers of polyurethane, according to soft and hard segments ratio demand, isocyanates and poly- two
The molar ratio of (many) member alcohol is 5:95 to 95:Within the scope of 5.
Above-mentioned steps 3) in, the alcohols chain extender is for example：1,4 1 butanediols, neopentyl glycol, 1,6-HD, glycerine,
Trimethylolpropane, diethylene glycol (DEG), triethylene glycol etc..It is preferably heated to 50-120 DEG C and carries out chain extending reaction 1-2 hours.Alcohols chain extender
Addition by di-n-butylamine titrate isocyano method calculate obtain.
Above-mentioned steps 4) in, the heat conductive filler can be particle, fiber, thin slice of one or more high heat conductance etc.
The filler of shape.According to the species of isocyanates, poly- two (many) first alcohol and heat conductive filler, corresponding thereto compatible is added
Agent, carrying out mechanical agitation, sonic oscillation makes solution dispersed.
Above-mentioned steps 5) polymerization curing reaction is carried out preferably at a temperature of 50-100 DEG C.
Above-mentioned steps 6) 0.001~1mm film can be turned into hot pressing, cut into the size matched with heater members
Using.
The solid-solid thermal interfacial material of the present invention when installing first, as shown in Fig. 2 being first to heat to higher than solid-solid phase alternating temperature
0-50 DEG C of degree, after after its softening, is pasted onto between heater members and radiator, and gradually pressure is applied to opposite side along side,
It is expelled from air；Stop after heating, using natural cooling, eliminate the residual stress of thermal interfacial material, enhancing thermal interfacial material with
The combination interface of heater members and radiator；After phase transition temperature, soft segment is recrystallized, and thermal interfacial material turns into shape invariance
Solid, and keep combining closely with heater members and radiator.
The solid-solid phase-change thermal interfacial material that the present invention is provided is using block polymers of polyurethane as matrix, with high heat conductance
The material of the forms such as grain, fiber, thin slice is filler, after heater members operating temperature exceedes phase transition temperature, and hot interface occurs
From a kind of solid-state phase to the transformation of another solid-state phase, heat transference efficiency it is original it is higher on the basis of occur it is essential significantly
Lifting, with the outstanding advantage that contact area is big, heat transfer efficiency is high, phase transition temperature modification scope is big.The solid-solid phase heating interface
Material is due to the addition of high heat conductance filler, and itself has higher thermal conductivity；After solid-solid phase-change temperature, soft segment from
Crystalline state is changed into amorphous state, and mobility strengthens, and thermal conductivity is further enhanced, and effectively can adhere to and infiltrate several
On the surface of any shape and roughness, micro-pore is filled up, air is supplanted, contact area is greatly enhanced, reduces boundary
The temperature difference between face；There is higher enthalpy of phase change simultaneously, heat is absorbed when helping to undergo phase transition.
To sum up, no liquid and gas are produced in solid-solid phase-change thermal interfacial material of the invention, phase transition process, with flexible
Good, effect of impregnation is strong, heat transference efficiency is high, storing heat is big for property, suitable phase transition temperature, convenient formation, Volume Changes are small, performance
The advantages of stable and service life is long.
Brief description of the drawings
The preparation method flow chart of Fig. 1 solid-solid phase-change thermal interfacial materials of the present invention.
Fig. 2 are installed and operation principle schematic diagram at solid-solid phase heating interface of the present invention first.
Embodiment
Below in conjunction with the accompanying drawings, the present invention, the model of but do not limit the invention in any way are expanded on further by embodiment
Enclose.
Referring to Fig. 1, solid-solid phase-change thermal interfacial material is prepared by following step：
1st, the poly-dihydric alcohol of molecular weight 6000 is dried in vacuo 3 hours at 110 DEG C, is weighed 7.68g, is added to the two of 100mL
Diluted in NMF solvent, mechanical agitation is uniform, until poly-dihydric alcohol is completely dissolved, obtains mixed solution.
2nd, 1.79g methyl diphenylene diisocyanates are slowly added in mixed solution, the sustained response 2 at a temperature of 60 DEG C
Hour, form performed polymer.
3rd, 0.53g BDO chain extender is added in performed polymer, 70 DEG C is heated to and carries out chain extending reaction 2 hours.
The method that the addition of chain extender titrates isocyano by di-n-butylamine, which is calculated, to be obtained.
4th, in the reactant solution that chain extending reaction is completed, 0.5g graphenes are added, silane coupler is added and it is carried out
Surface is modified, and mechanical agitation, sonic oscillation make solution dispersed afterwards.
5th, solution heating carries out heating polymerization curing reaction at a temperature of 80 DEG C, while being dried in vacuo, until complete
It is changed into solid-state, obtains the enhanced block polymers of polyurethane base composite wood of high heat conductance filler that can occur solid-solid phase-change
Material：Content of soft segmer is 81%, 75-85 DEG C of solid-solid phase-change temperature, and thermal conductivity is more than 1W/ (mK).
6th, by composite heating and melting, the film that thickness is 0.1mm thickness is hot pressed into, cuts into and is matched with heater members
Size, obtain solid-solid phase-change thermal interfacial material.
7th, thermal interfacial material is first to heat to 90 DEG C when installing first, after after its softening, is pasted onto heater members and radiating
Between device, gradually apply pressure to opposite side along side, be expelled from air.Stop after heating, using natural cooling, eliminate heat
The residual stress of boundary material, enhancing thermal interfacial material and heater members and the combination interface of radiator.After phase transition temperature,
Soft segment is recrystallized, thermal interfacial material turns into the solid of shape invariance, and keeps combining closely with heater members and radiator.
Claims (10)
1. it is solid-solid phase-change thermal interfacial material a kind of phase-change thermal interface material, including at least one block polymers of polyurethane is made
For matrix material, and it is dispersed at least one of matrix material heat conductive filler；The block polymers of polyurethane includes
Soft segment strand and hard section strand, after temperature exceedes phase transition temperature, soft segment strand is changed into amorphous state from crystalline state, should
Thermal interfacial material occurs from a kind of solid-state phase to the transformation of another solid-state phase.
2. phase-change thermal interface material as claimed in claim 1, it is characterised in that in the phase-change thermal interface material, by weight
Gauge, the block polymers of polyurethane accounts for 5%-99.99%, and the heat conductive filler accounts for 0.01%-95%.
3. phase-change thermal interface material as claimed in claim 1, it is characterised in that its solid-solid phase-change temperature is 30-120 DEG C.
4. phase-change thermal interface material as claimed in claim 1, it is characterised in that the soft segment of the block polymers of polyurethane point
Subchain is poly-dihydric alcohol and/or polyvalent alcohol strand, and the hard section strand is what isocyanates was obtained with chain extender reaction
Strand.
5. the preparation method of any phase-change thermal interface material of Claims 1 to 4, comprises the following steps：
1) by the poly-dihydric alcohol and/or polyvalent alcohol organic solvent diluting of one or more molecular weight 100~100000, obtain
Mixed solution；
2) in step 1) binary isocyanates and/or multicomponent isocyanate are added in obtained mixed solution, reaction forms pre-polymerization
Body；
3) alcohols chain extender is added in performed polymer, chain extending reaction is carried out；
4) one or more heat conductive fillers are added in the reactant solution that chain extending reaction is completed, and are added corresponding compatible
Agent, makes solution dispersed；
5) by step 4) heating of obtained solution carries out polymerization curing reaction, while being dried in vacuo, until being changed into consolidating completely
State, obtains block polymers of polyurethane based composites；
6) by step 5) obtained block polymers of polyurethane based composites heating and melting, hot pressing film forming obtains solid-solid phase-change
Thermal interfacial material.
6. preparation method as claimed in claim 5, it is characterised in that step 1) described in poly-dihydric alcohol and/or polyvalent alcohol
One or more in following material：Polyethylene glycol, polytetramethylene glycol, polypropylene glycol, polyvinyl alcohol, PTMG two
Alcohol and polyester-diol.
7. preparation method as claimed in claim 5, it is characterised in that step 2) described in binary isocyanates and/or polynary
One or more of the isocyanates in following material：Methyl diphenylene diisocyanate, toluene di-isocyanate(TDI), dimethyl
Biphenyl diisocyanate, hexamethylene diisocyanate, isoflurane chalcone diisocyanate, phenylene diisocyanate and the isocyanic acid of naphthalene two
Ester.
8. preparation method as claimed in claim 5, it is characterised in that step 3) described in alcohols chain extender be selected from following chemical combination
One or more in thing：1,4 1 butanediols, neopentyl glycol, 1,6-HD, glycerine, trimethylolpropane, diethylene glycol (DEG) and three
Glycol.
9. preparation method as claimed in claim 5, it is characterised in that step 2) added by binary isocyanates and/or polynary different
Cyanate and step 1) used in poly-dihydric alcohol and/or polyvalent alcohol mol ratio 5:95 to 95:In the range of 5.
10. preparation method as claimed in claim 5, it is characterised in that step 4) described in heat conductive filler be a kind of or many
Plant the filler of the particle, fiber and/or chip shape of high heat conductance.
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| CN108383968A (en) * | 2018-02-08 | 2018-08-10 | 中国工程物理研究院化工材料研究所 | High heat conduction polyurethane solid-solid phase transition material and preparation method thereof |
| CN108424503A (en) * | 2018-04-08 | 2018-08-21 | 李维治 | A kind of high-effect composite polyurethane phase-change material and preparation method thereof |
| CN108624296A (en) * | 2018-07-11 | 2018-10-09 | 桂林电子科技大学 | A kind of composite solid-solid phase-change and preparation method thereof of boron nitride enhancing heat conduction |
| CN108751801A (en) * | 2018-06-26 | 2018-11-06 | 长安大学 | A kind of polyurethane/carbon black composite solid-solid phase-change modified asphalt mixture and preparation method thereof |
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| CN109762130A (en) * | 2019-01-21 | 2019-05-17 | 温州医科大学附属第二医院、温州医科大学附属育英儿童医院 | One kind can be recycled defervescence plaster used |
| CN109913181A (en) * | 2019-03-29 | 2019-06-21 | 上海亘多材料科技有限公司 | Encapsulate the polyurethane wall material microcapsules and preparation method thereof of phase-change material |
| CN110964174A (en) * | 2019-12-16 | 2020-04-07 | 长安大学 | Solid-solid phase change material for actively cooling asphalt pavement, preparation method and application |
| CN111479837A (en) * | 2017-10-25 | 2020-07-31 | 陶氏环球技术有限责任公司 | Flexible packaging material for preserving food freshness |
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