CN106188903A - Phase-change heat conductive material and preparation method thereof - Google Patents
Phase-change heat conductive material and preparation method thereof Download PDFInfo
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- CN106188903A CN106188903A CN201610748821.2A CN201610748821A CN106188903A CN 106188903 A CN106188903 A CN 106188903A CN 201610748821 A CN201610748821 A CN 201610748821A CN 106188903 A CN106188903 A CN 106188903A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C08L23/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
- C08L23/22—Copolymers of isobutene; Butyl rubber ; Homo- or copolymers of other iso-olefins
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
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- 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
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- C08L2205/00—Polymer mixtures characterised by other features
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- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The present invention relates to phase-change heat conductive material technical field, specifically, relate to a kind of phase-change heat conductive material and preparation method thereof, described phase-change heat conductive material is by polyolefin, paraffin, conduction powder and coupling agent composition, the low melt point paraffin wherein used, not only good with compatible polyolefin, preparation-obtained phase-change heat conductive material is also made to have relatively low phase transition temperature, excellent heat stability and weatherability, can be repeatedly used for a long, improve phase transition temperature in traditional phase-change heat conductive material higher, and the production cost caused owing to adding some ethylene propylene diene rubbers or viscosifier increases, the problem such as the feature of environmental protection and poor stability.Present invention also offers the preparation method of phase-change heat conductive material, after described preparation method is by first mixing the paraffin of low melting point, coupling agent with polyolefin, adds heat filling, finally prepare phase-change heat conductive material, this preparation method technique is simple, easy to operate.
Description
Technical field
The present invention relates to phase-change heat conductive material technical field, in particular to a kind of phase-change heat conductive material and preparation thereof
Method.
Background technology
Along with microelectronics and the development of large scale integrated circuit, circuit components high concentration, the heat dissipation problem of components and parts
Have become as one of vital key in design.If the heat conduction problem of electronic component solves bad, will directly affect
Normal to various electronic equipments uses and the life-span.In order to solve the heat dissipation problem of heat-generating electronic elements, under normal circumstances at electricity
The heating face of sub-element adjoins fin and dispels the heat.But, the surface of electronic component and fin can not be the most smooth, and two
The air gap is inevitably produced when person contacts.The existence of the air gap makes the efficiency of fin be substantially reduced, in order to solve
This problem and occur in that phase-change heat conductive material.
Phase-change heat conductive material refers to the thermoplastic that can carry out changing at a certain temperature between solid-state and liquid.Phase
Becoming Heat Conduction Material to be placed between electronic component and fin, it presents solid-state at normal temperatures, is absorbing the heat liter that thermal source distributes
Temperature becomes liquid after more than phase transition temperature, thus fills the air gap between electronic component and fin, moistening heat conduction circle
Face, it is achieved good interface heat conductivility；And become solid after being cooled to below phase transition temperature, thus it is existing to avoid spilling
As.The phase transition temperature of existing phase-change heat conductive material, generally more than 50 DEG C, requires higher occasion for some heat conduction, this
The phase transition temperature planting phase-change heat conductive material is clearly the highest, unsuitable for application.
In consideration of it, need a kind of phase transition temperature low, there is high efficient heat dissipation performance, can be applicable to the phase of high heat conduction requirement occasion
Become Heat Conduction Material.
Summary of the invention
For the problem of above-mentioned existence, an object of the present invention is to provide a kind of phase-change heat conductive material, described phase
Becoming Heat Conduction Material to be made up of polyolefin, paraffin, heat filling and coupling agent, the low melt point paraffin wherein used, not only with polyene
Hydrocarbon phase capacitive is good, also makes preparation-obtained phase-change heat conductive material have a relatively low phase transition temperature, and efficient heat dispersion is excellent
Good heat stability and weatherability, it is adaptable to heat conduction requires high occasion and can be repeatedly used for a long, and improves traditional phase transformation
In Heat Conduction Material, phase transition temperature is higher, and the production cost caused owing to adding some ethylene propylene diene rubbers or viscosifier
The problems such as increase, the feature of environmental protection and poor stability.
The two of the purpose of the present invention are to provide the preparation method of a kind of phase-change heat conductive material, described preparation method to pass through
After first the paraffin of low melting point, coupling agent being mixed with polyolefin, add heat filling, finally prepare phase-change heat conductive material.This
Preparation method technique is simple, and easy to operate, prepared phase-change heat conductive material phase transition temperature is low, has efficient thermal diffusivity
Can, it is adaptable to heat conduction requires high occasion and can be repeatedly used for a long.It addition, the temperature during being used by regulation and pressure
Power so that the thickness of this phase-change heat conductive material is the most thinning, thermal impedance meeting step-down, heat transfer performance is the most excellent.
In order to realize the above-mentioned purpose of the present invention, spy by the following technical solutions:
A kind of phase-change heat conductive material, in parts by weight, described phase-change heat conductive material is mainly made up of following components:
Described paraffin is low melt point paraffin, and described melting point of paraffin wax is 30-50 DEG C.
The typical but non-limiting parts by weight of described polyolefin are 100 parts, 105 parts, 110 parts, 115 parts, 120 parts, 125
Part, 130 parts, 135 parts, 140 parts, 145 parts or 150 parts.
Paraffin is as phase change heat storage material, and its fusing point is closely bound up with the phase transition temperature of phase-change heat conductive material.For ensureing phase
Become Heat Conduction Material can undergo phase transition at a lower temperature, abundant wetting interface surface, disperse heat timely, therefore select low melting point
Paraffin.Described melting point of paraffin wax is 30-50 DEG C, the typical but non-limiting fusing point of described paraffin can be 30 DEG C, 32 DEG C, 35
DEG C, 37 DEG C, 38 DEG C, 40 DEG C, 42 DEG C, 45 DEG C, 46 DEG C, 48 DEG C and 50 DEG C.
In the present invention, paraffin can be by multiple different model, the mixing of the paraffin of different melting points.
The typical but non-limiting parts by weight of described paraffin are 60 parts, 65 parts, 70 parts, 75 parts, 80 parts, 85 parts, 90 parts,
95 parts or 100 parts.
Phase-change heat conductive material mainly by fill heat filling improve heat conductivity, so heat filling loading number
Impact on heat conductivity is critically important.In the case of the loading smaller (less than 30%) of heat filling, do not have between filler
Effectively connect, it is impossible to playing bridging action to form thermal conducting path, heat-conducting effect is inconspicuous.So phase-change heat conductive material is to heat conduction
The loading of filler has certain requirement.
In the present invention, the typical but non-limiting parts by weight of described heat filling be 500 parts, 520 parts, 550 parts,
580 parts, 600 parts, 620 parts, 650 parts, 660 parts, 680 parts, 700 parts, 720 parts, 750 parts, 760 parts, 780 parts or 800 parts.
In order to improve heat filling dispersion in polyolefin, use coupling agent that heat filling is carried out surface process.?
In the present invention, preferably silane coupler, the kind of described silane coupler can be aminopropyl triethoxysilane (KH550),
3-glycydoxy trimethoxy silane (KH560), methacryloxypropyl trimethoxy silane
(KH570), mercaptopropyl trimethoxysilane (KH580), mercaptopropyltriethoxysilane (KH590), vinyl triethoxyl silicon
Alkane (A151), vinyltrimethoxy silane (A171), 3-glycydoxy methyldiethoxysilane (Si-
563), in ethylenediaminepropyltriethoxysilane (KH792) or ethylenediamine hydroxypropyl methyl dimethoxysilane (KBM602)
Plant or the combination of at least two.
The typical but non-limiting parts by weight of described coupling agent are 0.1 part, 0.2 part, 0.3 part, 0.4 part, 0.5 part, 0.6
Part, 0.8 part, 0.9 part or 1 part.
Of the present invention " mainly by ... composition ", it is intended that it is in addition to described component, it is also possible to include other components, this
Other components a little give the characteristic that described phase-change heat conductive material is different.Such as, described phase-change heat conductive material can also include thickening
Agent and antioxidant etc..In addition, of the present invention " mainly by ... composition ", it is also possible to replace with enclosed " being " or
" by ... composition ".
Preferably, a kind of phase-change heat conductive material, in parts by weight, described phase-change heat conductive material is by following components system
Become:
Described paraffin is low melt point paraffin, and described melting point of paraffin wax is 30-50 DEG C.
This phase-change heat conductive material is made up of polyolefin, paraffin, heat filling and coupling agent, the low melting point stone wherein used
Wax, not only good with compatible polyolefin, also make preparation-obtained phase-change heat conductive material have relatively low phase transition temperature, efficiently
Heat dispersion, excellent heat stability and weatherability, it is adaptable to heat conduction requires high occasion can being repeatedly used for a long, improvement
In traditional phase-change heat conductive material, phase transition temperature is higher, and leads owing to adding some ethylene propylene diene rubbers or viscosifier
The problems such as the production cost increase, the feature of environmental protection and the poor stability that cause.
Further, a kind of phase-change heat conductive material, in parts by weight, described phase-change heat conductive material is by following components system
Become:
Described paraffin is low melt point paraffin, and described melting point of paraffin wax is 30-45 DEG C.
By selecting further and adjusting each component ratio, select the paraffin that fusing point is lower, so that the present invention
The phase-change heat conductive material of gained has lower phase transition temperature, the most just can undergo phase transition so that heat conduction with phase change material
Expect to be become liquid, filling interface the air gap from solid-state, reduce interface resistance and resist, reach good radiating effect.
Further, the phase transition temperature of described phase-change heat conductive material is 30-55 DEG C, it is preferred that described phase-change heat conductive material
Phase transition temperature be 30-50 DEG C.
The phase transition temperature of phase-change heat conductive material is the lowest, illustrates just can undergo phase transition under reaching relatively low operating temperature, energy
The air gap between filling interface, siphons away interface heat in time, reaches the purpose of heat radiation, is applicable to the field that heat conduction requirement is high
Close.
Further, described polyolefinic viscosity 10000-60000cps.
The typical but non-limiting viscosity of described polyolefin is 10000,15000,20000,24000,30000,40000,
45000,50000,55000 or 60000cps.
Further, the one during described polyolefin is selected from polyisobutylene, polybutene or polyisoprene or at least two
Combination.
In the present invention, described polyolefin is preferably polyisobutylene.Polyisobutylene is with isobutene. for a small amount of positive fourth of advocating peace
The liquid of alkene copolymerization.Polyisobutylene has the performances such as nonflammable, chemical stability good, acidproof, alkaline-resisting, and electrical insulating property is good.
Polyisobutylene mixes with paraffin, can improve toughness and the adhesiveness of paraffin, increases pull resistance in terms of tension intensity, and low
The brittleness of product is improved under gentle moisture conditions.Further, polyisobutylene is selected from the PB2400 in Guangzhou, the PB5500 in Guangzhou
Or the combination of a kind of or at least two in the H-2100 of Britain.
Further, the one during described heat filling is aluminium oxide, magnesium oxide, aluminium nitride or boron nitride or at least two
Combination, or described heat filling is a kind of or the different-grain diameter of at least two heat filling combines.
Described heat filling is many based on metal-oxide with nitride conduction powder, and this type of conduction powder has higher
Thermal conductivity.
Utilize the thickness collocation of the heat filling of different-grain diameter, the gap between filler can be made to be sufficient filling with so that
Heat conductivility promotes further.
Further, described heat filling is a kind of or the combination of the difformity of at least two heat filling；And/or, institute
Stating heat filling is nano heat-conductive filler.
The shape of described heat filling can be spherical, lamellar, column or needle-like.In the present invention, described heat conduction is filled out
That expects is preferably spherical, more preferably ball-aluminium oxide.Ball-aluminium oxide have high heat conduction, high insulation, high rigidity,
The advantage such as high temperature resistant, wear-resisting, corrosion-resistant, can obtain higher heat conductivity with minimum loading.
Generally phase-change heat conductive material uses micron order heat filling, and preferably employs nanometer conductive filling in this programme.
Due to nano heat-conductive filler fine size, specific surface area is big, surface can be high, and heat filling processes can effectively carry through Ultrafine
Himself heat conductivility high, and then increase thermal conductivity and the mechanical property of phase-change heat conductive material.
In order to realize providing one can be prepared by polyolefin, paraffin, heat filling and coupling agent multicomponent heat conduction with phase change material
The purpose of the preparation method of material, the preparation method of the present invention adopts the technical scheme that
(1) coupling agent of the polyolefin of formula ratio, the paraffin of formula ratio and formula ratio is mixed, heated and stirred to uniformly,
Obtain liquid mixture；
(2), after the heat filling of formula ratio being dried, mix with the described liquid mixture in step (1), at vacuum bar
Stir under part, obtain raw mixture；
(3) described raw mixture is cooled down molding, obtain phase-change heat conductive material.
After preparation method of the present invention is by first mixing low melt point paraffin, coupling agent with polyolefin, adds and lead
Hot filler, finally prepares phase-change heat conductive material.This preparation method technique is simple and convenient to operate, prepared heat conduction with phase change material
Material phase transition temperature is low, has excellent heat transfer performance and convenient use.It addition, the temperature during being used by regulation and pressure
Power so that the thickness of this phase-change heat conductive material is the most thinning, thermal impedance can be lower, and heat transfer performance is the most excellent.
Further, described preparation method specifically includes following steps:
(1) mix in the coupling agent of the polyolefin of formula ratio, the paraffin of formula ratio and formula ratio is joined heated and stirred pond
Closing, at 80-160 DEG C, heated and stirred is to uniformly, obtains liquid mixture；
(2) heat filling of formula ratio is put into baking oven in 80-120 DEG C dry after, join in heated and stirred pond, with
Described liquid mixture mixing in step (1), stirs 0.5-2h under vacuum, obtains raw mixture；
(3) it is applied on mould release membrance carry out being cooled to type at 70-90 DEG C of lower roll by described raw mixture, obtains heat conduction with phase change
Material.
Each step in preparation method is expanded on further and optimizes so that prepared phase-change heat conductive material has more excellent
Good heat conductivility and mechanical property.
Compared with prior art, the invention has the beneficial effects as follows:
(1) the invention provides a kind of phase-change heat conductive material, described phase-change heat conductive material is by polyolefin, paraffin, heat conduction
Filler and coupling agent composition, the low melt point paraffin wherein used, not only good with compatible polyolefin, also make preparation-obtained
Phase-change heat conductive material has relatively low phase transition temperature, excellent heat stability and weatherability, can be repeatedly used for a long, improve biography
In the phase-change heat conductive material of system, phase transition temperature is higher, and causes owing to adding some ethylene propylene diene rubbers or viscosifier
The problems such as production cost increase, the feature of environmental protection and poor stability.
(2) present invention also offers the preparation method of a kind of phase-change heat conductive material, described preparation method is by first by low
After melting waxes, coupling agent mix with polyolefin, add heat filling, finally prepare phase-change heat conductive material.This preparation method
Technique is simple, and easy to operate, prepared phase-change heat conductive material phase transition temperature is low, has efficient heat dispersion, it is adaptable to
Heat conduction requires high occasion and can be repeatedly used for a long.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, technical scheme will be carried out below
Clear, complete description.Obviously, described embodiment is only a part of embodiment of the present invention rather than whole embodiments.
Based on the embodiment in the present invention, the institute that those of ordinary skill in the art are obtained on the premise of not making creative work
There is other embodiments, broadly fall into the scope that the present invention is protected.
Embodiment 1
A kind of phase-change heat conductive material that the present invention provides, in parts by weight, is made up of following components:
Wherein, the viscosity of polyisoprene is 50000cps, and melting point of paraffin wax is 48 DEG C, and aluminium oxide is spherical, average particle
Footpath is 40 μm.
Embodiment 2
The preparation method of embodiment 1 phase-change heat conductive material, comprises the following steps:
(1) weigh polyisoprene 100 parts that viscosity is 50000cps, fusing point is 100 parts of paraffin and the coupling agent of 48 DEG C
KH550 0.1 part mixes in putting into heated and stirred pond, in 100 DEG C of heated and stirred to uniformly, obtains liquid mixture.
(2) weigh the aluminium oxide 550 parts that mean diameter is 40 μm, put into after baking oven dries in 90 DEG C, and in step (1)
Described liquid mixture mixing, stir 0.5h under vacuum, obtain raw mixture.
(3) it is applied on mould release membrance carry out being cooled to type at 70 DEG C of lower rolls by described raw mixture, obtains heat conduction with phase change material
Material.
Embodiment 3
A kind of phase-change heat conductive material that the present invention provides, in parts by weight, is made up of following components:
Wherein, the H-2100 of Britain selected by polyisobutylene, and the viscosity of polyisobutylene and polybutene is 40000cps, poly-different
Weight proportion between butylene and polybutene is 1:1, and melting point of paraffin wax is 45 DEG C, and the mean diameter of magnesium oxide is 20 μm, nitridation
The mean diameter of aluminum is 40 μm, and the proportioning between magnesium oxide and aluminium nitride is 5:8.
Embodiment 4
The preparation method of embodiment 3 phase-change heat conductive material, comprises the following steps:
(1) weigh viscosity and be polyisobutylene and polybutene (weight proportion is 1:1) totally 120 parts, the fusing point of 40000cps
It is 90 parts of the paraffin of 45 DEG C and coupling agent KH560 0.8 part joins mixing in heated and stirred pond, 110 DEG C of heated and stirred to all
After even, obtain liquid mixture.
(2) weigh magnesium oxide and the aluminium nitride (proportioning is 5:8) totally 650 parts of 40 μm that mean diameter is 20 μm, put into baking
After drying in 90 DEG C in case, mix with the described liquid mixture in step (1), stir 1h under vacuum, obtain raw material
Mixture.
(3) it is applied on mould release membrance carry out being cooled to type at 80 DEG C of lower rolls by described raw mixture, obtains heat conduction with phase change material
Material.
Embodiment 5
A kind of phase-change heat conductive material that the present invention provides, in parts by weight, is made up of following components:
Wherein, polyisobutylene is made up of the polyisobutylene PB2400 and polyisobutylene PB5500 in Guangzhou, polyisobutylene
The weight ratio of PB2400 and polyisobutylene PB5500 is 1:2, and the viscosity of polyisobutylene PB2400 is 24000cps, polyisobutylene
The viscosity of PB5500 is 55000cps, and melting point of paraffin wax is 32 DEG C, and aluminium oxide is spherical, and mean diameter is 60 μm.
Embodiment 6
The preparation method of embodiment 5 phase-change heat conductive material, comprises the following steps:
(1) weigh polyisobutylene PB2400 40 parts that viscosity is 24000cps, viscosity is the polyisobutylene of 55000cps
PB5500 80 parts, fusing point are that 80 parts and coupling agent Si-563 0.8 part of the paraffin of 32 DEG C puts into mixing in heated and stirred pond,
100 DEG C of heated and stirred, to after uniformly, obtain liquid mixture.
(2) weigh the aluminium oxide 750 parts that mean diameter is 60 μm, put into baking oven in 100 DEG C dry after, with step (1)
In described liquid mixture mixing, stir 1h under vacuum, obtain raw mixture.
(3) it is applied on mould release membrance carry out being cooled to type at 80 DEG C of lower rolls by described raw mixture, obtains heat conduction with phase change material
Material.
Embodiment 7
A kind of phase-change heat conductive material that the present invention provides, in parts by weight, is made up of following components:
Wherein, the viscosity of polyisoprene is 35000cps, and polyisobutylene is the PB2400 in Guangzhou, and viscosity is
24000cps, melting point of paraffin wax is 38 DEG C, and aluminium oxide is spherical, and mean diameter is 60 μm, and boron nitride is lamellar, and mean diameter is
40 μm, the weight proportion of the boron nitride of aluminium oxide sum is 1:1.
Embodiment 8
The preparation method of embodiment 7 phase-change heat conductive material, comprises the following steps:
(1) weigh polyisoprene 50 parts that viscosity is 35000cps, viscosity is the polyisobutylene PB2400 of 24000cps
100 parts, fusing point is 60 parts of the paraffin of 38 DEG C and coupling agent A171 1 part puts into mixing in heated and stirred pond, 150 DEG C of heating
After being stirred until homogeneous, obtain liquid mixture.
(2) weigh aluminium oxide and the boron nitride (proportioning is 1:1) totally 800 parts of 40 μm that mean diameter is 60 μm, put into baking
After drying in 120 DEG C in case, mix with the described liquid mixture in step (1), stir 2h under vacuum, obtain raw material
Mixture.
(3) it is applied on mould release membrance carry out being cooled to type at 90 DEG C of lower rolls by described raw mixture, obtains heat conduction with phase change material
Material.
Embodiment 9
A kind of phase-change heat conductive material that the present invention provides, in parts by weight, is made up of following components:
Wherein, polyisobutylene is made up of the polyisobutylene PB2400 and polyisobutylene PB5500 in Guangzhou, polyisobutylene
The weight ratio of PB2400 and polyisobutylene PB5500 is 1:2, and the viscosity of polyisobutylene PB2400 is 24000cps, polyisobutylene
The viscosity of PB5500 is 55000cps, and melting point of paraffin wax is 32 DEG C, and aluminium oxide is spherical, and mean diameter is 60nm.
Embodiment 10
The preparation method of embodiment 9 phase-change heat conductive material, comprises the following steps:
(1) weigh polyisobutylene PB2400 40 parts that viscosity is 24000cps, viscosity is the polyisobutylene of 55000cps
PB5500 80 parts, fusing point are that 80 parts and coupling agent Si-563 0.8 part of the paraffin of 32 DEG C puts into mixing in heated and stirred pond,
100 DEG C of heated and stirred, to after uniformly, obtain liquid mixture.
(2) weigh the aluminium oxide 750 parts that mean diameter is 60nm, put into baking oven in 100 DEG C dry after, with step (1)
In described liquid mixture mixing, stir 1h under vacuum, obtain raw mixture.
(3) it is applied on mould release membrance carry out being cooled to type at 80 DEG C of lower rolls by described raw mixture, obtains heat conduction with phase change material
Material.
Embodiment 11
A kind of phase-change heat conductive material that the present invention provides, in parts by weight, is made up of following components:
Wherein, polyisobutylene is made up of the polyisobutylene PB2400 and polyisobutylene PB5500 in Guangzhou, polyisobutylene
The weight ratio of PB2400 and polyisobutylene PB5500 is 1:2, and the viscosity of polyisobutylene PB2400 is 24000cps, polyisobutylene
The viscosity of PB5500 is 55000cps, and melting point of paraffin wax is 48 DEG C, and aluminium oxide is spherical, and mean diameter is 60 μm.
Embodiment 12
The preparation method of embodiment 11 phase-change heat conductive material, comprises the following steps:
(1) weigh polyisobutylene PB2400 40 parts that viscosity is 24000cps, viscosity is the polyisobutylene of 55000cps
PB5500 80 parts, fusing point are that 80 parts and coupling agent Si-563 0.8 part of the paraffin of 48 DEG C puts into mixing in heated and stirred pond,
100 DEG C of heated and stirred, to after uniformly, obtain liquid mixture.
(2) weigh the aluminium oxide 750 parts that mean diameter is 60 μm, put into baking oven in 100 DEG C dry after, with step (1)
In described liquid mixture mixing, stir 1h under vacuum, obtain raw mixture.
(3) it is applied on mould release membrance carry out being cooled to type at 80 DEG C of lower rolls by described raw mixture, obtains heat conduction with phase change material
Material.
Comparative example 1
A kind of phase-change heat conductive material, in parts by weight, is made up of following components:
Wherein, the viscosity of polyisoprene is 50000cps, and melting point of paraffin wax is 48 DEG C, and aluminium oxide is spherical, average particle
Footpath is 40 μm.
Comparative example 2
The preparation method of comparative example 1 phase-change heat conductive material, comprises the following steps:
(1) weigh polyisoprene 100 parts that viscosity is 50000cps, fusing point is 100 parts of paraffin, the coupling agent of 48 DEG C
KH550 0.1 part, ethylene propylene diene rubber 10 parts and polyborosiloxane viscosifier 10 parts mix in putting into heated and stirred pond,
100 DEG C of heated and stirred, to uniformly, obtain liquid mixture.
(2) weigh the aluminium oxide 550 parts that mean diameter is 40 μm, put into after baking oven dries in 90 DEG C, and in step (1)
Described liquid mixture mixing, stir 0.5h under vacuum, obtain raw mixture.
(3) it is applied on mould release membrance carry out being cooled to type at 70 DEG C of lower rolls by described raw mixture, obtains heat conduction with phase change material
Material.
Experimental example 1
Heat conductivity reflection is the material capacity of heat transmission under unit volume, and the heat conductivity of Heat Conduction Material is the biggest, then
Its heat conductivity is the best.
The phase-change heat conductive material of embodiment 1,3,5,7,9,11 and comparative example 1 gained is made size is 100mm × 100mm
× 0.1mm thin slice experiment Analysis, uses DRL-III heat conduction coefficient tester to detect its heat conductivity, specific performance parameter
As shown in the table:
As can be seen from the table, phase-change heat conductive material before phase transformation and after phase transformation heat conductivity there occurs and increase largely
Adding, the changing value of heat conductivity is all more than 20% on the whole.This explanation phase-change heat conductive material occurs under phase transition temperature really
Phase transformation, can effectively fill the air gap between electronic component and fin, siphon away interface heat, reaches the mesh of heat radiation
's.It should be noted that the paraffin melting point of selection is the lowest, the phase transition temperature of its prepared phase-change heat conductive material is the lowest, this
The phase transition temperature of bright phase-change heat conductive material is between 30-50 DEG C.
Embodiment 9 is the control experiment of embodiment 5, and difference between the two is that the size of heat filling is different.Implement
The heat filling used in example 5 is micron order, and the heat filling used in embodiment 9 is nanoscale.As can be seen from the table, real
No matter the phase-change heat conductive material executing example 9 is superior to the phase-change heat conductive material of embodiment 5 on heat conductivility or mechanical property.Can
Seeing, nanometer conductive filling can be effectively improved the heat conductivility of himself, so increase phase-change heat conductive material thermal conductivity and
Physical property.
Embodiment 11 is the controlled trial of embodiment 5, and difference between the two is that melting point of paraffin wax is different.Embodiment 5
In use the paraffin that fusing point is 32 DEG C, embodiment 11 uses the paraffin that fusing point is 48 DEG C.As can be seen from the table,
The phase transition temperature of the phase-change heat conductive material of embodiment 5 is significantly lower than the phase transition temperature of embodiment 11.Visible, melting point of paraffin wax and phase
The phase transition temperature becoming Heat Conduction Material is closely bound up, i.e. paraffin melting point is the lowest, and the fusing point of prepared phase-change heat conductive material is the lowest.
As the contrast test of embodiment 1, comparative example 1 is to the addition of again EPDM on the basis of the raw material of embodiment 1
Rubber and polyborosiloxane class viscosifier, the raw material that comparative example 1 uses consists of the composition of conventional phase-change heat conductive material.From table
It can be seen that the heat conductivity of embodiment 1 is slightly larger than the heat conductivity of comparative example 1, the phase alternating temperature of embodiment 1 phase-change heat conductive material
The phase transition temperature of degree slightly below comparative example 1 phase-change heat conductive material.But, the hot strength comparative example to be far above 1 of embodiment 1
Hot strength.It follows that the heat conductivility that the interpolation of ethylene propylene diene rubber and polyborosiloxane class viscosifier is to Heat Conduction Material
Impact is little, but can affect the mechanical property of phase-change heat conductive material so that the hot strength of phase-change heat conductive material reduces.And three
Unit's EP rubbers and the interpolation of polyborosiloxane class viscosifier, add the production cost of phase-change heat conductive material undoubtedly.So this
The technical scheme that thered is provided of invention improves traditional heat conduction with phase change material due to ethylene propylene diene rubber or the existence of viscosifier
The problems such as the production cost increase, the feature of environmental protection and the poor stability that cause.
The phase-change heat conductive material that the present invention provides is high molecular polymer, and the density at 23 DEG C is 1.92g/cm3, applicable for temperature
Degree scope is-55～120 DEG C, and cold-hot impact cycle is more than 1000 times.This phase-change heat conductive material has excellent heat dispersion
Phase transition temperature with relatively low, can be applicable to electro-heat equipment, is specifically related to be not required to the occasion of electric insulation, such as computer industry,
IC market, Mobile Industry, network communication apparatus, automotive electronics, LED illumination, household electric appliances and new-energy automobile are dynamic
The fields such as power power supply.
Last it is noted that various embodiments above is only in order to illustrate technical scheme, it is not intended to limit；To the greatest extent
The present invention has been described in detail by pipe with reference to foregoing embodiments, it will be understood by those within the art that: it depends on
So the technical scheme described in foregoing embodiments can be modified, or the most some or all of technical characteristic is entered
Row equivalent；And these amendments or replacement, do not make the essence of appropriate technical solution depart from various embodiments of the present invention technology
The scope of scheme.
Claims (10)
1. a phase-change heat conductive material, it is characterised in that in parts by weight, described phase-change heat conductive material is mainly by following group
Divide and make:
Described paraffin is low melt point paraffin, and described melting point of paraffin wax is 30-50 DEG C.
Phase-change heat conductive material the most according to claim 1, it is characterised in that in parts by weight, described heat conduction with phase change
Material is made up of following components:
Described paraffin is low melt point paraffin, and described melting point of paraffin wax is 30-50 DEG C.
Phase-change heat conductive material the most according to claim 1, it is characterised in that in parts by weight, described heat conduction with phase change
Material is made up of following components:
Described paraffin is low melt point paraffin, and described melting point of paraffin wax is 30-45 DEG C.
4. according to the phase-change heat conductive material described in claim 1-3 any one, it is characterised in that described phase-change heat conductive material
Phase transition temperature is 30-50 DEG C.
5. according to the phase-change heat conductive material described in claim 1-3 any one, it is characterised in that described polyolefinic viscosity
10000-60000cps。
Phase-change heat conductive material the most according to claim 4, it is characterised in that described polyolefin is selected from polyisobutylene, poly-fourth
One in alkene or polyisoprene or at least two combination.
7. according to the phase-change heat conductive material described in claim 1-3 any one, it is characterised in that described heat filling is oxidation
One or at least two in aluminum, magnesium oxide, aluminium nitride or boron nitride combine, or described heat filling is one or at least two
Plant the different-grain diameter combination of heat filling.
8. according to the phase-change heat conductive material described in claim 1-3 any one, it is characterised in that described heat filling is a kind of
Or the difformity combination of at least two heat filling；And/or, described heat filling is nano heat-conductive filler.
9. the preparation method of the phase-change heat conductive material described in claim 1-8 any one, it is characterised in that include walking as follows
Rapid:
(1) being mixed by the coupling agent of the polyolefin of formula ratio, the paraffin of formula ratio and formula ratio, heated and stirred, to uniformly, obtains
Liquid mixture；
(2), after the heat filling of formula ratio being dried, mix, under vacuum with the described liquid mixture in step (1)
Stir, obtain raw mixture；
(3) described raw mixture is cooled down molding, obtain phase-change heat conductive material.
Preparation method the most according to claim 9, it is characterised in that comprise the steps:
(1) mix in the coupling agent of the polyolefin of formula ratio, the paraffin of formula ratio and formula ratio is joined heated and stirred pond,
At 80-160 DEG C, heated and stirred is to uniformly, obtains liquid mixture；
(2) heat filling of formula ratio is put into after baking oven dries in 80-120 DEG C, in joining heated and stirred pond and step
(1) liquid mixture described in mixes, and stirs 0.5-2h under vacuum, obtains raw mixture；
(3) it is applied on mould release membrance carry out being cooled to type at 70-90 DEG C of lower roll by described raw mixture, obtains heat conduction with phase change material
Material.
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| CN108587570A (en) * | 2018-03-23 | 2018-09-28 | 南方科技大学 | A kind of insulation phase-change heat conductive material and preparation method thereof |
| CN109913183A (en) * | 2019-04-12 | 2019-06-21 | 哈尔滨理工大学 | A kind of insulating heat-conductive preparation of sections method with phase-change characteristic |
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| CN112895214A (en) * | 2021-01-15 | 2021-06-04 | 中裕软管科技股份有限公司 | Thermal insulation material for repairing thermal power pipe and method for preparing thermal power repairing pipe |
| CN113652205A (en) * | 2021-08-17 | 2021-11-16 | 山东电亮亮信息科技有限公司 | Heat-conducting insulating phase-change heat-absorbing composite potting material and potting method thereof |
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| CN107722942A (en) * | 2017-11-10 | 2018-02-23 | 苏州环明电子科技有限公司 | Phase transformation high heat conduction boundary material and preparation method thereof |
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| CN109913183A (en) * | 2019-04-12 | 2019-06-21 | 哈尔滨理工大学 | A kind of insulating heat-conductive preparation of sections method with phase-change characteristic |
| CN110317580A (en) * | 2019-07-18 | 2019-10-11 | 深圳前海量子翼纳米碳科技有限公司 | A kind of high latent heat phase-transition heat-storage heat-absorbing material of insulation |
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| CN112895214A (en) * | 2021-01-15 | 2021-06-04 | 中裕软管科技股份有限公司 | Thermal insulation material for repairing thermal power pipe and method for preparing thermal power repairing pipe |
| CN113652205A (en) * | 2021-08-17 | 2021-11-16 | 山东电亮亮信息科技有限公司 | Heat-conducting insulating phase-change heat-absorbing composite potting material and potting method thereof |
| CN114106370A (en) * | 2021-11-17 | 2022-03-01 | 深圳航美新材料科技有限公司 | Low-density composite phase-thinned membrane material and preparation method thereof |
| CN114106370B (en) * | 2021-11-17 | 2024-03-12 | 深圳航美新材料科技有限公司 | Low-density composite phase-change film material and preparation method thereof |
| CN114181670A (en) * | 2021-12-28 | 2022-03-15 | 中国科学院工程热物理研究所 | Flexible high-thermal-conductivity composite phase change film and preparation method thereof |
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