CN108034256A - A kind of explosion-proof silica gel pad of high heat conduction low-gravity lithium battery and preparation method thereof - Google Patents
A kind of explosion-proof silica gel pad of high heat conduction low-gravity lithium battery and preparation method thereof Download PDFInfo
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- CN108034256A CN108034256A CN201711246176.5A CN201711246176A CN108034256A CN 108034256 A CN108034256 A CN 108034256A CN 201711246176 A CN201711246176 A CN 201711246176A CN 108034256 A CN108034256 A CN 108034256A
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Abstract
The present invention provides a kind of explosion-proof silica gel pad of high heat conduction low-gravity lithium battery, include by weight：100 parts of methyl vinyl silicone rubber, 200 400 parts of aluminium oxide, 10 20 parts of boron nitride, 12 parts of vulcanizing agent, 20 parts of silica gel fire retardant, 36 parts of silane coupling agent, 36 parts of hydroxy silicon oil and 5 20 parts of graphene.Present invention also offers a kind of preparation method of the explosion-proof silica gel pad of high heat conduction low-gravity lithium battery.Present invention process is simple and practicable, and mild condition, method safety are easy to operate, required device simple, and production cost is low, it is easy to accomplish batch production.The explosion-proof silica gel pad insulating properties of high heat conduction low-gravity graphene composite lithium ion battery prepared by this method is good, and its vertical thermal conductivity brings up to more than 1.6W/mk, and its horizontal thermal conductivity factor brings up to more than 5W/mk, proportion is less than 2.0, hardness is more than 40SHOREA, tensile strength is more than 250PSI, and rebound degree reaches more than 50%, and flame retardant rating reaches UL94V0 requirements.
Description
Technical field
The invention belongs to the preparation method of silica gel pad, is more particularly to a kind of explosion-proof silica gel of high heat conduction low-gravity lithium battery
The preparation method of gasket.
Background technology
With the development of science and technology, electronic component increasingly levels off to densification and miniaturization, so as to electronics device
The stability of part proposes the requirement of higher, used by the reliability and its performance of electronic product depend greatly on
Whether heat sink material and heat sink conception are reasonable.Statistics shows that electronic component temperature often raises 2 DEG C, its reliability decrease
10%, temperature reduces by 8 DEG C, and the service life of electronic component will double.Therefore, thermal interfacial material is played the part of in information technology field
The role drilled is more and more important.How to further improve the conductibility of thermal interfacial material and reduce thermal resistance, be still current electronic seal
The considerable problem that dress is faced with heat dissipation work.Envelope used at present fills and the polymeric material of encapsulation predominantly synthesis
Material, wherein with epoxy resin, polyurethane and rubber are most widely used.Silicon rubber can be protected for a long time within the scope of very wide temperature
Will not absorb heat heat release when holding elasticity, vulcanization, and have excellent electric property and chemical stability, be that electric assembly fills
The preferred material of envelope.
Silicon rubber is a kind of special synthetic rubber, and using silicon oxygen bond as main chain, and general rubber is using C-C keys as main chain
Structure.Since the particularity of its structure determines that it has high-low temperature resistant, high voltage withstanding, resistance to ozone aging, radiation resistance, height thoroughly
Gas and excellent chemical inertness is shown to media such as lubricating oil.In addition, (- 50-250 DEG C) of use temperature range is broad,
Elastic good, anti creepage trace and electric corrosion performance are good, especially still have the characteristics that excellent hydrophobicity performance after its surface contamination.
Therefore, silicon rubber is used as heat conduction substrate, and a kind of elastic heat conducting insulating materials of excellent properties is combined with high heat conduction filler
It is of great significance.
The effect of heat filling is that thermal conducting path is formed in base material so as to improve the thermal conductivity of heat conductive silica gel, therefore
Lifting of the formation of effective thermal conducting path for material thermal conductivity is most important.The additive amount for improving heat filling can help to
The structure of thermal conducting path, but as the increase of heat filling, product cost also accordingly increase, mechanical performance also can be under
Drop, passage of heat deficiency inside currently used heat conductive silica gel, it is poor to cause the heat conductivility of silicagel pad, limits its application
Scope.The more excellent heat filling of heat conductivility is selected, is to solve the problems, such as one of this preferred solution.
Graphene is the new material for the individual layer laminated structure for having carbon atom to form, and thermal conductivity factor is up to 530W/ (m.k), and
And such two-dimensional structure has the specific surface area of super large and good chemical stability.On the other hand, in face of electronics member device
This following development trend requirement of the lighting of part, the low-density of graphene will be helpful to the obvious reduction of its product proportion.
Obviously, these excellent performances make graphene become a kind of preferably novel heat-conducting filler.But graphene is easily reunited,
Filling intrinsic silicon can influence the formation of thermal conducting path because of reunion.This patent is directed to this problem, it is proposed that corresponding to solve
Scheme.
The content of the invention
The object of the present invention is to provide the height that a kind of thermal conductivity factor is higher, heat conductivility and flame-resistant insulation performance are more excellent
The preparation method of the explosion-proof silica gel pad of heat conduction low-gravity lithium battery.
According to an aspect of the invention, there is provided a kind of explosion-proof silica gel pad of high heat conduction low-gravity lithium battery, by weight
Part meter includes：100 parts of methyl vinyl silicone rubber, 200-400 parts of aluminium oxide, 10-20 parts of boron nitride, 1-2 parts of sulphur
Agent, 20 parts of silica gel fire retardant, 3-6 parts of silane coupling agent, the graphene of 3-6 parts of hydroxy silicon oil and 5-20 part.
A kind of preparation method of the explosion-proof silica gel pad of high heat conduction low-gravity lithium battery, includes the following steps：
Step 1: boron nitride and graphene are surface-treated：With water with ethanol 1：1~2：1 volume ratio configuration
Boron nitride and graphene, are impregnated in silane coupling agent aqueous solution by ethanol water respectively, then through homogenous disperse, suction filtration, dry
It is dry, beat powder, boron nitride powder and graphene powder is made；
Step 2: aluminium oxide is added in homogenizer, after carrying out processing 3-5min to aluminium oxide with silane coupling agent, fall
Enter boron nitride and graphene powder carries out high-speed stirred and/or ultrasound and/or high-pressure homogeneous and/or ball milling and/or supercritical phase
The mixed processing of associated methods, is made mixed powder；
Step 3: adding methyl ethylene silica gel in masticator, kneading first, is slowly added to mixed powder and fire-retardant
Simultaneously kneading is uniform for agent, and cooling, kneading again, is blended into vulcanizing agent, and rubber compound is made；
Step 4: by rubber compound back mixing on a mill, finished composition is made；
Step 5: by after finished composition tabletting, it is placed in plate vulcanization machine die, it is high temperature vulcanized, high heat conduction low-gravity is made
The explosion-proof silica gel pad of lithium battery.
In some embodiments, the silane coupling agent is γ-(methacryloxypropyl) propyl trimethoxy silicane, 3-
One or more in aminopropyltriethoxywerene werene, vinyl three ('beta '-methoxy ethyoxyl) silane, selected boron nitride are
Hexagonal boron nitride, 4-8 μm of particle diameter, selected graphene powder are graphene prepared by mechanical stripping method, and the graphene number of plies is 1~10
Layer, size are 7-12 μm.
In some embodiments, the aluminium oxide is compounded by the small particle alumina particle of big particle diameter alumina particle sum
Form, the particle diameter of the big particle diameter alumina particle is 30-60 μm, and the particle diameter of the small particle alumina particle is 3-8 μm, institute
The mass ratio for stating big particle diameter alumina particle and small particle alumina particle is 1:3-1:4.
In some embodiments, the dosage of the silane coupling agent in the step 2 is the 1-2% of the quality of aluminium oxide.
In some embodiments, the aluminium oxide：The boron nitride：The mass ratio of the graphene is 40:3:1.
In some embodiments, the processing time added in the step 2 after silane coupling agent is 3-5min, described
The time of mixed processing is 5-10min.
In some embodiments, the time of kneading first is 30-50min, and cooling time is 4~6h.
In some embodiments, vulcanizing press curing temperature is 150-170 DEG C, sulfide stress 3-10Mpa, during vulcanization
Between 2-3min.
Its advantage is：The present invention utilizes the mixing of different-grain diameter aluminium oxide, boron nitride and graphene powder, makes stone
Ink is dilute to be not susceptible to reunite in rubber, is uniformly dispersed, and will not destroy itself framework of graphene and other carbon materials, is kept
Graphene and the excellent performance of other carbon materials in itself；Pass through the surface preparation to aluminium oxide, boron nitride, graphene particle
And blending, interpolation slit, realize reasonable distribution of the filler grain in silica gel matrix and fully fusion, it is excellent using graphene powder
Heat conductivility, finally realize improve silica gel pad heat conductivility；Powder is modified by being surface-treated, and is more easy to silica gel
With reference to utilizing the excellent heat conducting performance of graphene powder so that filer content declines, and compares market in the case of the identical thermal conductivity of gasket
Upper product density smaller mechanical performance is more preferably；Different-grain diameter, variety classes heat filling compounding, it is interparticle to reduce heat filling
Gap, hence it is evident that improve thermal conductivity factor.Present invention process is simple and practicable, and mild condition, method safety are easy to operate, required equipment letter
Easily, production cost is low, it is easy to accomplish batch production.The explosion-proof silica gel pad of high heat conduction low-gravity lithium battery prepared by this method
Insulating properties is good, and its vertical thermal conductivity brings up to more than 1.6W/mk, and its horizontal thermal conductivity factor brings up to 5W/mk
More than, proportion is less than 2.0, and hardness is more than 40SHOREA, and tensile strength is more than 250PSI, and rebound degree reaches more than 50%, resistance
Combustion grade reaches UL94V0 requirements.
Embodiment
With reference to specific embodiment, the present invention is described further.
Embodiment 1
A kind of explosion-proof silica gel pad of high heat conduction low-gravity lithium battery, is prepared in the following way：
(1) boron nitride and graphene are surface-treated：Under room temperature, graphene is added in 50% ethanol water,
Add the silane coupling agent KH570 of graphene quality 2%, be dispersed with stirring 2 it is small when after, homogenizer homogeneous three times, it is small to continue dipping 2
When, it is filtered dry, 24h is dried at 150 DEG C, it is spare to beat powder, the same graphene of boron nitride processing mode.
(2) 150 parts 7 μm add in homogenizer with 50 parts of 40 μm of aluminium oxide, after drenching 3 parts of A-172, high-speed stirring of starting shooting
5min is mixed, 15 parts of boron nitride is subsequently poured into and 5 parts of graphene powders continues mixed at high speed 8min；
(3) after adding 100 parts of methyl vinyl silicone rubbers in masticator, start is kneaded, and is slowly added to mixed powder and beautiful jade
Enter 3 parts of hydroxy silicon oils, 20 parts of fire retardants are continuously added after kneading is uniform and kneading is uniform, after parking 4h coolings, input is pinched again
Mill, is mixed into 1.5 parts of vulcanizing agents.
(4) by the back mixing on a mill of obtained rubber compound.
(5) by after finished composition tabletting, it is placed in plate vulcanization machine die, 170 DEG C, high temperature vulcanized under 5Mpa, 3min, to obtain the final product
High heat conductive insulating silica gel pad.
The obtained explosion-proof silica gel pad of high heat conduction low-gravity lithium battery includes 100 parts of methyl vinyl silicone rubber, 200 parts
Aluminium oxide, 15 parts of boron nitride, 1.5 parts of vulcanizing agent, 20 parts of silica gel fire retardant, 3 parts of silane coupling agent, 3 parts of hydroxyl
Base silicone oil and 5 parts of graphene.
Heat conductive silica gel thermal conductivity factor is measured with standard ASTMD5470 thermal constants analyzer, what is measured vertically leads
Hot coefficient is 1.6W/Mk, horizontal thermal conductivity factor 5.0W/mk, hardness 57SHOREA, proportion 1.98, and tensile strength is
256.6PSI, rebound degree 59%, flame retardant rating UL94V0.
Embodiment 2
A kind of explosion-proof silica gel pad of high heat conduction low-gravity lithium battery, is prepared in the following way：
(1) boron nitride and graphene are surface-treated：Under room temperature, graphene is added in 50% ethanol water,
Add the silane coupling agent KH570 of graphene quality 2%, be dispersed with stirring 2 it is small when after, homogenizer homogeneous three times, it is small to continue dipping 2
When, it is filtered dry, 24h is dried at 150 DEG C, it is spare to beat powder, the same graphene of boron nitride processing mode.
(2) 150 parts 7 μm add in homogenizer with 50 parts of 40 μm of aluminium oxide, after drenching 3 parts of A-172, high-speed stirring of starting shooting
5min is mixed, 10 parts of boron nitride is subsequently poured into and 10 parts of graphene powders continues mixed at high speed 8min；
(3) after adding 100 parts of methyl vinyl silicone rubbers in masticator, start is kneaded, and is slowly added to mixed powder and beautiful jade
Enter 3 parts of hydroxy silicon oils, 20 parts of fire retardants are continuously added after kneading is uniform and kneading is uniform, after parking 4h coolings, input is pinched again
Mill, is mixed into 1.5 parts of vulcanizing agents.
(4) by the back mixing on a mill of obtained rubber compound.
(5) by after finished composition tabletting, it is placed in plate vulcanization machine die, 170 DEG C, high temperature vulcanized under 5Mpa, 3min, to obtain the final product
The explosion-proof silica gel pad of high heat conduction low-gravity lithium battery.
The obtained explosion-proof silica gel pad of high heat conduction low-gravity lithium battery includes 100 parts of methyl vinyl silicone rubber, 200 parts
Aluminium oxide, 10 parts of boron nitride, 1.5 parts of vulcanizing agent, 20 parts of silica gel fire retardant, 3 parts of silane coupling agent, 3 parts of hydroxyl
Base silicone oil and 10 parts of graphene.
Heat conductive silica gel thermal conductivity factor is measured with standard ASTMD5470 thermal constants analyzer, what is measured vertically leads
Hot coefficient is 1.69W/Mk, horizontal thermal conductivity factor 5.25W/mk, hardness 67SHOREA, proportion 1.95, tensile strength
For 268.2PSI, rebound degree 54%, flame retardant rating UL94V0.
Embodiment 3
A kind of explosion-proof silica gel pad of high heat conduction low-gravity lithium battery, is prepared in the following way：
(1) boron nitride and graphene are surface-treated：Under room temperature, graphene is added in 50% ethanol water,
Add the silane coupling agent KH570 of graphene quality 2%, be dispersed with stirring 2 it is small when after, homogenizer homogeneous three times, it is small to continue dipping 2
When, it is filtered dry, 24h is dried at 150 DEG C, it is spare to beat powder, the same graphene of boron nitride processing mode.
(2) 150 parts 7 μm add in homogenizer with 50 parts of 40 μm of aluminium oxide, after drenching 3 parts of A-172, high-speed stirring of starting shooting
5min is mixed, 10 parts of boron nitride is subsequently poured into and 15 parts of graphene powders continues mixed at high speed 8min；
(3) after adding 100 parts of methyl vinyl silicone rubbers in masticator, start is kneaded, and is slowly added to mixed powder and beautiful jade
Enter 3 parts of hydroxy silicon oils, 20 parts of fire retardants are continuously added after kneading is uniform and kneading is uniform, after parking 4h coolings, input is pinched again
Mill, is mixed into 1.5 parts of vulcanizing agents.
(4) by the back mixing on a mill of obtained rubber compound.
(5) by after finished composition tabletting, it is placed in plate vulcanization machine die, 170 DEG C, high temperature vulcanized under 5Mpa, 3min, to obtain the final product
The explosion-proof silica gel pad of high heat conduction low-gravity lithium battery.
The obtained explosion-proof silica gel pad of high heat conduction low-gravity lithium battery includes 100 parts of methyl vinyl silicone rubber, 200 parts
Aluminium oxide, 10 parts of boron nitride, 1.5 parts of vulcanizing agent, 20 parts of silica gel fire retardant, 3 parts of silane coupling agent, 3 parts of hydroxyl
Base silicone oil and 15 parts of graphene.
Heat conductive silica gel thermal conductivity factor is measured with standard ASTMD5470 thermal constants analyzer, what is measured vertically leads
Hot coefficient is 1.62W/Mk, horizontal thermal conductivity factor 5.83W/mk, hardness 62SHOREA, proportion 1.93, tensile strength
For 257.4PSI, rebound degree 56%, flame retardant rating UL94V0.
As described above, the explosion-proof silica gel pad of high heat conduction low-gravity lithium battery of the present invention has higher thermal conductivity, relatively low
Proportion and preferable insulating properties, in addition, fire resistance, mobile performance and shock resistance are more excellent.
Described above has fully disclosed the embodiment of the present invention.It is pointed out that it is familiar with the field
Scope of the technical staff to any change that the embodiment of the present invention is done all without departing from claims of the present invention.
Correspondingly, the scope of claim of the invention is also not limited only to previous embodiment.
Claims (9)
1. a kind of explosion-proof silica gel pad of high heat conduction low-gravity lithium battery, it is characterised in that include by weight：100 parts of first
Base vinylsiloxane rubber, 200-400 parts of aluminium oxide, 10-20 parts of boron nitride, 1-2 parts of vulcanizing agent, 20 parts of silica gel are fire-retardant
Agent, 3-6 parts of silane coupling agent, the graphene of 3-6 parts of hydroxy silicon oil and 5-20 part.
2. the preparation method of the explosion-proof silica gel pad of high heat conduction low-gravity lithium battery as claimed in claim 1, it is characterised in that bag
Include following steps：
Step 1: boron nitride and graphene are surface-treated：With water with ethanol 1：1~2：1 volume ratio configuration ethanol
Boron nitride and graphene, are impregnated in silane coupling agent aqueous solution by aqueous solution respectively, then through homogenous disperse, suction filtration, drying, beat
Powder, is made boron nitride powder and graphene powder；
Step 2: aluminium oxide is added in homogenizer, after carrying out processing 3-5min to aluminium oxide with silane coupling agent, nitrogen is poured into
Change boron and graphene powder carries out high-speed stirred and/or ultrasound and/or high-pressure homogeneous and/or ball milling and/or supercritical phase combines
The mixed processing of method, is made mixed powder；
Step 3: adding methyl ethylene silica gel in masticator, kneading first, is slowly added to mixed powder and fire retardant simultaneously
Kneading is uniform, and cooling, kneading again, is blended into vulcanizing agent, and rubber compound is made；
Step 4: by rubber compound back mixing on a mill, finished composition is made；
Step 5: by after finished composition tabletting, it is placed in plate vulcanization machine die, it is high temperature vulcanized, high heat conduction low-gravity lithium electricity is made
The explosion-proof silica gel pad in pond.
3. the preparation method of the explosion-proof silica gel pad of high heat conduction low-gravity lithium battery according to claim 2, it is characterised in that
The silane coupling agent is γ-(methacryloxypropyl) propyl trimethoxy silicane, 3-aminopropyltriethoxysilane, ethene
One or more in base three ('beta '-methoxy ethyoxyl) silane, selected boron nitride are hexagonal boron nitride, and 4-8 μm of particle diameter is selected
Graphene powder is graphene prepared by mechanical stripping method, and the graphene number of plies is 1~10 layer, and size is 7-12 μm.
4. the preparation method of the explosion-proof silica gel pad of high heat conduction low-gravity lithium battery according to claim 2, it is characterised in that
The aluminium oxide is formed by big particle diameter alumina particle and small particle alumina particle compounding, the big particle diameter alumina particle
Particle diameter is 30-60 μm, and the particle diameter of the small particle alumina particle is 3-8 μm, the big particle diameter alumina particle and small particle
The mass ratio of alumina particle is 1:3-1:4.
5. the preparation method of the explosion-proof silica gel pad of high heat conduction low-gravity lithium battery according to claim 2, it is characterised in that
The dosage of silane coupling agent in the step 2 is the 1-2% of the quality of aluminium oxide.
6. the preparation method of the explosion-proof silica gel pad of high heat conduction low-gravity lithium battery according to claim 2, it is characterised in that
The aluminium oxide：The boron nitride：The mass ratio of the graphene is 40:3:1.
7. the preparation method of the explosion-proof silica gel pad of high heat conduction low-gravity lithium battery according to claim 2, it is characterised in that
The processing time added in the step 2 after silane coupling agent is 3-5min, and the time of the mixed processing is 5-10min.
8. the preparation method of the explosion-proof silica gel pad of high heat conduction low-gravity lithium battery according to claim 2, it is characterised in that
The time of kneading first is 30-50min, and cooling time is 4~6h.
9. the preparation method of the explosion-proof silica gel pad of high heat conduction low-gravity lithium battery according to claim 2, it is characterised in that
Vulcanizing press curing temperature is 150-170 DEG C, sulfide stress 3-10Mpa, vulcanization time 2-3min.
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Cited By (8)
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| CN108546414A (en) * | 2018-05-18 | 2018-09-18 | 深圳市金菱通达电子有限公司 | The dedicated lightweight Heat Conduction Material of new energy battery |
| CN111621139A (en) * | 2020-06-29 | 2020-09-04 | 江西伟普科技有限公司 | Wave-absorbing heat-conducting flexible composite material and preparation method thereof |
| WO2021005535A1 (en) * | 2019-07-09 | 2021-01-14 | Saudi Arabian Oil Company | Methods for the production of nanocomposites for high temperature electrochemical energy storage devices |
| CN112467305A (en) * | 2020-11-24 | 2021-03-09 | 江苏厚生新能源科技有限公司 | High-flame-retardance high-heat-conductivity lithium battery diaphragm and preparation method thereof |
| CN113105743A (en) * | 2021-03-31 | 2021-07-13 | 华南理工大学 | Heat-conducting ceramic silicon rubber material and preparation method thereof |
| US11239466B2 (en) | 2018-01-09 | 2022-02-01 | Saudi Arabian Oil Company | Nanocomposite cathode materials for use in batteries |
| CN114213850A (en) * | 2021-12-28 | 2022-03-22 | 江苏达胜高聚物股份有限公司 | High-thermal-conductivity silicone rubber cable material and preparation method and application thereof |
| US11658286B2 (en) | 2018-01-09 | 2023-05-23 | Saudi Arabian Oil Company | Nanocomposite electrode materials for use in high temperature and high pressure rechargeable batteries |
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Application publication date: 20180515 |