CN108003558A - A kind of phase-change heat conductive material of low transformation temperature and preparation method thereof - Google Patents
A kind of phase-change heat conductive material of low transformation temperature and preparation method thereof Download PDFInfo
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- CN108003558A CN108003558A CN201711290625.6A CN201711290625A CN108003558A CN 108003558 A CN108003558 A CN 108003558A CN 201711290625 A CN201711290625 A CN 201711290625A CN 108003558 A CN108003558 A CN 108003558A
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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
- C08L57/00—Compositions of unspecified polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C08L57/02—Copolymers of mineral oil hydrocarbons
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0812—Aluminium
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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Abstract
The present invention discloses a kind of phase-change heat conductive material of low transformation temperature and preparation method thereof, and the phase-change heat conductive material of the low transformation temperature includes the component of following mass fraction：Low melt wax 5~10%, basic long chain hydrocarbon resin 10~20%, antioxidant 0.1~3.0%, crosslinking agent 0.4~2.0%, coupling agent 1.5~3.0% and conductive particle 65~80%.The phase-change heat conductive material of low transformation temperature provided by the invention has good heat-conductive characteristic and stable storage performance, and easy to use and long-time service is not vulnerable, can be widely used for the heat conduction connection between all kinds of heat source generators and radiator.
Description
Technical field
The present invention relates to Heat Conduction Material technical field, the phase-change heat conductive material of more particularly to a kind of low transformation temperature and its preparation
Method.
Background technology
In general, in the heat dissipation design of electronic product, Heat Conduction Material can be usually used, such as heat-conducting silicone grease etc., uses
Heat conduction connection between heat source generator and radiator, can improve the heat dissipation performance of electronic product.But existing heat conduction
The problem of material generally existing thermal conduction effect is poor, and long-time service stability is bad.
The content of the invention
The main object of the present invention is to propose a kind of phase-change heat conductive material of low transformation temperature and preparation method thereof, it is intended to is improved
The thermal conduction effect of Heat Conduction Material, and improve the long-time service stability of Heat Conduction Material.
To achieve the above object, the phase-change heat conductive material of a kind of low transformation temperature proposed by the present invention, including following quality point
Several components：Low melt wax 5~10%, basic long chain hydrocarbon resin 10~20%, antioxidant 0.1~3.0%, crosslinking agent 0.4
~2.0%, coupling agent 1.5~3.0% and conductive particle 65~80%.
Preferably, the low melt wax includes at least one of paraffin, soft wax, beeswax and Organosilicon wax.
Preferably, the basic long chain hydrocarbon resin include C10~C20 alkane compounds, polybutadiene and its modified body,
At least one of polyisoprene and its modified body.
Preferably, the antioxidant include 2,2 '-di-2-ethylhexylphosphine oxide (4- methyl-6-tert-butylphenols), antioxidant 1076 with
And at least one of antioxidant 1010.
Preferably, the crosslinking agent includes ethyl orthosilicate, methyl orthosilicate, trimethoxy silane, aluminium isopropoxide, acetic acid
At least one of zinc and titanium acetylacetone.
Preferably, the coupling agent is gamma-aminopropyl-triethoxy-silane, γ-glycydoxy trimethoxy
Base silane, γ-methacryloxypropyl trimethoxy silane, N- β-(aminoethyl)-γ-aminopropyltrimethoxysilane,
The double titanate coupling agent of vinyltrimethoxysilane, Di(dioctylpyrophosphato) ethylene titanate, phosphate and
At least one of three oleic acid acyloxy titanate esters of isopropyl.
Preferably, the conductive particle includes at least one of aluminium powder, copper powder, aluminium oxide and aluminium nitride.
The present invention also proposes a kind of preparation method of the phase-change heat conductive material of low transformation temperature as described above, including following step
Suddenly：
Heat up after low melt wax, basic long chain hydrocarbon resin, antioxidant and coupling agent are mixed, and stir and form paste
Thing；
Crosslinking agent is added into paste, continues stirring and forms cross-linking products；
Conductive particle is added into cross-linking products, vacuum defoamation processing is carried out after stirring, the phase transformation for obtaining low transformation temperature is led
Hot material.
In technical solution provided by the invention, using low melt wax, basic long chain hydrocarbon resin and conductive particle to be main former
Expect the phase-change heat conductive material prepared, there is good heat-conductive characteristic and stable storage performance, easy to use and long-time service
It is not vulnerable, it can be widely used for the heat conduction connection between all kinds of heat source generators and radiator.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer, is the conventional production that can be obtained by commercially available purchase
Product.
A kind of phase-change heat conductive material of low transformation temperature proposed by the present invention, includes the component of following mass fraction：Low melting point
Wax 5~10%, basic long chain hydrocarbon resin 10~20%, antioxidant 0.1~3.0%, crosslinking agent 0.4~2.0%, coupling agent
1.5~3.0% and conductive particle 65~80%.
In technical solution provided by the invention, using low melt wax, basic long chain hydrocarbon resin and conductive particle to be main former
Expect the phase-change heat conductive material prepared, there is good heat-conductive characteristic and stable storage performance, easy to use and long-time service
It is not vulnerable, it can be widely used for the heat conduction connection between all kinds of heat source generators and radiator.
The low melt wax includes at least one of paraffin, soft wax, beeswax and Organosilicon wax.The low melt wax can
To be that the one or more in paraffin, soft wax, beeswax and Organosilicon wax mix, in embodiments of the present invention, with fusing point
It is preferred for 35~45 DEG C, advantageously reduces the transformation temperature of phase-change heat conductive material, its additive amount accounts for the total matter of the phase-change heat conductive material
The 6~8% of amount are optimal.
The basic long chain hydrocarbon resin includes C10~C20 alkane compounds, polybutadiene and its modified body, poly- isoamyl
At least one of diene and its modified body.Phase changing resin based on the basic long chain hydrocarbon resin, leads the phase transformation
The form of hot material can be varied with temperature and changed, when the feature component of electronic product works heating, by solid
State becomes liquid, there is provided certain latent heat and contribute to the heat dissipation of component；When the feature component of electronic product does not work,
Phenomena such as reverting to initial solid-state, diffusion or lower drop will not occur, long-time service stability is more reliable.In the embodiment of the present invention
In, to select the resin of C12~C18 to be preferred, and its additive amount accounts for 10~15% timeliness of the phase-change heat conductive material gross mass
Fruit is optimal.
The antioxidant includes 2,2 '-di-2-ethylhexylphosphine oxide (4- methyl-6-tert-butylphenols), antioxidant 1076 and antioxidant
At least one of 1010.The effect of the antioxidant is to delay or suppress the progress of polymer oxidizing process, so as to prevent to gather
The aging of compound simultaneously extends its service life, it is however generally that, its additive amount is 0.1~5%.In embodiments of the present invention, it is described
Antioxidant can be 2, one in 2 '-di-2-ethylhexylphosphine oxide (4- methyl-6-tert-butylphenols), antioxidant 1076 and antioxidant 1010
Kind or a variety of mixtures, what its additive amount accounted for the phase-change heat conductive material gross mass 0.1~1.4% is preferred.
The crosslinking agent include ethyl orthosilicate, methyl orthosilicate, trimethoxy silane, aluminium isopropoxide, zinc acetate and
At least one of titanium acetylacetone.By selecting suitable crosslinking agent and its additive amount, the heat conduction with phase change material can be improved
The sag resistance energy of material, so as to ensure that the phase-change heat conductive material has good sag-resistant performance.In embodiments of the present invention,
What the additive amount of the crosslinking agent accounted for the phase-change heat conductive material gross mass 0.5~2% is preferred.
The coupling agent for gamma-aminopropyl-triethoxy-silane, γ-glycydoxy trimethoxy silane,
γ-methacryloxypropyl trimethoxy silane, N- β-(aminoethyl)-γ-aminopropyltrimethoxysilane, vinyl three
The double titanate coupling agents of methoxy silane, Di(dioctylpyrophosphato) ethylene titanate, phosphate and isopropyl three
At least one of oleic acid acyloxy titanate esters.The addition of coupling agent helps to improve the stability of the phase-change heat conductive material,
Therefore, the storage stability of the phase-change heat conductive material can be improved by selecting suitable coupling agent and its additive amount
With application operating performance, what its additive amount accounted for the phase-change heat conductive material gross mass 0.5~2% is preferred.
The conductive particle includes at least one of aluminium powder, copper powder, aluminium oxide and aluminium nitride.The conductive particle
Effect be conduction heat, the higher material of thermal conductivity factor should be selected, by select suitable conductive particle species and its shape and
Particle diameter, can reach adjusting and optimize heat transfer and the heat diffusivity energy of the phase-change heat conductive material.In embodiments of the present invention, institute
Conductive particle is stated as all kinds of conductive powders with different-grain diameter (being illustrated in the embodiment of the present invention exemplified by 2~5 μm) distribution
Body, including aluminium powder, copper powder, aluminium oxide and 70~80% are preferred.
The present invention also proposes a kind of preparation method of the phase-change heat conductive material of low transformation temperature as described above, including following step
Suddenly：
Step S10, heat up, and stir after mixing low melt wax, basic long chain hydrocarbon resin, antioxidant and coupling agent
Form paste；
In embodiments of the present invention, raw material can be mixed using planetary power mixer, concrete operations are：Press
After ratio weighs low melt wax, basic long chain hydrocarbon resin, antioxidant and coupling agent, put into planetary power mixer, rise
70~80 DEG C of high temperature value, stirs 30~45min, forms uniform paste.
Step S20, crosslinking agent is added into paste, continues stirring and forms cross-linking products；
The crosslinking agent weighed in proportion is added in paste into planetary power mixer, continues to stir 10min, extremely
Crosslinking agent is completely dissolved.
Step S30, conductive particle is added into cross-linking products, vacuum defoamation processing is carried out after stirring, obtains low transformation temperature
Phase-change heat conductive material.
After crosslinking agent to be added is completely dissolved, conductive particle is added portionwise, stirs 60~90min, observation is uniformly mixed
Afterwards, carry out vacuum defoamation and handle 30~45min, vacuum defoamation is completed to obtain the phase-change heat conductive material of low transformation temperature.
Technical scheme is described in further detail below in conjunction with specific embodiment, it will be appreciated that following real
Example is applied only to explain the present invention, is not intended to limit the present invention.
Embodiment 1
(1) raw material is weighed：40# soft waxs 5%, C12 hydrocarbon resins 15%, antioxidant 1076 0.1%, trimethoxy silane
0.4%th, γ-methacryloxypropyl trimethoxy silane 3.0% and ball-aluminium oxide (D50=2 μm) 76.5%.
(2) prepared by phase-change heat conductive material：40# soft waxs, C12 hydrocarbon resins, antioxidant are added in planet power mixer
1076 and γ-methacryloxypropyl trimethoxy silane, rise temperature is to 75 DEG C, and stirring 45min is into uniform paste
Thing；Then trimethoxy silane is added, stirring 10min to trimethoxy silane is completely dissolved, then ball-aluminium oxide is added portionwise,
75min is stirred, is observed to vacuum defoamation processing 45min after mixing, is carried out, up to phase-change heat conductive material.
Embodiment 2
(1) raw material is weighed：40# soft waxs 8%, C18 hydrocarbon resins 20%, 2,2 '-di-2-ethylhexylphosphine oxide (4- methyl-6-tert butyl
Phenol) 1.5%, trimethoxy silane 2.0%, three oleic acid acyloxy titanate esters 2.5% of isopropyl and aluminium powder (D50=2 μm)
66%.
(2) prepared by phase-change heat conductive material：40# soft waxs, C18 hydrocarbon resins, 2,2 '-Asia are added in planet power mixer
Methyl double (4- methyl-6-tert-butylphenols) and three oleic acid acyloxy titanate esters of isopropyl, rise temperature is to 70 DEG C, stirring
45min is into homogeneous paste；Then trimethoxy silane is added, stirring 10min to trimethoxy silane is completely dissolved, then in batches
Aluminium powder is added, stirs 75min, is observed to vacuum defoamation processing 45min after mixing, is carried out, up to phase-change heat conductive material.
Embodiment 3
(1) raw material is weighed：35# Organosilicon waxes 10%, C15 hydrocarbon resins 15%, antioxidant 1010 3.0%, acetylacetone,2,4-pentanedione
Titanium 1.0%, γ-methacryloxypropyl trimethoxy silane 1.5% and aluminium powder (D50=2 μm) 74.5%.
(2) prepared by phase-change heat conductive material：35# Organosilicon waxes, C15 hydrocarbon resins are added in planet power mixer, is resisted
Oxygen agent 1010 and γ-methacryloxypropyl trimethoxy silane, rise temperature is to 70 DEG C, and 45min is into uniform for stirring
Paste；Then titanium acetylacetone is added, stirring 10min to trimethoxy silane is completely dissolved, then aluminium powder is added portionwise, and is stirred
75min, is observed to vacuum defoamation processing 45min after mixing, is carried out, up to phase-change heat conductive material.
Embodiment 4
(1) raw material is weighed：Paraffin 6%, C12 hydrocarbon resins 17%, 2,2 '-di-2-ethylhexylphosphine oxide (4- methyl-6-tert butyl benzene
Phenol) 1.0%, trimethoxy silane 1.3%, three oleic acid acyloxy titanate esters 2.2% of isopropyl and aluminium oxide (D50=5 μm)
24.5% and aluminium powder (D50=2 μm) 48%.
(2) prepared by phase-change heat conductive material：Paraffin, C12 hydrocarbon resins, 2,2 '-methylene are added in planet power mixer
Base double (4- methyl-6-tert-butylphenols) and three oleic acid acyloxy titanate esters of isopropyl, rise temperature is to 70 DEG C, stirring
45min is into homogeneous paste；Then trimethoxy silane is added, stirring 10min to trimethoxy silane is completely dissolved, then in batches
Aluminium oxide and aluminium powder are added, stirs 75min, observes to vacuum defoamation processing 45min after mixing, is carried out, is led up to phase transformation
Hot material.
Respectively with Henkel phase-change heat conductive material PSX, Japanese SHIN-ETSU HANTOTAI's heat-conducting silicone grease 7762 as a comparison case 1 and comparative example 2, press
The quasi- ASTM-5470D of sighting target and method for testing shear strength are tested, and indices are as shown in table 1.
Every test index of the Heat Conduction Material of 1 each embodiment of table and comparative example
As shown in Table 1, compared to comparative example, the interface of the phase-change heat conductive material of low transformation temperature provided in an embodiment of the present invention
Impedance is lower, can provide outstanding interface thermal conductivity effect, and shows good heat conductivility (wherein embodiment 4 shows most
It is good)；And thermal impedance change of the phase-change heat conductive material provided by the invention under different causticity test conditions is small, all samples are all opened up
Reveal the reliability more more excellent than heat-conducting silicone grease in comparative example 2 with long term heat transfer stability.
In conclusion the phase-change heat conductive material of low transformation temperature provided by the invention, can meet outstanding heat-conductive characteristic,
Can meet again the longer time using the reliability under validity and particular service requirement, also with good storage stability,
Thermal impedance is low, outstanding to the wetting effect of numerous base materials, can meet that the heat dissipation of current semiconductor components and devices/high-capacity LED will
Ask, and since itself is in paste, use is also more convenient convenient.
It these are only the preferred embodiment of the present invention, be not intended to limit the scope of the invention, it is every to utilize this hair
The equivalent structure or equivalent flow shift that bright description is made, is directly or indirectly used in other relevant technology necks
Domain, is included within the scope of the present invention.
Claims (8)
1. a kind of phase-change heat conductive material of low transformation temperature, it is characterised in that include the component of following mass fraction：Low melt wax 5
~10%, basic long chain hydrocarbon resin 10~20%, antioxidant 0.1~3.0%, crosslinking agent 0.4~2.0%, coupling agent 1.5~
3.0% and conductive particle 65~80%.
2. the phase-change heat conductive material of low transformation temperature as claimed in claim 1, it is characterised in that the low melt wax includes stone
At least one of wax, soft wax, beeswax and Organosilicon wax.
3. the phase-change heat conductive material of low transformation temperature as claimed in claim 1, it is characterised in that the basic long chain hydrocarbon resin
Including at least one of C10~C20 alkane compounds, polybutadiene and its modified body, polyisoprene and its modified body.
4. the phase-change heat conductive material of low transformation temperature as claimed in claim 1, it is characterised in that the antioxidant includes 2,2 '-
At least one of di-2-ethylhexylphosphine oxide (4- methyl-6-tert-butylphenols), antioxidant 1076 and antioxidant 1010.
5. the phase-change heat conductive material of low transformation temperature as claimed in claim 1, it is characterised in that the crosslinking agent includes positive silicic acid
At least one of ethyl ester, methyl orthosilicate, trimethoxy silane, aluminium isopropoxide, zinc acetate and titanium acetylacetone.
6. the phase-change heat conductive material of low transformation temperature as claimed in claim 1, it is characterised in that the coupling agent is γ-ammonia third
Ethyl triethoxy silicane alkane, γ-glycydoxy trimethoxy silane, γ-methacryloxypropyl trimethoxy
Base silane, N- β-(aminoethyl)-γ-aminopropyltrimethoxysilane, vinyltrimethoxysilane, double (two octyloxy Jiao's phosphorus
Perester radical) ethylene titanate esters, at least one in the double three oleic acid acyloxy titanate esters of titanate coupling agent and isopropyl of phosphate
Kind.
7. the phase-change heat conductive material of low transformation temperature as claimed in claim 1, it is characterised in that the conductive particle includes aluminium
At least one of powder, copper powder, aluminium oxide and aluminium nitride.
8. a kind of preparation method of the phase-change heat conductive material of low transformation temperature as described in claim 1 to 7 any one, its feature
It is, includes the following steps：
Heat up after low melt wax, basic long chain hydrocarbon resin, antioxidant and coupling agent are mixed, and stir and form paste；
Crosslinking agent is added into paste, continues stirring and forms cross-linking products；
Conductive particle is added into cross-linking products, vacuum defoamation processing is carried out after stirring, obtains the heat conduction with phase change material of low transformation temperature
Material.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109021932A (en) * | 2018-08-30 | 2018-12-18 | 桂林电子科技大学 | Graphene oxide/silver particles complex intensifying paraffin wax type phase-changing energy storage material and preparation method thereof |
| CN109337652A (en) * | 2018-10-23 | 2019-02-15 | 佛山科学技术学院 | A kind of window frame composite phase-change material composition |
| CN109517582A (en) * | 2018-10-23 | 2019-03-26 | 佛山科学技术学院 | A kind of retaining wall composite phase-change material composition |
| 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 |
| CN114716832A (en) * | 2022-04-26 | 2022-07-08 | 南京天诗新材料科技有限公司 | Low-shrinkage special wax material for electronic capacitor and preparation method thereof |
| WO2022183391A1 (en) * | 2021-03-03 | 2022-09-09 | Dow Global Technologies Llc | Curable polyolefin composition and cured product |
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| CN104650817A (en) * | 2015-02-12 | 2015-05-27 | 平湖阿莱德实业有限公司 | Heat conductive phase-change material and production method thereof |
| CN105348821A (en) * | 2015-11-06 | 2016-02-24 | 深圳德邦界面材料有限公司 | Phase change graphite heat conduction material with high thermal conductivity and preparation method |
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- 2017-12-07 CN CN201711290625.6A patent/CN108003558A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104650817A (en) * | 2015-02-12 | 2015-05-27 | 平湖阿莱德实业有限公司 | Heat conductive phase-change material and production method thereof |
| CN105348821A (en) * | 2015-11-06 | 2016-02-24 | 深圳德邦界面材料有限公司 | Phase change graphite heat conduction material with high thermal conductivity and preparation method |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109021932A (en) * | 2018-08-30 | 2018-12-18 | 桂林电子科技大学 | Graphene oxide/silver particles complex intensifying paraffin wax type phase-changing energy storage material and preparation method thereof |
| CN109337652A (en) * | 2018-10-23 | 2019-02-15 | 佛山科学技术学院 | A kind of window frame composite phase-change material composition |
| CN109517582A (en) * | 2018-10-23 | 2019-03-26 | 佛山科学技术学院 | A kind of retaining wall composite phase-change material composition |
| 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 |
| CN110317580B (en) * | 2019-07-18 | 2021-05-14 | 深圳前海量子翼纳米碳科技有限公司 | Insulating high latent heat phase change heat storage and absorption material |
| WO2022183391A1 (en) * | 2021-03-03 | 2022-09-09 | Dow Global Technologies Llc | Curable polyolefin composition and cured product |
| CN114716832A (en) * | 2022-04-26 | 2022-07-08 | 南京天诗新材料科技有限公司 | Low-shrinkage special wax material for electronic capacitor and preparation method thereof |
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