CN104140678B - Self-adhesive heat-conducting silicone grease and preparation method thereof - Google Patents
Self-adhesive heat-conducting silicone grease and preparation method thereof Download PDFInfo
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- CN104140678B CN104140678B CN201410305597.0A CN201410305597A CN104140678B CN 104140678 B CN104140678 B CN 104140678B CN 201410305597 A CN201410305597 A CN 201410305597A CN 104140678 B CN104140678 B CN 104140678B
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- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 55
- 239000004519 grease Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000853 adhesive Substances 0.000 title abstract 4
- 238000011049 filling Methods 0.000 claims abstract description 22
- 239000003054 catalyst Substances 0.000 claims abstract description 20
- 238000000227 grinding Methods 0.000 claims abstract description 14
- 239000003112 inhibitor Substances 0.000 claims abstract description 14
- 239000000084 colloidal system Substances 0.000 claims abstract description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 16
- 239000006210 lotion Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 12
- 238000009826 distribution Methods 0.000 claims description 11
- 229910052697 platinum Inorganic materials 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- 238000009472 formulation Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- JQZGUQIEPRIDMR-UHFFFAOYSA-N 3-methylbut-1-yn-1-ol Chemical group CC(C)C#CO JQZGUQIEPRIDMR-UHFFFAOYSA-N 0.000 claims description 3
- 229910017083 AlN Inorganic materials 0.000 claims description 3
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 3
- 229910052582 BN Inorganic materials 0.000 claims description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 238000009775 high-speed stirring Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 8
- 239000006185 dispersion Substances 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 abstract 2
- 238000010276 construction Methods 0.000 abstract 1
- 238000009792 diffusion process Methods 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 6
- 230000035939 shock Effects 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 238000000280 densification Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000004990 Smectic liquid crystal Substances 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006253 efflorescence Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Landscapes
- Lubricants (AREA)
- Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)
Abstract
The invention belongs to the field of heat-conducting silicone greases, and discloses self-adhesive heat-conducting silicone grease and a preparation method of the self-adhesive heat-conducting silicone grease. The heat-conducting silicone grease consists of the following components in parts by weight: 20-50 parts of a component A, 0.8-5 parts of a component B, 0.1-0.5 part of a catalyst, 60-120 parts of a heat-conducting filling material and 0.1-0.5 part of an inhibitor. The preparation method comprises the following steps: weighing the component A, the component B, the catalyst, the heat-conducting filling material and the inhibitor according to the weight parts of a formula, putting into a stirring kettle, and uniformly stirring at a high speed until flowing paste is obtained; then performing grinding and dispersion treatment on the flowing paste on a high-speed colloid grinder, and then slowly and finely grinding the paste on a three-roll grinder; finally performing vacuum pumping treatment to obtain the self-adhesive heat-conducting silicone grease. The heat-conducting silicone grease disclosed by the invention has high heat-conducting performance and good utilization and weather-resistant performance, and has the advantages of good self-adhesion, low diffusion rate, good rework performance, easiness in construction, and the like.
Description
Technical field
The invention belongs to heat-conducting silicone grease field, and in particular to a kind of heat-conducting silicone grease with tack and preparation method thereof.
Background technology
With the development of science and technology, electronic product is intended to densification, miniaturization and densification, components and parts on circuit board
Integrated level more and more higher, with the requirement to heat dispersion is also improved, thus have developed many heat dissipation technologys and radiating material
Material.
Heat-conducting silicone grease is commonly called as thermal grease, typically with organic silicone as primary raw material, adds heat-resisting, excellent thermal conductivity material
Organosilicon smectic compound made by material, can be used for the heat conduction of the electronic devices and components such as power amplifier, transistor, electron tube, CPU
And radiating, so as to the electric property for ensureing electronic instrument and meter etc. is stablized.
About the existing more report of development of heat-conducting silicone grease, also there are some products on sale on market, but generally existing one
A little shortcomings, the such as bi-component heat-conducting silicone grease crosslinking curing time is short, it is necessary to which extemporaneous preparation is used；One pack system heat-conducting silicone grease viscosity is low,
Diffusivity is big, there is trickling property, is susceptible to base-material and separates with heat filling, causes the efflorescence of heat-conducting silicone grease coating broken and thermal conductivity
It is deteriorated；And be then difficult to add the heat filling of high solids content using high-viscosity base-material, product heat conductivility is poor；Heat-conducting silicone grease is certainly
Viscosity is low, doing over again property is poor, is not easy to repeat to glue take maintenance.
The content of the invention
In order to overcome the shortcoming and deficiency of prior art, the primary and foremost purpose of the present invention is to provide a kind of with tack
Heat-conducting silicone grease, the heat-conducting silicone grease with tack has tack, and thermal conductivity is good, and diffusivity is low, will not flow automatically
Drop down；
Another object of the present invention is to provide the preparation method of the above-mentioned heat-conducting silicone grease with tack.
The purpose of the present invention is achieved through the following technical solutions：
A kind of heat-conducting silicone grease with tack, its composition of raw materials is made up of each component of following parts by weight：
Shown in the structural formula of said components A such as formula (I)：
In above-mentioned formula (I), m=250～280, n=3～5；
The structural formula of said components B is as shown in logical formula (II)：
In above-mentioned logical formula (II), p=10～15, q=20～30.
Preferably, the catalyst is platinum catalyst；It is furthermore preferred that the platinum catalyst is the catalysis of Karst platinum
Agent；
Preferably, the thermal conductivity value of the heat filling is 30～300W/mK, and particle diameter is 8～40um.
Preferably, the heat filling is aluminum oxide, titanium oxide, magnesia, zinc oxide, boron nitride, aluminium nitride or nitridation
One or more of silicon.
Preferably, the inhibitor is methyl butynol or vinyl ring body.
The preparation method of the above-mentioned heat-conducting silicone grease with tack, comprises the steps：Group is weighed by formulation weight part
A, component B, catalyst, heat filling and inhibitor is divided to be placed in stirred tank, high-speed stirred uniformly extremely obtains mobility lotion；Then
By gained mobility lotion, grinding distribution is processed on colloid mills, the slow finely ground mill on three-roll grinder；Finally carry out
Process is vacuumized, the heat-conducting silicone grease with tack is obtained.
Preferably, the speed of the high-speed stirred is 1000～5000rpm；
Preferably, the grinding distribution number of processing is 1～3 time；
Preferably, the number of times of the slow finely ground mill is 1～3 time；
Preferably, the vacuum for vacuumizing process is -0.095MPa.
The present invention has the following advantages and effect relative to prior art：Thermal conductive silicon with tack of the present invention
Fat, the screening and dosage optimization by each component in formula, products obtained therefrom has high-termal conductivity and good use weather resistance,
And have the advantages that tack is good, diffusivity is low, heavy industry good and it is easy to construct.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention not limited to this.
Embodiment 1
A kind of heat-conducting silicone grease with tack, its composition of raw materials is made up of each component of following parts by weight：
Shown in the structural formula of said components A such as formula (I)：
In above-mentioned formula (I), m=250, n=3；
The structural formula of component B is as shown in logical formula (II)：
In above-mentioned logical formula (II), p=10, q=30.
Wherein, the catalyst is Karst platinum catalyst；
The thermal conductivity value of the heat filling is 37W/mK, and particle diameter is 8～20nm；
The heat filling is aluminum oxide；
The inhibitor is methyl butynol.
The preparation method of the above-mentioned heat-conducting silicone grease with tack, comprises the steps：Group is weighed by formulation weight part
A, component B, catalyst, heat filling and inhibitor is divided to be placed in stirred tank, high-speed stirred uniformly extremely obtains mobility lotion；Then
By gained mobility lotion, grinding distribution is processed on colloid mills, the slow finely ground mill on three-roll grinder；Finally carry out
Process is vacuumized, the heat-conducting silicone grease with tack is obtained.
Wherein, the speed of the high-speed stirred is 1000rpm；
The grinding distribution number of processing is 1 time；
The number of times of the slow finely ground mill is 3 times；
The vacuum for vacuumizing process is -0.095Mpa.
Embodiment 2
A kind of heat-conducting silicone grease with tack, its composition of raw materials is made up of each component of following parts by weight：
Shown in the structural formula of said components A such as formula (I)：
In above-mentioned formula (I), m=260, n=4；
The structural formula of component B is as shown in logical formula (II)：
In above-mentioned logical formula (II), p=15, q=25.
Wherein, the catalyst is Karst platinum catalyst；
The thermal conductivity value of the heat filling is 125W/mK, and particle diameter is 8～20nm；
The heat filling is boron nitride；
The inhibitor is vinyl ring body.
The preparation method of the above-mentioned heat-conducting silicone grease with tack, comprises the steps：Group is weighed by formulation weight part
A, component B, catalyst, heat filling and inhibitor is divided to be placed in stirred tank, high-speed stirred uniformly extremely obtains mobility lotion；Then
By gained mobility lotion, grinding distribution is processed on colloid mills, the slow finely ground mill on three-roll grinder；Finally carry out
Process is vacuumized, the heat-conducting silicone grease with tack is obtained.
Wherein, the speed of the high-speed stirred is 5000rpm；
The grinding distribution number of processing is 2 times；
The number of times of the slow finely ground mill is 1 time；
The vacuum for vacuumizing process is -0.095Mpa.
Embodiment 3
A kind of heat-conducting silicone grease with tack, its composition of raw materials is made up of each component of following parts by weight：
Shown in the structural formula of said components A such as formula (I)：
In above-mentioned formula (I), m=280, n=5；
The structural formula of component B is as shown in logical formula (II)：
In above-mentioned logical formula (II), p=10, q=25.
Wherein, the catalyst is platinum catalyst；
The thermal conductivity value of the heat filling is 270W/mK, and particle diameter is 8～15um；
The heat filling is aluminium nitride；
The inhibitor is vinyl ring body.
The preparation method of the above-mentioned heat-conducting silicone grease with tack, comprises the steps：Group is weighed by formulation weight part
A, component B, catalyst, heat filling and inhibitor is divided to be placed in stirred tank, high-speed stirred uniformly extremely obtains mobility lotion；Then
By gained mobility lotion, grinding distribution is processed on colloid mills, the slow finely ground mill on three-roll grinder；Finally carry out
Process is vacuumized, the heat-conducting silicone grease with tack is obtained.
Wherein, the speed of the high-speed stirred is 2500rpm；
The grinding distribution number of processing is 3 times；
The number of times of the slow finely ground mill is 1 time；
The vacuum for vacuumizing process is -0.095Mpa.
Embodiment 4
A kind of heat-conducting silicone grease with tack, its composition of raw materials is made up of each component of following parts by weight：
Shown in the structural formula of said components A such as formula (I)：
In above-mentioned formula (I), m=260, n=4；
The structural formula of component B is as shown in logical formula (II)：
In above-mentioned logical formula (II), p=15, q=30.
Wherein, the catalyst is platinum catalyst；
The thermal conductivity value of the heat filling is 300W/mK, and particle diameter is 20～40um；
The heat filling is silicon nitride；
The inhibitor is vinyl ring body.
The preparation method of the above-mentioned heat-conducting silicone grease with tack, comprises the steps：Group is weighed by formulation weight part
A, component B, catalyst, heat filling and inhibitor is divided to be placed in stirred tank, high-speed stirred uniformly extremely obtains mobility lotion；Then
By gained mobility lotion, grinding distribution is processed on colloid mills, the slow finely ground mill on three-roll grinder；Finally carry out
Process is vacuumized, the heat-conducting silicone grease with tack is obtained.
Wherein, the speed of the high-speed stirred is 2800rpm；
The grinding distribution number of processing is 2 times；
The number of times of the slow finely ground mill is 2 times；
The vacuum for vacuumizing process is -0.095Mpa.
Performance test：
The heat-conducting silicone grease with tack of the gained of embodiment 1～4 is carried out into performance test, performance test is included in following
Hold：Viscosity, thermal conductivity, thermal resistance and heat resistance.
Viscosity：By the heat-conducting silicone grease rotation viscometer with tack of the gained of embodiment 1～4 under the rotating speed of 2rpm
Measurement viscosity, as a result as shown in table 1；
Thermal conductivity：The heat-conducting silicone grease with tack of the gained of embodiment 1～4 is applied to into the testboard of thermal conductivity tester
On face, THICKNESS CONTROL is 2mm, determines the heat conductivity value of viscosity silicone grease, as a result as shown in table 1；
Thermal resistance：The heat-conducting silicone grease with tack of the gained of embodiment 1～4 is applied on the testing stand of thermal resistance instrument,
THICKNESS CONTROL is 2mm, determines the heat conductivity value of viscosity silicone grease, as a result as shown in table 1；
Heat resistance：Heat resistance determination test includes degradation and cold shock testing.Degradation is to implement
The heat-conducting silicone grease with tack of the gained of example 1～4 is toasted 24 hours under 150 DEG C of high temperature；Cold shock testing is to implement
The heat-conducting silicone grease with tack of the gained of example 1～4 is circulated 100 times at -50 DEG C～120 DEG C.Degradation and thermal shock are tried
Test result as shown in table 1.
The heat-conducting silicone grease testing experiment result with tack of the present invention of table 1.
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Viscosity (Pas) | 254 | 320 | 300 | 335 |
| Thermal conductivity (W/mK) | 1.2 | 1.5 | 2.0 | 2.9 |
| Thermal resistance (mm2·K/W) | 1.67 | 1.33 | 1.0 | 1.0 |
| Aging rear thermal resistance (mm2·K/W) | 1.55 | 1.26 | 0.97 | 0.81 |
| Thermal resistance (mm after thermal shock2·K/W) | 1.47 | 1.18 | 0.95 | 0.79 |
As shown in Table 1, the heat conductivity of heat-conduction silicone grease with tack of the present invention is excellent, and conservation rate is good；And have
Good tack, repeatable gluing takes, convenient to install and keep in repair.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention not by above-described embodiment
Limit, other any Spirit Essences without departing from the present invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (8)
1. a kind of heat-conducting silicone grease with tack, it is characterised in that the composition of raw materials of the heat-conducting silicone grease with tack is
It is made up of each component of following parts by weight：
Shown in the structural formula of said components A such as formula (I)：
In above-mentioned formula (I), m=250～280, n=3～5；
The structural formula of said components B is as shown in logical formula (II)：
In above-mentioned logical formula (II), p=10～15, q=20～30；
The thermal conductivity value of the heat filling is 30～300W/mK, and particle diameter is 8～40um；
The heat filling be aluminum oxide, titanium oxide, magnesia, zinc oxide, boron nitride, aluminium nitride or silicon nitride in one kind with
On.
2. a kind of heat-conducting silicone grease with tack according to claim 1, it is characterised in that：The catalyst is urged for platinum
Agent.
3. a kind of heat-conducting silicone grease with tack according to claim 1, it is characterised in that：The inhibitor is methyl
Butynol or vinyl ring body.
4. the preparation method of the heat-conducting silicone grease with tack according to any one of claims 1 to 3, it is characterised in that bag
Include following steps：Component A, component B, catalyst, heat filling and inhibitor are weighed by formulation weight part to be placed in stirred tank, it is high
Speed is evenly stirred until to obtain mobility lotion；Then by gained mobility lotion, grinding distribution is processed on colloid mills, then at
Slow finely ground mill on three-roll grinder；Finally carry out vacuumizing process, obtain the heat-conducting silicone grease with tack.
5. the preparation method of the heat-conducting silicone grease with tack according to claim 4, it is characterised in that：The high-speed stirring
The speed mixed is 1000～5000rpm.
6. the preparation method of the heat-conducting silicone grease with tack according to claim 4, it is characterised in that：The grinding point
Scattered number of processing is 1～3 time.
7. the preparation method of the heat-conducting silicone grease with tack according to claim 4, it is characterised in that：It is described slow finely ground
The number of times of mill is 1～3 time.
8. the preparation method of the heat-conducting silicone grease with tack according to claim 4, it is characterised in that：It is described to vacuumize
The vacuum of process is -0.095MPa.
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| CN201410305597.0A CN104140678B (en) | 2014-06-29 | 2014-06-29 | Self-adhesive heat-conducting silicone grease and preparation method thereof |
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| CN201410305597.0A CN104140678B (en) | 2014-06-29 | 2014-06-29 | Self-adhesive heat-conducting silicone grease and preparation method thereof |
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| CN104140678B true CN104140678B (en) | 2017-04-12 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10155894B2 (en) | 2014-07-07 | 2018-12-18 | Honeywell International Inc. | Thermal interface material with ion scavenger |
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| KR20160094385A (en) | 2013-12-05 | 2016-08-09 | 허니웰 인터내셔날 인코포레이티드 | STANNOUS METHANSULFONATE SOLUTION WITH ADJUSTED pH |
| EP3227399B1 (en) | 2014-12-05 | 2021-07-14 | Honeywell International Inc. | High performance thermal interface materials with low thermal impedance |
| CN105315958A (en) * | 2015-10-28 | 2016-02-10 | 苏州天脉导热科技有限公司 | Addition heat-conducting self-adhesive silicone rubber and preparation method thereof |
| US10312177B2 (en) | 2015-11-17 | 2019-06-04 | Honeywell International Inc. | Thermal interface materials including a coloring agent |
| US10781349B2 (en) | 2016-03-08 | 2020-09-22 | Honeywell International Inc. | Thermal interface material including crosslinker and multiple fillers |
| US10501671B2 (en) | 2016-07-26 | 2019-12-10 | Honeywell International Inc. | Gel-type thermal interface material |
| CN106590550A (en) * | 2016-12-15 | 2017-04-26 | 深圳德邦界面材料有限公司 | Heat conduction silicone grease and preparation method thereof |
| US11041103B2 (en) | 2017-09-08 | 2021-06-22 | Honeywell International Inc. | Silicone-free thermal gel |
| US10428256B2 (en) | 2017-10-23 | 2019-10-01 | Honeywell International Inc. | Releasable thermal gel |
| US11072706B2 (en) | 2018-02-15 | 2021-07-27 | Honeywell International Inc. | Gel-type thermal interface material |
| US11373921B2 (en) | 2019-04-23 | 2022-06-28 | Honeywell International Inc. | Gel-type thermal interface material with low pre-curing viscosity and elastic properties post-curing |
| CN110724381A (en) * | 2019-09-25 | 2020-01-24 | 无锡易佳美电子科技有限公司 | Preparation method of heat conduction grease capable of preventing pumping in cold and hot impact environment |
| CN111849169B (en) * | 2020-07-14 | 2023-02-17 | 广东乐普泰新材料科技有限公司 | Heat-conducting silicone grease and preparation method thereof |
| CN113801640A (en) * | 2021-09-24 | 2021-12-17 | 合肥联宝信息技术有限公司 | Wave-absorbing heat-conducting shielding composition and preparation method thereof |
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| CN103571207A (en) * | 2012-07-22 | 2014-02-12 | 上海利隆化工化纤有限公司 | Heat-conductve silicone grease composition used for plasma display screens and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US10155894B2 (en) | 2014-07-07 | 2018-12-18 | Honeywell International Inc. | Thermal interface material with ion scavenger |
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