CN103122237A - Heat-conducting glue and preparation method thereof - Google Patents
Heat-conducting glue and preparation method thereof Download PDFInfo
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- CN103122237A CN103122237A CN2013100540151A CN201310054015A CN103122237A CN 103122237 A CN103122237 A CN 103122237A CN 2013100540151 A CN2013100540151 A CN 2013100540151A CN 201310054015 A CN201310054015 A CN 201310054015A CN 103122237 A CN103122237 A CN 103122237A
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Abstract
The invention discloses heat-conducting glue. The heat-conducting glue comprises the following main components in percentage by mass: 35%-55% of heat-conducting powder, 1.0%-4.5% of modifier and the adhesive, wherein the heat-conducting powder is nanoscale heat-conducting powder with the particle size less than or equal to 50nm, the adhesive is organic silica gel, and the modifier is a silane coupling agent. The invention also discloses a preparation method of the heat-conducting glue. The preparation method comprises the following steps of: firstly modifying the surfaces of the anoscale heat-conducting powder, and then filling the modified anoscale heat-conducting powder into an adhesive matrix. The heat-conducting glue prepared by the method has stable performance and high heat conductivity coefficients. Nano-powder is not adopted in a preparation process, so that the substantial increase of viscosity of the adhesive, which is caused by the introduction of lots of nano-powder, is avoided.
Description
Technical field
The present invention relates to the heat-conducting glue field, particularly relate to a kind of heat-conducting glue and preparation method.
Background technology
Along with more and more densification and the microminiaturization of assembling of unicircuit and microelectronic device, electronic component becomes less and moves with more speed, and its Working environment sharply changes to the high temperature direction.2 ℃ of the every risings of electronic devices and components temperature, its reliability decrease 10%, therefore in time heat radiation becomes the important factor that affects its work-ing life and use properties.Need in aerospace, electronics, the field such as electric to be applied to dispel the heat and the heat-conducting glue at heat transfer position, the amount of heat that can in time fall apart and produce except in the electronics use, all significant to its reliability of densification, miniaturization and raising, tightness and the work-ing life of electronic devices and components.
Heat-conducting glue mainly contains following several types: a kind of is to add the heat conduction powder with high thermal conductivity coefficient in the glue material, as ceramic powder, graphite composite powder or metal-powder, this heat-conducting glue, form restriction because of weighting agent, can only fill less ratio, and in use volatile small-molecule substance and mummification, so the thermal conductivity of this class heat-conducting glue is less; Another kind is the proportioning that improves content, purity and the particle shape of precious metal powder in the glue material, and the shortcoming of this class heat-conducting glue is expensive and unstable properties.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of heat-conducting glue and preparation method, and made heat-conducting glue stable performance thermal conductivity is high.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of heat-conducting glue is provided, its principal constituent according to mass percent is: 35% ~ 55%, properties-correcting agent 1.0% ~ 4.5%, all the other are glue paste, described heat conduction powder is that particle diameter is less than or equal to the nano level heat conduction powder of 50nm, described glue paste is the organic silica gel class, and described properties-correcting agent is silane coupling agent.
In a preferred embodiment of the present invention, described heat conduction powder is MgO, Ag, SiO
2In one or more mixing.
Another object of the present invention is to provide a kind of preparation method of heat-conducting glue, and concrete steps comprise:
(100), the surface modification of nano heat-conductive powder: take in proportion nano heat-conductive powder and properties-correcting agent, nano heat-conductive powder and properties-correcting agent are added in the first solvent mix, and adjusting pH value, after the suspension of gained disperses 50min with ultrasonic wave, put into the thermostat water bath heating, stir, in 75 ℃ of backflow 1.5h until powder all suspend, then with powder with deionized water wash, suction filtration, at last modified powder is put into the nano heat-conductive powder after modification that air dry oven dries standby;
(200), the nano heat-conductive powder is inserted glue paste: the nano heat-conductive powder and the glue paste that obtain in above-mentioned steps are proportionally taken, nano heat-conductive powder and glue paste are added in the second solution mix, ultrasonic wave is disperseed 0.5h after strong stirring 1h under room temperature, fully mix complete, vacuum is deviate from solvent and bubble, and final curing forms the heat-conducting glue finished product.
In a preferred embodiment of the present invention, the first solvent in described step (100) is the solvent that toluene and deionized water mix according to volume ratio 1:1.5.
In a preferred embodiment of the present invention, the nano heat-conductive powder in described step (100) after resulting modification also need adopt the acetone reflux to carry out soxhlet extraction and remove the properties-correcting agent that surface physics coats.
In a preferred embodiment of the present invention, in described step (200), the mode that the curing of heat-conducting glue adopts segmentation to solidify: 130 ℃ 1h+160 ℃ 4h+200 ℃ of 1.5h.
The invention has the beneficial effects as follows: heat-conducting glue of the present invention and preparation method, made heat-conducting glue stable performance thermal conductivity is high.In preparation process, adopt nano-powder, can not cause increasing considerably of tackiness agent viscosity because of a large amount of introducings of nano-powder.
Embodiment
The below is described in detail preferred embodiment of the present invention, thereby so that advantages and features of the invention can be easier to be it will be appreciated by those skilled in the art that, protection scope of the present invention is made more explicit defining.
Embodiment one:
Raw material: particle diameter is the MgO powder 100g of 30nm, silane coupling agent 3g, silica gel 150g
Preparation process: at first the MgO powder is placed in the dry 24h of vacuum drying oven of 120 ℃ with impurity such as the organism of removing powder preparation process surface adsorption, moisture; Then the MgO powder is carried out surface modification: the coupling agent of 100g powder and 3g, the solvent that 1000ml toluene and deionized water mix according to volume ratio 1:1.5, after again the suspension of gained being disperseed 50min with ultrasonic wave, put into the thermostat water bath heating, stir, in 75 ℃ of backflow 1.5h until powder all suspend, then with powder deionized water wash, suction filtration, at last modified powder is put into air dry oven and dry; Last above-mentioned modified powder carries out soxhlet extraction with the acetone reflux and removes the properties-correcting agent that surface physics coats, and vacuum-drying is standby.Then the nano-powder after modification is filled in the glue paste material: nano-powder and silica gel is solution blending in proportion, can add a small amount of suspension aids, and ultrasonic 0.5h is to guarantee the powder good dispersion after strong stirring 1h under room temperature.Fully mixing is complete, and the heat-conducting glue performed polymer is poured in the grinding tool of preheating in baking oven, and vacuum is deviate from solvent and bubble, and curing then heats up: 130 ℃ 1h+160 ℃ 4h+200 ℃ of 1.5h obtains finished product one.
Embodiment two:
Raw material: particle diameter is the MgO powder of 40nm and the mixed powder 100g of Ag powder, silane coupling agent 4g, silica gel 180g
Preparation process: at first mixed powder is placed in the dry 24h of vacuum drying oven of 120 ℃ with impurity such as the organism of removing powder preparation process surface adsorption, moisture; Then mixed powder is carried out surface modification: the coupling agent of 100g powder and 4g, the solvent that 1000ml toluene and deionized water mix according to volume ratio 1:1.5, after again the suspension of gained being disperseed 50min with ultrasonic wave, put into the thermostat water bath heating, stir, in 75 ℃ of backflow 1.5h until powder all suspend, then with powder deionized water wash, suction filtration, at last modified powder is put into air dry oven and dry; Last above-mentioned modified powder carries out soxhlet extraction with the acetone reflux and removes the properties-correcting agent that surface physics coats, and vacuum-drying is standby.Then the nano-powder after modification is filled in the glue paste material: nano-powder and silica gel is solution blending in proportion, can add a small amount of suspension aids, and ultrasonic 0.5h after strong stirring 1h under room temperature guarantees the powder good dispersion.Fully mixing is complete, and the heat-conducting glue performed polymer is poured in the grinding tool of preheating in baking oven, and vacuum is deviate from solvent and bubble, and curing then heats up: 130 ℃ 1h+160 ℃ 4h+200 ℃ of 1.5h obtains finished product two.
The nano heat-conductive powder has higher thermal conductivity, volume specific resistance and impelling strength through after modification; This is that the thermal resistance between particle and basal body interface descends because filler grain improves through after surface treatment and the interface between matrix, thermal conductivity improves.
Heat-conducting glue of the present invention and preparation method, made heat-conducting glue stable performance thermal conductivity is high, more than thermal conductivity reaches 36W/mK.In preparation process, adopt nano-powder, can not cause increasing considerably of tackiness agent viscosity because of a large amount of introducings of nano-powder.
The above is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or equivalent flow process conversion that utilizes description of the present invention to do; or directly or indirectly be used in other relevant technical fields, all in like manner be included in scope of patent protection of the present invention.
Claims (6)
1. heat-conducting glue, it is characterized in that, its principal constituent according to mass percent is: heat conduction powder 35% ~ 55%, properties-correcting agent 1.0% ~ 4.5%, all the other are glue paste, described heat conduction powder is that particle diameter is less than or equal to the nano level heat conduction powder of 50nm, described glue paste is the organic silica gel class, and described properties-correcting agent is silane coupling agent.
2. heat-conducting glue according to claim 1, is characterized in that, described heat conduction powder is MgO, Ag, SiO
2In one or more mixing.
3. the preparation method of described heat-conducting glue according to claim 1 and 2, is characterized in that, concrete steps comprise:
(100), the surface modification of nano heat-conductive powder: take in proportion nano heat-conductive powder and properties-correcting agent, nano heat-conductive powder and properties-correcting agent are added in the first solvent mix, after the suspension of gained disperses 50min with ultrasonic wave, heat, stir, in 75 ℃ of backflow 1.5h until powder all suspend, then with powder with deionized water wash, suction filtration, at last modified powder is put into loft drier and dries, the nano heat-conductive powder that obtains after modification is standby;
(200), the nano heat-conductive powder is inserted glue paste: the nano heat-conductive powder and the glue paste that obtain in above-mentioned steps are proportionally taken, nano heat-conductive powder and glue paste are added in the second solution mix, ultrasonic wave is disperseed 0.5h after strong stirring 1h under room temperature, fully mix complete, vacuum is deviate from solvent and bubble, and final curing forms the heat-conducting glue finished product.
4. the preparation method of heat-conducting glue according to claim 3, is characterized in that, the first solvent in described step (100) is the solvent that toluene and deionized water mix according to volume ratio 1:1.5.
5. the preparation method of heat-conducting glue according to claim 3, is characterized in that, the nano heat-conductive powder in described step (100) after resulting modification also need adopt the acetone reflux to carry out soxhlet extraction and remove the properties-correcting agent that surface physics coats.
6. the preparation method of heat-conducting glue according to claim 3, is characterized in that, in described step (200), and the mode that the curing of heat-conducting glue adopts segmentation to solidify: 130 ℃ 1h+160 ℃ 4h+200 ℃ of 1.5h.
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| CN2013100540151A CN103122237A (en) | 2013-02-20 | 2013-02-20 | Heat-conducting glue and preparation method thereof |
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| CN2013100540151A CN103122237A (en) | 2013-02-20 | 2013-02-20 | Heat-conducting glue and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104031601A (en) * | 2014-05-28 | 2014-09-10 | 浙江大学 | Insulative adhesive for preparing metallic and soft magnetic composite material and using method thereof |
| CN105778510A (en) * | 2016-05-09 | 2016-07-20 | 中国科学院合肥物质科学研究院 | Method for preparing thermally conductive composite material with directivity |
| CN107987748A (en) * | 2017-12-28 | 2018-05-04 | 张家港康得新光电材料有限公司 | The preparation method and applications of heat conduction pressure sensitive adhesive |
| CN108624280A (en) * | 2018-05-08 | 2018-10-09 | 中国工程物理研究院化工材料研究所 | A kind of preparation method of high-capacity optical fiber laser heat-conducting glue |
| CN112980360A (en) * | 2021-03-31 | 2021-06-18 | 上海西怡新材料科技有限公司 | Light diffusion function heat-conducting adhesive and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311238A (en) * | 2007-05-25 | 2008-11-26 | 上海橡胶制品研究所 | Light-coloured high temperature resistant organic silicone adhesive/sealant |
| CN102876282A (en) * | 2012-09-13 | 2013-01-16 | 上海大学 | Preparation method of transparent organic silica glue for encapsulating nano SiO2 modified COB-LEDs |
-
2013
- 2013-02-20 CN CN2013100540151A patent/CN103122237A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311238A (en) * | 2007-05-25 | 2008-11-26 | 上海橡胶制品研究所 | Light-coloured high temperature resistant organic silicone adhesive/sealant |
| CN102876282A (en) * | 2012-09-13 | 2013-01-16 | 上海大学 | Preparation method of transparent organic silica glue for encapsulating nano SiO2 modified COB-LEDs |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104031601A (en) * | 2014-05-28 | 2014-09-10 | 浙江大学 | Insulative adhesive for preparing metallic and soft magnetic composite material and using method thereof |
| CN105778510A (en) * | 2016-05-09 | 2016-07-20 | 中国科学院合肥物质科学研究院 | Method for preparing thermally conductive composite material with directivity |
| CN107987748A (en) * | 2017-12-28 | 2018-05-04 | 张家港康得新光电材料有限公司 | The preparation method and applications of heat conduction pressure sensitive adhesive |
| CN108624280A (en) * | 2018-05-08 | 2018-10-09 | 中国工程物理研究院化工材料研究所 | A kind of preparation method of high-capacity optical fiber laser heat-conducting glue |
| CN112980360A (en) * | 2021-03-31 | 2021-06-18 | 上海西怡新材料科技有限公司 | Light diffusion function heat-conducting adhesive and preparation method and application thereof |
| CN112980360B (en) * | 2021-03-31 | 2022-07-15 | 上海西怡新材料科技有限公司 | Light diffusion functional heat-conducting adhesive and preparation method and application thereof |
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Application publication date: 20130529 |