CN102876261A - Water-based silicon-acrylic heat-conducting composition, silicon-acrylic heat-conducting bonding sheet and preparation method of silicon-acrylic heat-conducting bonding sheet - Google Patents
Water-based silicon-acrylic heat-conducting composition, silicon-acrylic heat-conducting bonding sheet and preparation method of silicon-acrylic heat-conducting bonding sheet Download PDFInfo
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- CN102876261A CN102876261A CN2012103681551A CN201210368155A CN102876261A CN 102876261 A CN102876261 A CN 102876261A CN 2012103681551 A CN2012103681551 A CN 2012103681551A CN 201210368155 A CN201210368155 A CN 201210368155A CN 102876261 A CN102876261 A CN 102876261A
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Abstract
The invention belongs to the technical field of heat-conducting interface materials and discloses a water-based silicon-acrylic heat-conducting composition which comprises emulsion, heat-conducting inorganic powder and flame retardants, wherein the emulsion comprises carboxyl-containing silicon-acrylic emulsion, cyano-group-containing silicon-acrylic emulsion and epoxy-group-containing silicon-acrylic emulsion. Organic silicon is used for modifying acrylic acid, carboxylic, cyanophoric and epoxy silicon-acrylic polymers are compounded and mixed with the heat-conducting powder and flame-retardant powder, and immersional wetting of cyano-groups to an interface and facilitation of carboxyls on epoxy group open loop reaction are fully used, so that the heat-conducting composition excellent in high-and-low temperature performance, good in initial bonding and heat conduction and flame-retardant is obtained by means of mutual synergy. A silicon-acrylic heat-conducting bonding sheet prepared by the water-based silicon-acrylic heat-conducting composition has the advantages that the heat-conducting coefficient reaches 0.8W/(m.K), flame retardance reaches UL94V-0 level, initial bonding is good, the torque resistance is larger than 20kgf cm, breakdown voltage is larger than 25Kv/mm, and the temperature resistant range is 20-160 DEG C. Besides, the silicon-acrylic heat-conducting bonding sheet is low in curing temperature when bonding, and only 120 DEG C is needed.
Description
Technical field
The present invention relates to thermally conductive composition, heat conduction adhesive sheet of a kind of high adhesion and preparation method thereof, especially a kind of adopt the water-based organosilicon crylic acid latex as the thermally conductive composition of caking agent, use adhesive sheet that this thermally conductive composition makes and preparation method thereof.
Background technology
In fields such as industrial electronic, electrical equipment, communications, development trend along with raising, electron device high integration and the product High Density Packaging of circuit work frequency, heating in electron device and the circuit working is growing on and on, the rising of temperature is day by day serious on the impact of electronic product work, and the importance of heat management more and more highlights.It is calculated that, when electron device is worked between 70～80 ℃, 1 ℃ of the every rising of working temperature, device reliability just descends 5%, and the thermal diffusivity of power device is the problem of must emphasis considering in product reliability assessment.The convenience in the miniaturization of electron device and lightweight and when assembling requires also more and more highlyer on the other hand, more and more in the assembling of component adopts bonding form to substitute original fastened by screw.Therefore, the solid conductive heat adhesives utmost point that has excellent heat conductivity and structure bonding force concurrently is pursued, and this material also requires to have preferably resistant of high or low temperature, electric insulating quality and flame retardancy simultaneously, does not still have over-all properties all to satisfy the product that electronic industry requires at present.
Summary of the invention
The problem that exists in order to solve above-mentioned prior art, the invention provides a kind of water-based silicon the third thermally conductive composition, silicon the third heat conduction adhesive sheet that adopts said composition to make has good thermal conductivity and stronger structure bonding force, and high temperature performance is good, electric insulation intensity is high, fire-retardant.
The technical solution used in the present invention is: a kind of water-based silicon the third thermally conductive composition, it comprises emulsion, heat conduction inorganic powder and fire retardant, described emulsion comprise carboxylic organosilicon crylic acid latex, cyano-containing organosilicon crylic acid latex, contain the organosilicon crylic acid latex of epoxy group(ing).
Preferably, described emulsion also comprises tackifier emulsion, can improve being glued the initial bonding strength at interface.The preferred rosin based resin of tackifier obtains the oil-in-water-type tackifier emulsion with emulsification after its melting.
Preferably, also can add defoamer, flow agent in the described emulsion to improve processes.
Preferably, the monomer for preparing described carboxylic organosilicon crylic acid latex comprises methyl methacrylate (MMA), Isooctyl acrylate monomer (EHA), butyl acrylate (BA), hydroxyethyl methylacrylate (HEMA), vinylformic acid (AA), vinyltriethoxysilane (A-151) and Sodium styrene sulfonate (NaSS).Preferably, the content (weight) of vinylformic acid in the described monomer (AA) monomer is 4～6%, more preferably 5%, and this moment, Calcium ion stability, freeze-thaw stability, stability in storage, mechanical stability, the alkali resistance of emulsion were better, gel content is lower, can reach 0.15%.
Preferably, the monomer for preparing the organosilicon crylic acid latex of described cyano-containing comprises methyl methacrylate (MMA), Isooctyl acrylate monomer (EHA), butyl acrylate (BA), hydroxyethyl methylacrylate (HEMA), vinyl cyanide (AN), vinyltriethoxysilane (A-151) and Sodium styrene sulfonate (NaSS).Preferably, the content (weight) of vinyl cyanide in the described monomer (AN) monomer is 9～11%, more preferably 10%, and this moment, Calcium ion stability, freeze-thaw stability, stability in storage, mechanical stability, the alkali resistance of emulsion were better, gel content is lower, can reach 0.2%.
Preferably, the described monomer that contains the organosilicon crylic acid latex of epoxy group(ing) of preparation comprises methyl methacrylate (MMA), Isooctyl acrylate monomer (EHA), butyl acrylate (BA), hydroxyethyl methylacrylate (HEMA), glycidyl methacrylate (GMA), vinyltriethoxysilane (A-151) and Sodium styrene sulfonate (NaSS).Preferably, the content (weight) of glycidyl methacrylate in the described monomer (GMA) monomer is 4～6%, more preferably 5%, and this moment, Calcium ion stability, freeze-thaw stability, stability in storage, mechanical stability, the alkali resistance of emulsion were better, gel content is lower, can reach 0.2%.
Preferably, the above-mentioned silicone content (weight) that contains the organosilicon crylic acid latex of each functional group is 7～9%, more preferably 8%, make keep when can reach preferably heatproof, weathering resistance polyreaction steadily; Second-order transition temperature is preferably-45～-55 ℃, more preferably-50 ℃, can make tack and force of cohesion keep preferably balance.
Preferably, described heat conduction inorganic powder comprises the heat conduction powder of at least two kinds of particle diameters, and the tap density of heat conduction inorganic powder requires to be not less than 1.6g/cm
3, be preferably 1.6～3.0g/cm
3, 1.7～2.5g/cm more preferably
3The average particle size range of the selected powder of heat conduction inorganic powder is preferably 0.01～50 micron, more preferably 0.1～40 micron; The heat conduction inorganic powder is preferably chosen from following material: Al
2O
3, MgO, ZnO, Fe
2O
3, CaO, BeO, ZrO
2, TiO
2, SiO
2, AlN, Si
3N
4, ZrN, BN, SiC, BC, more preferably Al
2O
3, MgO, BeO, TiO
2, SiO
2, AlN, SiC; The better situation of heat conduction inorganic powder is to carry out pre-treatment before the adapted, the preferred method of pre-treatment be use coupling agent for example hexamethyldisilazane, methyltrimethoxy silane, vinyltrimethoxy silane, dimethyldimethoxysil,ne or 3-glycidoxy trimethoxy siloxane to the powder processing of spraying.
Preferably, described fire retardant is phosphorus-nitrogen containing flame retardant.More preferably ammonium polyphosphate, encapsulated red phosphorus, melamine cyanurate, tetramethylolmethane are (2.5～3.5) according to weight ratio: (0.5～1.5): (1.5～2.5): the compound of (0.5～1.5), for example ammonium polyphosphate by weight: encapsulated red phosphorus: melamine cyanurate: tetramethylolmethane is 3:1:2:1.
Preferably, the weight ratio of described emulsion, heat conduction inorganic powder and fire retardant is: (3～5): (4～6): (0.5～1.5), preferred ratio is 4:5:1.
The present invention also provides a kind of silicon the third heat conduction adhesive sheet, the heat conduction adhesive film that it comprises glasscloth and is compound in described glasscloth two sides, and described heat conduction adhesive film is made by above-mentioned water-based silicon the third thermally conductive composition drying slaking.
The preparation method of silicon the third heat conduction adhesive sheet of the present invention may further comprise the steps:
B1, employing emulsion polymerisation process prepare respectively the organosilicon crylic acid latex of carboxylic organosilicon crylic acid latex, cyano-containing and contain the organosilicon crylic acid latex of epoxy group(ing);
B2, emulsion is mixed with heat conduction inorganic powder, fire retardant and stir, grind through sand mill and make the heat conduction rubber cement;
B3, heat conduction rubber cement curtain coating on lining form is become heat conduction adhesive film and dry slaking, preferred dry slaking condition is 60～80 ℃, 5～20 minutes;
B4, glasscloth is placed between two heat conduction adhesive films that invest on the lining form compound through roll-in, heat conduction adhesive film and glasscloth are bonded together, obtain silicon the third heat conduction adhesive sheet.
The preferred soap-free polymerization of emulsion polymerisation process can reduce small-molecular emulsifier to the impact of product performance.Drip first acrylic acid or the like and functional monomer during polyreaction and drip again organosilane monomer after 1.5～2.5 hours, form organosilicon core-shell emulsion particle outside, can give full play to organosilyl modification advantage.
The technique effect that the present invention is useful: water-based silicon the third thermally conductive composition of the present invention, use organosilicon-modified acrylic, with carboxyl, cyano group, composite conductive powder, the fireproof powder of being mixed again of epoxy group(ing) siloxane-acrylate copolymer, take full advantage of cyano group to the immersional wetting at interface and the carboxyl promoter action to epoxy ring-opening, mutually work in coordination with and obtained the heat-conductive composite material that a kind of high temperature performance is good, bonding strength is high, thermal conductivity is good and fire-retardant, and employing water-based material, preparation and the discharging of application process VOC free meet the environmental protection theory.
Adopt the silicon third heat conduction adhesive sheet of this water-based silicon the third thermally conductive composition preparation, its thermal conductivity reaches 0.8W/ (m.K), the fire-retardant UL94 V-0 level that reaches, tack is good, twisting resistance is greater than 20kgfcm, and voltage breakdown is greater than 25kV/mm, and temperature resistant range is-20～160 ℃; And solidification value is low when bonding, only needs 120 ℃.
Preparation method's raw material of the present invention is easy to get, and technique is simple, and safety and environmental protection is convenient to industrialization.
Embodiment
Contain the preparation of the organosilicon crylic acid latex of function base
Being the A material with (methyl) acrylic monomer with after containing the monomer pre-emulsification of corresponding function group, will be that B expects after the organosilane monomer pre-emulsification.Reactive emulsifier, water adding are equipped with in the four-hole boiling flask of agitator, prolong, thermometer, be warming up to 75 ℃-90 ℃, add part initiator ammonium persulfate (APS) aqueous solution after temperature is recovered, begin to drip the A material, behind dropping 1～3h, beginning drips B material and remaining A material, the APS aqueous solution simultaneously, in 1.5-2h, drip off, be incubated approximately 1-3h, be cooled to room temperature, transfer PH to 7-7.5 with ammoniacal liquor, can obtain containing the organosilicon crylic acid latex of corresponding function base.
The preparation of tackifier emulsion
Adopt the rosin based resin (＜85 ℃) of low softening point to be heated to molten state, add emulsifying agent and water, the W/O contrary transfers O/W under 90 ℃ of rapid stirrings, namely gets the oil-in-water-type tackifier emulsion.
The preparation of heat conduction adhesive sheet
Required emulsion is mixed, add defoamer, flow agent, stir, add heat conduction inorganic powder, fire retardant, suitable quantity of water, high-speed stirring 1h crosses sand mill 30min, gets the heat conduction rubber cement;
The heat conduction rubber cement that the upper step was made is in the certain thickness heat conduction adhesive film of curtain coating on the BOPP film and dry slaking 5～20 minutes under 60～80 ℃, condition, glasscloth is placed on the middle roll-in of two films, glass and heat conduction adhesive film namely are bonded together, and obtain silicon the third heat conduction adhesive sheet.
Embodiment 1
Prepare carboxylic organosilicon crylic acid latex
Accurately take by weighing methyl methacrylate 29.15g, Isooctyl acrylate monomer 122.62g, butyl acrylate 65.88g, Hydroxyethyl acrylate 2.2g, vinylformic acid 11.15g, n-Hexadecane 2g, sodium lauryl sulphate 0.15g, water 60g carries out pre-emulsification, namely gets pre-emulsion A.
Accurately take by weighing vinyltriethoxysilane 25g, Arlacel-80 0.1g, sodium lauryl sulphate 0.1g, water 20g and carry out pre-emulsification, namely get pre-emulsion B.
Sodium styrene sulfonate 0.2g, water 160g are incorporated in the four-hole bottle of belt stirrer, prolong, thermometer, and high-speed stirring 20 minutes is warming up to 80 ℃, add the part APS aqueous solution after temperature is recovered, begin to drip part A material, when dropping to 1-3h, A material, the APS aqueous solution that beginning drips simultaneously the B material, is left, in 1.5-2h, drip off, be incubated approximately 1-3h, be cooled to room temperature, transfer PH to 7-7.5 with ammoniacal liquor, can obtain the 1# emulsion, the obvious blue light of milky white colour band, viscosity is 200cps.
Embodiment 2
The organosilicon crylic acid latex of preparation cyano-containing
Accurately take by weighing methyl methacrylate 20.15g, Isooctyl acrylate monomer 122.62g, butyl acrylate 65.88g, Hydroxyethyl acrylate 2.2g, vinyl cyanide 22.15g, n-Hexadecane 2g, sodium lauryl sulphate 0.15g, water 60g carries out pre-emulsification, namely gets pre-emulsion A.
Accurately take by weighing vinyltriethoxysilane 25g, Arlacel-80 0.1g, sodium lauryl sulphate 0.1g, water 20g and carry out pre-emulsification, namely get pre-emulsion B.
Sodium styrene sulfonate 0.2g, water 160g are incorporated in the four-hole bottle of belt stirrer, prolong, thermometer, and high-speed stirring 20 minutes is warming up to 80 ℃, add the part APS aqueous solution after temperature is recovered, begin to drip part A material, when dropping to 1-3h, A material, the APS aqueous solution that beginning drips simultaneously the B material, is left, in 1.5-2h, drip off, be incubated approximately 1-3h, be cooled to room temperature, transfer PH to 7-7.5 with ammoniacal liquor, can obtain the 2# emulsion, the obvious blue light of milky white colour band, viscosity is 130cps.
Embodiment 3
Preparation contains the organosilicon crylic acid latex of epoxy group(ing)
Accurately take by weighing methyl methacrylate 29.55g, Isooctyl acrylate monomer 122.62g, butyl acrylate 65.88g, Hydroxyethyl acrylate 2.2g, glycidyl methacrylate 11.75g, n-Hexadecane 2g, sodium lauryl sulphate 0.15g, water 60g carries out pre-emulsification, namely gets pre-emulsion A.
Accurately take by weighing vinyltriethoxysilane 25g, Arlacel-80,0.1g, sodium lauryl sulphate 0.1g, water 20g and carry out pre-emulsification, namely get pre-emulsion B.
Sodium styrene sulfonate 0.2g, water 160g are incorporated in the four-hole bottle of belt stirrer, prolong, thermometer, and high-speed stirring 20 minutes is warming up to 80 ℃, add the part APS aqueous solution after temperature is recovered, begin to drip part A material, when dropping to 1-3h, A material, the APS aqueous solution that beginning drips simultaneously the B material, is left, in 1.5-2h, drip off, be incubated approximately 1-3h, be cooled to room temperature, transfer PH to 7-7.5 with ammoniacal liquor, can obtain the 3# emulsion, the obvious blue light of milky white colour band, viscosity is 125cps.
Embodiment 4
The preparation tackifier emulsion
Take by weighing Gum Rosin 70g in the four-hole bottle of 250ml, be heated to 90 ℃ and reach molten state, take by weighing span-80 3.5g, water 126.5g stirring and dissolving gets emulsifier aqueous solution, under high-speed stirring, in the Gum Rosin of melting, slowly add the good emulsifier aqueous solution of dissolving, the aqueous solution transfers the O/W phase to by the W/O contrary, can obtain solid content and be 35% tackifying resin 4# emulsion.
Embodiment 5
Preparation heat conduction adhesive sheet
Take by weighing 1# emulsion 47.60g, 2# emulsion 47.60g, 3# emulsion 95.24g, 4# emulsion 9.52, defoamer 1.5g, flow agent 1g mix.Take by weighing conductive powder 250g, phosphorus nitrogen is that fireproof powder 50g, water 150g mix, and then slowly joins in the mixed emulsion that has mixed, high-speed stirring 1h crosses sand mill 30min, gets the heat conduction rubber cement.It is the heat conduction adhesive film of 0.06mm and in 70 ℃ of lower slaking drying treatment 10min that heat conduction rubber cement curtain coating on the BOPP film is become thickness, glasscloth is placed on the middle roll-in of two films, and glass and heat conduction adhesive film are bonded together, and obtain silicon the third heat conduction adhesive sheet.
Prepared silicon the third heat conduction adhesive sheet tack is good, and measuring thermal conductivity according to ASTM D5470 method is 0.8W/ (mK).Be used for metal-oxide-semiconductor and heat sink heat transfer of aluminum, 180 ℃ solidify 15min, are 25kgfcm with Japanese 40FTD2-S torsionmeter test twisting resistance, press the GBT1695-2005 method and measure breakdown voltage strength greater than 25kV/mm, reach the V-0 level by UL94 standard testing flame retardant resistance.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that implementation of the present invention is confined to these explanations.For the general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, can also make some simple deduction or replace, all should be considered as belonging to protection scope of the present invention.
Claims (10)
1. water-based silicon third thermally conductive composition, it comprises emulsion, heat conduction inorganic powder and fire retardant, described emulsion comprise carboxylic organosilicon crylic acid latex, cyano-containing organosilicon crylic acid latex, contain the organosilicon crylic acid latex of epoxy group(ing).
2. water-based silicon the third thermally conductive composition according to claim 1, it is characterized in that: described emulsion also comprises tackifier emulsion.
3. water-based silicon the third thermally conductive composition according to claim 1 and 2, it is characterized in that: the monomer for preparing described carboxylic organosilicon crylic acid latex comprises methyl methacrylate, Isooctyl acrylate monomer, butyl acrylate, hydroxyethyl methylacrylate, vinylformic acid, vinyltriethoxysilane and Sodium styrene sulfonate.
4. water-based silicon the third thermally conductive composition according to claim 1 and 2, it is characterized in that: the monomer for preparing the organosilicon crylic acid latex of described cyano-containing comprises methyl methacrylate, Isooctyl acrylate monomer, butyl acrylate, hydroxyethyl methylacrylate, vinyl cyanide, vinyltriethoxysilane and Sodium styrene sulfonate.
5. water-based silicon the third thermally conductive composition according to claim 1 and 2 is characterized in that: prepare the described monomer that contains the organosilicon crylic acid latex of epoxy group(ing) and comprise methyl methacrylate, Isooctyl acrylate monomer, butyl acrylate, hydroxyethyl methylacrylate, glycidyl methacrylate, vinyltriethoxysilane and Sodium styrene sulfonate.
6. water-based silicon the third thermally conductive composition according to claim 1 and 2, it is characterized in that: described heat conduction inorganic powder comprises the heat conduction powder of at least two kinds of particle diameters, and the tap density of described heat conduction inorganic powder is not less than 1.6g/cm
3
7. water-based silicon the third thermally conductive composition according to claim 1 and 2, it is characterized in that: described fire retardant is phosphorus-nitrogen containing flame retardant.
8. water-based silicon the third thermally conductive composition according to claim 1 and 2, it is characterized in that: the weight ratio of described emulsion, heat conduction inorganic powder and fire retardant is: (3～5): (4～6): (0.5～1.5).
9. silicon third heat conduction adhesive sheet, the heat conduction adhesive film that it comprises glasscloth and is compound in described glasscloth two sides, described heat conduction adhesive film is made by each described water-based silicon third thermally conductive composition drying slaking of claim 1～8.
10. the preparation method of silicon third a heat conduction adhesive sheet as claimed in claim 9 may further comprise the steps:
B1, employing emulsion polymerisation process prepare respectively the organosilicon crylic acid latex of carboxylic organosilicon crylic acid latex, cyano-containing and contain the organosilicon crylic acid latex of epoxy group(ing);
B2, emulsion is mixed with heat conduction inorganic powder, fire retardant and stir, grind through sand mill and make the heat conduction rubber cement;
B3, heat conduction rubber cement curtain coating on lining form is become heat conduction adhesive film and dry slaking;
B4, glasscloth is placed between two heat conduction adhesive films that invest on the lining form compound through roll-in, heat conduction adhesive film and glasscloth are bonded together, obtain silicon the third heat conduction adhesive sheet.
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| CN104356978A (en) * | 2014-12-03 | 2015-02-18 | 张亦彬 | Preparation method of adhesive |
| CN104629375A (en) * | 2015-02-11 | 2015-05-20 | 深圳市安品有机硅材料有限公司 | Ceramizable fireproof fire-resistant silicone rubber |
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| CN101423734A (en) * | 2008-12-05 | 2009-05-06 | 武汉科技学院 | Method for preparing organosilicon modified acrylic ester binding agent |
| CN101671523A (en) * | 2009-10-01 | 2010-03-17 | 厦门大学 | Aqueous flame-retardant and thermal-insulated coating and preparation method thereof |
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| JP2006117783A (en) * | 2004-10-21 | 2006-05-11 | Hokuetsu Paper Mills Ltd | Removable pressure-sensitive recording paper sheet |
| CN101423734A (en) * | 2008-12-05 | 2009-05-06 | 武汉科技学院 | Method for preparing organosilicon modified acrylic ester binding agent |
| CN101671523A (en) * | 2009-10-01 | 2010-03-17 | 厦门大学 | Aqueous flame-retardant and thermal-insulated coating and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104356978A (en) * | 2014-12-03 | 2015-02-18 | 张亦彬 | Preparation method of adhesive |
| CN104356978B (en) * | 2014-12-03 | 2015-08-12 | 张亦彬 | A kind of preparation method of binding agent |
| CN104629375A (en) * | 2015-02-11 | 2015-05-20 | 深圳市安品有机硅材料有限公司 | Ceramizable fireproof fire-resistant silicone rubber |
| CN104629375B (en) * | 2015-02-11 | 2017-05-10 | 深圳市安品有机硅材料有限公司 | Ceramizable fireproof fire-resistant silicone rubber |
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