CN102876261B - 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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- CN102876261B CN102876261B CN201210368155.1A CN201210368155A CN102876261B CN 102876261 B CN102876261 B CN 102876261B CN 201210368155 A CN201210368155 A CN 201210368155A CN 102876261 B CN102876261 B CN 102876261B
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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 water-based organosilicon crylic acid latex as the thermally conductive composition of caking agent, apply 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 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.According to calculating, when electron device is worked between 70～80 ℃, 1 ℃ of the every rising of working temperature, the reliability of device just declines 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 good resistant of high or low temperature, electric insulating quality and flame retardancy simultaneously, does not still have over-all properties all to meet the product that electronic industry requires at present.
Summary of the invention
The problem existing 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, and it comprises emulsion, heat conduction inorganic powder and fire retardant, described emulsion comprises the organosilicon crylic acid latex of carboxylic organosilicon crylic acid latex, cyano-containing, containing 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 oil-in-water-type tackifier emulsion by emulsification after its melting.
Preferably, in described emulsion, also can add defoamer, flow agent to improve processes.
Preferably, the monomer of 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 described monomer (AA) monomer is 4～6%, more preferably 5%, and now the Calcium ion stability of emulsion, freeze-thaw stability, stability in storage, mechanical stability, alkali resistance are better, gel content is lower, can reach 0.15%.
Preferably, the monomer of 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 described monomer (AN) monomer is 9～11%, more preferably 10%, and now the Calcium ion stability of emulsion, freeze-thaw stability, stability in storage, mechanical stability, alkali resistance are better, gel content is lower, can reach 0.2%.
Preferably, the monomer of the described organosilicon crylic acid latex containing 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 described monomer (GMA) monomer is 4～6%, more preferably 5%, and now the Calcium ion stability of emulsion, freeze-thaw stability, stability in storage, mechanical stability, alkali resistance are better, gel content is lower, can reach 0.2%.
Preferably, the silicone content (weight) of the above-mentioned organosilicon crylic acid latex containing each functional group is 7～9%, more preferably 8%, when making to reach good heatproof, weathering resistance, keep polyreaction steadily; Second-order transition temperature is preferably-45～-55 ℃, more preferably-50 ℃, can make tack and force of cohesion keep good 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
3; The 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; 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; Heat conduction inorganic powder preferably situation is before adapted, to carry out pre-treatment, 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, comprises the following steps:
B1, employing emulsion polymerisation process are prepared respectively the organosilicon crylic acid latex of carboxylic organosilicon crylic acid latex, cyano-containing and are contained the organosilicon crylic acid latex of epoxy group(ing);
B2, emulsion mixed and stirred with heat conduction inorganic powder, fire retardant, through sand mill, grinding and make heat conduction rubber cement;
B3, heat conduction rubber cement curtain coating on lining form is become to heat conduction adhesive film dry slaking, preferably dry slaking condition is 60～80 ℃, 5～20 minutes;
B4, glasscloth is placed between two heat conduction adhesive films that invest on 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 the impact of small-molecular emulsifier on product performance.During polyreaction, first drip acrylic acid or the like and functional monomer and after 1.5～2.5 hours, drip again organosilane monomer, 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, with organosilicon-modified acrylic, by carboxyl, cyano group, composite conductive powder, the fireproof powder of being mixed again of epoxy group(ing) siloxane-acrylate copolymer, make full use of cyano group to the immersional wetting at interface and carboxyl the 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 discharge of application process VOC free, meet environmental protection theory.
Silicon the third heat conduction adhesive sheet that adopts this water-based silicon third thermally conductive composition to prepare, 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
By (methyl) acrylic monomer with containing being A material after the monomer pre-emulsification of corresponding function group, will after organosilane monomer pre-emulsification, be B material.Reactive emulsifier, water are added in the four-hole boiling flask that agitator, prolong, thermometer are housed, be warming up to 75 ℃-90 ℃, add part initiator ammonium persulfate (APS) aqueous solution after temperature is recovered, start to drip A material, drip after 1～3h, start to drip B material and remaining A material, the APS aqueous solution simultaneously, in 1.5-2h, drip off, be incubated about 1-3h, be cooled to room temperature, with ammoniacal liquor, adjust PH to 7-7.5, can obtain the organosilicon crylic acid latex containing corresponding function base.
the preparation of tackifier emulsion
Adopt the rosin based resin (85 ℃ of <) of low softening point to be heated to molten state, add emulsifying agent and water, under 90 ℃ of rapid stirrings, W/O contrary transfers O/W to, obtains 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, obtains heat conduction rubber cement;
The certain thickness heat conduction adhesive film of the heat conduction rubber cement that upper step is made curtain coating on BOPP film dry slaking 5～20 minutes under 60～80 ℃, condition, glasscloth is placed on to the middle roll-in of two films, glass and heat conduction adhesive film are bonded together, and obtain silicon the third heat conduction adhesive sheet.
embodiment 1
prepare carboxylic organosilicon crylic acid latex
Accurately take 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, obtains pre-emulsion A.
Accurately take vinyltriethoxysilane 25g, Arlacel-80 0.1g, sodium lauryl sulphate 0.1g, water 20g and carry out pre-emulsification, obtain 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, start to drip part A material, while dropping to 1-3h, start to drip B material, remaining A material, the APS aqueous solution simultaneously, in 1.5-2h, drip off, be incubated about 1-3h, be cooled to room temperature, with ammoniacal liquor, adjust PH to 7-7.5, can obtain 1# emulsion, the obvious blue light of milky white colour band, viscosity is 200cps.
embodiment 2
the organosilicon crylic acid latex of preparing cyano-containing
Accurately take 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, obtains pre-emulsion A.
Accurately take vinyltriethoxysilane 25g, Arlacel-80 0.1g, sodium lauryl sulphate 0.1g, water 20g and carry out pre-emulsification, obtain 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, start to drip part A material, while dropping to 1-3h, start to drip B material, remaining A material, the APS aqueous solution simultaneously, in 1.5-2h, drip off, be incubated about 1-3h, be cooled to room temperature, with ammoniacal liquor, adjust PH to 7-7.5, can obtain 2# emulsion, the obvious blue light of milky white colour band, viscosity is 130cps.
embodiment 3
preparation is containing the organosilicon crylic acid latex of epoxy group(ing)
Accurately take 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, obtains pre-emulsion A.
Accurately take vinyltriethoxysilane 25g, Arlacel-80,0.1g, sodium lauryl sulphate 0.1g, water 20g and carry out pre-emulsification, obtain 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, start to drip part A material, while dropping to 1-3h, start to drip B material, remaining A material, the APS aqueous solution simultaneously, in 1.5-2h, drip off, be incubated about 1-3h, be cooled to room temperature, with ammoniacal liquor, adjust PH to 7-7.5, can obtain 3# emulsion, the obvious blue light of milky white colour band, viscosity is 125cps.
embodiment 4
preparation tackifier emulsion
Take Gum Rosin 70g in the four-hole bottle of 250ml, be heated to 90 ℃ and reach molten state, take span-80 3.5g, water 126.5g stirring and dissolving obtains emulsifier aqueous solution, under high-speed stirring, in the Gum Rosin of melting, slowly add the emulsifier aqueous solution having dissolved, the aqueous solution transfers O/W phase to by W/O contrary, can obtain solid content and be 35% tackifying resin 4# emulsion.
embodiment 5
preparation heat conduction adhesive sheet
Take 1# emulsion 47.60g, 2# emulsion 47.60g, 3# emulsion 95.24g, 4# emulsion 9.52, defoamer 1.5g, flow agent 1g are uniformly mixed.Take conductive powder 250g, phosphorus nitrogen is that fireproof powder 50g, water 150g are uniformly mixed, and then slowly joins in the mixed emulsion having mixed, high-speed stirring 1h, crosses sand mill 30min, obtains heat conduction rubber cement.By heat conduction rubber cement curtain coating on BOPP film become thickness be the heat conduction adhesive film of 0.06mm and at 70 ℃ slaking drying treatment 10min, glasscloth is placed on to the middle roll-in of two films, 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 according to ASTM D5470 method, measuring thermal conductivity is 0.8W/ (mK).For metal-oxide-semiconductor and heat sink heat transfer of aluminum, 180 ℃ of curing 15min, are 25kgfcm with Japanese 40FTD2-S torsionmeter test twisting resistance, measure breakdown voltage strength be greater than 25kV/mm by GBT1695-2005 method, by UL94 standard testing flame retardant resistance, reach V-0 level.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For 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 (6)
1. water-based silicon third thermally conductive composition, it comprises emulsion, heat conduction inorganic powder and fire retardant, described emulsion comprises carboxylic organosilicon crylic acid latex, the organosilicon crylic acid latex of cyano-containing, containing the organosilicon crylic acid latex of epoxy group(ing), the monomer of preparing described carboxylic organosilicon crylic acid latex comprises methyl methacrylate, Isooctyl acrylate monomer, butyl acrylate, hydroxyethyl methylacrylate, vinylformic acid, vinyltriethoxysilane and Sodium styrene sulfonate, the monomer of 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, the monomer of the described organosilicon crylic acid latex containing epoxy group(ing) of preparation comprises methyl methacrylate, Isooctyl acrylate monomer, butyl acrylate, hydroxyethyl methylacrylate, glycidyl methacrylate, vinyltriethoxysilane and Sodium styrene sulfonate, described emulsion, the weight ratio of heat conduction inorganic powder and fire retardant is: (3～5): (4～6): (0.5～1.5).
2. water-based silicon the third thermally conductive composition according to claim 1, 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, 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.
4. water-based silicon the third thermally conductive composition according to claim 1 and 2, is characterized in that: described fire retardant is phosphorus-nitrogen containing flame retardant.
5. a 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 water-based silicon the third thermally conductive composition drying slaking described in claim 1～4 any one.
6. a preparation method for silicon the third heat conduction adhesive sheet as claimed in claim 5, comprises the following steps:
B1, employing emulsion polymerisation process are prepared respectively the organosilicon crylic acid latex of carboxylic organosilicon crylic acid latex, cyano-containing and are contained the organosilicon crylic acid latex of epoxy group(ing);
B2, emulsion mixed and stirred with heat conduction inorganic powder, fire retardant, through sand mill, grinding and make heat conduction rubber cement;
B3, heat conduction rubber cement curtain coating on lining form is become to heat conduction adhesive film dry slaking;
B4, glasscloth is placed between two heat conduction adhesive films that invest on 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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