CN102952403A - Additive organosilicon heat-conducting electronic potting adhesive and manufacturing method thereof - Google Patents
Additive organosilicon heat-conducting electronic potting adhesive and manufacturing method thereof Download PDFInfo
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- CN102952403A CN102952403A CN2011102531957A CN201110253195A CN102952403A CN 102952403 A CN102952403 A CN 102952403A CN 2011102531957 A CN2011102531957 A CN 2011102531957A CN 201110253195 A CN201110253195 A CN 201110253195A CN 102952403 A CN102952403 A CN 102952403A
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Abstract
The invention relates to an additive organosilicon heat-conducting electronic potting adhesive and a preparation method thereof. The preparation method comprises the following steps: adding 100 parts of alpha,omega-divinylpolydimethylsiloxane, 0-20 parts of filler and 120-360 parts of special heat-conducting filler into a kneader, dehydrating at 100-180 DEG C under the vacuum degree of -0.06 to -0.1 MPa for 1-4 hours, and cooling to obtain a base material; adding 100 parts of base material, 10-30 parts of alpha,omega-divinylpolydimethylsiloxane and 0.01-2 parts of catalyst into a planetary stirring machine at room temperature, and stirring under the vacuum degree of -0.06 to -0.1 MPa at the stirring speed of 50-100rpm for 10-30 minutes to obtain a component A; and adding 100 parts of base material, 5-20 parts of crosslinking agent and 0.1-3 parts of silane coupling agent into a planetary stirring machine at room temperature, and stirring under the vacuum degree of -0.06 to -0.1 MPa at the stirring speed of 50-100rpm for 10-30 minutes to obtain a component B. The components A and B constitute the heat-conducting organosilicon potting adhesive which has the advantages of no pollution for the substrate, excellent heat conductivity, high storage stability and excellent operability, wherein the heat conductivity coefficient is 1.0, and the fire-protection grade is up to FV-0. The heat-conducting filler compounded by different particle sizes can effectively improve the addition proportion, the storage stability of the finished product and the flowability of the product in use.
Description
One, technical field
The present invention relates to a kind of additional organosilicon heat conductive electronic pouring sealant and manufacture method thereof, especially use additional organosilicon heat conductive electronic pouring sealant and manufacture method thereof through composite heat conductive filler.
Two, background technology
Organic silica gel has excellent ageing resistance, physics inertia, electric property, water proof and dust proof etc., can vulcanize at normal temperatures and pressures (the energy accelerated cure speed of heating), development is swift and violent after last century, imported Chinese market the eighties into, product application extensively, consumption increases sharply, and is widely used in the industries such as building, automobile, electric, mechanical, chemical industry, food.
Addition-type silicon rubber can keep elasticity at 60～200 ℃ long-term, do not absorb heat during curing, not heat release, do not shrink after the curing, have good electrical property and chemical stability, water-fast, the anti-ozone of energy, weather-resistant, behind its embedding electronic product, can play protection against the tide, protection against corrosion, shockproof, dustproof effect, stable electrical sub-element parameter.Though common silicon rubber has certain thermal conductivity, thermal conductivity relatively poor (about about 0.2).
Along with emerging energy-conservation new forms of energy product such as electronic product especially LED, sun power etc. to high-power future development; be accompanied by the increase of electronic devices and components thermal value in the auxiliary; urgent need is transmitted the heat of its generation to the external world; in order to avoid burn out electronic devices and components because of the accumulation of heat; these auxiliaries directly contact atmospheric environment simultaneously; constantly accept hot and cold, dried, wet replacing; need to have and organic silica gel moistureproof, dustproof, oil-stain-preventing to be protected by its embedding; thereby prolong its work-ing life, make it to conform to the characteristics of the long lifetime green energy conservation of LED, sun power.
The heat conductivility that affects silica gel is not only relevant with the thermal conductivity of thermally conductive material own, and contacts with size distribution, form, the interface of heat conductive filler, and intramolecular combination degree etc. are closely related.Existing heat conductive filler kind is more, such as Al
2O
3, SiO
2, BN, AlN, ZnO, SiC, B
2O
3(poisonous) etc.Select the filler of high thermal conductivity coefficient, consider filler forms the heat conduction network chain in silicon rubber complexity, be conducive to improve the thermal conductivity of silicon rubber.Nano level heat conductive filler can increase by 10 times than the thermal conductivity of conventional heat conductive filler, but price also rises more than 10 times simultaneously.Condensation considers the heat conductivility, add-on of filler to use properties, raw materials cost, the production environmental requirement of product, the present invention adopts the inorganic heat conductive filler that mixes type, in the situation that suitable proportion adds, has higher heat conductivility, the flowability that is suitable for using, the production cost that qualified electrical property and client are easy to accept, the large-scale promotion application of suitable existing market.
Three, summary of the invention
The purpose of this invention is to provide a kind of additional organosilicon heat conductive electronic pouring sealant and preparation method thereof.Be characterized in adopting α, ω-divinyl polydimethylsiloxane is base-material, mix the inorganic heat conductive filler of type as thermally conductive material, an amount of mineral filler is as the mechanical property activator, with an amount of linking agent, coupling agent, and catalyzer, be mixed with respectively A, B component, obtain the electronics heat conduction joint sealant of, excellent thermal conductivity pollution-free to base material, water proof and dust proof through (or room temperature) sulfuration addition reaction of heating.The use that mixes the inorganic heat conductive filler of type reaches in the situation of thermal conductivity more than 1.0 product, and the shrinking percentage after the storage of joint sealant, viscosity and mobile and the sulfuration is all improved greatly.
Technical scheme provided by the invention is:
1, two-pack is heated, and (room temperature) vulcanized, the electronics heat conduction organosilicon filling and sealing gum, and the starting material and the parts by weight that comprise are:
The A component
The B component
Wherein:
α, ω-divinyl polydimethylsiloxane structural formula is
N=50 in the formula～2000, R is-CH
3,-CH
2CH
3
2, additional organosilicon heat conductive electronic pouring sealant according to claim 1, the described mineral filler of its feature are a kind of in calcium carbonate superfine powder, active nano calcium, superfine silicon dioxide powder, silica powder, ultrafine kaolin, titanium dioxide, the aluminium hydroxide.
3, additional organosilicon heat conductive electronic pouring sealant according to claim 1 is characterized in that described heat conductive filler is at least a in aluminum oxide, nano aluminium oxide, silicon-dioxide, aluminium nitride, nano aluminum nitride, boron nitride, nm-class boron nitride, the silicon carbide.
4, additional organosilicon heat conductive electronic pouring sealant according to claim 1 is characterized in that described catalyzer is platinum catalyst.
5, additional organosilicon heat conductive electronic pouring sealant according to claim 1 is characterized in that described linking agent is containing hydrogen silicone oil at least a of methyl blocking of end hydrogen silicone oil, the low polymerization degree of low polymerization degree.
6, additional organosilicon heat conductive electronic pouring sealant according to claim 1 is characterized in that described coupling agent is vinyltrimethoxy silane, glycidoxy-propyltrimethoxy silane, contains polysiloxane at least a of epoxy group(ing).
7, the manufacture method of the sub-joint sealant of additional organosilicon heat conduction electrical network the steps include:
(1) with α, 120～360 parts of 100 parts of ω-divinyl polydimethylsiloxane, 0～20 part of filler, heat conductive filler join in the kneader, 100～180 ℃, vacuum tightness-0.06～-dewatered 1～4 hour under the 0.1MPa, make base-material after the cooling for subsequent use;
(2) at room temperature, with 100 parts of base-materials, α, in 10～30 parts of ω-divinyl polydimethylsiloxane, 0.01～2 part of adding of the catalyzer planetary mixer, maintenance vacuum tightness-0.06～-0.1MPa, stirring velocity is 50～100rpm, stirs 10～30 minutes, makes the A component;
(3) at room temperature, in 100 parts of base-materials, 5～20 parts of linking agents, 0.1～3 part of adding of silane coupling agent planetary mixer, maintenance vacuum tightness-0.06～-0.1MPa, stirring velocity is 50～100rpm, stirs 10～30 minutes, makes the B component;
(4) this A, B component are the additional organosilicon heat conductive electronic pouring sealant, during use this A, B component are mixed use by weight 1: 1 ratio.
Advantage of the present invention is:
1) product adopts different-grain diameter, the difform inorganic heat conductive filler that mixes, have advantages of nontoxic, easily purchase without burn into environmentally safe, raw material.
2) in the situation of equal result of use, but the first mate increases the add-on of heat conductive filler, thereby heat-conducting effect is significantly improved.
3) product preparation method is simple, and production unit does not need to increase separately, thereby greatly improves the production efficiency of product, and product system is close with company's currently available products, produces without the three wastes in the production.
4) product is easy to use, weather, temp. variation resistant performance excellence, and the Applicable temperature scope is wide; the fire prevention thermal conductivity is good; because reactionless deposits yields in the sulfidation, to the base material of electronic product without corrosion, protection electronics unit's equipment and the performance of electronic equipment had no adverse effect.
Four, embodiment
Characteristics of the present invention are with α, and ω-divinyl polydimethylsiloxane adopts to mix the inorganic heat conductive filler of type, make, thermal conductivity pollution-free to base material, the excellent additional organosilicon heat conductive electronic pouring sealant of storge quality.
Two-pack is heated, and (room temperature) vulcanized, electronics fire prevention organic silicon potting adhesive, and the starting material and the parts by weight that comprise are:
The A component
The B component
The manufacture method of additional organosilicon heat conductive electronic pouring sealant the steps include:
(1) with α, 120～360 parts of 100 parts of ω-divinyl polydimethylsiloxane, 0～20 part of filler, heat conductive filler join in the kneader, 100～180 ℃, vacuum tightness-0.06～-dewatered 1～4 hour under the 0.1MPa, make base-material after the cooling;
(2) at room temperature, with 100 parts of base-materials, α, in 10～30 parts of ω-divinyl polydimethylsiloxane, 0.01～2 part of adding of the catalyzer planetary mixer, maintenance vacuum tightness-0.06～-0.1MPa, stirring velocity is 50～100rpm, stirs 10～30 minutes, makes the A component;
(3) at room temperature, in 100 parts of base-materials, 5～20 parts of linking agents, 0.1～3 part of adding of silane coupling agent planetary mixer, maintenance vacuum tightness-0.06～-0.1MPa, stirring velocity is 50～100rpm, stirs 10～30 minutes, makes the B component;
(4) this A, B component are the additional organosilicon heat conductive electronic pouring sealant, during use this A, B component are mixed use by weight 1: 1 ratio.
Need to prove: above-described α, ω-divinyl polydimethylsiloxane, mineral filler, heat conductive filler, linking agent, silane coupling agent, the equal buyable of catalyzer obtain; Described kneader, planetary mixer and other utility appliance are existing conventional equipment.
Below by embodiment the present invention is carried out concrete description, be necessary to be pointed out that at this following examples only for the present invention is described in detail, can not be interpreted as the restriction to protection scope of the present invention.In each embodiment, except indicating especially, the equal buyable of raw materials obtains.
Embodiment 1:
Viscosity is the α of 500mPas viscosity during with 25 ± 2 ℃, and 100 parts of ω-divinyl polydimethylsiloxane, are put into kneader and mediated 3 hours under 180 ℃ of temperature, vacuum tightness-0.08MPa 120 parts of ball-aluminium oxides, after the cooling base-material.At room temperature, with 100 parts of base-materials, α, in 10 parts of ω-divinyl polydimethylsiloxane, 0.2 part of adding of the platinum catalyst planetary mixer, keep vacuum tightness-0.08MPa, stirring velocity is 70rpm, stirs 20 minutes, makes the A component; At room temperature, in 100 parts of base-materials, 8 parts of containing hydrogen silicone oils of end, 2 parts of addings of vinyltrimethoxy silane planetary mixer, keep vacuum tightness-0.08MPa, stirring velocity is 70rpm, stirs 20 minutes, makes the B component.The product performance test result is shown in Table 1.
Embodiment 2:
Viscosity is the α of 500mPas viscosity during with 25 ± 2 ℃, and 100 parts of ω-divinyl polydimethylsiloxane, are put into kneader and mediated 3 hours under 180 ℃ of temperature, vacuum tightness-0.08MPa 120 parts of boron nitride, after the cooling base-material.At room temperature, with 100 parts of base-materials, α, in 10 parts of ω-divinyl polydimethylsiloxane, 0.2 part of adding of the platinum catalyst planetary mixer, keep vacuum tightness-0.08MPa, stirring velocity is 70rpm, stirs 20 minutes, makes the A component; At room temperature, in 100 parts of base-materials, 8 parts of end containing hydrogen silicone oil linking agents, 2 parts of addings of vinyltrimethoxy silane coupling agent planetary mixer, keep vacuum tightness-0.08MPa, stirring velocity is 70rpm, stirs 20 minutes, makes the B component.The product performance test result is shown in Table 1.
Embodiment 3:
Viscosity is the α of 500mPas viscosity during with 25 ± 2 ℃, and 100 parts of ω-divinyl polydimethylsiloxane, are put into kneader and mediated 3 hours under 180 ℃ of temperature, vacuum tightness-0.08MPa 120 parts of aluminium nitride, after the cooling base-material.At room temperature, with 100 parts of base-materials, α, in 10 parts of ω-divinyl polydimethylsiloxane, 0.2 part of adding of the platinum catalyst planetary mixer, keep vacuum tightness-0.08MPa, stirring velocity is 70rpm, stirs 20 minutes, makes the A component; At room temperature, in 100 parts of base-materials, 8 parts of containing hydrogen silicone oils of end, 2 parts of addings of vinyltrimethoxy silane planetary mixer, keep vacuum tightness-0.08MPa, stirring velocity is 70rpm, stirs 20 minutes, makes the B component.The product performance test result is shown in Table 1.
Embodiment 4:
Viscosity is the α of 500mPas viscosity during with 25 ± 2 ℃, and 100 parts of ω-divinyl polydimethylsiloxane mix aluminum oxide
1.120 parts, put into kneader and under 180 ℃ of temperature, vacuum tightness-0.08MPa, mediated 3 hours, after the cooling base-material.At room temperature, with 100 parts of base-materials, α, in 10 parts of ω-divinyl polydimethylsiloxane, 0.2 part of adding of the platinum catalyst planetary mixer, keep vacuum tightness-0.08MPa, stirring velocity is 70rpm, stirs 20 minutes, makes the A component; At room temperature, in 100 parts of base-materials, 8 parts of containing hydrogen silicone oils of end, 2 parts of addings of vinyltrimethoxy silane planetary mixer, keep vacuum tightness-0.08MPa, stirring velocity is 70rpm, stirs 20 minutes, makes the B component.The product performance test result is shown in Table 1.
Comparative example 1:
Viscosity is the α of 500mPas viscosity during with 25 ± 2 ℃, 100 parts of ω-divinyl polydimethylsiloxane, and 60 parts of nano aluminium oxides, 20 parts of fillers are put into kneader and were mediated 3 hours under 180 ℃ of temperature, vacuum tightness-0.08MPa, get base-material after the cooling.At room temperature, with 100 parts of base-materials, α, in 10 parts of ω-divinyl polydimethylsiloxane, 0.2 part of adding of the platinum catalyst planetary mixer, keep vacuum tightness-0.08MPa, stirring velocity is 70rpm, stirs 20 minutes, makes the A component; At room temperature, in 100 parts of base-materials, 8 parts of containing hydrogen silicone oils of end, 2 parts of addings of vinyltrimethoxy silane planetary mixer, keep vacuum tightness-0.08MPa, stirring velocity is 70rpm, stirs 20 minutes, makes the B component.The product performance test result is shown in Table 1.
Comparative example 2:
Viscosity is the α of 500mPas viscosity during with 25 ± 2 ℃, and 100 parts of ω-divinyl polydimethylsiloxane, are put into kneader and mediated 3 hours under 180 ℃ of temperature, vacuum tightness-0.08MPa 120 parts in silicon carbide, after the cooling base-material.At room temperature, with 100 parts of base-materials, α, in 10 parts of ω-divinyl polydimethylsiloxane, 0.2 part of adding of the platinum catalyst planetary mixer, keep vacuum tightness-0.08MPa, stirring velocity is 70rpm, stirs 20 minutes, makes the A component; At room temperature, in 100 parts of base-materials, 8 parts of containing hydrogen silicone oils of end, 2 parts of addings of vinyltrimethoxy silane planetary mixer, keep vacuum tightness-0.08MPa, stirring velocity is 70rpm, stirs 20 minutes, makes the B component.The product performance test result is shown in Table 1.
Table 1 product performance test result
Annotate
1.Select the ball-aluminium oxide of different-grain diameter, be mixed by a certain percentage;
Annotate
2.Deaeration time test method is as follows: with after the sample mix approximately 300 ± 5g place smooth mouthful of container of 300ml, stirred 2 minutes with toolsetting, make sample mix even, put into the vacuum-pumping container that the glass visor is housed, open vacuum pump and vacuumize and begin simultaneously timing, keep vacuum tightness to be-0.08MPa.Observe sample deaeration situation by visor, timing stops when taking off to sample is still, and this time is the deaeration time;
Annotate
3.The accelerated storage stability testing method is as follows: sample is respectively charged in the encloses container, puts into 40 ℃ of baking ovens, regularly measure its viscosity variation, layering sepage situation every day; From falling behind, can the observation cutter head be with sedimentation thickness and the situation that stir with toolsetting, to determine its precipitation situation.Can not penetrate settled layer to 15 days or cutter head and stop test.
Can find out by above test-results, use the α of low viscosity (500cs), ω-divinyl polydimethylsiloxane can obtain lower kinematic viscosity; Make thermal conducting agent with the different-grain diameter ball-aluminium oxide that mixes through certain proportion, than the inorganic thermal conducting agent of other kind is mobile better, the deaeration time is shorter, package stability better, comprehensive cost performance is higher.
Claims (7)
1. additional organosilicon heat conductive electronic pouring sealant, the starting material and the parts by weight that comprise are:
The A component
The B component
Wherein:
α, ω-divinyl polydimethylsiloxane structural formula is
N=50 in the formula～2000, R is-CH
3,-CH
2CH
3
2. additional organosilicon heat conductive electronic pouring sealant according to claim 1, the described mineral filler of its feature are a kind of in calcium carbonate superfine powder, active nano calcium, superfine silicon dioxide powder, silica powder, ultrafine kaolin, titanium dioxide, the aluminium hydroxide.
3. additional organosilicon heat conductive electronic pouring sealant according to claim 1 is characterized in that described heat conductive filler is at least a in aluminum oxide, nano aluminium oxide, silicon-dioxide, aluminium nitride, nano aluminum nitride, boron nitride, nm-class boron nitride, the silicon carbide.
4. additional organosilicon heat conductive electronic pouring sealant according to claim 1 is characterized in that described catalyzer is platinum catalyst.
5. additional organosilicon heat conductive electronic pouring sealant according to claim 1 is characterized in that described linking agent is containing hydrogen silicone oil at least a of methyl blocking of end hydrogen silicone oil, the low polymerization degree of low polymerization degree.
6. additional organosilicon heat conductive electronic pouring sealant according to claim 1 is characterized in that described coupling agent is vinyltrimethoxy silane, glycidoxy-propyltrimethoxy silane, contains polysiloxane at least a of epoxy group(ing).
7. the manufacture method of additional organosilicon heat conductive electronic pouring sealant the steps include:
(1) with α, 120～360 parts of 100 parts of ω-divinyl polydimethylsiloxane, 0～20 part of filler, heat conductive filler join in the kneader, 100～180 ℃, vacuum tightness-0.06～-dewatered 1～4 hour under the 0.1MPa, make base-material after the cooling;
(2) at room temperature, with 100 parts of base-materials, α, in 10～30 parts of ω-divinyl polydimethylsiloxane, 0.01～2 part of adding of the catalyzer planetary mixer, maintenance vacuum tightness-0.06～-0.1MPa, stirring velocity is 50～100rpm, stirs 10～30 minutes, makes the A component;
(3) at room temperature, in 100 parts of base-materials, 5～20 parts of linking agents, 0.1～3 part of adding of silane coupling agent planetary mixer, maintenance vacuum tightness-0.06～-0.1MPa, stirring velocity is 50～100rpm, stirs 10～30 minutes, makes the B component;
(4) this A, B component are the additional organosilicon heat conductive electronic pouring sealant, during use this A, B component are mixed use by weight 1: 1 ratio.
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Application publication date: 20130306 |