CN116536027A - Low-stress organosilicon two-component pouring sealant and preparation method thereof - Google Patents
Low-stress organosilicon two-component pouring sealant and preparation method thereof Download PDFInfo
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- CN116536027A CN116536027A CN202310581860.8A CN202310581860A CN116536027A CN 116536027 A CN116536027 A CN 116536027A CN 202310581860 A CN202310581860 A CN 202310581860A CN 116536027 A CN116536027 A CN 116536027A
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- 239000000565 sealant Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000945 filler Substances 0.000 claims abstract description 76
- 229920002545 silicone oil Polymers 0.000 claims abstract description 61
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000000463 material Substances 0.000 claims abstract description 55
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 53
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 51
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 48
- 239000002245 particle Substances 0.000 claims abstract description 47
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910052802 copper Inorganic materials 0.000 claims abstract description 38
- 239000010949 copper Substances 0.000 claims abstract description 38
- 239000001257 hydrogen Substances 0.000 claims abstract description 37
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 37
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 32
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 28
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 239000003112 inhibitor Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 14
- 239000003446 ligand Substances 0.000 claims description 14
- 229910052710 silicon Inorganic materials 0.000 claims description 14
- 239000010703 silicon Substances 0.000 claims description 14
- 239000012691 Cu precursor Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 230000003301 hydrolyzing effect Effects 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000003638 chemical reducing agent Substances 0.000 claims description 5
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- -1 polydimethylsiloxane Polymers 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- 239000005046 Chlorosilane Substances 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 125000003368 amide group Chemical group 0.000 claims description 2
- 125000002843 carboxylic acid group Chemical group 0.000 claims description 2
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical group Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims description 2
- 230000018044 dehydration Effects 0.000 claims description 2
- 238000006297 dehydration reaction Methods 0.000 claims description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 125000004076 pyridyl group Chemical group 0.000 claims description 2
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical group O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 19
- 239000002994 raw material Substances 0.000 abstract description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 18
- 239000011231 conductive filler Substances 0.000 description 17
- UJYZRMROGXVXFD-UHFFFAOYSA-N 1-hex-1-ynylcyclohexan-1-ol Chemical compound CCCCC#CC1(O)CCCCC1 UJYZRMROGXVXFD-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- 150000002431 hydrogen Chemical class 0.000 description 9
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 9
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- DLLABNOCKQMTEJ-UHFFFAOYSA-N chloro-dodecyl-dimethylsilane Chemical compound CCCCCCCCCCCC[Si](C)(C)Cl DLLABNOCKQMTEJ-UHFFFAOYSA-N 0.000 description 8
- 239000000084 colloidal system Substances 0.000 description 8
- 239000006228 supernatant Substances 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 6
- 229910000365 copper sulfate Inorganic materials 0.000 description 5
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 229960005070 ascorbic acid Drugs 0.000 description 4
- 235000010323 ascorbic acid Nutrition 0.000 description 4
- 239000011668 ascorbic acid Substances 0.000 description 4
- 238000004382 potting Methods 0.000 description 4
- 230000008439 repair process Effects 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 238000007259 addition reaction Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- KFDVPJUYSDEJTH-UHFFFAOYSA-N 4-ethenylpyridine Chemical compound C=CC1=CC=NC=C1 KFDVPJUYSDEJTH-UHFFFAOYSA-N 0.000 description 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- GZGREZWGCWVAEE-UHFFFAOYSA-N chloro-dimethyl-octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[Si](C)(C)Cl GZGREZWGCWVAEE-UHFFFAOYSA-N 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Sealing Material Composition (AREA)
Abstract
A low-stress organosilicon double-component pouring sealant and a preparation method thereof are provided, wherein the pouring sealant comprises a component A and a component B; the component A comprises 80 parts of base material, 15-20 parts of methyl silicone oil and 0.5-1 part of platinum catalyst; the component B comprises 80 parts of base material, 15-20 parts of methyl silicone oil, 1.5-2 parts of hydrogen-containing silicone oil and 0.01-0.05 part of inhibitor; the base material comprises 5-25 parts of single-ended vinyl silicone oil, 5-15 parts of first heat conducting filler, 20-40 parts of second heat conducting filler, 5-15 parts of methyl silicone oil and 0.1-0.6 part of filler treating agent; the first heat conduction filler comprises nano copper particles and a silicon dioxide layer coated on the surfaces of the nano copper particles. According to the preparation method, the single-ended vinyl silicone oil is used as the raw material, so that the reaction sites between the single-ended vinyl silicone oil and the hydrogen-containing silicone oil are effectively reduced, meanwhile, on the basis of guaranteeing the heat conduction performance of the heat conduction filler, the addition amount of the heat conduction filler is further reduced, the internal stress of the cured organosilicon pouring sealant is reduced, and meanwhile, the fluidity of the organosilicon pouring sealant is improved and the hardness of the organosilicon pouring sealant is reduced.
Description
Technical Field
The invention relates to the field of organic silicon pouring sealants, in particular to a low-stress organic silicon double-component pouring sealant and a preparation method thereof.
Background
In recent years, the demands for integration and miniaturization of electronic components have been increasing, and the demands for potting materials have been increasing. The addition type organic silicon pouring sealant has been widely used in the field of element packaging because of its characteristics of small molecule release prevention, no shrinkage, elasticity in the temperature range of-50 to 200 ℃, and the like.
However, the viscosity of the addition type silicone potting adhesive is relatively large and the fluidity is poor due to the large addition of the heat conductive filler, so that it is difficult to infiltrate into minute gaps, particularly gaps smaller than 1 mm. In addition, the colloid can gradually increase the hardness under the high and low temperature conditions, so that internal stress is generated on the device, and meanwhile, the colloid is softer and higher in viscosity, and if secondary repair is performed, the micro device is easily damaged.
The patent with the application number of 201910675359.1 discloses a double-component organic silicon pouring sealant, which comprises an A component and a B component with equal mass; the component A comprises a base material, double-end vinyl silicone oil, methyl silicone oil and a platinum catalyst; the component B comprises a base material, methyl silicone oil, hydrogen-containing silicone oil, hydrogen-terminated silicone oil, a tackifier, black paste and an inhibitor; the base material comprises double-end vinyl silicone oil, a heat-conducting filler and a filler treating agent, and the tackifier is a silane coupling agent with epoxy groups and vinyl groups, so that the adhesive has excellent flowing property and lower stress, and is strong in viscosity and difficult to be suitable for filling and sealing of micro devices needing repairing.
Disclosure of Invention
The invention provides a low-stress organic silicon double-component pouring sealant and a preparation method thereof, which are used for overcoming the defect that the organic silicon double-component pouring sealant in the prior art is difficult to realize balance of low stress, high flow property and low bonding property.
In order to achieve the aim of the invention, the invention is realized by the following technical scheme:
in the first aspect, the invention firstly provides a low-stress organosilicon two-component pouring sealant, which comprises a component A and a component B;
the component A comprises 80 parts of base material, 15-20 parts of methyl silicone oil and 0.5-1 part of platinum catalyst;
the component B comprises 80 parts of base material, 15-20 parts of methyl silicone oil, 1.5-2 parts of hydrogen-containing silicone oil and 0.01-0.05 part of inhibitor;
the base material comprises 5-25 parts of single-ended vinyl silicone oil, 5-15 parts of first heat conducting filler, 20-40 parts of second heat conducting filler, 5-15 parts of methyl silicone oil and 0.1-0.6 part of filler treating agent;
the first heat conduction filler comprises nano copper particles and a silicon dioxide layer coated on the surfaces of the nano copper particles.
Through the research of the applicant of the present invention, the stress of the organosilicon pouring sealant is derived from the process of forming the addition reaction between hydrogen-containing silicone oil and vinyl silicone oil, namely the process of converting the hydrogen and double bond structure into a saturated structure. The lower the vinyl content of the vinyl silicone oil and the hydrogen content of the hydrogen-containing silicone oil, i.e. the fewer the reaction sites between the two, the lower the stress of the silicone potting adhesive.
At present, the organosilicon pouring sealant in the prior art generally adopts vinyl silicone oil with vinyl groups at both ends as a raw material. However, since both ends participate in the addition reaction with the hydrogen-containing silicone oil, both ends of the main chain are drawn and fixed after the reaction is finished, and cannot rotate freely, so that the main chain encounters resistance in the process of adjusting the structure of the main chain, and internal stress is generated in the pouring sealant.
In order to overcome the above phenomenon, silicone oil containing vinyl groups at one end is used as a raw material. Because only one end participates in the reaction and the other end can still freely rotate in the process of adding hydrogen-containing silicone oil, the chain segment can still freely adjust the structure after the reaction is finished, and the generation of internal stress is obviously reduced. Meanwhile, due to the reduction of the connecting sites, the viscosity and the bonding performance of the micro-device are obviously reduced, and the micro-device is more easily separated from the micro-device, so that the micro-device is convenient to repair.
In addition, the viscosity of the pouring sealant is further reduced by innovating the formula of the heat conducting filler so as to improve the fluidity of the pouring sealant. In the present application, a method of compounding a first heat conductive filler and a second heat conductive filler is employed, wherein the first heat conductive filler is composed of nano copper particles and a silica layer. Because the heat conduction performance of the metal copper particles is far higher than that of conventional inorganic heat conduction fillers (such as silica micropowder, alumina powder and the like), the addition of the first heat conduction filler can greatly reduce the addition amount of the total heat conduction filler on the premise of keeping the same heat conduction rate, effectively avoid the influence of excessive heat conduction fillers on the potting adhesive, and ensure that the metal copper particles have better fluidity.
In addition, the surface of the nano copper particle is coated with a silicon dioxide layer, so that the conductivity is extremely low, the influence of nano copper on the conductivity of the whole pouring sealant is effectively avoided, and the nano copper particle can be applied to the electronic component packaging technology. The silicon dioxide layer and the main chain of the organic silicon pouring sealant are of Si-O-Si structures, so that the compatibility between the silicon dioxide layer and the organic silicon pouring sealant is high. But the silica layer in the first thermally conductive filler and the surface of the second thermally conductive filler generally have a more-OH hydrophilic structure. Therefore, the first and second heat conducting fillers are subjected to surface modification by adopting the filler treating agent, so that the filler treating agent can react with the-OH hydrophilic structure on the surface of the silicon dioxide to form an oleophilic structure, and the filler and the silicone oil are favorably mixed.
Finally, under the premise of ensuring the colloid performance, the formula is added with sufficient methyl silicone oil, so that the surface of the solidified colloid is smooth and flat, has small viscosity, and can not cause damage to micro devices during secondary repair.
Preferably, the preparation method of the first heat conductive filler comprises the following steps:
dissolving a copper precursor and trialkoxysilane with a ligand group in water, adding an acidic reducing agent, reducing the copper precursor to obtain nano copper particles, hydrolyzing the trialkoxysilane with the ligand group to form a silicon dioxide layer, coating the nano copper particles to obtain nano copper particles coated with the silicon dioxide layer, filtering, washing, drying and carrying out heat treatment in a vacuum environment to obtain the first heat-conducting filler.
The nano copper particles in the first heat-conducting filler are formed by reducing a copper precursor under the action of a reducing agent. After the nano copper particles are prepared, the ligand groups in the trialkoxysilane with the ligand groups can be mutually attracted and matched with the nano copper particles, so that the nano copper particles are coated in the nano copper particles. Because the acidic reducing agent is used for catalyzing the reduction of the copper precursor, the alkoxy groups in the trialkoxysilane with the ligand groups can form a crosslinked silicon dioxide layer in the hydrolytic condensation process, so that the nano copper particles are tightly packed inside, and the protection of the nano copper particles is realized.
Preferably, the ligand group in the trialkoxysilane with ligand group includes any one of pyrrolidone group, amide group, pyridyl group and carboxylic acid group.
Preferably, the copper precursor includes any one of copper chloride, copper sulfate, and copper acetate.
Preferably, the acidic reducing agent comprises any one of citric acid, ascorbic acid, oxalic acid and oxalic acid.
Preferably, the reduction temperature is 70-85 ℃ and the reaction time is 3-5 h.
Preferably, the single-ended vinyl silicone oil is linear vinyl polydimethylsiloxane;
the vinyl content of the single-ended vinyl silicone oil is 0.15-0.25%, and the viscosity is 500-1000 mPa.s.
Preferably, the second heat conduction filler is silica powder and/or alumina;
the average particle diameter of the silica micropowder and/or alumina is 5-20 mu m.
Preferably, the viscosity of the methyl silicone oil is 100 mPas-1000 mPas.
Preferably, the hydrogen content of the hydrogen-containing silicone oil is 0.1 to 0.36%.
Preferably, the filler treating agent is chlorosilane containing an alkyl group having 12 to 20 carbon atoms.
In a second aspect, the invention also provides a method for preparing the low-stress organosilicon two-component pouring sealant, which comprises the following steps:
1) Preparing a base material: blending and dehydrating single-ended vinyl silicone oil, a first heat-conducting filler, a second heat-conducting filler and methyl silicone oil, then adding a filler treating agent to treat the first heat-conducting filler and the second heat-conducting filler, and then continuing blending and dehydrating to obtain a base material;
2) And (3) preparing a component A: uniformly mixing the base material, the methyl silicone oil and the platinum catalyst, and vacuumizing to remove bubbles to obtain a component A;
3) And (3) preparing a component B: uniformly mixing the base material, the methyl silicone oil, the hydrogen-containing silicone oil and the inhibitor, and vacuumizing to remove bubbles to obtain a component B;
4) Preparing organic silicon pouring sealant: the component A prepared in the step 2) and the component B prepared in the step 3) are mixed according to the weight ratio of 1:1, and vacuumizing to remove bubbles, thus obtaining the organic silicon pouring sealant.
Preferably, the step (1) is specifically as follows:
blending and dehydrating single-end vinyl silicone oil, a first heat conducting filler, a second heat conducting filler and methyl silicone oil at the temperature of 120-130 ℃ and the vacuum degree of less than or equal to minus 0.095MPa for 1-5 h; cooling to 70-90 ℃, adding a filler treating agent, and preserving heat for 0.5-2 h; and raising the temperature to 120-130 ℃ again, and carrying out blending dehydration for 1-2 h under the vacuum degree of less than or equal to minus 0.095MPa to obtain the base material.
Therefore, the invention has the following beneficial effects:
(1) The single-ended vinyl silicone oil is used as the raw material, so that the reaction sites between the single-ended vinyl silicone oil and the hydrogen-containing silicone oil are effectively reduced, the internal stress of the cured organosilicon pouring sealant is reduced, the fluidity of the organosilicon pouring sealant is improved, and the hardness of the organosilicon pouring sealant is reduced;
(2) The application improves the heat-conducting filler to a certain extent, further reduces the addition amount of the heat-conducting filler on the basis of ensuring the heat-conducting property of the heat-conducting filler, reduces the viscosity of the organic pouring sealant and improves the fluidity of the organic pouring sealant;
(3) Under the condition of ensuring the colloid performance, the formula is added with more methyl silicone oil, so that the surface of the solidified colloid is smoother, the viscosity is small, and the damage of micro devices can not be caused during secondary repair.
Detailed Description
The invention is further described below in connection with specific embodiments. Those of ordinary skill in the art will be able to implement the invention based on these descriptions. In addition, the embodiments of the present invention referred to in the following description are typically only some, but not all, embodiments of the present invention. Therefore, all other embodiments, which can be made by one of ordinary skill in the art without undue burden, are intended to be within the scope of the present invention, based on the embodiments of the present invention.
[ preparation of trialkoxysilane with ligand group ]
Trialkoxysilane A1 16.4 (0.1 mol) triethoxysilane and 11.1 (0.1 mol) vinylpyrrolidone were dissolved in 200ml toluene under nitrogen atmosphere, 3000ppm of Karster catalyst was added, the reaction was heated and refluxed for 3 hours, then the reaction was stopped, 1g of activated carbon was added thereto, stirred at room temperature for 30 minutes, and then filtered, and toluene in the filtrate was distilled off to obtain trialkoxysilane A1, the reaction schematic formula of which is shown in the following formula (1):
trialkoxysilane A2 16.4 (0.1 mol) triethoxysilane and 10.5 (0.1 mol) 4-vinylpyridine were dissolved in 200ml toluene under nitrogen atmosphere, 3000ppm of Karster catalyst was added, the reaction was heated and refluxed for 3 hours, then the reaction was stopped, 1g of activated carbon was added thereto, stirred at room temperature for 30 minutes, and then filtered, toluene in the filtrate was distilled off to obtain trialkoxysilane A2, the reaction scheme of which is shown in the following formula (2):
trialkoxysilane A3 16.4 (0.1 mol) triethoxysilane and 9.8 (0.1 mol) maleic anhydride were dissolved in 200ml toluene under nitrogen atmosphere protection, 3000ppm Kanst catalyst was added, reflux reaction was carried out at elevated temperature for 3 hours, then the reaction was stopped, 1g of activated carbon was added thereto, stirred at room temperature for 30 minutes, then filtration was carried out, toluene in the filtrate was distilled off, and trialkoxysilane A3 was obtained, the reaction scheme of which was shown in the following formula (3):
[ preparation of first Heat conductive filler ]
First heat conductive filler B1: 16g (0.1 mol) of copper sulfate, 27.5g (0.1 mol) of triethoxysilane A1 are dissolved in 50g of water to form a solution A. 25g of ascorbic acid was dissolved in 60g of water to form solution B. And (3) dropwise adding the solution A into the solution B, stirring at 75 ℃ for reaction for 5 hours, reducing the copper precursor to obtain nano copper particles, hydrolyzing triethoxysilane A1 to form a silicon dioxide layer so as to coat the nano copper particles, obtaining nano copper particle precipitate coated with the silicon dioxide layer, centrifuging the precipitate 4000r/min, removing supernatant, washing with ethanol in a vibrating manner for 5 minutes, centrifuging again, removing supernatant, and heating to 110 ℃ in a vacuum environment for 5 hours to obtain the first heat-conducting filler B1.
First heat conductive filler B2: 16g (0.1 mol) of copper sulfate, 27g (0.1 mol) of triethoxysilane A2 are dissolved in 50g of water to form a solution A. 25g of citric acid was dissolved in 50g of water to form solution B. And (3) dropwise adding the solution A into the solution B, stirring at 75 ℃ for reaction for 5 hours, reducing the copper precursor to obtain nano copper particles, hydrolyzing triethoxysilane A2 to form a silicon dioxide layer so as to coat the nano copper particles, obtaining nano copper particle precipitate coated with the silicon dioxide layer, centrifuging the precipitate 4000r/min, removing supernatant, washing with ethanol in a vibrating manner for 5 minutes, centrifuging again, removing supernatant, and heating to 110 ℃ in a vacuum environment for 5 hours to obtain the first heat-conducting filler B2.
First heat conductive filler B3: 16g (0.1 mol) of copper sulfate, 26g (0.1 mol) of triethoxysilane A3 are dissolved in 50g of water to form a solution A. 25g of ascorbic acid was dissolved in 60g of water to form solution B. And (3) dropwise adding the solution A into the solution B, stirring at 75 ℃ for reaction for 5 hours, reducing the copper precursor to obtain nano copper particles, hydrolyzing triethoxysilane A3 to form a silicon dioxide layer so as to coat the nano copper particles, obtaining nano copper particle precipitate coated with the silicon dioxide layer, centrifuging the precipitate 4000r/min, removing supernatant, washing with ethanol in a vibrating manner for 5 minutes, centrifuging again, removing supernatant, and heating to 110 ℃ in a vacuum environment for 5 hours to obtain the first heat-conducting filler B3.
First heat conductive filler B4: 16g (0.1 mol) of copper sulfate, 21g (0.1 mol) of tetraethoxysilane were dissolved in 50g of water to form a solution A. 25g of ascorbic acid was dissolved in 60g of water to form solution B. And (3) dropwise adding the solution A into the solution B, stirring at 75 ℃ for reaction for 5 hours, reducing the copper precursor to obtain nano copper particles, hydrolyzing tetraethoxysilane to form a silicon dioxide layer so as to coat the nano copper particles, obtaining nano copper particle sediment coated with the silicon dioxide layer, centrifuging 4000r/min of the sediment, removing supernatant, oscillating and washing with ethanol for 5 minutes, centrifuging again, removing supernatant, and heating to 110 ℃ in a vacuum environment for 5 hours to obtain the first heat-conducting filler B4.
Example 1
A low-stress organosilicon double-component pouring sealant comprises a component A and a component B;
the component A comprises 80 parts of base material, 18 parts of methyl silicone oil and 0.8 part of 3000ppm platinum catalyst;
the component B comprises 80 parts of base material, 15 parts of methyl silicone oil, 1.8 parts of hydrogen silicone oil with hydrogen content of 0.25%, and 0.03 part of 1-hexynyl-1-cyclohexanol;
the base material comprises 20 parts of single-end vinyl silicone oil with the vinyl content of 0.2% and the viscosity of 800 mPas, 1 part of a first heat-conducting filler B, 35 parts of a second heat-conducting filler (spherical alumina with the average particle size of 10 mu m), 10 parts of methyl silicone oil and 0.5 part of dodecyl dimethyl chlorosilane.
The preparation method comprises the following steps:
(1) Preparing a base material: blending and dehydrating single-end vinyl silicone oil, a first heat-conducting filler B1, a second heat-conducting filler and methyl silicone oil at the temperature of 120-130 ℃ and the vacuum degree of-0.095 MPa for 2h; cooling to 80 ℃, adding a filler treating agent, and preserving heat for 1h; then raising the temperature to 120-130 ℃ and blending and dehydrating for 2 hours under the vacuum degree of-0.095 MPa to obtain a base material;
(2) And (3) preparing a component A: uniformly mixing the base material, the methyl silicone oil and the platinum catalyst, and vacuumizing to remove bubbles to obtain a component A;
(3) And (3) preparing a component B: uniformly mixing the base material, the methyl silicone oil, the hydrogen-containing silicone oil and the inhibitor, and vacuumizing to remove bubbles to obtain a component B;
(4) Preparing organic silicon pouring sealant: the component A prepared in the step 2) and the component B prepared in the step 3) are mixed according to the weight ratio of 1:1, and vacuumizing to remove bubbles, thus obtaining the organic silicon pouring sealant.
Example 2
A low-stress organosilicon double-component pouring sealant comprises a component A and a component B;
the component A comprises 80 parts of base material, 18 parts of methyl silicone oil and 0.8 part of 3000ppm platinum catalyst;
the component B comprises 80 parts of base material, 15 parts of methyl silicone oil, 1.8 parts of hydrogen silicone oil with hydrogen content of 0.25%, and 0.03 part of 1-hexynyl-1-cyclohexanol;
the base material comprises 20 parts of single-end vinyl silicone oil with the vinyl content of 0.2% and the viscosity of 800 mPas, 2 parts of a first heat-conducting filler B, 35 parts of a second heat-conducting filler (spherical alumina with the average particle size of 10 mu m), 10 parts of methyl silicone oil and 0.5 part of dodecyl dimethyl chlorosilane.
The preparation method is shown in example 1.
Example 3
A low-stress organosilicon double-component pouring sealant comprises a component A and a component B;
the component A comprises 80 parts of base material, 18 parts of methyl silicone oil and 0.8 part of 3000ppm platinum catalyst;
the component B comprises 80 parts of base material, 15 parts of methyl silicone oil, 1.8 parts of hydrogen silicone oil with hydrogen content of 0.25%, and 0.03 part of 1-hexynyl-1-cyclohexanol;
the base material comprises 20 parts of single-end vinyl silicone oil with the vinyl content of 0.2% and the viscosity of 800 mPas, 3 parts of a first heat-conducting filler B, 35 parts of a second heat-conducting filler (spherical alumina with the average particle size of 10 mu m), 10 parts of methyl silicone oil and 0.5 part of dodecyl dimethyl chlorosilane.
The preparation method is shown in example 1.
Example 4
A low-stress organosilicon double-component pouring sealant comprises a component A and a component B;
the component A comprises 80 parts of base material, 18 parts of methyl silicone oil and 0.5 part of 3000ppm platinum catalyst;
the component B comprises 80 parts of base material, 15 parts of methyl silicone oil, 1.5 parts of hydrogen silicone oil with hydrogen content of 0.1 percent and 0.01 part of 1-hexynyl-1-cyclohexanol;
the base material comprises 5 parts of single-end vinyl silicone oil with the vinyl content of 0.15% and the viscosity of 1000 mPas, 35 parts of a first heat conducting filler B, 20 parts of a second heat conducting filler (spherical alumina with the average particle size of 10 mu m), 15 parts of methyl silicone oil and 0.1 part of dodecyl dimethyl chlorosilane.
The preparation method is shown in example 1.
Example 5
A low-stress organosilicon double-component pouring sealant comprises a component A and a component B;
the component A comprises 80 parts of base material, 20 parts of methyl silicone oil and 1 part of 3000ppm platinum catalyst;
the component B comprises 80 parts of base material, 20 parts of methyl silicone oil, 2 parts of hydrogen silicone oil with hydrogen content of 0.36%, and 0.05 part of 1-hexynyl-1-cyclohexanol;
the base material comprises 25 parts of single-end vinyl silicone oil with the vinyl content of 0.25% and the viscosity of 500 mPa.s, 3 parts of a first heat-conducting filler B, 30 parts of a second heat-conducting filler (spherical alumina with the average particle size of 10 mu m) and 0.6 part of dodecyl dimethyl chlorosilane.
The preparation method is shown in example 1.
Example 6
A low-stress organosilicon double-component pouring sealant comprises a component A and a component B;
the component A comprises 80 parts of base material, 15 parts of methyl silicone oil and 1 part of 3000ppm platinum catalyst;
the component B comprises 80 parts of base material, 20 parts of methyl silicone oil, 2 parts of hydrogen silicone oil with hydrogen content of 0.36%, and 0.03 part of 1-hexynyl-1-cyclohexanol;
the base material comprises 25 parts of single-end vinyl silicone oil with the vinyl content of 0.25% and the viscosity of 500 mPa.s, 3 parts of a first heat-conducting filler B, 36 parts of a second heat-conducting filler (spherical alumina with the average particle size of 10 mu m) and 0.3 part of octadecyl dimethyl chlorosilane.
The preparation method is shown in example 1.
Comparative example 1
A low-stress organosilicon double-component pouring sealant comprises a component A and a component B;
the component A comprises 80 parts of base material, 18 parts of methyl silicone oil and 0.8 part of 3000ppm platinum catalyst;
the component B comprises 80 parts of base material, 15 parts of methyl silicone oil, 1.8 parts of hydrogen silicone oil with hydrogen content of 0.25%, and 0.03 part of 1-hexynyl-1-cyclohexanol;
the base material comprises 20 parts of single-end vinyl silicone oil with the vinyl content of 0.2% and the viscosity of 800 mPa.s, 65 parts of second heat conduction filler (spherical alumina with the average particle size of 10 mu m), 10 parts of methyl silicone oil and 0.5 part of dodecyl dimethyl chlorosilane.
The preparation method is shown in example 1.
Comparative example 2
A low-stress organosilicon double-component pouring sealant comprises a component A and a component B;
the component A comprises 80 parts of base material, 18 parts of methyl silicone oil and 0.8 part of 3000ppm platinum catalyst;
the component B comprises 80 parts of base material, 15 parts of methyl silicone oil, 1.8 parts of hydrogen silicone oil with hydrogen content of 0.25%, and 0.03 part of 1-hexynyl-1-cyclohexanol;
the base material comprises 20 parts of double-end vinyl silicone oil with the vinyl content of 0.2% and the viscosity of 800 mPas, 1 part of a first heat-conducting filler B, 35 parts of a second heat-conducting filler (spherical alumina with the average particle size of 10 mu m), 10 parts of methyl silicone oil and 0.5 part of dodecyl dimethyl chlorosilane.
The preparation method is shown in example 1.
Comparative example 3
A low-stress organosilicon double-component pouring sealant comprises a component A and a component B;
the component A comprises 80 parts of base material, 18 parts of methyl silicone oil and 0.8 part of 3000ppm platinum catalyst;
the component B comprises 80 parts of base material, 15 parts of methyl silicone oil, 1.8 parts of hydrogen silicone oil with hydrogen content of 0.25%, and 0.03 part of 1-hexynyl-1-cyclohexanol;
the base material comprises 20 parts of single-end vinyl silicone oil with the vinyl content of 0.2% and the viscosity of 800 mPas, 4 parts of a first heat-conducting filler B, 35 parts of a second heat-conducting filler (spherical alumina with the average particle size of 10 mu m), 10 parts of methyl silicone oil and 0.5 part of dodecyl dimethyl chlorosilane.
The preparation method is shown in example 1.
Examples 1 to 5 and comparative examples 1 to 3 were tested for leveling property, thermal conductivity, conductivity and hardness, respectively.
Wherein:
leveling property: dripping 0.5ml of the glue solution into a polytetrafluoroethylene groove with a certain angle, and testing the length of the glue solution after 3 min.
Thermal conductivity coefficient: the thermal conductivity was measured according to GB/T10297-2015.
Hardness: and curing the pouring sealant to obtain a colloid, and testing the Shore hardness of the colloid.
The test results are shown in table 1 below:
from the results shown in the table, the organosilicon two-component pouring sealant has good leveling property, so that the organosilicon two-component pouring sealant can permeate into a tiny gap, and is used for pouring and sealing tiny electronic components. Meanwhile, after curing, the material has lower hardness, so that the internal stress is lower, and the thermal conductivity and the dielectric constant are excellent.
By comparing example 1 with comparative example 1, it was found that the first heat conductive filler was not added in comparative example 1, and therefore, in order to achieve a close heat conductivity, more of the second heat conductive filler was added in comparative example 1, resulting in a decrease in leveling property and an increase in hardness.
Comparing example 1 with comparative example 2, it was found that the hardness of the cured single-ended vinyl silicone oil is significantly improved after the single-ended vinyl silicone oil is replaced by double-ended vinyl silicone oil, which indicates that the single-ended vinyl silicone oil can effectively reduce the internal stress of the pouring sealant.
Comparing example 1 with comparative example 3, it was found that, after the type of the first heat conductive filler was changed, since the first heat conductive filler B4 did not introduce a ligand during the preparation process, the silica could not completely coat the copper nanoparticle, resulting in a decrease in dielectric constant thereof, indicating that the introduction of a ligand has a significant effect on the conductivity of the first heat conductive filler.
Claims (10)
1. The low-stress organosilicon double-component pouring sealant is characterized by comprising a component A and a component B;
the component A comprises 80 parts of base material, 15-20 parts of methyl silicone oil and 0.5-1 part of platinum catalyst;
the component B comprises 80 parts of base material, 15-20 parts of methyl silicone oil, 1.5-2 parts of hydrogen-containing silicone oil and 0.01-0.05 part of inhibitor; the base material comprises 5-25 parts of single-ended vinyl silicone oil, 5-15 parts of first heat conducting filler, 20-40 parts of second heat conducting filler, 5-15 parts of methyl silicone oil and 0.1-0.6 part of filler treating agent;
the first heat conduction filler comprises nano copper particles and a silicon dioxide layer coated on the surfaces of the nano copper particles.
2. The low stress organosilicon two-component pouring sealant according to claim 1, wherein,
the preparation method of the first heat conduction filler comprises the following steps:
dissolving a copper precursor and trialkoxysilane with a ligand group in water, adding an acidic reducing agent, reacting to reduce the copper precursor to obtain nano copper particles, hydrolyzing the trialkoxysilane with the ligand group to form a silicon dioxide layer so as to coat the nano copper particles, obtaining nano copper particles coated with the silicon dioxide layer, filtering, washing, drying and carrying out heat treatment in a vacuum environment to obtain the first heat-conducting filler.
3. The low stress organosilicon two-component pouring sealant according to claim 2, wherein,
the ligand group in the trialkoxysilane with ligand group comprises any one of pyrrolidone group, amide group, pyridyl group and carboxylic acid group.
4. A low stress silicone two-component pouring sealant according to any one of claims 1 to 3, characterized in that,
the single-ended vinyl silicone oil is linear vinyl polydimethylsiloxane;
the vinyl content of the single-ended vinyl silicone oil is 0.15-0.25%, and the viscosity is 500-1000 mPa.s.
5. A low stress organosilicon two-component pouring sealant according to claim 1-3, characterized in that,
the second heat conduction filler is silica micropowder and/or alumina;
the average particle diameter of the silica micropowder and/or alumina is 5-20 mu m.
6. A low stress organosilicon two-component pouring sealant according to claim 1-3, characterized in that,
the viscosity of the methyl silicone oil is 100 mPas-1000 mPas.
7. A low stress organosilicon two-component pouring sealant according to claim 1-3, characterized in that,
the hydrogen content of the hydrogen-containing silicone oil is 0.1-0.36%.
8. A low stress organosilicon two-component pouring sealant according to claim 1-3, characterized in that,
the filler treating agent is chlorosilane containing alkyl groups with 12-20 carbons.
9. A method for preparing the low stress organosilicon two-component pouring sealant according to any one of claims 1 to 8, which is characterized by comprising the following steps:
1) Preparing a base material: blending and dehydrating single-ended vinyl silicone oil, a first heat-conducting filler, a second heat-conducting filler and methyl silicone oil, then adding a filler treating agent to treat the first heat-conducting filler and the second heat-conducting filler, and then continuing blending and dehydrating to obtain a base material;
2) And (3) preparing a component A: uniformly mixing the base material, the methyl silicone oil and the platinum catalyst, and vacuumizing to remove bubbles to obtain a component A;
3) And (3) preparing a component B: uniformly mixing the base material, the methyl silicone oil, the hydrogen-containing silicone oil and the inhibitor, and vacuumizing to remove bubbles to obtain a component B;
4) Preparing organic silicon pouring sealant: the component A prepared in the step 2) and the component B prepared in the step 3) are mixed according to the weight ratio of 1:1, and vacuumizing to remove bubbles, thus obtaining the organic silicon pouring sealant.
10. The method of claim 9, wherein the step of determining the position of the substrate comprises,
the step (1) is specifically as follows:
blending and dehydrating single-end vinyl silicone oil, a first heat conducting filler, a second heat conducting filler and methyl silicone oil at the temperature of 120-130 ℃ and the vacuum degree of less than or equal to minus 0.095MPa for 1-5 h; cooling to 70-90 ℃, adding a filler treating agent, and preserving heat for 0.5-2 h; and raising the temperature to 120-130 ℃ again, and carrying out blending dehydration for 1-2 h under the vacuum degree of less than or equal to minus 0.095MPa to obtain the base material.
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