CN115109561A - Organic silicon gel and preparation method applying IGBT packaging - Google Patents
Organic silicon gel and preparation method applying IGBT packaging Download PDFInfo
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- CN115109561A CN115109561A CN202210860375.XA CN202210860375A CN115109561A CN 115109561 A CN115109561 A CN 115109561A CN 202210860375 A CN202210860375 A CN 202210860375A CN 115109561 A CN115109561 A CN 115109561A
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- percha
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 25
- 239000010703 silicon Substances 0.000 title claims abstract description 25
- 238000004806 packaging method and process Methods 0.000 title claims description 16
- 238000002360 preparation method Methods 0.000 title description 8
- 238000001879 gelation Methods 0.000 title description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 62
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 56
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 48
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 42
- 239000000899 Gutta-Percha Substances 0.000 claims abstract description 41
- 240000000342 Palaquium gutta Species 0.000 claims abstract description 41
- 229920000588 gutta-percha Polymers 0.000 claims abstract description 41
- 229920002545 silicone oil Polymers 0.000 claims abstract description 40
- 229920005610 lignin Polymers 0.000 claims abstract description 33
- 239000003054 catalyst Substances 0.000 claims abstract description 31
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 31
- 239000002245 particle Substances 0.000 claims abstract description 30
- -1 polysiloxane Polymers 0.000 claims abstract description 30
- 239000003112 inhibitor Substances 0.000 claims abstract description 22
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 17
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910000077 silane Inorganic materials 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims description 39
- 239000000203 mixture Substances 0.000 claims description 27
- 229910052739 hydrogen Inorganic materials 0.000 claims description 26
- 239000001257 hydrogen Substances 0.000 claims description 26
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 21
- 239000002904 solvent Substances 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 19
- 239000003292 glue Substances 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 9
- 238000004821 distillation Methods 0.000 claims description 8
- 238000004513 sizing Methods 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 238000003786 synthesis reaction Methods 0.000 claims description 7
- 239000003963 antioxidant agent Substances 0.000 claims description 6
- 230000003078 antioxidant effect Effects 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 229920001971 elastomer Polymers 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 3
- AZIQALWHRUQPHV-UHFFFAOYSA-N prop-2-eneperoxoic acid Chemical compound OOC(=O)C=C AZIQALWHRUQPHV-UHFFFAOYSA-N 0.000 claims description 3
- 239000000306 component Substances 0.000 description 46
- 239000000499 gel Substances 0.000 description 44
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 12
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 7
- 238000013016 damping Methods 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 238000001308 synthesis method Methods 0.000 description 6
- 150000002431 hydrogen Chemical class 0.000 description 4
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 3
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 3
- 241000208689 Eucommia ulmoides Species 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 239000008096 xylene Substances 0.000 description 3
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000002444 silanisation Methods 0.000 description 2
- IFTRQJLVEBNKJK-UHFFFAOYSA-N Aethyl-cyclopentan Natural products CCC1CCCC1 IFTRQJLVEBNKJK-UHFFFAOYSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- 239000004970 Chain extender Substances 0.000 description 1
- 241000208688 Eucommia Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- IIEWJVIFRVWJOD-UHFFFAOYSA-N ethyl cyclohexane Natural products CCC1CCCCC1 IIEWJVIFRVWJOD-UHFFFAOYSA-N 0.000 description 1
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
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Classifications
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- 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
- C09J11/08—Macromolecular additives
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
- H01L21/56—Encapsulations, e.g. encapsulation layers, coatings
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
- H01L23/293—Organic, e.g. plastic
- H01L23/296—Organo-silicon compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the technical field of silicone gel, in particular to an organic silicone gel, which comprises a component A and a component B: wherein, the component A comprises: 50-100 parts of vinyl silicone oil and 0.1-10 parts of platinum catalyst by mass; wherein, the component B comprises: 50-100 parts of vinyl silicone oil, 10-50 parts of silane modified gutta-percha particles, 0.1-1 part of cross-linking agent, 0.1-20 parts of lignin modified hydrogenous polysiloxane and 0.1-10 parts of inhibitor; the component A and the component B are mixed according to the mass ratio of 5-0.5: 1 to obtain the organic silicon gel.
Description
Technical Field
The invention relates to the technical field of silicone gel, in particular to an organic silicone gel and a preparation method applying IGBT packaging.
Background
At present, the IGBT module is widely applied to the fields of rail transit, automotive electronics, power grids, communication, household appliances and the like, and is one of the core components of electronic products. In practical application, the IGBT module is often required to operate in severe environments such as high temperature change, high humidity, high temperature, and the like, and therefore, higher requirements are put on the sealing protection of the IGBT.
The organic silicon gel has various excellent performances such as good temperature resistance, weather resistance, shock absorption and self-repairing performance and is widely applied to IGBT module packaging, but the existing organic silicon gel is generally an addition system, so that in practical application, obvious performance weakness of poor bonding performance exists, and risks are brought to the sealing performance of IGBT packaging, meanwhile, the organic silicon gel often needs good construction manufacturability, and the cross-linking density is low generally, so that the damping performance is weak, and challenges are brought to the shock absorption performance of the organic silicon gel.
Disclosure of Invention
The invention aims to solve the technical problems brought forward by the technical background and provides an organic silicon gel and a preparation method applying IGBT packaging.
In order to achieve the above purpose, the present invention is widely applied to the technical scheme of silicone gel, and particularly provides the following technical scheme: a silicone gel comprising a component a and a component B:
wherein, the component A comprises:
50-100 parts of vinyl silicone oil,
0.1-10 parts of platinum catalyst by mass;
wherein, the component B comprises:
50-100 parts of vinyl silicone oil,
10-50 parts of silane modified gutta-percha particles,
0.1 to 1 part of a crosslinking agent,
0.1 to 20 parts of lignin modified hydrogenous polysiloxane,
0.1-10 parts of inhibitor, and mixing the raw materials in parts by weight;
the component A and the component B are mixed according to the mass ratio of 5-0.5: 1 to obtain the organic silicon gel.
Preferably, the component A is prepared by adding vinyl silicone oil into a platinum catalyst, uniformly stirring, and finally performing vacuum defoaming treatment under the pressure of 0.08-0.1 MPa.
Preferably, the component B is prepared by sequentially adding vinyl silicone oil, silanized modified gutta-percha particles, a cross-linking agent, lignin modified hydrogenpolysiloxane, an inhibitor and an antioxidant into a stirring kettle, uniformly stirring, and finally performing defoaming treatment under the pressure of 0.08-0.1 MPa.
Preferably, the content of the vinyl silicone oil is 0.1-5% by mass, wherein the viscosity is 1000-10000 mPa.s.
Preferably, the cross-linking agent is hydrogen-terminated polydimethylmethylhydrogensiloxane, the hydrogen mass ratio of which is 0.03-0.3%, and the viscosity of which is 10-1000 mPas.
Preferably, the inhibitor is a vinyl ring inhibitor, and the vinyl content of the inhibitor is 0.01-1%.
Preferably, the synthesis of the silane-modified gutta percha particle comprises the following steps:
cutting endosperm of gutta Percha into small particles, transferring into a round bottom flask equipped with a magnetic stirrer, adding solvent, and heating to 50-100 deg.C; and dropwise adding a mixture of H2O2 and pure water under stirring of a stirrer, wherein the mass ratio of the mixture of H2O2 and pure water is 0.1-10: 1;
stirring the mixture at 50-100 deg.C for 2-6 hr, and centrifuging to remove impurities and water to obtain purified gutta-percha solution;
adding the purified gutta-percha solution and a platinum catalyst into a four-neck round-bottom flask, stirring the mixture at 20-60 ℃ for 1-3h, heating to 90-120 ℃ for reaction for 1-4h, and then carrying out reduced pressure distillation to remove the solvent to obtain the silane modified gutta-percha particles.
Preferably, the synthesis of the lignin-modified hydrogenpolysiloxane comprises the following steps:
mixing 1-100g of hydrogen-containing polysiloxane, 1-100g of hydroxyl acrylate and a solvent, heating to 30-60 ℃, then dripping a platinum catalyst, heating to 70-100 ℃, and stirring for 1-4 hours;
adding 10-100g lignin, heating to 80-120 deg.C, stirring for 1-4h, filtering to remove solid lignin, distilling under reduced pressure, and removing solvent to obtain lignin-modified hydrogenous polysiloxane.
According to the above, the preparation method of the organic silicon gel applied IGBT package comprises the following steps:
placing the IGBT module at 80-100 ℃ for pre-drying for 20-24 h before glue filling to remove residual moisture;
when the glue starts, the component A and the component B are mixed according to the mass ratio of 5-0.5: 1, uniformly mixing to obtain a sizing material;
pouring the sizing material into the preheated IGBT module, and defoaming in vacuum for 5-10 min under the pressure of 0.08-0.1 MPa;
and (4) after the glue filling and bonding is finished, curing for 1-5 hours at the temperature of 80-120 ℃ to finish packaging the IGBT module.
Compared with the prior art, the invention has the beneficial effects that:
(1) the gutta-percha is purified from the biomass eucommia ulmoides tree and then is subjected to silanization modification to obtain modified gutta-percha particles which are better compatible with the organic silicon body, and the mechanical strength of the organic silicon gel is effectively improved, the damping performance of the organic silicon gel is improved, and the damping performance of the organic silicon gel is improved by introducing the gutta-percha particles;
(2) according to the invention, lignin is subjected to silanization modification, and a lignin group is introduced into the main chain of the polysiloxane group, so that the hydroxyl content in an organic silicon gel system is effectively increased, and the bonding performance and the waterproof performance of the organic silicon gel are effectively improved;
(3) the invention comprises the following steps that A component and B component are mixed according to the mass ratio of 5-0.5: 1 to obtain the organic silicon gel, and the organic silicon gel with high adhesion and high damping can be obtained by the design; the crosslinking density is effectively designed and adjusted by adjusting the molar ratio of Si to Vi to H, so that the hardness and the repairability of the silica gel are ensured;
(4) the invention adopts the organic silicon gel to package the IGBT, so that the packaged IGBT has good sealing performance, good damping performance, strong shock absorption performance and strong temperature resistance.
Drawings
FIG. 1 shows the performance test results of silicone gel prepared according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment provided by the invention comprises the following steps:
a silicone gel comprising a component a and a component B:
wherein, the component A comprises:
50-100 parts of vinyl silicone oil,
0.1-10 parts of platinum catalyst by mass;
wherein, the component B comprises:
50-100 parts of vinyl silicone oil,
10-50 parts of silane modified gutta-percha particles,
0.1 to 1 part of a crosslinking agent,
0.1 to 20 parts of lignin modified hydrogenous polysiloxane,
0.1-10 parts of inhibitor, and mixing the raw materials in parts by weight;
the component A and the component B are mixed according to the mass ratio of 5-0.5: 1 to obtain the organic silicon gel.
Further, the component A is prepared by adding vinyl silicone oil into a platinum catalyst, uniformly stirring, and finally performing vacuum defoaming treatment under the pressure of 0.08-0.1 MPa.
Further, the component B is prepared by sequentially adding vinyl silicone oil, silanized modified gutta-percha particles, a cross-linking agent, lignin modified hydrogenpolysiloxane, an inhibitor and an antioxidant into a stirring kettle, uniformly stirring, and finally performing defoaming treatment under the pressure of 0.08-0.1 MPa.
Further, in order to improve the viscosity of the silicone gel, the technical scheme adopted is as follows:
the vinyl silicone oil is methyl vinyl silicone oil, the mass ratio of the content of the vinyl silicone oil is 0.1-5%, wherein the viscosity is 10000 mPa.s, the electronic grade methyl vinyl silicone oil adopts a special synthesis process, the product does not contain metal ions such as potassium, sodium and the like, and the volatile matter is less than 0.2%.
Further, in order to improve the strength and toughness of the silicone gel, the technical scheme adopted is as follows:
the cross-linking agent is hydrogen-terminated polydimethylmethylhydrogensiloxane, the terminal group and the side group of which both contain Si-H groups, so that the cross-linking agent and the chain extender can play a role, and the strength and the toughness of the organic silicon gel are improved. The hydrogen content is 0.03-0.3%, the viscosity is 10-1000 mPa.s, and the volatilization is less than 0.2%.
Furthermore, the inhibitor is a vinyl ring inhibitor, and the vinyl content of the inhibitor is 0.01-1%.
Further, the synthesis of the silane modified gutta percha particle comprises the following steps:
cutting endosperm of gutta Percha into small particles, transferring into a round bottom flask equipped with a magnetic stirrer, adding solvent, and heating to 50-100 deg.C; and dropwise adding a mixture of H2O2 and pure water under stirring of a stirrer, wherein the mass ratio of the mixture of H2O2 and pure water is 0.1-10: 1;
stirring the mixture at 50-100 deg.C for 2-6 hr, and centrifuging to remove impurities and water to obtain purified gutta-percha solution;
adding the purified gutta-percha solution and a platinum catalyst into a four-neck round-bottom flask, stirring the mixture at 20-60 ℃ for 1-3h, heating to 90-120 ℃ for reaction for 1-4h, and then carrying out reduced pressure distillation to remove the solvent to obtain silane modified gutta-percha particles;
wherein the endosperm of the gutta-percha is one or more of folium Eucommiae, root Eucommiae, and seed shell of Eucommiae cortex; the solvent is one or a combination of toluene, xylene, cyclohexane, petroleum ether and cyclopentane; the curing agent is methyl phenyl hydrogen-containing silicone oil, the mass ratio of hydrogen content is 0.1-0.8%, the mass ratio of phenyl content is 10-50%, the purity is more than 99.98%, and the viscosity is 10-1000mPa & s.
Further, the synthesis of the lignin modified hydrogenpolysiloxane comprises the following steps:
mixing 1-100g of hydrogen-containing polysiloxane, 1-100g of hydroxyl acrylate and a solvent, heating to 30-60 ℃, then dripping a platinum catalyst, heating to 70-100 ℃, and stirring for 1-4 hours;
adding 10-100g lignin, heating to 80-120 deg.C, stirring for 1-4h, filtering to remove solid lignin, distilling under reduced pressure, and removing solvent to obtain lignin-modified hydrogenous polysiloxane.
According to the above, the method for packaging the IGBT by using the silicone gel comprises the following steps:
placing the IGBT module at 80-100 ℃ for pre-drying for 20-24 h before glue filling to remove residual moisture;
when the glue starts, the component A and the component B are mixed according to the mass ratio of 5-0.5: 1, uniformly mixing to obtain a sizing material;
pouring the sizing material into the preheated IGBT module, and defoaming in vacuum for 5-10 min under the pressure of 0.08-0.1 MPa;
and (4) after the glue filling and bonding is finished, curing for 1-5 hours at the temperature of 80-120 ℃ to finish packaging the IGBT module.
Wherein the hydrogen-containing polysiloxane is methyl phenyl hydrogen-containing silicone oil, the mass ratio of hydrogen content is 0.1-0.8%, the mass ratio of phenyl content is 10-50%, the purity is more than 99.98%, and the viscosity is 10-1000mPa & s; the hydroxy acrylic ester is one or a combination of hydroxyethyl acrylate and hydroxyethyl methacrylate; the solvent is one or a combination of toluene, xylene, ethyl acetate, cyclohexane and cyclopentane; the lignin is one or more of acid lignin, alkali lignin and lignin salt.
Example 1
The organic silicon gel comprises a component A and a component B, wherein the component A is prepared by mixing the following raw materials in parts by weight:
90kg of vinyl silicone oil is added,
0.2kg of platinum catalyst;
the component B is prepared by mixing the following raw materials in parts by mass:
wherein the vinyl silicone oil is electronic grade methyl-end vinyl silicone oil with 0.30 percent of vinyl content, and the viscosity is 1000 mPa.s; the cross-linking agent is hydrogen-terminated polydimethylmethylhydrosiloxane, the hydrogen content of which is 0.50 percent and the viscosity of which is 15mPa & s; wherein the platinum catalyst is a transception platinum catalyst (5000 ppm); the inhibitor is vinyl ring body, and the vinyl content is 0.05%; the molar ratio of Si-Vi: Si: H in the silicone gel was 1.2.
The silane modified gutta-percha particles are self-made in a laboratory, and the synthesis method comprises the following steps:
(1) 100g of eucommia ulmoides seed husk was cut into small particles, and then transferred to a round-bottomed flask equipped with a magnetic stirrer, and 300g of ethyl acetate was added, the mixer was heated to 60 ℃, and a mixture of H2O2 and pure water (mass ratio: 1) was added dropwise with stirring. The mixture was stirred at 90 ℃ for 6 hours. Centrifuging to remove impurities and water to obtain purified gutta-percha solution.
(2) The purified gutta percha solution and platinum catalyst were added to a four-necked round bottom flask, and the mixture was stirred at 60 ℃ for 3 hours. Methyl phenyl hydrogen-containing silicone oil (hydrogen-containing mass ratio of 0.16%) was added dropwise to the flask. The mixture was stirred at 60 ℃ for 3 hours and then heated to 120 ℃ for 4 hours. And carrying out reduced pressure distillation to remove the solvent, thereby obtaining the silane modified gutta-percha particles.
The lignin modified hydrogenous polysiloxane is self-made in a laboratory, and the synthesis method comprises the following steps:
(1) 50g of hydrogen-containing polysiloxane (with the hydrogen mass ratio of 0.25 percent), 22g of hydroxyethyl acrylate and dimethylbenzene are mixed and uniformly mixed, the temperature is raised to 60 ℃, then a platinum catalyst is dripped, the temperature is raised to 100 ℃, and the mixture is stirred for 4 hours.
(2) Adding 100g of lignin, heating to 90 ℃, stirring for 4h, filtering to remove solid lignin, carrying out reduced pressure distillation, and removing the solvent to obtain the lignin-modified hydrogenous polysiloxane.
The preparation method of the organosilicone gel comprises the following steps:
(1) adding the vinyl silicone oil into a platinum catalyst, uniformly stirring, and finally carrying out vacuum defoaming treatment under the pressure of 0.1MPa to obtain a component A;
(2) sequentially adding vinyl silicone oil, silanized modified gutta-percha particles, a cross-linking agent, lignin modified hydrogen-containing polysiloxane, an inhibitor and an antioxidant into a stirring kettle, uniformly stirring, and finally performing defoaming treatment under the pressure of 0.1MPa to obtain the component B.
The application of the silicone gel in the IGBT packaging of the embodiment specifically comprises the following steps:
(1) placing the IGBT module at 100 ℃ for pre-drying for 24 hours to remove residual moisture before glue pouring;
(2) when glue pouring is started, mixing the component A and the component B according to a mass ratio of 1:1, uniformly mixing to obtain a sizing material;
(3) pouring the rubber material into the preheated IGBT module, and defoaming for 10min under the pressure of 0.08 in vacuum;
(4) and after the glue is poured, curing for 1h at the temperature of 120 ℃ to finish the packaging of the IGBT module.
The silicone gel of this example was tested for properties and the results are shown in table 1.
Example 2
The organic silicon gel comprises a component A and a component B, wherein the component A is prepared by mixing the following raw materials in parts by mass:
95kg of vinyl silicone oil is added,
0.2kg of platinum catalyst;
the component B is prepared by mixing the following raw materials in parts by mass:
wherein the vinyl silicone oil is electronic grade methyl-end vinyl silicone oil with 0.22 percent of vinyl content, and the viscosity is 2000 mPa.s; the cross-linking agent is hydrogen-terminated polydimethylmethylhydrosiloxane, the hydrogen content of which is 0.40 percent and the viscosity of which is 25mPa & s; wherein the platinum catalyst is a transception platinum catalyst (5000 ppm); the inhibitor is vinyl ring body, and the vinyl content is 0.05%; the molar ratio of Si-Vi: Si: H in the silicone gel was 1.43.
The silane modified gutta-percha particles are self-made in a laboratory, and the synthesis method comprises the following steps:
(1) 80g of eucommia ulmoides leaf was cut into small particles, and then transferred to a round-bottomed flask equipped with a magnetic stirrer, and 300g of ethyl acetate was added, the mixer was heated to 70 ℃, and a mixture of H2O2 and pure water (mass ratio of 1.4:1) was added dropwise with stirring. The mixture was stirred at 80 ℃ for 4 hours. Centrifuging to remove impurities and water to obtain purified gutta-percha solution.
(2) The purified gutta percha solution and platinum catalyst were added to a four-necked round bottom flask, and the mixture was stirred at 50 ℃ for 2 h. Methyl phenyl hydrogen-containing silicone oil (hydrogen-containing mass ratio of 0.23%) was added dropwise to the flask. The mixture was stirred at 50 ℃ for 3 hours and then heated to 120 ℃ for reaction for 3 hours. And distilling under reduced pressure to remove the solvent to obtain the silane modified gutta percha particles.
The lignin modified hydrogenous polysiloxane is self-made in a laboratory, and the synthesis method comprises the following steps:
(1) 100g of hydrogen-containing polysiloxane (with the mass ratio of hydrogen being 0.15 percent), 34g of hydroxyethyl methacrylate and ethyl acetate are mixed and evenly mixed, the temperature is raised to 50 ℃, then a platinum catalyst is dripped, the temperature is raised to 110 ℃, and the mixture is stirred for 4 hours.
(2) Adding 80g of alkali lignin, heating to 80 ℃, stirring for 2h, filtering to remove solid lignin, carrying out reduced pressure distillation, and removing the solvent to obtain the lignin-modified hydrogen-containing polysiloxane.
The preparation method of the silicone gel of the embodiment comprises the following steps:
(1) adding the vinyl silicone oil into a platinum catalyst, uniformly stirring, and finally carrying out vacuum defoaming treatment under the pressure of 0.1MPa to obtain a component A;
(2) sequentially adding vinyl silicone oil, silanized modified gutta-percha particles, a cross-linking agent, lignin modified hydrogen-containing polysiloxane, an inhibitor and an antioxidant into a stirring kettle, uniformly stirring, and finally performing defoaming treatment under the pressure of 0.1MPa to obtain the component B.
The application of the silicone gel in the IGBT packaging of the embodiment specifically comprises the following steps:
(1) placing the IGBT module at 110 ℃ for pre-drying for 24 hours before glue pouring to remove residual moisture;
(2) when glue pouring is started, the component A and the component B are mixed according to the mass ratio of 1.2: 1, uniformly mixing to obtain a sizing material;
(3) pouring the rubber material into the preheated IGBT module, and defoaming for 15min in vacuum under the pressure of 0.08;
(4) and (5) after the glue is poured, curing for 3 hours at the temperature of 80 ℃ to finish the packaging of the IGBT module.
The silicone gel of this example was tested for properties and the results are shown in table 1.
Example 3
The organic silicon gel comprises a component A and a component B, wherein the component A is prepared by mixing the following raw materials in parts by mass:
110kg of vinyl silicone oil is added into the paint,
0.2kg of platinum catalyst;
the component B is prepared by mixing the following raw materials in parts by mass:
wherein the vinyl silicone oil is electronic grade methyl-end vinyl silicone oil with 0.76 percent of vinyl content, and the viscosity is 200 mPa.s; the cross-linking agent is hydrogen-terminated polydimethylmethylhydrogensiloxane, the hydrogen content of which is 0.32 percent and the viscosity of which is 15mPa & s; wherein the platinum catalyst is a transception platinum catalyst (5000 ppm); the inhibitor is vinyl ring body, and the vinyl content is 0.05%; the molar ratio of Si-Vi: Si: H in the silicone gel was 1.15.
The silane modified gutta-percha particles are self-made in a laboratory, and the synthesis method comprises the following steps:
(1) 70g of eucommia bark was cut into small particles, which were then transferred to a round-bottomed flask equipped with a magnetic stirrer, and 200g of xylene was added, the mixer was heated to 60 ℃, and a mixture of H2O2 and pure water (mass ratio: 3:1) was added dropwise with stirring. The mixture was stirred at 100 ℃ for 5 hours. Centrifuging to remove impurities and water to obtain purified gutta-percha solution.
(2) The purified gutta percha solution and the platinum catalyst were added to a four-necked round-bottom flask, and the mixture was stirred at 60 ℃ for 3 hours. Methyl phenyl hydrogen-containing silicone oil (hydrogen-containing mass ratio of 0.32%) was added dropwise to the flask. The mixture was stirred at 60 ℃ for 4 hours and then heated to 120 ℃ for 4 hours. And carrying out reduced pressure distillation to remove the solvent, thereby obtaining the silane modified gutta-percha particles.
The lignin modified hydrogenous polysiloxane is self-made in a laboratory, and the synthesis method comprises the following steps:
(1) 100g of hydrogen-containing polysiloxane (with the mass ratio of hydrogen being 0.15 percent), 32g of hydroxyethyl acrylate and dimethylbenzene are mixed and evenly mixed, the temperature is raised to 60 ℃, then a platinum catalyst is dripped, the temperature is raised to 80 ℃, and the mixture is stirred for 3 hours.
(2) Adding 50g of lignin salt, heating to 90 ℃, stirring for 4h, filtering to remove solid lignin, carrying out reduced pressure distillation, and removing the solvent to obtain the lignin-modified hydrogenous polysiloxane.
The preparation method of the silicone gel of the embodiment comprises the following steps:
(1) adding the vinyl silicone oil into a platinum catalyst, uniformly stirring, and finally carrying out vacuum defoaming treatment under the pressure of 0.1MPa to obtain a component A;
(2) sequentially adding vinyl silicone oil, silanized modified gutta-percha particles, a cross-linking agent, lignin modified hydrogen-containing polysiloxane, an inhibitor and an antioxidant into a stirring kettle, uniformly stirring, and finally performing defoaming treatment under the pressure of 0.1MPa to obtain the component B.
The application of the silicone gel in the IGBT packaging of the embodiment specifically comprises the following steps:
(1) placing the IGBT module at 100 ℃ for pre-drying for 24 hours to remove residual moisture before glue pouring;
(2) when glue pouring is started, the component A and the component B are mixed according to the mass ratio of 1.2: 1, uniformly mixing to obtain a sizing material;
(3) pouring the rubber material into the preheated IGBT module, and defoaming for 10min under the pressure of 0.08 in vacuum;
(4) and after the glue is poured, curing for 1h at the temperature of 100 ℃ to finish packaging the IGBT module.
The silicone gel of this example was tested for properties and the results are shown in table 1.
In summary, the performance of the silicone gels of examples 1-3 were tested and the results are shown in Table 1.
Wherein the damping and adhesion properties in table 1 were determined using a texture analyzer; the process is as follows: setting the original position of the probe and the position of the sample to be penetrated, stabilizing for a period of time after reaching the original position, and then returning to the original position, wherein the force applied to the probe obtains a curve along with the change of displacement, and different materials can respond to different characteristic curves.
As can be seen from the experimental data in Table 1, the silicone gel of the present invention can endure a high temperature of 220 ℃ for a long time, is not yellowed, and can maintain good hardness, damping performance and adhesion performance; and the dielectric property, the mechanical property, the operation process property and other comprehensive properties are also excellent.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (9)
1. A silicone gel characterized by: comprises a component A and a component B:
wherein, the component A comprises:
50-100 parts of vinyl silicone oil,
0.1-10 parts of platinum catalyst by weight;
wherein, the component B comprises:
50-100 parts of vinyl silicone oil,
10-50 parts of silane modified gutta-percha particles,
0.1 to 1 part of a crosslinking agent,
0.1 to 20 parts of lignin modified hydrogenous polysiloxane,
0.1-10 parts of inhibitor is prepared by mixing the raw materials;
the component A and the component B are mixed according to the mass ratio of 5-0.5: 1 to obtain the organic silicon gel.
2. A silicone gel in accordance with claim 1, wherein: the component A is prepared by adding vinyl silicone oil into a platinum catalyst, uniformly stirring, and finally performing vacuum defoaming treatment under the pressure of 0.08-0.1 MPa.
3. A silicone gel in accordance with claim 1, wherein: and the component B is prepared by sequentially adding vinyl silicone oil, silanized modified gutta-percha particles, a cross-linking agent, lignin modified hydrogenpolysiloxane, an inhibitor and an antioxidant into a stirring kettle, uniformly stirring, and finally performing defoaming treatment under the pressure of 0.08-0.1 MPa.
4. A silicone gel in accordance with claim 1, wherein: the content mass ratio of the vinyl silicone oil is 0.1-5%, wherein the viscosity is 1000-10000mPa & s.
5. A silicone gel in accordance with claim 1, wherein: the cross-linking agent is hydrogen-terminated polydimethylmethylhydrogensiloxane, the hydrogen mass ratio of which is 0.03-0.3%, wherein the viscosity is 10-1000mPa & s.
6. A silicone gel in accordance with claim 1, wherein: the inhibitor is a vinyl ring inhibitor, and the vinyl content of the inhibitor is 0.01-1%.
7. A silicone gel in accordance with claim 1, wherein: the synthesis of the silane modified gutta-percha particles comprises the following steps:
cutting endosperm of gutta Percha into small particles, transferring into a round bottom flask equipped with a magnetic stirrer, adding solvent, and heating to 50-100 deg.C; and dropwise adding a mixture of H2O2 and pure water under stirring of a stirrer, wherein the mass ratio of the mixture of H2O2 and pure water is 0.1-10: 1;
stirring the mixture at 50-100 deg.C for 2-6 hr, and centrifuging to remove impurities and water to obtain purified gutta-percha solution;
adding the purified gutta-percha solution and a platinum catalyst into a four-neck round-bottom flask, stirring the mixture at 20-60 ℃ for 1-3h, heating to 90-120 ℃ for reaction for 1-4h, and then carrying out reduced pressure distillation to remove the solvent to obtain the silane modified gutta-percha particles.
8. A silicone gel in accordance with claim 1, wherein: the synthesis of the lignin modified hydrogenpolysiloxane comprises the following steps:
mixing 1-100g of hydrogen-containing polysiloxane, 1-100g of hydroxyl acrylate and a solvent, heating to 30-60 ℃, then dripping a platinum catalyst, heating to 70-100 ℃, and stirring for 1-4 h;
adding 10-100g lignin, heating to 80-120 deg.C, stirring for 1-4h, filtering to remove solid lignin, distilling under reduced pressure, and removing solvent to obtain lignin-modified hydrogenous polysiloxane.
9. The method of preparing a silicone gel application IGBT package according to any one of claims 1-8, characterized in that:
placing the IGBT module at 80-100 ℃ before glue pouring, and pre-drying for 20-24 h to remove residual moisture;
when the glue starts, the component A and the component B are mixed according to the mass ratio of (5-0.5): 1, uniformly mixing to obtain a sizing material;
pouring the rubber material into the preheated IGBT module, and performing vacuum deaeration for 5-10 min under the pressure of 0.08-0.1 MPa;
and (4) after the glue filling and bonding is finished, curing for 1-5 hours at the temperature of 80-120 ℃ to finish packaging the IGBT module.
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| CN115820207A (en) * | 2023-01-05 | 2023-03-21 | 重庆云潼科技有限公司 | Lignin-based silicon gel and preparation method thereof, application of lignin-based silicon gel in IGBT and IGBT packaging structure |
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| CN102964844A (en) * | 2012-12-31 | 2013-03-13 | 上海回天化工新材料有限公司 | Transparent organic silica gel for electronic encapsulation |
| CN103045159A (en) * | 2013-01-31 | 2013-04-17 | 株洲时代新材料科技股份有限公司 | Double-component organic silica gel for packaging of large power IGBT (insulated bipolar translator) and preparation method thereof |
| CN106336469A (en) * | 2016-09-12 | 2017-01-18 | 沈阳化工大学 | Synthesis method of self-repairing elastomer material based on eucommia rubber |
| CN106397635A (en) * | 2016-08-31 | 2017-02-15 | 北京化工大学 | Biobased silicon-containing alternating EP rubber and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102964844A (en) * | 2012-12-31 | 2013-03-13 | 上海回天化工新材料有限公司 | Transparent organic silica gel for electronic encapsulation |
| CN103045159A (en) * | 2013-01-31 | 2013-04-17 | 株洲时代新材料科技股份有限公司 | Double-component organic silica gel for packaging of large power IGBT (insulated bipolar translator) and preparation method thereof |
| CN106397635A (en) * | 2016-08-31 | 2017-02-15 | 北京化工大学 | Biobased silicon-containing alternating EP rubber and preparation method thereof |
| CN106336469A (en) * | 2016-09-12 | 2017-01-18 | 沈阳化工大学 | Synthesis method of self-repairing elastomer material based on eucommia rubber |
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| CN115820207A (en) * | 2023-01-05 | 2023-03-21 | 重庆云潼科技有限公司 | Lignin-based silicon gel and preparation method thereof, application of lignin-based silicon gel in IGBT and IGBT packaging structure |
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