CN105504823A - High-temperature-resistant organosilicone powder encapsulating material and preparation method thereof - Google Patents
High-temperature-resistant organosilicone powder encapsulating material and preparation method thereof Download PDFInfo
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- CN105504823A CN105504823A CN201610057401.XA CN201610057401A CN105504823A CN 105504823 A CN105504823 A CN 105504823A CN 201610057401 A CN201610057401 A CN 201610057401A CN 105504823 A CN105504823 A CN 105504823A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of 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; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- 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
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- 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
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- 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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- 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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- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a high-temperature-resistant organosilicone powder encapsulating material and a preparation method thereof. The high-temperature-resistant organosilicone powder encapsulating material is mainly prepared from, by weight, 20-50 parts of organosilicone resin, 0.1-5 parts of catalyst, 1-5 parts of pigment, 40-70 parts of filler, 3-6 parts of flexibilizer, 0.3-1 part of thixotropic agent, 0.1 part of coupling reagent, 0.5 part of defoamer and 0.1-5 parts of other auxiliaries. The preparation method of the encapsulating material comprises the steps of mixing, extruding, crushing and classification and thixotropic agent mixing. Encapsulating is conducted through a fluidized bed with compressed air in the using process. The encapsulating material does not contain solvents such as xylene and isopropanol, poisonous and harmful micromolecules are not emitted in the solidification process, and the high-temperature-resistant organosilicone powder encapsulating material is excellent in insulating property, green, environmentally friendly, resistant to high temperature, fast in heat dissipation and suitable for high-temperature-resistant electron components such as piezoresistors and thermistors.
Description
Technical field
The present invention relates to a kind of high-temperature resistant silicone powder encapsulating material, it be a kind of based on silicone resin, the heat conductive filler such as silica flour or aluminum oxide is main stuffing, the electronic devices and components encapsulating material of solvent-free, high temperature resistant, excellent insulating property.
Background technology
In Electronic Packaging field, main employing epoxy resin, resol and silicone resin are as matrix resin, coordinate solidifying agent, filler, auxiliary agent to reach the effect of insulation, heat-resisting, exclusion of water steam, for thermistor, its working temperature is minimum reaches-40 DEG C, reach as high as 250 DEG C, therefore resistance to gentleness heat radiation becomes the crucial Con trolling index of thermistor encapsulating material, and under the overall situation day by day strengthened in current environmental consciousness, the important requirement green, environmental protection also becomes thermistor encapsulating material.
Field more than 200 DEG C is required in heatproof, thermistor mainly adopts solvent-type organosilicon impregnation enveloping material, this kind of encapsulating material has excellent high thermal resistance, thermal diffusivity, insulativity and flame retardant resistance, but also there is serious problem, these problems mainly contain: 1, solvent, and this type of impregnation enveloping material adopts toluene, dimethylbenzene, Virahol, propyl carbinol equal solvent mostly, have solvent to release in solidification process, contaminate environment, endangers healthy; 2, solidification intensity is low, and because this type of encapsulating material uses solvent and filler in a large number, organic part contained by final cured article is little, and material is hard and crisp, easily embrittlement occurs during post-treatment, limits the application of product.
Require in 180 DEG C of fields in heatproof, thermistor mainly adopts solvent-borne type resin impregnating encapsulating material, this kind of encapsulating material has excellent high thermal resistance, thermal diffusivity, insulativity and flame retardant resistance, but there is the problem identical with organosilicon impregnation enveloping material: 1, solvent, this type of impregnation enveloping material adopts toluene, dimethylbenzene, Virahol, propyl carbinol equal solvent mostly, there is solvent to release in solidification process, contaminate environment, endanger healthy; 2, solidification intensity is low, and because this type of encapsulating material uses solvent and filler in a large number, organic part contained by final cured article is little, and material is hard and crisp, easily embrittlement occurs during post-treatment, limits the application of product.
In sum, there is larger problem in current thermistor impregnation enveloping material, therefore, provides a kind of environmental protection, high temperature resistant, that rapid heat dissipation, intensity are high novel encapsulating material has great using value and environment protection significance.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of thermistor high temperature resistance phenolic aldehyde powder encapsulating material is provided, solve the solvent harm problem of existing phenolic impregnated encapsulating material and the problem of intensity difference.
The technical scheme that the present invention realizes object is as follows:
A kind of high-temperature resistant silicone powder encapsulating material, composed of the following components: silicone resin 20 ~ 50 parts, catalyzer 0.1 ~ 5 part, pigment 1 ~ 5 part, filler 40 ~ 70 parts, toughner 3 ~ 6 parts, thixotropic agent 0.3 ~ 1 part, coupling agent 0.1 part, defoamer 0.5 part, other auxiliary agents 0.1 ~ 5 part, amount to 100 parts, each component by weight.
And described silicone resin is the combination of one or more in methyl silicon resin, phenyl methyl silicone resin, phenyl polysiloxane, MQ silicone resin, vinyl polysiloxane, polyester modification silicone resin, epoxide modified silicone resin, phenol aldehyde modified silicone resin.
And described catalyzer is aluminium acetylacetonate, dibutyl tin dilaurate, tin protochloride, isoflurane chalcone diisocyanate and derivative, 1, the combination of one or more in 2 aminoundecane-earboxylic acids, aminosilane.
And, described filler be the combination of one or more in aluminium sesquioxide, silicon nitride, graphite, light calcium carbonate, water-ground limestone, barium sulfate, titanium dioxide, glass powder with low melting point, silicon powder, mica powder, talcum powder, kaolin.
And described packing material size is between 75 μm ~ 18 μm.
And described pigment is the combination of one or more in aluminium powder, chrome green, carbon black, chrome yellow, the husky Huang of the Chinese, ultramarine, the blue or green orchid of phthalein, red iron oxide.
And described toughner is the combination of one or more in carboxy nitrile rubber, nbr carboxyl terminal, thiorubber, polyethers, polysulfones, polyimide, nano-calcium carbonate, nano titanium oxide, acrylic elastomer, chloroprene rubber, chlorosulfonated polyethylene, ABS resin, SBS resin, SEBS resin, Vinyl Acetate Copolymer, containing hydrogen silicone oil, hydroxy silicon oil, silicon rubber, viton, polyvinyl butyral acetal.
And described thixotropic agent is the combination of one or more in wilkinite, white carbon black, gaseous oxidation aluminium, polyamide wax.
Prepare a method for high-temperature resistant silicone powder encapsulating material, step is as follows:
(1) mix, in formula, each component all needs by 100 eye mesh screens, except coupling agent and thixotropic agent, each component all mixes in high-speed mixer, mixing velocity 20 ~ 80Hz, adopts the mode of spraying to add coupling agent after 10 ~ 30 minutes, continuing mixing 40 ~ 90 minutes, is raw material after completing mixing;
(2) extrude, mixed rear raw material input forcing machine and extruded, forcing machine rotating speed 30 ~ 50Hz, district's temperature 50 ~ 100 DEG C, two district's temperature 70 ~ 130 DEG C, three district's temperature 70 ~ 130 DEG C;
(3) crushing and classification, adopts the disintegrating apparatus with separator, rotating screen, dust removal cabinet to pulverize, and gained powder need by 80 ~ 200 eye mesh screens, and now powder is work in-process;
(4) mix thixotropic agent, 1 ~ 3kg is got from work in-process, add the thixotropic agent of work in-process total mass 1.0 ~ 3.0 ‰, disperse in high speed disintegrator, frequency is 100 ~ 300 hertz, 1 ~ 3 minute time, is dropped in mixing tank by all work in-process and mixes after having disperseed, hybrid frequency 1 ~ 10Hz, mixing time 30 ~ 120 minutes.
The using method of organosilicon encapsulating material, is divided into components and parts preheating, fluidized-bed encapsulation, components and parts heating levelling, secondary encapsulating, thermofixation 5 steps.
Advantage of the present invention and positively effect are:
Present invention, avoiding and avoid use solvent, environmental protection, healthy useful to operator; Add the intensity of cured article, tighter to the protection of thermistor.
Embodiment
Below embodiments of the invention are further described; The present embodiment is descriptive, is not determinate, can not limit protection scope of the present invention thus.
Embodiment 1
A kind of high-temperature resistant silicone powder encapsulating material, each component composed as follows:
Each component by weight.
The preparation concrete steps of organosilicon encapsulating material are as follows:
(1) mix, except coupling agent and thixotropic agent, each component all mixes in high-speed mixer, mixing velocity 50Hz, adopts the mode of spraying to add coupling agent after 10 minutes, continues mixing 40 minutes, is raw material after completing mixing;
(2) extrude, mixed rear raw material input forcing machine and extruded, forcing machine rotating speed 30Hz, district's temperature 70 C, two district's temperature 90 DEG C, three district's temperature 90 DEG C;
(3) crushing and classification, adopts the disintegrating apparatus with separator, rotating screen, dust removal cabinet to pulverize, and gained powder need by 120 eye mesh screens, and now powder is work in-process;
(4) mix thixotropic agent, in work in-process, add thixotropic agent, and mix in mixing tank, hybrid frequency 1Hz, mixing time 30 minutes.
The using method of organosilicon encapsulating material should operate as follows:
(1) the preheating of components and parts, components and parts need to heat wherein preheating 10 minutes at baking oven, continuous tunnel furnace etc.;
(2) encapsulate, the element after preheating is encapsulated through fluidized-bed encapsulation equipment;
(3) levelling, after encapsulating, components and parts enter the heating installation such as baking oven, continuous tunnel furnace 2 minutes, and surface containment material reaches levelling state;
(4) repeat (2) (3) two steps;
(5) solidify, the present invention adopts the method for thermofixation, and 150 DEG C solidify 0.5 hour, and 180 degrees Celsius solidify 2 hours.
Embodiment 2
A kind of high-temperature resistant silicone powder encapsulating material, each component composed as follows:
Each component by weight.
The preparation concrete steps of organosilicon encapsulating material are as follows:
(1) mix, except coupling agent and thixotropic agent, each component all mixes in high-speed mixer, mixing velocity 50Hz, adopts the mode of spraying to add coupling agent after 10 minutes, continues mixing 40 minutes, is raw material after completing mixing;
(2) extrude, mixed rear raw material input forcing machine and extruded, forcing machine rotating speed 30Hz, district's temperature 70 C, two district's temperature 90 DEG C, three district's temperature 90 DEG C;
(3) crushing and classification, adopts the disintegrating apparatus with separator, rotating screen, dust removal cabinet to pulverize, and gained powder need by 120 eye mesh screens, and now powder is work in-process;
(4) mix thixotropic agent, in work in-process, add thixotropic agent, and mix in mixing tank, hybrid frequency 1Hz, mixing time 30 minutes.
The using method of organosilicon encapsulating material should operate as follows:
(1) the preheating of components and parts, components and parts need to heat wherein preheating 10 minutes at baking oven, continuous tunnel furnace etc.;
(2) encapsulate, the element after preheating is encapsulated through fluidized-bed encapsulation equipment;
(3) levelling, after encapsulating, components and parts enter the heating installation such as baking oven, continuous tunnel furnace 2 minutes, and surface containment material reaches levelling state;
(4) repeat (2) (3) two steps;
(5) solidify, the present invention adopts the method for thermofixation, and 150 DEG C solidify 0.5 hour, and 180 degrees Celsius solidify 2 hours.
Comparative example 1
This routine organosilicon impregnation enveloping material used is divided into A, B two components, uses step as follows:
1, mix, mix in following ratio,
Silicone fluid impregnant component A10kg
Dimethylbenzene 3kg
Silicone fluid impregnant B component 100g
For subsequent use after mixing rear placement 24h.
2, dipping coating, immerses in silicone fluid impregnant by thermistor, leave standstill and slowly take out after 2 seconds.
3, air-dry, after having flooded, need draughty indoor standing and drying 8 hours.
4, solidify, adopt the method for thermofixation, ladder-elevating temperature solidifies, 70 DEG C of * 30min → 100 DEG C * 30min arrow 140 DEG C of * 30min → 160 DEG C * 2h.
Table 1 organosilicon encapsulating material and organosilicon impregnation enveloping material performance comparison
Note: cold-hot impact: be that the destructive test that ftractures is occurred in the environment of high temperature and low temperature successively alternation to the coating of electronic devices and components; The design temperature of high temperature and time length all can require to set according to difference, and low temperature is also like this; The resistance to high temperature of coating and a low temperature, be called a circulation; The cycle index of coating before cracking is more, and its cold-hot impact property is better.
Cold-hot impact condition involved in the present invention: high temperature is set as+125 DEG C, and low temperature is set as-40 DEG C, and a high temperature and a low temperature continuous time are 30min, voltage dependent resistor magnetic sheet used, diameter 20 Φ, often organizes experiment 10 prints.
Claims (10)
1. a high-temperature resistant silicone powder encapsulating material, it is characterized in that: composed of the following components: silicone resin 20 ~ 50 parts, catalyzer 0.1 ~ 5 part, pigment 1 ~ 5 part, filler 40 ~ 70 parts, toughner 3 ~ 6 parts, thixotropic agent 0.3 ~ 1 part, coupling agent 0.1 part, defoamer 0.5 part, other auxiliary agents 0.1 ~ 5 part, amount to 100 parts, each component by weight.
2. a kind of high-temperature resistant silicone powder encapsulating material according to claim 1, is characterized in that: described silicone resin is the combination of one or more in methyl silicon resin, phenyl methyl silicone resin, phenyl polysiloxane, MQ silicone resin, vinyl polysiloxane, polyester modification silicone resin, epoxide modified silicone resin, phenol aldehyde modified silicone resin.
3. a kind of high-temperature resistant silicone powder encapsulating material according to claim 1, it is characterized in that: described catalyzer is aluminium acetylacetonate, dibutyl tin dilaurate, tin protochloride, isoflurane chalcone diisocyanate and derivative, 1, the combination of one or more in 2 aminoundecane-earboxylic acids, aminosilane.
4. a kind of high-temperature resistant silicone powder encapsulating material according to claim 1, is characterized in that: described filler be aluminium sesquioxide, silicon nitride, graphite, light calcium carbonate, water-ground limestone, barium sulfate, titanium dioxide, glass powder with low melting point, silicon powder, mica powder, talcum powder, the combination of one or more in kaolin.
5. a kind of high-temperature resistant silicone powder encapsulating material according to claim 1, is characterized in that: described packing material size is between 75 μm ~ 18 μm.
6. a kind of high-temperature resistant silicone powder encapsulating material according to claim 1, is characterized in that: described pigment is the combination of one or more in aluminium powder, chrome green, carbon black, chrome yellow, the husky Huang of the Chinese, ultramarine, the blue or green orchid of phthalein, red iron oxide.
7. a kind of high-temperature resistant silicone powder encapsulating material according to claim 1, is characterized in that: described toughner is the combination of one or more in carboxy nitrile rubber, nbr carboxyl terminal, thiorubber, polyethers, polysulfones, polyimide, nano-calcium carbonate, nano titanium oxide, acrylic elastomer, chloroprene rubber, chlorosulfonated polyethylene, ABS resin, SBS resin, SEBS resin, Vinyl Acetate Copolymer, containing hydrogen silicone oil, hydroxy silicon oil, silicon rubber, viton, polyvinyl butyral acetal.
8. a kind of high-temperature resistant silicone powder encapsulating material according to claim 1, is characterized in that: described thixotropic agent is the combination of one or more in wilkinite, white carbon black, gaseous oxidation aluminium, polyamide wax.
9. prepare a method for high-temperature resistant silicone powder encapsulating material according to claim 1, it is characterized in that: step is as follows:
(1) mix, in formula, each component all needs by 100 eye mesh screens, except coupling agent and thixotropic agent, each component all mixes in high-speed mixer, mixing velocity 20 ~ 80Hz, adopts the mode of spraying to add coupling agent after 10 ~ 30 minutes, continuing mixing 40 ~ 90 minutes, is raw material after completing mixing;
(2) extrude, mixed rear raw material input forcing machine and extruded, forcing machine rotating speed 30 ~ 50Hz, district's temperature 50 ~ 100 DEG C, two district's temperature 70 ~ 130 DEG C, three district's temperature 70 ~ 130 DEG C;
(3) crushing and classification, adopts the disintegrating apparatus with separator, rotating screen, dust removal cabinet to pulverize, and gained powder need by 80 ~ 200 eye mesh screens, and now powder is work in-process;
(4) mix thixotropic agent, 1 ~ 3kg is got from work in-process, add the thixotropic agent of work in-process total mass 1.0 ~ 3.0 ‰, disperse in high speed disintegrator, frequency is 100 ~ 300 hertz, 1 ~ 3 minute time, is dropped in mixing tank by all work in-process and mixes after having disperseed, hybrid frequency 1 ~ 10Hz, mixing time 30 ~ 120 minutes.
10. the using method of organosilicon encapsulating material described in claim 1, is characterized in that: be divided into components and parts preheating, fluidized-bed encapsulation, components and parts heating levelling, secondary encapsulating, thermofixation 5 steps.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105907098A (en) * | 2016-05-19 | 2016-08-31 | 苏州倍力特物流设备有限公司 | Composite polysiloxane resin packaging material and preparation method thereof |
| CN107163834A (en) * | 2017-05-31 | 2017-09-15 | 兴勤（常州）电子有限公司 | A kind of organic resin coating composition |
| CN107201104A (en) * | 2017-06-21 | 2017-09-26 | 东莞市振鑫电子有限公司 | For coated alloy inductance and the new material and preparation method on piezo-resistance surface |
| CN107459926A (en) * | 2017-09-20 | 2017-12-12 | 江南载福粉末涂料（张家港）有限公司 | A kind of automobile exhaust pipe and muffler powdery paints and preparation method thereof |
| CN107686634A (en) * | 2017-10-18 | 2018-02-13 | 徐宏伟 | A kind of LED heat sink material and its preparation technology |
| CN109130376A (en) * | 2018-09-07 | 2019-01-04 | 江苏天泽教育咨询有限公司 | A kind of environment-friendly type aqueous plastic material |
| CN110387190A (en) * | 2018-04-16 | 2019-10-29 | 常州市源长新材料科技有限公司 | A kind of high-temperature resistant silicone powdery paints, preparation method and spraying method |
| CN113462115A (en) * | 2021-06-29 | 2021-10-01 | 上海艾镇新材料有限公司 | High-weather-resistance spraying-free ABS (acrylonitrile butadiene styrene) composite material and preparation method thereof |
| WO2022017023A1 (en) * | 2020-07-22 | 2022-01-27 | 长鑫存储技术有限公司 | Lead-free glass paste, chip resistor, and preparation method therefor |
| CN114149201A (en) * | 2021-11-30 | 2022-03-08 | 南京先正电子股份有限公司 | High-power aluminum shell resistor encapsulating material and preparation method thereof |
| CN114874625A (en) * | 2022-05-30 | 2022-08-09 | 东莞市港田高分子材料有限公司 | High-temperature-resistant high-purity organic silica gel material |
| US11802076B2 (en) | 2020-07-22 | 2023-10-31 | Changxin Memory Technologies, Inc. | Lead-free glass paste, chip resistor and method for producing same |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105907098A (en) * | 2016-05-19 | 2016-08-31 | 苏州倍力特物流设备有限公司 | Composite polysiloxane resin packaging material and preparation method thereof |
| CN107163834A (en) * | 2017-05-31 | 2017-09-15 | 兴勤（常州）电子有限公司 | A kind of organic resin coating composition |
| CN107201104A (en) * | 2017-06-21 | 2017-09-26 | 东莞市振鑫电子有限公司 | For coated alloy inductance and the new material and preparation method on piezo-resistance surface |
| CN107459926A (en) * | 2017-09-20 | 2017-12-12 | 江南载福粉末涂料（张家港）有限公司 | A kind of automobile exhaust pipe and muffler powdery paints and preparation method thereof |
| CN107459926B (en) * | 2017-09-20 | 2019-11-15 | 江南载福粉末涂料（张家港）有限公司 | A kind of automobile exhaust pipe and muffler powdery paints and preparation method thereof |
| CN107686634A (en) * | 2017-10-18 | 2018-02-13 | 徐宏伟 | A kind of LED heat sink material and its preparation technology |
| CN110387190A (en) * | 2018-04-16 | 2019-10-29 | 常州市源长新材料科技有限公司 | A kind of high-temperature resistant silicone powdery paints, preparation method and spraying method |
| CN109130376A (en) * | 2018-09-07 | 2019-01-04 | 江苏天泽教育咨询有限公司 | A kind of environment-friendly type aqueous plastic material |
| WO2022017023A1 (en) * | 2020-07-22 | 2022-01-27 | 长鑫存储技术有限公司 | Lead-free glass paste, chip resistor, and preparation method therefor |
| US11802076B2 (en) | 2020-07-22 | 2023-10-31 | Changxin Memory Technologies, Inc. | Lead-free glass paste, chip resistor and method for producing same |
| CN113462115A (en) * | 2021-06-29 | 2021-10-01 | 上海艾镇新材料有限公司 | High-weather-resistance spraying-free ABS (acrylonitrile butadiene styrene) composite material and preparation method thereof |
| CN114149201A (en) * | 2021-11-30 | 2022-03-08 | 南京先正电子股份有限公司 | High-power aluminum shell resistor encapsulating material and preparation method thereof |
| CN114874625A (en) * | 2022-05-30 | 2022-08-09 | 东莞市港田高分子材料有限公司 | High-temperature-resistant high-purity organic silica gel material |
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