CN109161375A - Organic silicon potting adhesive and preparation method thereof - Google Patents
Organic silicon potting adhesive and preparation method thereof Download PDFInfo
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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
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- 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
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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Abstract
This application provides one kind mechanical irrigation silicon sealing and preparation method thereof.The organic silicon potting adhesive is formed by mass parts number scale are as follows: both-end vinyl silicone oil, 100 parts；Containing hydrogen silicone oil, 25 parts~60 parts；Vinyl MQ silicon resin, 20 parts~30 parts；Heat Conduction Material, 20 parts~40 parts；Silane coupling agent, 3 parts~15 parts；The organic silicon potting adhesive further includes platinum water and inhibitor；Concentration of the platinum water in the organic silicon potting adhesive is 500ppm~3000ppm；The content of the inhibitor is the 6%~8% of the organic silicon potting adhesive gross mass.There is good heating conduction after the organic silicon potting adhesive solidification, while also there is good mechanical property and thermal stability after organic silicon potting adhesive solidification.
Description
Technical field
This application involves casting glue technical fields more particularly to one kind mechanical irrigation silicon sealing and preparation method thereof.
Background technique
Encapsulating can assign electronic device globality, make internal element, route have good resistance to foreign impacts, vibration
Ability avoids internal element, route from directly exposing, improves waterproof, the moisture-proof and insulation performance of electronic device.Epoxy resin encapsulated
Matter is crisp after adhesive curing, poor heat resistance.Compared with epoxy resin, organic silicon potting adhesive solidification after matter it is soft, have good toughness and
High- and low-temperature resistance performance, can significantly more efficient elimination internal stress show electronic device within the scope of relatively wide temperature
It is good to foreign impacts, the resistance of vibration out；Simultaneously because its excellent heat resistance, in the long-term use,
Also it is not easy xanthochromia；But the thermal conductivity of organic silicon potting adhesive is poor, cannot remove the heat of electronic device generation in time, is easy
Keep inside of electronic component temperature excessively high so that damage, or even generation are dangerous.Therefore, developing heat conduction organosilicon filling and sealing gum becomes inevitable
Trend.
The applying date is that the Chinese patent application CN106833509A on December 30th, 2016 uses boron nitride, aluminium oxide, stone
Black alkene improves the heating conduction of organic silicon potting adhesive；The Chinese patent application that the applying date is on 2 27th, 2017
CN106833511A improves organosilicon using white carbon black, silicon nitride, aluminium oxide, calcium carbonate, boron nitride, carbon nanotube, hydrotalcite
The heating conduction of casting glue, but the poor compatibility of above-mentioned heat filling and organic silicon potting adhesive, seriously affect organic silicon potting adhesive
Toughness, mechanical strength and hot property after solidification；The applying date is the Chinese patent application on November 28th, 2017
CN107880843A improves the heating conduction of organic silicon potting adhesive using inorganic filler aluminium nitride and titanium dioxide；The applying date is
The Chinese patent application CN107286902A on July 12nd, 2017 improves the heating conduction of organic silicon potting adhesive using boron phosphide,
But it is all made of organic solvent and is modified to inorganic filler progress surface, uneconomical and pollution environment.
Summary of the invention
In view of the problems in the background art, the application is designed to provide a kind of organic silicon potting adhesive and its preparation
Method has good heating conduction, while also having after organic silicon potting adhesive solidification after the organic silicon potting adhesive solidification
There are good mechanical property and thermal stability.
In order to achieve the above object, the application's in a first aspect, this application provides a kind of organic silicon potting adhesives, by matter
Measure number note, composition are as follows: both-end vinyl silicone oil, 100 parts；Containing hydrogen silicone oil, 25 parts~60 parts；Vinyl MQ silicon resin, 20 parts
~30 parts；Heat Conduction Material, 20 parts~40 parts；Silane coupling agent, 3 parts~15 parts；The organic silicon potting adhesive further includes platinum water
And inhibitor；Content of the platinum water in the organic silicon potting adhesive is 500ppm~3000ppm；The inhibitor contains
Amount is the 6%~8% of the organic silicon potting adhesive gross mass.
In the second aspect of the application, this application provides a kind of preparation method of organic silicon potting adhesive, it is used to prepare this
The organic silicon potting adhesive for applying for first aspect, comprising steps of S1, Heat Conduction Material is placed in ball mill with silane coupling agent and is carried out
Then first time ball milling mixing is added Vinyl MQ silicon resin and carries out second of ball milling mixing, then by the object after ball milling mixing
Material is mixed and is stirred with containing hydrogen silicone oil；S2 by platinum water and inhibitor mixed and carries out first time stirring, then with step
The material that S1 is obtained mixes and carries out second of stirring, is subsequently added into both-end vinyl silicone oil and carries out third time stirring, later
Vacuum row's bubble is carried out, organic silicon potting adhesive is obtained.
Compared with the existing technology, the application has the beneficial effect that
Heat Conduction Material is introduced in the organic silicon potting adhesive of the application, can uniformly be divided under the action of silane coupling agent
It is dispersed in the space network polymer for the tridimensional network that both-end vinyl silicone oil, containing hydrogen silicone oil and Vinyl MQ silicon resin are formed,
There is preferable heating conduction, the thermal conductivity after the organic silicon potting adhesive solidifies can achieve after solidifying organic silicon potting adhesive
1.5W/ (mk)~2.1W/ (mk), while also having good mechanical property and heat steady after organic silicon potting adhesive solidification
Qualitative energy, tensile strength are 0.9MPa~3.1MPa, and elongation at break is 202.6%~312.8%, temperature of initial decomposition
It is 421.2 DEG C~462.3 DEG C.
Specific embodiment
The following detailed description of the organic silicon potting adhesive and preparation method thereof according to the application.
Illustrate the organic silicon potting adhesive according to the application first aspect first, by mass parts number scale, composition are as follows: both-end ethylene
Base silicone oil, 100 parts；Containing hydrogen silicone oil, 25 parts~60 parts；Vinyl MQ silicon resin, 20 parts~30 parts；Heat Conduction Material, 20 parts~40
Part；Silane coupling agent, 3 parts~15 parts；The organic silicon potting adhesive further includes platinum water and inhibitor, and the platinum water is described
Content in organic silicon potting adhesive is 500ppm~3000ppm, and the content of the inhibitor is the total matter of the organic silicon potting adhesive
The 6%~8% of amount.
In the organic silicon potting adhesive according to the application first aspect, the organic silicon potting adhesive is by being heating and curing
When, under the catalytic action of platinum water, both-end vinyl silicone oil, Vinyl MQ silicon resin can be by occurring silicon with containing hydrogen silicone oil
Addition reaction of hydrogen generates chemical bonding, forms the three-dimensional polymer of tridimensional network, wherein containing hydrogen silicone oil plays crosslinking agent
Effect, Vinyl MQ silicon resin play the role of reinforcing filler, and silane coupling agent can be effectively improved by bonding action and be led
Binding force between hot material and the three-dimensional polymer of tridimensional network, so that Heat Conduction Material be allow firmly to be attached to three
In the three-dimensional polymer for tieing up reticular structure.Due to both-end vinyl silicone oil, Vinyl MQ silicon resin, containing hydrogen silicone oil and other groups
The mixing divided needs certain time, to avoid these components from reacting before being heating and curing, has organic silicon potting adhesive steady
Fixed performance goes on smoothly in order to which subsequent heat is cured, it usually needs inhibitor is added in organic silicon potting adhesive, it is ensured that
Organic silicon potting adhesive not only can have stable performance, but also can the smoothly solidification completion encapsulating in being heating and curing.
Have after the organic silicon potting adhesive solidification of the application plus preferable heating conduction, thermal coefficient can achieve
1.5W/ (mk)~2.1W/ (mk), while also having good mechanical property and heat steady after organic silicon potting adhesive solidification
Qualitative energy, tensile strength are 0.9MPa~3.1MPa, and elongation at break is 202.6%~312.8%, temperature of initial decomposition
It is 421.2 DEG C~462.3 DEG C.
In the organic silicon potting adhesive according to the application first aspect, the viscosity of the both-end vinyl silicone oil is
1Pas~100Pas.
In the organic silicon potting adhesive according to the application first aspect, the both-end vinyl silicone oil can be viscous by difference
The both-end vinyl silicone oil of degree forms, and each component in organic silicon potting adhesive can be enable to be sufficiently mixed in this way, fill organosilicon
Reaction of each component in heat curing process in sealing is more abundant, and then the net after making organic silicon potting adhesive be heating and curing
The distribution of chain chain length is wide, excellent in mechanical performance.Preferably, the both-end vinyl that the both-end vinyl silicone oil is 1Pas by viscosity
Both-end vinyl silicone oil that both-end vinyl silicone oil that silicone oil, viscosity are 5Pas, viscosity are 10Pas, viscosity 20Pas
Both-end vinyl silicone oil, viscosity be 50Pas both-end vinyl silicone oil, viscosity be 100Pas both-end vinyl silicone oil
Composition.
In the organic silicon potting adhesive according to the application first aspect, the viscosity of the containing hydrogen silicone oil is 20mPas
~500mPas.
In the organic silicon potting adhesive according to the application first aspect, the containing hydrogen silicone oil can containing by different viscosities
Hydrogen silicone oil composition, can enable each component in organic silicon potting adhesive be sufficiently mixed in this way, make each group in organic silicon potting adhesive
Reaction point in heat curing process is more abundant, and then the network chain chain length distribution after making organic silicon potting adhesive be heating and curing
Width, excellent in mechanical performance.Preferably, the containing hydrogen silicone oil is 20mPas by viscosity containing hydrogen silicone oil, viscosity 50mPas
Containing hydrogen silicone oil, viscosity be 200mPas containing hydrogen silicone oil, viscosity be 500mPas containing hydrogen silicone oil composition.
In the organic silicon potting adhesive according to the application first aspect, the Vinyl MQ silicon resin medium vinyl
Mass content is 1.2%~2.7%.
In the organic silicon potting adhesive according to the application first aspect, the Heat Conduction Material is selected from silicon carbide, nitridation
Aluminium, boron nitride, zinc oxide, at least two in graphene.
In the organic silicon potting adhesive according to the application first aspect, the silicon carbide, aluminium nitride, boron nitride, oxygen
The average grain diameter for changing zinc is 40nm~150nm.Preferably, the average grain diameter of the silicon carbide is 40nm, and the aluminium nitride is put down
Equal partial size is 50nm, and the average grain diameter of the boron nitride is 150nm, and the average grain diameter of the zinc oxide is 50nm.
In the organic silicon potting adhesive according to the application first aspect, the graphene is selected from graphene nanometer sheet.
In the organic silicon potting adhesive according to the application first aspect, the purity of the graphene is greater than 90%.
In the organic silicon potting adhesive according to the application first aspect, the silane coupling agent is selected from KH-570, KH-
One or both of 560.
In the organic silicon potting adhesive according to the application first aspect, the inhibitor inhibits selected from maleic acid esters
Agent.
In the organic silicon potting adhesive according to the application first aspect, the solidification temperature of the organic silicon potting adhesive is
60 DEG C~130 DEG C, curing time is 2h~5h.
In the organic silicon potting adhesive according to the application first aspect, the organic silicon potting adhesive can be used for electronics device
The encapsulating of part, but the application of the organic silicon potting adhesive of the application is not restricted to this.
Secondly explanation is used to prepare the application first according to the preparation method of the organic silicon potting adhesive of the application second aspect
Organic silicon potting adhesive described in aspect, comprising steps of S1, Heat Conduction Material and silane coupling agent are placed in ball mill and carry out first
Secondary ball milling mixing, then be added Vinyl MQ silicon resin carry out second of ball milling mixing, then by after ball milling mixing material with
Containing hydrogen silicone oil is mixed and is stirred；S2 by platinum water and inhibitor mixed and carries out first time stirring, then obtains with step S1
To material mix and carry out second of stirring, be subsequently added into both-end vinyl silicone oil and carry out third time stirring, carry out later
Vacuum row's bubble, obtains organic silicon potting adhesive.
In the preparation method of the organic silicon potting adhesive according to the application second aspect, in step sl, described
The time of ball milling mixing is 30min~60min, and the revolving speed of the first time ball milling mixing is 200r/min~400r/
min。
In the preparation method of the organic silicon potting adhesive according to the application second aspect, in step sl, described
The time of secondary ball milling mixing is 30min~60min, and the revolving speed of second of ball milling mixing is 100r/min~300r/
min。
It is in step sl, described to stir in the preparation method of the organic silicon potting adhesive according to the application second aspect
The time mixed is 120min~180min, and the revolving speed of the stirring is 1000r/min~2000r/min.
In the preparation method of the organic silicon potting adhesive according to the application second aspect, in step s 2, described
The time once stirred is 20min~40min, and the revolving speed of the first time stirring is 700r/min~900r/min.
In the preparation method of the organic silicon potting adhesive according to the application second aspect, in step s 2, described
The time of secondary agitation is 20min~40min, and the revolving speed of second of stirring is 1500r/min~2500r/min.
In the preparation method of the organic silicon potting adhesive according to the application second aspect, in step s 2, described
The time of triple mixing is 60min~120min, and the revolving speed of the third time stirring is 2000r/min~3500r/min.
Below with reference to embodiment, the application is further described.It should be understood that these embodiments be merely to illustrate the application without
For limiting scope of the present application.
Embodiment 1
By average grain diameter be 40nm silicon carbide 12.0g, average grain diameter be 150nm boron nitride 6.0g, graphene nano
Piece 2.0g, KH-560 7.0g are placed in ball mill, at room temperature ball milling mixing 30min, wherein the revolving speed of ball mill
300r/min；Then the Vinyl MQ silicon resin 30.0g that vinyl mass content is 2% is added, ball milling is mixed at room temperature
Close 30min, wherein the revolving speed 200r/min of ball mill；Then by viscosity be 20mPas containing hydrogen silicone oil 10.0g, viscosity be
Containing hydrogen silicone oil 18.0g that the containing hydrogen silicone oil 18.0g of 50mPas, viscosity are 100mPas, viscosity are the hydrogeneous of 200mPas
Silicone oil 4.0g is mixed with above-mentioned material, at room temperature mechanical stirring 120min, wherein the revolving speed of stirring is 1000r/min.
12.0g maleic acid ester inhibitors are mixed with 0.3g platinum water and mechanical stirring 30min at room temperature,
In, the revolving speed 800r/min of stirring is mixed with afore-mentioned materials, at room temperature mechanical stirring 30min later, wherein stirring
Revolving speed be 2000r/min.Then by viscosity be 1Pas both-end vinyl silicone oil 10.0g, viscosity be 5Pas both-end
The both-end vinyl that both-end vinyl silicone oil 47.0g that vinyl silicone oil 14.0g, viscosity are 10Pas, viscosity are 20Pas
The both-end vinyl silicone oil that both-end vinyl silicone oil 10.0g that silicone oil 14.0g, viscosity are 50Pas, viscosity are 100Pas
5.0g is mixed with above-mentioned material, at room temperature mechanical stirring 60min, wherein the revolving speed of stirring is 3000r/min.
By above-mentioned gained organic silicon potting adhesive after vacuum defoamation, solidify 3h in 130 DEG C of environment, carries out subsequent property later
It can test.
Embodiment 2
By average grain diameter be 50nm aluminium nitride 16.0g, average grain diameter be 150nm boron nitride 14.0g, average grain diameter be
Zinc oxide 10.0g, KH-570 10.0g, the KH-560 4.0g of 50nm is placed in ball mill, at room temperature ball milling mixing
60min, wherein the revolving speed 300r/min of ball mill.Then the Vinyl MQ silicon resin that vinyl mass content is 2% is added
20.0g, at room temperature ball milling mixing 60min, wherein the revolving speed 200r/min of ball mill.It then is 20mPa by viscosity
Containing hydrogen silicone oil 15.0g that containing hydrogen silicone oil 14.0g that the containing hydrogen silicone oil 8.0g of s, viscosity are 50mPas, viscosity are 100mPas,
Viscosity is that the containing hydrogen silicone oil 3.0g of 200mPas is mixed with above-mentioned material, at room temperature mechanical stirring 180min, wherein
The revolving speed of stirring is 2000r/min.
11.2g maleic acid ester inhibitors are mixed with 0.4g platinum water and mechanical stirring 20min at room temperature,
In, the revolving speed 800r/min of stirring is mixed with afore-mentioned materials, at room temperature mechanical stirring 30min later, wherein stirring
Revolving speed be 2500r/min；Then by viscosity be 1Pas both-end vinyl silicone oil 10.0g, viscosity be 5Pas both-end
The both-end vinyl that both-end vinyl silicone oil 27.0g that vinyl silicone oil 33.0g, viscosity are 10Pas, viscosity are 20Pas
The both-end vinyl silicone oil that both-end vinyl silicone oil 10.0g that silicone oil 17.0g, viscosity are 50Pas, viscosity are 100Pas
3.0g is mixed with above-mentioned material, at room temperature mechanical stirring 90min, wherein the revolving speed of stirring is 2500r/min.
By above-mentioned gained organic silicon potting adhesive after vacuum defoamation, solidify 3h in 120 DEG C of environment, carries out subsequent property later
It can test.
Embodiment 3
By average grain diameter be 40nm silicon carbide 20.0g, be 50nm aluminium nitride 10.0g, KH-570 by average grain diameter
10.0g is placed in ball mill, in room temperature condition elder generation ball milling mixing 60min, wherein the revolving speed of ball mill is 400r/min；Then
The Vinyl MQ silicon resin 25.0g that vinyl mass content is 2% is added, at room temperature ball milling mixing 30min, wherein
The revolving speed 200r/min of ball mill；Later by viscosity be 20mPas containing hydrogen silicone oil 10.0g, viscosity be the hydrogeneous of 50mPas
The containing hydrogen silicone oil 3.0g that containing hydrogen silicone oil 17.0g that silicone oil 17.0g, viscosity are 100mPas, viscosity are 200mPas with it is above-mentioned
Material mixes, at room temperature mechanical stirring 180min, wherein the revolving speed of stirring is 1500r/min.
12.0g maleic acid ester inhibitors are mixed with 0.7g platinum water and mechanical stirring 30min at room temperature,
In, the revolving speed 800r/min of stirring is mixed with afore-mentioned materials, at room temperature mechanical stirring 30min later, wherein stirring
Revolving speed be 2000r/min；Then by viscosity be 1Pas both-end vinyl silicone oil 9.0g, viscosity be 5Pas both-end second
The both-end vinyl silicon that both-end vinyl silicone oil 17.0g that alkenyl silicone oil 48.0g, viscosity are 10Pas, viscosity are 20Pas
The both-end vinyl silicone oil 5.0g that both-end vinyl silicone oil 7.0g that oily 14.0g, viscosity are 50Pas, viscosity are 100Pas
It is mixed with above-mentioned material, at room temperature mechanical stirring 90min, wherein the revolving speed of stirring is 3000r/min.
By above-mentioned gained organic silicon potting adhesive after vacuum defoamation, solidify 3h in 60 DEG C of environment, carries out subsequent property later
It can test.
Embodiment 4
By average grain diameter be 40nm silicon carbide 12.0g, by average grain diameter be 50nm aluminium nitride 12g, by average grain diameter
It is placed in ball mill for the zinc oxide 6.0g, graphene nanometer sheet 5.0g, KH-570 12.0g of 50nm, at room temperature ball milling
Mix 30min, wherein the revolving speed 400r/min of ball milling；Then it is 2% Vinyl MQ silicon resin that vinyl mass content, which is added,
20.0g, at room temperature ball milling mixing 30min, wherein the revolving speed 200r/min of ball milling；It is later 20mPas by viscosity
Containing hydrogen silicone oil 4.0g, viscosity be 50mPas containing hydrogen silicone oil 22.0g, viscosity be 100mPas containing hydrogen silicone oil 22.0g,
Viscosity is that the containing hydrogen silicone oil 12.0g of 200mPas is mixed with above-mentioned material, at room temperature mechanical stirring 120min, wherein
The revolving speed of stirring is 1500r/min.
13.0g maleic acid ester inhibitors are mixed with 0.6g platinum water and mechanical stirring 30min at room temperature,
In you, the revolving speed 800r/min of stirring is mixed with afore-mentioned materials, at room temperature mechanical stirring 30min, wherein stir later
The revolving speed mixed is 2000r/min；Then by viscosity be 1Pas both-end vinyl silicone oil 30.0g, viscosity be the double of 5Pas
The both-end ethylene that both-end vinyl silicone oil 10.0g that vinyl-terminated silicone fluid 50.0g, viscosity are 10Pas, viscosity are 20Pas
The both-end vinyl silicone oil that both-end vinyl silicone oil 3.0g that base silicone oil 5.0g, viscosity are 50Pas, viscosity are 100Pas
2.0g is mixed with above-mentioned material, at room temperature mechanical stirring 60min, wherein the revolving speed of stirring is 3500r/min.
By above-mentioned gained organic silicon potting adhesive after vacuum defoamation, solidify 3h in 90 DEG C of environment, carries out subsequent property later
It can test.
Comparative example 1
By vinyl mass content be 2% Vinyl MQ silicon resin 30.0g, viscosity be 20mPas containing hydrogen silicone oil
Containing hydrogen silicone oil 18.0g that containing hydrogen silicone oil 18.0g that 10.0g, viscosity are 50mPas, viscosity are 100mPas, viscosity are
The containing hydrogen silicone oil 4.0g of 200mPas is mixed, at room temperature mechanical stirring 120min, wherein the revolving speed of stirring is
1000r/min。
12.0g dibutyl maleate is mixed with 0.3g platinum water and mechanical stirring 30min at room temperature, wherein
The revolving speed 800r/min of stirring, mixes with afore-mentioned materials, at room temperature mechanical stirring 30min later, wherein stirring turns
Speed is 2000r/min.Then by viscosity be 1Pas both-end vinyl silicone oil 10.0g, viscosity be 5Pas both-end ethylene
The both-end vinyl silicone oil that both-end vinyl silicone oil 47.0g that base silicone oil 14.0g, viscosity are 10Pas, viscosity are 20Pas
The both-end vinyl silicone oil 5.0g that both-end vinyl silicone oil 10.0g that 14.0g, viscosity are 50Pas, viscosity are 100Pas with
Above-mentioned material mixes, at room temperature mechanical stirring 60min, wherein the revolving speed of stirring is 3000r/min.
By above-mentioned gained organic silicon potting adhesive after vacuum defoamation, solidify 3h in 130 DEG C of environment, carries out subsequent property later
It can test.
Tensile strength and elongation at break after solidifying according to GB/T 528-2009 measurement organic silicon potting adhesive, using heat
Weight analysis instrument tests the temperature of initial decomposition after organic silicon potting adhesive solidifies, and tests organosilicon encapsulating using thermal conductivity measuring apparatus
Heating conduction after adhesive curing.
The performance test results of embodiment 1-4 and comparative example 1
| Tensile strength | Elongation at break | Temperature of initial decomposition | Thermal coefficient | |
| Embodiment 1 | 3.1MPa | 294.30% | 426.9℃ | 1.5W/(m·k) |
| Embodiment 2 | 2.8MPa | 209.70% | 448.1℃ | 2.0W/(m·k) |
| Embodiment 3 | 1.3MPa | 203.20% | 441.7℃ | 1.8W/(m·k) |
| Embodiment 4 | 1.0MPa | 205.70% | 454.1℃ | 1.9W/(m·k) |
| Comparative example 1 | 2.4MPa | 330.70% | 389.4℃ | 0.9W/(m·k) |
From the test result analysis of table 1 it is found that there is good heating conduction after organic silicon potting adhesive solidification, simultaneously
Also there is good mechanical property and thermal stability after the organic silicon potting adhesive solidification.
Claims (10)
1. a kind of organic silicon potting adhesive, which is characterized in that press mass parts number scale, composition are as follows:
Both-end vinyl silicone oil, 100 parts；
Containing hydrogen silicone oil, 25 parts~60 parts；
Vinyl MQ silicon resin, 20 parts~30 parts；
Heat Conduction Material, 20 parts~40 parts；
Silane coupling agent, 3 parts~15 parts；
The organic silicon potting adhesive further includes platinum water and inhibitor；
Content of the platinum water in the organic silicon potting adhesive is 500ppm~3000ppm；
The content of the inhibitor is the 6%~8% of the organic silicon potting adhesive gross mass.
2. organic silicon potting adhesive according to claim 1, which is characterized in that
The viscosity of the both-end vinyl silicone oil is 1Pas~100Pas；
The viscosity of the containing hydrogen silicone oil is 20mPas~500mPas.
3. organic silicon potting adhesive according to claim 2, which is characterized in that the both-end vinyl silicone oil is by viscosity
The both-end vinyl that both-end vinyl silicone oil that the both-end vinyl silicone oil of 1Pas, viscosity are 5Pas, viscosity are 10Pas
Both-end vinyl silicone oil that both-end vinyl silicone oil that silicone oil, viscosity are 20Pas, viscosity are 50Pas, viscosity are
The both-end vinyl silicone oil of 100Pas forms.
4. organic silicon potting adhesive according to claim 2, which is characterized in that the containing hydrogen silicone oil is 20mPas by viscosity
Containing hydrogen silicone oil, viscosity be 50mPas containing hydrogen silicone oil, viscosity be 200mPas containing hydrogen silicone oil, viscosity 500mPas
Containing hydrogen silicone oil composition.
5. organic silicon potting adhesive according to claim 1, which is characterized in that the Vinyl MQ silicon resin medium vinyl
Mass content is 1.2%~2.7%.
6. organic silicon potting adhesive according to claim 1, which is characterized in that the Heat Conduction Material is selected from silicon carbide, nitridation
Aluminium, boron nitride, zinc oxide, at least two in graphene.
7. organic silicon potting adhesive according to claim 6, which is characterized in that the silicon carbide, aluminium nitride, boron nitride, oxygen
The average grain diameter for changing zinc is 40nm~150nm.
8. organic silicon potting adhesive according to claim 6, which is characterized in that the graphene is selected from graphene nanometer sheet.
9. organic silicon potting adhesive according to claim 6, which is characterized in that the purity of the graphene is greater than 90%.
10. a kind of preparation method of organic silicon potting adhesive is used to prepare organosilicon encapsulating of any of claims 1-9
Glue, which is characterized in that comprising steps of
Heat Conduction Material and silane coupling agent are placed in progress first time ball milling mixing in ball mill, vinyl MQ are then added by S1
Silicone resin carries out second of ball milling mixing, and then the material after ball milling mixing is mixed and is stirred with containing hydrogen silicone oil；
S2 by platinum water and inhibitor mixed and carries out first time stirring, then mixes and carry out with the obtained material of step S1
Second of stirring, is subsequently added into both-end vinyl silicone oil and carries out third time stirring, carries out vacuum row's bubble later, obtains organosilicon
Casting glue.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811138177.2A CN109161375A (en) | 2018-09-28 | 2018-09-28 | Organic silicon potting adhesive and preparation method thereof |
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| CN201811138177.2A CN109161375A (en) | 2018-09-28 | 2018-09-28 | Organic silicon potting adhesive and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113403022A (en) * | 2021-06-24 | 2021-09-17 | 上海珏晟新材料科技有限公司 | Organic silicon heat-conducting pouring sealant and preparation method thereof |
| CN113999648A (en) * | 2021-12-20 | 2022-02-01 | 南通强生光电科技有限公司 | Graphene bottom sealing adhesive and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106833509A (en) * | 2016-12-30 | 2017-06-13 | 常州碳星科技有限公司 | A kind of heat conduction organosilicon rubber battery casting glue and preparation method thereof |
| CN107815286A (en) * | 2017-11-03 | 2018-03-20 | 航天特种材料及工艺技术研究所 | A kind of heat conduction embedding silica gel based on phase-change microcapsule and preparation method thereof |
| CN107892898A (en) * | 2017-11-09 | 2018-04-10 | 南京科孚纳米技术有限公司 | A kind of preparation method of high heat conduction low-gravity flame-proof organosilicon casting glue |
-
2018
- 2018-09-28 CN CN201811138177.2A patent/CN109161375A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106833509A (en) * | 2016-12-30 | 2017-06-13 | 常州碳星科技有限公司 | A kind of heat conduction organosilicon rubber battery casting glue and preparation method thereof |
| CN107815286A (en) * | 2017-11-03 | 2018-03-20 | 航天特种材料及工艺技术研究所 | A kind of heat conduction embedding silica gel based on phase-change microcapsule and preparation method thereof |
| CN107892898A (en) * | 2017-11-09 | 2018-04-10 | 南京科孚纳米技术有限公司 | A kind of preparation method of high heat conduction low-gravity flame-proof organosilicon casting glue |
Non-Patent Citations (6)
| Title |
|---|
| 张琳琳: "导热硅橡胶的制备与性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 章基凯: "《有机硅材料》", 31 October 1999, 中国物资出版社 * |
| 童英: "加成型有机硅导热灌封胶的制备与性能研究", 《中国优秀硕士学位论文全文数据库 B016-41》 * |
| 范华乐 等: "有机硅基体与填料表面处理对电子灌封胶性能的影响", 《广东化工》 * |
| 邝生鲁 等: "《现代精细化工高新技术与产品合成工艺》", 31 December 1997, 科学技术文献出版社 * |
| 黄文润: "《硅烷偶联剂及硅树脂》", 31 August 2010, 四川科学技术出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113403022A (en) * | 2021-06-24 | 2021-09-17 | 上海珏晟新材料科技有限公司 | Organic silicon heat-conducting pouring sealant and preparation method thereof |
| CN113999648A (en) * | 2021-12-20 | 2022-02-01 | 南通强生光电科技有限公司 | Graphene bottom sealing adhesive and preparation method thereof |
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