CN108441160A - A kind of integrated circuit board casting glue and preparation method thereof - Google Patents
A kind of integrated circuit board casting glue and preparation method thereof Download PDFInfo
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- CN108441160A CN108441160A CN201810370501.7A CN201810370501A CN108441160A CN 108441160 A CN108441160 A CN 108441160A CN 201810370501 A CN201810370501 A CN 201810370501A CN 108441160 A CN108441160 A CN 108441160A
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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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
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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
- 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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- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08L2201/02—Flame or fire retardant/resistant
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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
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- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Polyurethanes Or Polyureas (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of integrated circuit board casting glues, which is characterized in that by being 1 by weight：The component A and B component of (1 2) form；The component A includes the raw material of following weight percent：10 20 parts of surface modification silicon dopen Nano diamond, 60 80 parts of activated urethanes；The B component includes the raw material of following weight percent：60 80 parts of dimethyl hydroxyl silicon oil, 8 14 parts of catalyst；The catalyst is selected from one or more of triethylamine, triphenylphosphine, benzyl tributyl ammonium bromide；The casting glue of the disclosure of the invention has excellent electric property and anti-flammability, and strong with integrated circuit board substrate bonding power, can effectively extend the service life of electronic equipment.And the casting glue avoids addition type heat conducting silicon rubber molecule in nonpolarity, interfacial energy is low, with base material bad adhesion, when being used as electronics embedding, coating material, after expanding with heat and contract with cold for a long time, the stress of generation so that casting glue is removed with base material or internal electronic component shifts, and moisture is caused to enter inside component the problem that burn into short circuit occurs by gap.
Description
Technical field
The present invention relates to casting glue technical fields, multiple with polysiloxane-polyurethane more specifically to a kind of integrated circuit
Close electron pouring sealant and preparation method thereof.
Background technology
With the fast development of electronic science and technology, electronic component, device, instrument and instrument are continuous in the electronics industry
Develop, they have begun towards lighting, integrated, high performance, densification, high-precision and powerful direction
Development, this calorific value for inevitably resulting in electronic device greatly improves, and especially integrated circuit board heat-dissipating space is small, heat dissipation channel
It is crowded, there are amount of heat accumulations, if these heats disperse not in time, the stability of electronic component and reliable can be seriously affected
Property, so as to shorten the service life of electronic equipment.It is right in order to improve the electric property and stability of electronic component in integrated circuit
The casting glue that electronic equipment is potted protection not only requires good electrical insulation capability and adhesive property, also to have excellent
Different heat conductivility and flame retardant property.
Lacking using more organic silicon casting glue there are thermal conductivities low, anti-flammability and adhesive property difference in the prior art
Point has seriously affected its application range, another common casting glue material polyurethane material possesses best waterproof, acid resistance
Energy, flexibility and shock resistance are all preferable, but it when as Electronic Packaging glue, bubble ratio is more, and bubble is closeer,
It carries out vacuumizing encapsulating, operation is more complicated.
China Patent Publication No. is that CN 106753212A disclose a kind of PCB circuit board that the good transparency of caking property is high use
Organic silicon electronic potting adhesive is made of following raw materials according：Vinyl-terminated silicone fluid -1, vinyl-terminated silicone fluid -2,12% platinum catalysis
Agent, ethynylcyclohexanol, vinyl polysiloxane, 1- allyloxy -2,3- propylene oxide, 1,3,5,7- tetramethyl cyclotetrasiloxane silica
Alkane, silane coupling A 171, appropriate containing hydrogen silicone oil, montmorillonite, microencapsulated powder oil, hexamethyldisilazane, deionized water are suitable
Amount, appropriate absolute ethyl alcohol, to make up, organic silicon casting glue thermal conductivity is low, hinders by adding auxiliary agent for the casting glue which prepares
The defect of combustion property and adhesive property difference, but the addition of auxiliary agent excessively can cause viscosity excessive, influence mobility and mechanical property；.
Therefore, develop a kind of integrated circuit board casting glue haveing excellent performance, come make up in the prior art with organosilicon and
Polyurethane is the deficiency of the embedding glue material of representative, to promoting industrial development to be of great significance.
Invention content
The main purpose of the present invention is to provide a kind of integrated circuit board casting glue, which is easy to get, price
Cheap, preparation method is simple, and the casting glue being prepared has excellent electric property and anti-flammability, and and integrated circuit
Plate substrate bonding power is strong, can effectively extend the service life of electronic equipment.And the casting glue avoids addition type heat conducting silicon rubber
For molecule in nonpolarity, interfacial energy is low, and base material bad adhesion, as electronics embedding, coating material in use, prolonged
After expanding with heat and contract with cold, the stress of generation so that casting glue is removed with base material or internal electronic component shifts, and causes moisture logical
It crosses gap and enters inside component the problem that burn into short circuit occurs.
To achieve the above objectives, the technical solution adopted by the present invention is：A kind of integrated circuit board casting glue is by by weight
Than being 1：The component A and B component of (1-2) form,
The component A includes the raw material of following weight percent：10-20 parts of surface modification silicon dopen Nano diamond is lived
Change 60-80 parts of polyurethane；
The B component includes the raw material of following weight percent：60-80 parts of dimethyl hydroxyl silicon oil, 8-14 parts of catalyst；
The preparation method of the wherein described surface modification silicon dopen Nano diamond, includes the following steps：
1) silicon dopen Nano diamond：Nano diamond after drying is added to dimethyl silicone polymer in ethyl alcohol,
It is 1-2 hours ultrasonic, then dried 10-20 hours in vacuum drying chamber at 60-80 DEG C；Finally under nitrogen or atmosphere of inert gases
Calcining obtains the Nano diamond of silicon doping at 550 DEG C；
2) silicon dopen Nano diamond surface is modified：The silicon dopen Nano diamond being prepared in step 1) is scattered in
In ethyl alcohol, silane coupling agent KH560 is then added, stirs 4-6 hours at room temperature, then at 60-80 DEG C in vacuum drying chamber
It dries 10-20 hours；
Wherein, Nano diamond described in step 1), dimethyl silicone polymer, ethyl alcohol mass ratio be (3-5):2：(10-
15)；
The inert gas is selected from one or more of helium, neon, argon gas；
The diamond of silicon dopen Nano described in step 2), ethyl alcohol, silane coupling agent KH560 mass ratio be (3-5)：(15-
25)：(0.5-1)；
The catalyst is selected from one or more of triethylamine, triphenylphosphine, benzyl tributyl ammonium bromide；
The preparation method of the activated urethanes, includes the following steps：By Toluene-2,4-diisocyanate, 4- diisocyanate, tin dilaurate
Dibutyl tin is dissolved in toluene and forms solution in proportion, is stirred to react at 70-80 DEG C of nitrogen atmosphere 2-3 hour, is then added and gathers
Urethane, 4-5 hours in the toluene solution at 65-75 DEG C, after being washed 3-5 times with toluene, 65 in vacuum drying chamber~
It is 8~12 hours dry at 85 DEG C；
Preferentially, the Toluene-2,4-diisocyanate, 4- diisocyanate, dibutyl tin laurate, toluene, polyurethane mass ratio be
10:2：(60-100)：(20-30)；
A kind of preparation method of integrated circuit board casting glue, includes the following steps：
1) preparation of component A：Surface modification silicon dopen Nano diamond, activated urethanes are proportionally added into mixed at high speed
In machine, stirring 40-60 minutes is evacuated under room temperature in high-speed mixer, component A is made in vacuum degree 0.05-0.10MPa；
2) preparation of B component：At room temperature, catalyst, dimethyl hydroxyl silicon oil are proportionally added into high speed dispersor,
Evacuate stirring；Vacuum degree is 0.08-0.16MPa, and rotating speed 1100-1300rpm, mixing time is 40-60 minutes, and B groups are made
Point；
3) preparation of casting glue finished product：At normal temperatures, component A and B component are mixed in proportion, in vacuum degree
Deaeration 21-26 minutes under 0.08-0.16MPa, then at 70-80 DEG C curing molding prepare 2-4 hours, obtain casting glue at
Product；
Since above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：
(1) the integrated circuit board casting glue that the present invention designs, raw material are easy to get, and price is less expensive, each component preparation method
It is simple and practicable, it is not high to equipment requirement.
(2) the integrated circuit board casting glue that designs of the present invention, has excellent an electric property and anti-flammability, and with it is integrated
Circuit board substrate cohesive force is strong, can effectively extend the service life of electronic equipment.
(3) the integrated circuit board casting glue that the present invention designs does not use addition polymer, avoids addition thermal conductive
For silicon rubber molecule in nonpolarity, interfacial energy is low, and base material bad adhesion, as electronics embedding, coating material in use, long
After the expanding with heat and contract with cold of time, the stress of generation so that casting glue is removed with base material or internal electronic component shifts, and causes
Moisture enters inside component the problem that burn into short circuit occurs by gap.
(4) the integrated circuit board casting glue that the present invention designs improves resistance to height added with the Nano diamond of silicon doping
Temperature, insulation, sealing, waterproof heat conductivility and flame retardant property.
(5) the integrated circuit board casting glue that the present invention designs, the nanometer Buddha's warrior attendant that activated urethanes, surface modification silicon adulterate
Interaction forms three-dimensional net structure between stone and dimethyl hydroxyl silicon oil, is conducive to improve mechanical properties of rubber compound and chemistry is steady
It is qualitative；And this casting glue overcomes that polyurethane material is easy to foaming, potting operation is complicated and its organosilicon material thermal conductivity is low, fire-retardant
Property and adhesive property difference problem, combine the excellent properties of two class materials, have excellent adhesive property and electric property.
Specific implementation mode
It is described below for disclosing the present invention so that those skilled in the art can realize the present invention.It is excellent in being described below
Embodiment is selected to be only used as illustrating, it may occur to persons skilled in the art that other obvious modifications.
Raw material described in the present embodiment is purchased from Sinopharm Chemical Reagent Co., Ltd..
Embodiment 1
A kind of integrated circuit board casting glue is by by weight being 1：1 component A and B component composition,
The component A includes the raw material of following weight percent：10 parts of surface modification silicon dopen Nano diamond, activation are poly-
60 parts of urethane；
The B component includes the raw material of following weight percent：60 parts of dimethyl hydroxyl silicon oil, 8 parts of triethylamine；
The preparation method of the wherein described surface modification silicon dopen Nano diamond, includes the following steps：
1) silicon dopen Nano diamond：Nano diamond 30g and dimethyl silicone polymer 20g after drying is added to second
In alcohol 100g, then ultrasound 1 hour is dried 10 hours at 60 DEG C in vacuum drying chamber；Finally forge at 550 DEG C under nitrogen atmosphere
It burns and obtains the Nano diamond of silicon doping；
2) silicon dopen Nano diamond surface is modified：30g points of the silicon dopen Nano diamond that will be prepared in step 1)
It dissipates in ethyl alcohol 150g, silane coupling agent KH560 5g is then added, stir at room temperature 4 hours, then vacuum is dry at 60 DEG C
It is dried 10 hours in dry case；
The preparation method of the activated urethanes, includes the following steps：By Toluene-2,4-diisocyanate, 4- diisocyanate 10g, two bays
Sour dibutyl tin 2g is dissolved in toluene 60g and forms solution, is stirred to react 2 hours at 70 DEG C of nitrogen atmosphere, polyurethane is then added
20g is dry 8 small at 65 DEG C in vacuum drying chamber after washing 3 times with toluene 4 hours in the toluene solution at 65 DEG C
When；
A kind of preparation method of integrated circuit board casting glue, includes the following steps：
1) preparation of component A：Surface modification silicon dopen Nano diamond, activated urethanes are proportionally added into mixed at high speed
In machine, stirring 40 minutes is evacuated under room temperature in high-speed mixer, component A is made in vacuum degree 0.05MPa；
2) preparation of B component：At room temperature, triethylamine, dimethyl hydroxyl silicon oil are proportionally added into high speed dispersor,
Evacuate stirring；Vacuum degree is 0.08MPa, and rotating speed 1100rpm, mixing time is 40 minutes, and B component is made；
3) preparation of casting glue finished product：At normal temperatures, component A and B component are mixed in proportion, in vacuum degree
Deaeration 21 minutes under 0.08MPa, then curing molding 2 hours at 70 DEG C, obtain casting glue finished product.
Embodiment 2
A kind of integrated circuit board casting glue is by by weight being 1:1.2 component A and B component composition,
The component A includes the raw material of following weight percent：14 parts of surface modification silicon dopen Nano diamond, activation are poly-
66 parts of urethane；
The B component includes the raw material of following weight percent：68 parts of dimethyl hydroxyl silicon oil, 10 parts of triphenylphosphine；
The preparation method of the wherein described surface modification silicon dopen Nano diamond, includes the following steps：
1) silicon dopen Nano diamond：Nano diamond 40g and dimethyl silicone polymer 20g after drying is added to second
In alcohol 125g, then ultrasound 1.6 hours is dried 15 hours at 69 DEG C in vacuum drying chamber；Finally under argon atmosphere at 550 DEG C
Calcining obtains the Nano diamond of silicon doping；
2) silicon dopen Nano diamond surface is modified：39g points of the silicon dopen Nano diamond that will be prepared in step 1)
It dissipates in ethyl alcohol 200g, silane coupling agent KH560 8g is then added, stir at room temperature 5 hours, then vacuum is dry at 70 DEG C
It is dried 15 hours in dry case；
The preparation method of the activated urethanes, includes the following steps：By Toluene-2,4-diisocyanate, 4- diisocyanate 10g, two bays
Sour dibutyl tin 2g is dissolved in toluene 80g and forms solution, is stirred to react 2.6 hours at 76 DEG C of nitrogen atmosphere, poly- ammonia is then added
Ester 24g 4.5 hours in the toluene solution at 71 DEG C, after washing 4 times with toluene, is done in vacuum drying chamber at 75 DEG C
Dry 10 hours；
A kind of preparation method of integrated circuit board casting glue, includes the following steps：
1) preparation of component A：Surface modification silicon dopen Nano diamond, activated urethanes are proportionally added into mixed at high speed
In machine, stirring 50 minutes is evacuated under room temperature in high-speed mixer, component A is made in vacuum degree 0.09MPa；
2) preparation of B component：At room temperature, triphenylphosphine, dimethyl hydroxyl silicon oil are proportionally added into high speed dispersor
In, evacuate stirring；Vacuum degree is 0.13MPa, and rotating speed 1200rpm, mixing time is 48 minutes, and B component is made；
3) preparation of casting glue finished product：At normal temperatures, component A and B component are mixed in proportion, in vacuum degree
Deaeration 24 minutes under 0.12MPa, then curing molding 3 hours at 74 DEG C, obtain casting glue finished product.
Embodiment 3
A kind of integrated circuit board casting glue is by by weight being 1:1.5 component A and B component composition,
The component A includes the raw material of following weight percent：16 parts of surface modification silicon dopen Nano diamond, activation are poly-
72 parts of urethane；
The B component includes the raw material of following weight percent：72 parts of dimethyl hydroxyl silicon oil, benzyl tributyl ammonium bromide
11 parts；
The preparation method of the wherein described surface modification silicon dopen Nano diamond, includes the following steps：
1) silicon dopen Nano diamond：Nano diamond after drying is added to ethyl alcohol with dimethyl silicone polymer 43g
In 20g, then ultrasound 1.7 hours is dried 17 hours at 72 DEG C in vacuum drying chamber；Finally forged at 550 DEG C under neon atmosphere
It burns and obtains the Nano diamond of silicon doping；
2) silicon dopen Nano diamond surface is modified：40g points of the silicon dopen Nano diamond that will be prepared in step 1)
It dissipates in ethyl alcohol 220g, silane coupling agent KH560 9g is then added, stir at room temperature 5 hours, then vacuum is dry at 72 DEG C
It is dried 15 hours in dry case；
The preparation method of the activated urethanes, includes the following steps：By Toluene-2,4-diisocyanate, 4- diisocyanate 10g, two bays
Sour dibutyl tin 2g is dissolved in toluene 88g and forms solution, is stirred to react 2.7 hours at 75 DEG C of nitrogen atmosphere, poly- ammonia is then added
Ester 26g is dry at 81 DEG C in vacuum drying chamber after washing 5 times with toluene 5 hours in the toluene solution at 72 DEG C
10 hours；
A kind of preparation method of integrated circuit board casting glue, includes the following steps：
1) preparation of component A：Surface modification silicon dopen Nano diamond, activated urethanes are proportionally added into mixed at high speed
In machine, stirring 53 minutes is evacuated under room temperature in high-speed mixer, component A is made in vacuum degree 0.06MPa；
2) preparation of B component：At room temperature, benzyl tributyl ammonium bromide, dimethyl hydroxyl silicon oil are proportionally added into height
In fast dispersion machine, stirring is evacuated；Vacuum degree is 0.14MPa, and rotating speed 1250rpm, mixing time is 52 minutes, and B component is made；
3) preparation of casting glue finished product：At normal temperatures, component A and B component are mixed in proportion, in vacuum degree
Deaeration 23 minutes under 0.14MPa, then curing molding 3.6 hours at 76 DEG C, obtain casting glue finished product.
Embodiment 4
A kind of integrated circuit board casting glue is by by weight being 1:1.8 component A and B component composition,
The component A includes the raw material of following weight percent：20 parts of surface modification silicon dopen Nano diamond, activation are poly-
75 parts of urethane；
The B component includes the raw material of following weight percent：78 parts of dimethyl hydroxyl silicon oil, 13 parts of triethylamine；
The preparation method of the wherein described surface modification silicon dopen Nano diamond, includes the following steps：
1) silicon dopen Nano diamond：Nano diamond 46g and dimethyl silicone polymer 20g after drying is added to second
In alcohol 140g, then ultrasound 2 hours is dried 19 hours at 77 DEG C in vacuum drying chamber；Finally forged at 550 DEG C under argon atmosphere
It burns and obtains the Nano diamond of silicon doping；
2) silicon dopen Nano diamond surface is modified：45g points of the silicon dopen Nano diamond that will be prepared in step 1)
It dissipates in ethyl alcohol 235g, silane coupling agent KH560 9g is then added, at room temperature stirring 5.8 hours, then the vacuum at 78 DEG C
It is dried 19 hours in drying box；
The preparation method of the activated urethanes, includes the following steps：By Toluene-2,4-diisocyanate, 4- diisocyanate 10g, two bays
Sour dibutyl tin 2g is dissolved in toluene 95g and forms solution, is stirred to react 3 hours at 78 DEG C of nitrogen atmosphere, polyurethane is then added
28g, 5 hours in the toluene solution at 72 DEG C, after washing 4 times with toluene, in vacuum drying chamber dry 11 at 83 DEG C
Hour；
A kind of preparation method of integrated circuit board casting glue, includes the following steps：
1) preparation of component A：Surface modification silicon dopen Nano diamond, activated urethanes are proportionally added into mixed at high speed
In machine, stirring 58 minutes is evacuated under room temperature in high-speed mixer, component A is made in vacuum degree 0.09MPa；
2) preparation of B component：At room temperature, catalyst, dimethyl hydroxyl silicon oil are proportionally added into high speed dispersor,
Evacuate stirring；Vacuum degree is 0.14MPa, and rotating speed 1280rpm, mixing time is 56 minutes, and B component is made；
3) preparation of casting glue finished product：At normal temperatures, component A and B component are mixed in proportion, in vacuum degree
Deaeration 25 minutes under 0.14MPa, then curing molding 4 hours at 80 DEG C, obtain casting glue finished product.
Embodiment 5
A kind of integrated circuit board casting glue is by by weight being 1:2 component A and B component composition,
The component A includes the raw material of following weight percent：20 parts of surface modification silicon dopen Nano diamond, activation are poly-
80 parts of urethane；
The B component includes the raw material of following weight percent：80 parts of dimethyl hydroxyl silicon oil, 14 parts of triphenylphosphine；
The preparation method of the wherein described surface modification silicon dopen Nano diamond, includes the following steps：
1) silicon dopen Nano diamond：Nano diamond 50g and dimethyl silicone polymer 20g after drying is added to second
In alcohol 150g, then ultrasound 2 hours is dried 20 hours at 80 DEG C in vacuum drying chamber；Finally forge at 550 DEG C under nitrogen atmosphere
It burns and obtains the Nano diamond of silicon doping；
2) silicon dopen Nano diamond surface is modified：45g points of the silicon dopen Nano diamond that will be prepared in step 1)
It dissipates in ethyl alcohol 250g, silane coupling agent KH560 10g is then added, stir at room temperature 6 hours, then vacuum is dry at 80 DEG C
It is dried 20 hours in dry case；
The preparation method of the activated urethanes, includes the following steps：By Toluene-2,4-diisocyanate, 4- diisocyanate 10g, two bays
Sour dibutyl tin 2g is dissolved in toluene 100g and forms solution, is stirred to react 3 hours at 80 DEG C of nitrogen atmosphere, polyurethane is then added
30g, 5 hours in the toluene solution at 75 DEG C, after washing 5 times with toluene, in vacuum drying chamber dry 12 at 85 DEG C
Hour；
A kind of preparation method of integrated circuit board casting glue, includes the following steps：
1) preparation of component A：Surface modification silicon dopen Nano diamond, activated urethanes are proportionally added into mixed at high speed
In machine, stirring 60 minutes is evacuated under room temperature in high-speed mixer, component A is made in vacuum degree 0.10MPa；
2) preparation of B component：At room temperature, catalyst, dimethyl hydroxyl silicon oil are proportionally added into high speed dispersor,
Evacuate stirring；Vacuum degree is 0.16MPa, and rotating speed 1300rpm, mixing time is 60 minutes, and B component is made；
3) preparation of casting glue finished product：At normal temperatures, component A and B component are mixed in proportion, in vacuum degree
Deaeration 26 minutes under 0.16MPa, then curing molding 4 hours at 80 DEG C, obtain casting glue finished product.
Comparative example
The filling glue of commercially available tradition organosilicon.
Correlated performance test is carried out to sample obtained by above-described embodiment 1-5 and comparative example, test result is as shown in table 1,
Test method is as follows,
(1) viscosity：Foundation is measured according to standard GB/T 10247-2008；
(2) tensile strength, elongation at break：A, B component vacuum defoamation after mixing, it is 2mm to be coated uniformly on thickness
Mold on, deaeration 26 minutes at vacuum degree 0.16MPa, then at 80 DEG C curing molding after 4 hours press GB/T 528-
2009 tests；
(3) hardness：Shore A hardness is tested by GB/T 531-2008；
(4) dielectric strength：Dielectric strength is tested by GB/T1695-2005；
(5) volume resistivity：By GB/T1692-2008 test volume resistivity；
(6) thermal conductivity：Thermal conductivity is tested by GB/T 11205-2009；
(7) anti-flammability：Fire-retardant rank is tested by UL 94.
From following table as can be seen that compared with commercially available traditional organic silicon potting adhesive, casting glue tool disclosed by the embodiments of the present invention
There are preferable anti-flammability (V-0 grades), thermal coefficient (2.4-2.9W/m.K), electrical insulation capability (dielectric strength 34-44KV/mm, body
Product resistivity 5.1 × 1015-6.2×1015Q.cm), mechanical property (tensile strength 4.6-5.6MPa, elongation at break 300-
375%, hardness 76-78A), good mobility (viscosity 2200-2400mPa.s).
1 embodiment and comparative example properties of sample test result of table
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative example |
| Viscosity (mPa.s) | 2400 | 2350 | 2300 | 2240 | 2200 | 5500 |
| Hardness (ShoreA) | 76 | 78 | 75 | 79 | 78 | 60 |
| Tensile strength (MPa) | 4.6 | 4.9 | 5.3 | 5.6 | 5.6 | 2 |
| Elongation at break (%) | 300 | 330 | 350 | 362 | 375 | 182 |
| Dielectric strength (KV/mm) | 34 | 37 | 39 | 42 | 44 | 25 |
| Volume resistivity (× 1015Q.cm) | 5.1 | 5.3 | 5.6 | 5.9 | 6.2 | 2.2 |
| Thermal coefficient (W/m.K) | 2.4 | 2.5 | 2.6 | 2.8 | 2.9 | 1.5 |
| Fire-retardant rank (UL94) | V-0 | V-0 | V-0 | V-0 | V-0 | V-1 |
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and what is described in the above embodiment and the description is only the present invention
Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these variation and
Improvement is both fallen in the range of claimed invention.The present invention claims protection domain by appended claims and its
Equivalent defines.
Claims (9)
1. a kind of integrated circuit board casting glue, which is characterized in that by being 1 by weight：The component A and B component group of (1-2)
At；The component A includes the raw material of following weight percent：10-20 parts of surface modification silicon dopen Nano diamond, the poly- ammonia of activation
60-80 parts of ester；The B component includes the raw material of following weight percent：60-80 parts of dimethyl hydroxyl silicon oil, catalyst 8-14
Part.
2. a kind of integrated circuit board casting glue according to claim 1, which is characterized in that the surface modification silicon doping
The preparation method of Nano diamond, includes the following steps：
1) silicon dopen Nano diamond：Nano diamond after drying is added to dimethyl silicone polymer in ethyl alcohol, ultrasound
It 1-2 hours, is then dried 10-20 hours in vacuum drying chamber at 60-80 DEG C；Finally 550 under nitrogen or atmosphere of inert gases
Calcining obtains the Nano diamond of silicon doping at DEG C；
2) silicon dopen Nano diamond surface is modified：The silicon dopen Nano diamond being prepared in step 1) is scattered in ethyl alcohol
In, silane coupling agent KH560 is then added, stirs 4-6 hours at room temperature, then dries 10- in vacuum drying chamber at 60-80 DEG C
20 hours.
3. a kind of integrated circuit board casting glue according to claim 2, which is characterized in that nanogold described in step 1)
Hard rock, dimethyl silicone polymer, ethyl alcohol mass ratio be (3-5):2：(10-15).
4. a kind of integrated circuit board casting glue according to claim 2, which is characterized in that the inert gas is selected from helium
One or more of gas, neon, argon gas.
5. a kind of integrated circuit board casting glue according to claim 2, which is characterized in that silicon described in step 2) adulterates
Nano diamond, ethyl alcohol, silane coupling agent KH560 mass ratio be (3-5)：(15-25)：(0.5-1).
6. a kind of integrated circuit board casting glue according to claim 1, which is characterized in that the catalyst is selected from three second
One or more of amine, triphenylphosphine, benzyl tributyl ammonium bromide.
7. a kind of integrated circuit board casting glue according to claim 1, which is characterized in that the system of the activated urethanes
Preparation Method includes the following steps：By Toluene-2,4-diisocyanate, 4- diisocyanate, dibutyl tin laurate are dissolved in toluene and are formed in proportion
Solution is stirred to react 2-3 hours at 70-80 DEG C of nitrogen atmosphere, polyurethane is then added, the toluene at 65-75 DEG C
It is 8~12 hours dry at 65~85 DEG C in vacuum drying chamber after being washed 3-5 times with toluene 4-5 hours in solution.
8. a kind of integrated circuit board casting glue according to claim 1, which is characterized in that the Toluene-2,4-diisocyanate, 4- bis- are different
Cyanate, dibutyl tin laurate, toluene, polyurethane mass ratio be 10:2：(60-100)：(20-30).
9. a kind of integrated circuit board casting glue according to claim 1, which is characterized in that the integrated circuit board fills
The preparation method of sealing, includes the following steps：
1) preparation of component A：Surface modification silicon dopen Nano diamond, activated urethanes are proportionally added into high-speed mixer
In, stirring 40-60 minutes is evacuated under room temperature in high-speed mixer, component A is made in vacuum degree 0.05-0.10MPa；
2) preparation of B component：At room temperature, catalyst, dimethyl hydroxyl silicon oil are proportionally added into high speed dispersor, are evacuated
Stirring；Vacuum degree is 0.08-0.16MPa, and rotating speed 1100-1300rpm, mixing time is 40-60 minutes, and B component is made；
3) preparation of casting glue finished product：At normal temperatures, component A and B component are mixed in proportion, in vacuum degree 0.08-
Deaeration 21-26 minutes under 0.16MPa, then curing molding is prepared 2-4 hours at 70-80 DEG C, obtains casting glue finished product；According to
A kind of biodegradable environment-protective lubricant oil described in claim 1, which is characterized in that the 2,5-furandicarboxylic acid starch ester
Preparation method includes the following steps：2,5-furandicarboxylic acid is dissolved in tetrahydrofuran, starch, carbodiimide, 4- is then added
Dimethylamino pyridine stirs 2-3 hours in ice-water bath, after return stirring 18-24 hours at 40-50 DEG C, after pass through successively
Filtering washes 4-6 time, anhydrous magnesium sulfate water suction with organic solvent diluting, washing 3-5 time, saturated common salt, filters, then in 50-60
Solvent is evaporated off in DEG C backspin.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810370501.7A CN108441160A (en) | 2018-04-24 | 2018-04-24 | A kind of integrated circuit board casting glue and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810370501.7A CN108441160A (en) | 2018-04-24 | 2018-04-24 | A kind of integrated circuit board casting glue and preparation method thereof |
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| US20030011867A1 (en) * | 2001-07-09 | 2003-01-16 | Loxley Andrew L. | Electro-optic display and adhesive composition for use therein |
| CN105969287A (en) * | 2016-05-31 | 2016-09-28 | 苏州市奎克力电子科技有限公司 | Transparent waterproof encapsulating material |
| CN107142073A (en) * | 2017-05-05 | 2017-09-08 | 江苏海川卓越密封材料有限公司 | Improved seal glue composition and preparation method thereof |
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2018
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|---|---|---|---|---|
| US20030011867A1 (en) * | 2001-07-09 | 2003-01-16 | Loxley Andrew L. | Electro-optic display and adhesive composition for use therein |
| CN105969287A (en) * | 2016-05-31 | 2016-09-28 | 苏州市奎克力电子科技有限公司 | Transparent waterproof encapsulating material |
| CN107142073A (en) * | 2017-05-05 | 2017-09-08 | 江苏海川卓越密封材料有限公司 | Improved seal glue composition and preparation method thereof |
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