CN115449257A - Amidated boron nitride-graphene oxide heat-conducting and insulating ink and preparation method and application thereof - Google Patents
Amidated boron nitride-graphene oxide heat-conducting and insulating ink and preparation method and application thereof Download PDFInfo
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- CN115449257A CN115449257A CN202211122017.5A CN202211122017A CN115449257A CN 115449257 A CN115449257 A CN 115449257A CN 202211122017 A CN202211122017 A CN 202211122017A CN 115449257 A CN115449257 A CN 115449257A
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229910052796 boron Inorganic materials 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 88
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 78
- 229910052582 BN Inorganic materials 0.000 claims abstract description 54
- 239000000945 filler Substances 0.000 claims abstract description 23
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 238000000498 ball milling Methods 0.000 claims description 21
- YDKNBNOOCSNPNS-UHFFFAOYSA-N methyl 1,3-benzoxazole-2-carboxylate Chemical compound C1=CC=C2OC(C(=O)OC)=NC2=C1 YDKNBNOOCSNPNS-UHFFFAOYSA-N 0.000 claims description 21
- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 claims description 21
- 239000000725 suspension Substances 0.000 claims description 20
- 239000013078 crystal Substances 0.000 claims description 15
- 239000002270 dispersing agent Substances 0.000 claims description 14
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 claims description 14
- NQTADLQHYWFPDB-UHFFFAOYSA-N N-Hydroxysuccinimide Chemical compound ON1C(=O)CCC1=O NQTADLQHYWFPDB-UHFFFAOYSA-N 0.000 claims description 12
- 239000002518 antifoaming agent Substances 0.000 claims description 12
- -1 boron nitride amide Chemical class 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- 239000004202 carbamide Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 10
- 238000000967 suction filtration Methods 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- 239000000080 wetting agent Substances 0.000 claims description 10
- 150000001412 amines Chemical class 0.000 claims description 9
- 239000002131 composite material Substances 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 7
- XPAKVERFSWPGKO-UHFFFAOYSA-N 3-(ethyliminomethylideneamino)-1-n',1-n'-dimethylpropane-1,1-diamine Chemical compound CCN=C=NCCC(N)N(C)C XPAKVERFSWPGKO-UHFFFAOYSA-N 0.000 claims description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- 239000012304 carboxyl activating agent Substances 0.000 claims description 4
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims description 4
- 239000012752 auxiliary agent Substances 0.000 claims description 3
- 239000000178 monomer Substances 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- 229960003638 dopamine Drugs 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 abstract description 9
- 238000000576 coating method Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 9
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 6
- 238000005054 agglomeration Methods 0.000 abstract description 5
- 230000002776 aggregation Effects 0.000 abstract description 5
- 125000000524 functional group Chemical group 0.000 abstract description 5
- 230000017525 heat dissipation Effects 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 5
- 125000003277 amino group Chemical group 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000013329 compounding Methods 0.000 abstract description 3
- 239000000976 ink Substances 0.000 description 46
- 239000010410 layer Substances 0.000 description 18
- 239000004814 polyurethane Substances 0.000 description 17
- 229920002635 polyurethane Polymers 0.000 description 17
- 239000008367 deionised water Substances 0.000 description 16
- 229910021641 deionized water Inorganic materials 0.000 description 16
- LMDZBCPBFSXMTL-UHFFFAOYSA-N 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide Chemical compound CCN=C=NCCCN(C)C LMDZBCPBFSXMTL-UHFFFAOYSA-N 0.000 description 10
- 239000000463 material Substances 0.000 description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000012295 chemical reaction liquid Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000002041 carbon nanotube Substances 0.000 description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 description 3
- 238000010292 electrical insulation Methods 0.000 description 3
- 239000002114 nanocomposite Substances 0.000 description 3
- 239000002113 nanodiamond Substances 0.000 description 3
- 230000005476 size effect Effects 0.000 description 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 3
- 235000017557 sodium bicarbonate Nutrition 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
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- BDAGIHXWWSANSR-UHFFFAOYSA-N Formic acid Chemical compound OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
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- 125000003368 amide group Chemical group 0.000 description 1
- 230000001588 bifunctional effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001638 boron Chemical class 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
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- 239000005543 nano-size silicon particle Substances 0.000 description 1
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- 230000009467 reduction Effects 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/101—Inks specially adapted for printing processes involving curing by wave energy or particle radiation, e.g. with UV-curing following the printing
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Abstract
According to the amidated boron nitride-graphene oxide heat-conducting insulating ink, the amidated boron nitride-graphene oxide nano heat-conducting insulating filler is added, so that the heat conduction and the insulation of the ink are greatly improved, the problem that the insulating ink for electronic devices is poor in heat conduction effect is solved, the amidated boron nitride-graphene oxide nano heat-conducting insulating ink is used for coating the surface of a circuit board to enhance the heat conduction and heat dissipation capacity of the circuit board, the working stability of the circuit is improved, the production cost is further reduced, and the preparation method is simple and suitable for industrial production; the boron nitride and the graphene oxide are connected through the amido bond, so that the compounding stability of the boron nitride and the graphene oxide is enhanced, the agglomeration effect of the boron nitride is reduced, a reactive functional group is introduced, and the amido bond is formed by the amino group on the aminated boron nitride and the carboxyl group on the graphene oxide to covalently combine the boron nitride and the graphene.
Description
Technical Field
The invention relates to the technical field of insulating ink, in particular to amidated boron nitride-graphene oxide heat-conducting insulating ink and a preparation method and application thereof.
Background
With the development of society, the outer side of electronic device products is printed with ink to identify information. When the ink is printed on the surface of an electronic product, a compact ink layer is formed, and a connecting material in the ink is solidified into a film and firmly attached to the surface of an electronic device, so that heat dissipation is hindered. The phenomena of deformation and aging of components, short circuit of a circuit, reduction of service life and the like can be caused by excessive heat accumulation, and researches show that when the temperature of an electronic device is reduced by 1 ℃ within a rated working temperature range, the failure rate of the electronic device is reduced by 4 percent; and when the maximum set temperature is exceeded by 20 ℃, the failure rate reaches 100 percent. Therefore, in order to ensure the long-term safe normal work of electronic products, the key of prolonging the service life of the electronic products is to rapidly dissipate heat, and the development of heat-conducting ink which can meet the printing requirements of the electronic products and can dissipate heat in time becomes an important task at present. The heat-conducting ink is added with a filler or an auxiliary agent with heat-conducting property on the basis of the traditional ink so as to endow the ink with excellent heat-conducting property, wherein the high-efficiency heat-radiating material is the core and key components of the heat-conducting ink.
The successful preparation of the graphene opens the door of two-dimensional heat conduction materials, and then the two-dimensional heat conduction materials such as nano graphene, hexagonal boron nitride, nano diamond, carbon nano tubes, nano silicon nitride, maxene and the like are sequentially stripped to be used for heat dissipation of electronic devices, so that better research results are obtained. Among many heat conducting materials, the carbon-based material has the best heat conducting property, such as the theoretical heat conducting coefficient of a single-arm carbon nano tube of 6000W/mK, the theoretical heat conducting coefficient of a single-layer graphene of 5300W/mK and the theoretical heat conducting coefficient of a single-layer nano diamond of 2000W/mK, and the high-efficiency heat radiating material, such as the carbon nano tube and the graphene, has high heat conducting coefficient, but can conduct electricity, cannot meet the insulation requirement of a component, and has low safety, while the nano diamond has insulation property, but the high cost makes the merchant keep pace with the expectation, and cannot realize industrial production, compared with the boron nitride, although the heat conducting coefficient is slightly low, the boron nitride has the obvious advantages of good strippability, good electrical insulation property, unique size effect and the like,
therefore, a heat-conducting insulating ink which combines the performances of graphene and boron nitride and has insulating and heat-conducting performances, and a preparation method and application thereof are needed.
Disclosure of Invention
The invention provides amidated boron nitride-graphene oxide heat-conducting insulating ink, and aims to solve the technical problem that the prior art can not organically combine the excellent heat-conducting property of graphene and the excellent insulating property of boron nitride and use the graphene and the boron nitride in insulating ink so as to greatly improve the insulating property and the heat-conducting property of the ink.
The second purpose of the invention is to provide a preparation method of the amidated boron nitride-graphene oxide heat-conducting and insulating ink.
In order to achieve the first purpose, the invention adopts the technical scheme that:
the amidated boron nitride-graphene oxide heat-conducting and insulating ink consists of the following components: amidated boron nitride-graphene oxide nanofiller, a binder, a monomer, a photoinitiator and an auxiliary agent; the amidated boron nitride-graphene oxide nanofiller is added into the ink, so that the heat conduction performance and the insulation performance of the ink can be effectively improved, the addition amount is small, the characteristics of excellent strippability, electrical insulation and unique size effect of boron nitride are effectively utilized, the amidated boron nitride-graphene oxide nanofiller is organically combined with graphene with high heat conductivity coefficient, the agglomeration effect of boron nitride is reduced, and the reactive functional group is introduced, so that the problem of poor heat conduction of the existing ink is solved, the requirements of components on insulation performance can be met, the multifunctional reactive boron nitride-graphene oxide nanofiller has great theoretical and practical significance on safe use of electronic components, the composite stability of boron nitride and graphene is effectively enhanced, and the heat conduction insulation performance of the ink is greatly improved.
The preparation method of the amidated boron nitride-graphene oxide nanofiller comprises the following steps: s1, adding boron nitride crystals and amine substances into water, and performing ball milling for 4-24h; centrifuging for 10-60min after the ball milling is finished, collecting upper suspension, centrifuging the upper suspension for 30-60min, collecting lower precipitate, and drying for 1-2 h at the temperature of 50-100 ℃ to obtain the boron nitride amide;
s2, adding graphene oxide into water, uniformly stirring, and performing ultrasonic treatment at the temperature of 30-80 ℃ and with the power of 200-325W for 30-90min to obtain a graphene oxide dispersion liquid; adding the aminated boron nitride obtained in the step S1 into the obtained graphene oxide dispersion liquid, adjusting the pH value in the system, adding a carboxyl activating agent, stirring for 4-20 hours at a stirring speed of 300-500r/min until the mixture is uniformly dispersed, carrying out suction filtration on the mixed liquid for 15-30 hours, and drying to obtain the graphene oxide dispersion liquid; the aminated boron nitride is prepared by adopting a ball milling method, the agglomeration effect of the boron nitride is reduced, meanwhile, a reactive functional group is introduced, an amido bond is formed between an amino group on the aminated boron nitride and a carboxyl group on the graphene oxide to covalently combine the boron nitride and the graphene, and the amidated boron nitride-graphene oxide nano filler is prepared, so that the composite stability of the boron nitride and the graphene is enhanced, the heat conductivity and the insulativity of the composite nano filler in a coating are greatly improved, the problem of poor heat conduction effect of insulating ink for electronic devices is solved, the heat conduction and heat dissipation capability of a circuit board is enhanced when the aminated boron nitride-graphene oxide nano filler is used for coating the surface of the circuit board, the working stability of the circuit is improved, the production cost is further reduced, and the preparation method is simple and suitable for industrial production.
Preferably, the amine substance in step S1 is one or a combination of urea, ammonium chloride and dopamine, and the amine substance reacts with the boron nitride crystal to aminate the surface of boron nitride, so as to solve the disadvantage of poor direct compound stability of boron nitride and graphene oxide, and the amino group on the surface of aminated boron nitride and the carboxyl group on graphene oxide form an amide bond, thereby enhancing the compound stability of boron nitride and graphene and greatly improving the thermal conductivity of the filler for insulating ink.
Preferably, the mass ratio of the boron nitride crystal to the amine substance in the step S1 is 1 to 50, and the solid content of the boron nitride crystal and the amine substance added into water is 10 to 50 percent.
Preferably, the mass ratio of the aminated boron nitride to the graphene oxide in the step S2 is 1.
Preferably, the carboxyl activating agent in step S2 is a mixture of N-hydroxysuccinimide and amino 1-ethyl-3- (3-dimethylaminopropyl) carbodiimide; the ratio of the graphene oxide to the N-hydroxysuccinimide is 1.15-1; the graphene oxide and amino 1-ethyl-3- (3-dimethylaminopropyl) carbodiimide 1; by adopting NHS and EDC as carboxyl activators, formation of amido bonds on boron nitride and graphene oxide is facilitated, and the efficiency of the coupling reaction can be increased.
Preferably, the graphene oxide is prepared by a Hummers method or a modified Hummers method, and the concentration of the graphene oxide dispersion liquid in the step S2 is 0.08-10mg/ml.
Preferably, the proportion of the amidated boron nitride-graphene oxide nanofiller in the heat-conducting insulating ink is 0.1-10%.
Preferably, the composition consists of the following components:
neopentyl glycol diacrylate is adopted as a bifunctional monomer, and the acid value is less than or equal to 0.5; the viscosity is 6-12s, the polyurethane acrylate and the epoxy acrylate have good compatibility, and the polyurethane acrylate and the epoxy acrylate are matched with each other to have the characteristics of good flexibility, high glossiness and high adhesive force.
In order to achieve the second object, the invention adopts the technical scheme that:
a preparation method of the amidated boron nitride-graphene oxide heat conduction and insulation ink comprises the following steps:
1) Stirring the urethane acrylate, the epoxy acrylate and the neopentyl glycol diacrylate at the stirring speed of 1200-2400r/min for 5-10min;
2) Adding amidated boron nitride-graphene oxide nanofiller, and stirring at the stirring speed of 3000-3500r/min for 10-15min;
3) Adding a defoaming agent, a dispersing agent and a wetting agent, finally slowly adding a photoinitiator and a flatting agent, and stirring for 30-40min at a stirring speed of 4000r/min to obtain a mixture;
4) Crushing and grinding the mixture obtained in the step 3) for 1-6h, and filtering the mixture with a gauze of 200-1000 meshes to obtain the polyurethane acrylic ester/neopentyl glycol diacrylate dispersed filler, dispersing the filler and the main paint to form a molecular layer on the surface of the filler, gradually consuming a dispersing agent and a defoaming agent in the process of gradually adding the polyurethane acrylic ester and other components into the filler, and continuously supplementing the dispersing agent and the defoaming agent to uniformly disperse the polyurethane acrylic ester and other components and prevent bubbles from being generated or the polyurethane and other components are not uniformly dispersed; finally, adding a photoinitiator and a leveling agent to prevent the problem of overhigh coating viscosity caused by partial polymerization of urethane acrylate molecules in the preparation process of the coating; and all the components can be uniformly dispersed through different stirring speeds, so that good heat-conducting insulating ink is formed, and the ink is simple, convenient and strong in operability.
The application of the amidated boron nitride-graphene oxide heat-conducting and insulating ink as described in any one of the above aspects in printing and packaging of electronic appliances.
Compared with the prior art, the invention has the following advantages:
1. according to the amidated boron nitride-graphene oxide heat-conducting insulating ink, the amidated boron nitride-graphene oxide nano heat-conducting insulating filler is added, so that the heat conduction and the insulation of the ink are greatly improved, the problem that the insulating ink for electronic devices is poor in heat conduction effect is solved, the amidated boron nitride-graphene oxide nano heat-conducting insulating ink is used for coating the surface of a circuit board to enhance the heat conduction and heat dissipation capacity of the circuit board, the working stability of the circuit is improved, the production cost is further reduced, and the preparation method is simple and suitable for industrial production; the boron nitride and the graphene oxide are connected through the amido bond, so that the compounding stability of the boron nitride and the graphene oxide is enhanced, the agglomeration effect of the boron nitride is reduced, a reactive functional group is introduced, and the amido bond is formed by the amino group on the aminated boron nitride and the carboxyl group on the graphene oxide to covalently combine the boron nitride and the graphene.
2. According to the preparation method of the amidated boron nitride-graphene oxide heat-conducting insulating ink, the filler and the main paint are dispersed, so that a molecular layer for dispersing urethane acrylate, epoxy acrylate and neopentyl glycol diacrylate can be formed on the surface of the filler, then the dispersant and the defoamer are gradually consumed in the process of gradually adding the urethane acrylate and other components into the filler, and the dispersant and the defoamer are continuously supplemented, so that the urethane acrylate and other components are uniformly dispersed, and bubbles are prevented from being generated or the polyurethane and other components are not uniformly dispersed; finally, adding a photoinitiator and a leveling agent to prevent the problem of overhigh coating viscosity caused by partial polymerization of polyurethane acrylate molecules in the preparation process of the coating; and all the components can be uniformly dispersed through different stirring speeds, so that good heat-conducting insulating ink is formed, and the ink is simple, convenient and strong in operability.
3. The application of the heat-conducting and insulating ink of amidated boron nitride-graphene oxide in printing and packaging of electronic appliances has the characteristics of peelability, good electrical insulation, unique size effect, high safety coefficient and high heat conductivity coefficient.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings used in the description of the embodiments will be briefly described below.
Fig. 1 is an electrode SEM image of amidated boron nitride-graphene oxide nanofillers of the present application.
Fig. 2 is an electrode SEM image of simple physically blended boron nitride-graphene.
Fig. 3 is an infrared spectrum of amidated boron nitride-graphene oxide nanofiller prepared in example 5 of the present application.
Detailed Description
The following describes a specific embodiment of the present invention with reference to specific examples 1 to 8:
example 1:
(1) Under the condition of room temperature, 1.0g of boron nitride crystal and 30.0g of urea are taken and added into 125ml of deionized water, and then the mixture is placed into a planetary ball mill for ball milling for 4 hours, and the rotating speed is 500r/min; after the ball milling is finished, centrifuging the reaction liquid for 10 minutes under the condition of 500r/min, removing large blocks of boron nitride on the lower layer, and collecting the suspension on the upper layer; continuously centrifuging the upper suspension for 30 minutes under the condition of 5000r/min, placing the lower precipitate in a drying oven, and drying for 1 hour under the condition of 50 ℃ to obtain aminated boron nitride;
(2) Adding 20.0mg of graphene oxide into 40ml of deionized water, stirring to uniformly disperse the graphene oxide, and then carrying out ultrasonic treatment at 35 ℃ and 200w for 30 minutes to obtain a graphene oxide dispersion liquid; then, transferring the graphene oxide dispersion liquid into a three-neck flask, adding 4.0mg of aminated boron nitride prepared in the step (1), adjusting the pH to 7-9 by using 10.0wt% of sodium carbonate solution, adding 2.0mg of 1-ethyl- (3-dimethylaminopropyl) carbodiimide and 3.0mg of N-hydroxysuccinimide, stirring at room temperature (the rotating speed is 300 r/min), reacting for 4 hours, and finally performing suction filtration for 15 hours and drying to obtain the amidated boron nitride-graphene oxide nanofiller;
(3) According to the table 1, stirring urethane acrylate, epoxy acrylate and neopentyl glycol diacrylate at a stirring speed of 1200r/min for 5min, adding amidated boron nitride-graphene oxide nanofiller, stirring at a stirring speed of 3000r/min for 10min, slowly adding a photoinitiator, a leveling agent, an antifoaming agent, a dispersing agent and a wetting agent, stirring at a stirring speed of 4000r/min for 30min to obtain a mixture, crushing and grinding for 1h, and filtering with a 300-mesh gauze to obtain the polyurethane acrylic ester/epoxy acrylate/neopentyl glycol diacrylate nano filler/graphene oxide composite material.
Example 2:
(1) Under the condition of room temperature, 1.5g of boron nitride crystal and 60.0g of urea are taken and added into 200ml of deionized water, and then the mixture is placed into a planetary ball mill for ball milling for 6 hours, and the rotating speed is 600r/min; after the ball milling is finished, centrifuging the reaction liquid for 15 minutes under the condition of 1000r/min, removing large blocks of boron nitride on the lower layer, and collecting the suspension on the upper layer; continuously centrifuging the upper suspension for 40 minutes at 6000r/min, placing the lower precipitate in a drying oven, and drying for 1 hour at 60 ℃ to obtain aminated boron nitride;
(2) Adding 25.0mg of graphene oxide into 50ml of deionized water, stirring to uniformly disperse the graphene oxide, and performing ultrasonic treatment at 40 ℃ and 250w for 60 minutes to obtain a graphene oxide dispersion liquid; then transferring the graphene oxide dispersion liquid into a three-neck flask, adding 6.0mg of aminated boron nitride prepared in the step (1), adjusting the pH value to 7-9 by using a 10.0wt% sodium carbonate solution, adding 2.5mg of 1-ethyl- (3-dimethylaminopropyl) carbodiimide and 4.0mg of N-hydroxysuccinimide, stirring at room temperature (the rotating speed is 350 r/min), reacting for 5 hours, and finally performing suction filtration for 18 hours and drying to obtain the amidated boron nitride-graphene oxide nanofiller;
(3) According to the table 1, stirring urethane acrylate, epoxy acrylate and neopentyl glycol diacrylate for 6min at a stirring speed of 1400-r/min, adding amidated boron nitride-graphene oxide nanofiller, stirring for 11min at a stirring speed of 3100r/min, slowly adding a photoinitiator, a leveling agent, an antifoaming agent, a dispersing agent and a wetting agent, stirring for 31min at a stirring speed of 4000r/min to obtain a mixture, crushing and grinding for 2h, and filtering with a 200-mesh gauze to obtain the polyurethane acrylic ester, epoxy acrylate and neopentyl glycol diacrylate.
Example 3:
(1) Under the condition of room temperature, 2.0g of boron nitride crystal and 60.0g of urea are taken and added into 300ml of deionized water, and then the mixture is placed into a planetary ball mill for ball milling for 8 hours, and the rotating speed is 700r/min; after the ball milling is finished, centrifuging the reaction solution for 20 minutes under the condition of 1500r/min, removing large blocks of boron nitride on the lower layer, and collecting the suspension on the upper layer; continuously centrifuging the upper suspension for 30 minutes under the condition of 7000r/min, placing the lower-layer precipitate into a drying oven, and drying for 2 hours under the condition of 60 ℃ to obtain aminated boron nitride;
(2) Adding 30.0mg of graphene oxide into 50ml of deionized water, stirring to uniformly disperse the graphene oxide, and performing ultrasonic treatment at the temperature of 38 ℃ for 50 minutes at the speed of 250w to obtain a graphene oxide dispersion liquid; then transferring the graphene oxide dispersion liquid into a three-neck flask, adding 8.0mg of aminated boron nitride prepared in the step (1), adjusting the pH value to 7-9 by using a 10.0wt% sodium carbonate solution, adding 5.0mg of 1-ethyl- (3-dimethylaminopropyl) carbodiimide and 6.0mg of N-hydroxysuccinimide, stirring at room temperature (the rotating speed is 300 r/min), reacting for 6 hours, and finally performing suction filtration for 20 hours and drying to obtain the amidated boron nitride-graphene oxide nanofiller;
(3) According to the table 1, stirring urethane acrylate, epoxy acrylate and neopentyl glycol diacrylate at a stirring speed of 1600r/min for 7min, adding amidated boron nitride-graphene oxide nanofiller, stirring at a stirring speed of 3200r/min for 14min, slowly adding a photoinitiator, a leveling agent, an antifoaming agent, a dispersing agent and a wetting agent, stirring at a stirring speed of 4000r/min for 34min to obtain a mixture, crushing and grinding for 3h, and filtering with a 200-mesh gauze to obtain the polyurethane acrylic ester/epoxy acrylate/neopentyl glycol diacrylate nano filler/graphene oxide composite material.
Example 4:
(1) Under the condition of room temperature, 2.5g of boron nitride crystals and 100.0g of urea are taken and added into 300ml of deionized water, and then the mixture is placed into a planetary ball mill for ball milling for 10 hours, and the rotating speed is 750r/min; after the ball milling is finished, centrifuging the reaction liquid for 15 minutes under the condition of 1800r/min, removing large blocks of boron nitride on the lower layer, and collecting the suspension on the upper layer; continuously centrifuging the upper suspension for 35 minutes under the condition of 7500r/min, taking the lower precipitate, and drying in a drying oven for 1 hour under the condition of 70 ℃ to obtain the aminated boron nitride;
(2) Adding 40.0mg of graphene oxide into 60ml of deionized water, stirring to uniformly disperse the graphene oxide, and then carrying out ultrasonic treatment at 40 ℃ and 300w for 40 minutes to obtain a graphene oxide dispersion liquid; then transferring the graphene oxide dispersion liquid into a three-neck flask, adding 10.0mg of aminated boron nitride prepared in the step (1), adjusting the pH to 7-9 by using 10.0wt% of ammonia water solution, adding 10.0mg of 1-ethyl- (3-dimethylaminopropyl) carbodiimide and 15.0mg of N-hydroxysuccinimide, stirring at room temperature (the rotating speed is 400 r/min), reacting for 8 hours, and finally performing suction filtration for 24 hours and drying to obtain the amidated boron nitride-graphene oxide nanofiller;
(3) According to the table 1, stirring urethane acrylate, epoxy acrylate and neopentyl glycol diacrylate at a stirring speed of 1800r/min for 5min, adding amidated boron nitride-graphene oxide nanofiller, stirring at a stirring speed of 3300r/min for 10min, slowly adding a photoinitiator, a leveling agent, an antifoaming agent, a dispersing agent and a wetting agent, stirring at a stirring speed of 4000r/min for 30min to obtain a mixture, crushing and grinding for 4h, and filtering with a 250-mesh gauze to obtain the polyurethane acrylic ester/epoxy acrylate/neopentyl glycol diacrylate nano filler/graphene oxide nano filler/polyurethane composite material.
Example 5:
(1) Under the condition of room temperature, 3.0g of boron nitride crystal and 150.0g of urea are taken and added into 350ml of deionized water, and then the mixture is placed into a planetary ball mill for ball milling for 10 hours, and the rotating speed is 800r/min; after the ball milling is finished, centrifuging the reaction solution for 15 minutes under the condition of 2000r/min, removing large blocks of boron nitride on the lower layer, and collecting the suspension on the upper layer; continuously centrifuging the upper suspension for 45 minutes under the condition of 8000r/min, placing the lower precipitate in a drying oven, and drying for 1.5 hours under the condition of 80 ℃ to obtain the aminated boron nitride;
(2) Adding 60.0mg of graphene oxide into 100ml of deionized water, stirring to uniformly disperse the graphene oxide, and then carrying out ultrasonic treatment at 60 ℃ for 50 minutes at 200w to obtain a graphene oxide dispersion liquid; then transferring the graphene oxide dispersion liquid into a three-neck flask, adding 15.0mg of aminated boron nitride prepared in the step (1), adjusting the pH to 7-9 by using 10.0wt% of ammonia water solution, adding 12.0mg of 1-ethyl- (3-dimethylaminopropyl) carbodiimide and 15.0mg of N-hydroxysuccinimide, stirring at room temperature (the rotating speed is 500 r/min), reacting for 10 hours, finally carrying out suction filtration for 25 hours, and drying to obtain the amidated boron nitride-graphene oxide nanofiller;
(3) According to the table 1, stirring urethane acrylate, epoxy acrylate and neopentyl glycol diacrylate at a stirring speed of 2000r/min for 5min, adding amidated boron nitride-graphene oxide nanofiller, stirring at a stirring speed of 3000r/min for 10min, slowly adding a photoinitiator, a leveling agent, an antifoaming agent, a dispersing agent and a wetting agent, stirring at a stirring speed of 4000r/min for 30min to obtain a mixture, crushing and grinding for 5h, and filtering with a 250-mesh gauze to obtain the polyurethane acrylic ester, epoxy acrylate and neopentyl glycol diacrylate.
Example 6:
(1) Under the condition of room temperature, 2.0g of boron nitride crystal and 110.0g of urea are taken and added into 350ml of deionized water, and then the mixture is placed into a planetary ball mill for ball milling for 16 hours, and the rotating speed is 600r/min; after the ball milling is finished, centrifuging the reaction liquid for 15 minutes at 1200r/min, removing large blocks of boron nitride on the lower layer, and collecting the suspension on the upper layer; continuously centrifuging the upper suspension for 35 minutes under the condition of 6500r/min, placing the lower precipitate in a drying oven, and drying for 3 hours under the condition of 80 ℃ to obtain aminated boron nitride;
(2) Adding 65.0mg of graphene oxide into 80ml of deionized water, stirring to uniformly disperse the graphene oxide, and performing ultrasonic treatment at 35 ℃ and 250w for 60 minutes to obtain a graphene oxide dispersion liquid; then, transferring the graphene oxide dispersion liquid into a three-neck flask, adding 16.0mg of aminated boron nitride prepared in the step (1), adjusting the pH to 7-9 by using 10.0wt% of sodium bicarbonate solution, adding 10.0mg of 1-ethyl- (3-dimethylaminopropyl) carbodiimide and 15.0mg of N-hydroxysuccinimide, stirring at room temperature (the rotating speed is 400 r/min), reacting for 20 hours, and finally performing suction filtration for 24 hours and drying to obtain the amidated boron nitride-graphene oxide nanofiller;
(3) According to the table 1, stirring urethane acrylate, epoxy acrylate and neopentyl glycol diacrylate at a stirring speed of 2200r/min for 5min, adding amidated boron nitride-graphene oxide nanofiller, stirring at a stirring speed of 3000r/min for 10min, then slowly adding a photoinitiator, a leveling agent, a defoaming agent, a dispersing agent and a wetting agent, stirring at a stirring speed of 4000r/min for 30min to obtain a mixture, crushing and grinding for 6h, and filtering with a 500-mesh gauze to obtain the polyurethane acrylate/epoxy acrylate/neopentyl glycol diacrylate nano-composite material.
Example 7:
(1) Under the condition of room temperature, 0.5g of boron nitride crystal and 20.0g of urea are taken and added into 100ml of deionized water, and then the mixture is placed into a planetary ball mill for ball milling for 10 hours, and the rotating speed is 500r/min; after the ball milling is finished, centrifuging the reaction solution for 20 minutes under the condition of 1500r/min, removing large blocks of boron nitride on the lower layer, and collecting the suspension on the upper layer; continuously centrifuging the upper suspension for 30 minutes at 6000r/min, placing the lower precipitate in a drying oven, and drying for 8 hours at 60 ℃ to obtain aminated boron nitride;
(2) Adding 75.0mg of graphene oxide into 100ml of deionized water, stirring to uniformly disperse the graphene oxide, and then carrying out ultrasonic treatment at 40 ℃ and 200w for 80 minutes to obtain a graphene oxide dispersion liquid; then, transferring the graphene oxide dispersion liquid into a three-neck flask, adding 15.0mg of aminated boron nitride prepared in the step (1), adjusting the pH value to 7-9 by using 10.0wt% sodium bicarbonate solution, adding 12.0mg of 1-ethyl- (3-dimethylaminopropyl) carbodiimide and 14.0mg of N-hydroxysuccinimide, stirring at room temperature (the rotating speed is 400 r/min), reacting for 20 hours, and finally performing suction filtration for 20 hours and drying to obtain the amidated boron nitride-graphene oxide nanofiller;
(3) According to the table 1, stirring urethane acrylate, epoxy acrylate and neopentyl glycol diacrylate at a stirring speed of 2300r/min for 5min, adding amidated boron nitride-graphene oxide nanofiller, stirring at a stirring speed of 3000r/min for 10min, slowly adding a photoinitiator, a leveling agent, an antifoaming agent, a dispersing agent and a wetting agent, stirring at a stirring speed of 4000r/min for 30min to obtain a mixture, crushing and grinding for 6h, and filtering with a 800-mesh gauze to obtain the polyurethane acrylic ester/epoxy acrylate/neopentyl glycol diacrylate nano filler/graphene oxide composite material.
Example 8:
(1) At room temperature, 3.0g of boron nitride crystal and 30.0g of urea are taken and added into 100ml of deionized water, and then the mixture is placed into a planetary ball mill for ball milling for 15 hours, wherein the rotating speed is 650r/min; after the ball milling is finished, centrifuging the reaction solution for 25 minutes at 1800r/min, removing large blocks of boron nitride on the lower layer, and collecting the suspension on the upper layer; continuously centrifuging the upper suspension for 45 minutes under the condition of 7500r/min, placing the lower precipitate in a drying oven, and drying for 9 hours under the condition of 50 ℃ to obtain the aminated boron nitride;
(2) Adding 80.0mg of graphene oxide into 500ml of deionized water, stirring to uniformly disperse the graphene oxide, and then carrying out ultrasonic treatment at 45 ℃ and 300w for 40 minutes to obtain a graphene oxide dispersion liquid; then transferring the graphene oxide dispersion liquid into a three-neck flask, adding 10.0mg of aminated boron nitride prepared in the step (1), adjusting the pH value to 7-9 by using 10.0wt% sodium bicarbonate solution, adding 10.0mg of 1-ethyl- (3-dimethylaminopropyl) carbodiimide and 20.0mg of N-hydroxysuccinimide, stirring at room temperature (the rotating speed is 500 r/min), reacting for 18 hours, finally performing suction filtration for 25 hours, and drying to obtain the amidated boron nitride-graphene oxide nanofiller;
(3) According to the table 1, stirring urethane acrylate, epoxy acrylate and neopentyl glycol diacrylate at a stirring speed of 2400r/min for 5min, adding amidated boron nitride-graphene oxide nanofiller, stirring at a stirring speed of 3000r/min for 10min, slowly adding a photoinitiator, a leveling agent, an antifoaming agent, a dispersing agent and a wetting agent, stirring at a stirring speed of 4000r/min for 30min to obtain a mixture, crushing and grinding for 3h, and filtering with a 800-mesh gauze to obtain the polyurethane acrylic ester/epoxy acrylate/neopentyl glycol diacrylate nano filler/graphene oxide composite material.
Table 1: component table of amidated boron nitride-graphene oxide heat-conducting and insulating ink
When the amidated boron nitride-graphene oxide nanocomposite material of example 5 was subjected to electron microscope scanning, it can be seen from the scanning electron microscope picture (fig. 2) that the surface of the boron nitride-graphene oxide nanocomposite bonded by amide bonds became very rough and the edges thereof were loaded with many fine graphene oxide particles, compared to the simple physical blending of boron nitride-graphene.
Meanwhile, the amidated boron nitride-graphene oxide thermal conductive and insulating inks prepared in examples 1 to 8 were subjected to in-plane thermal conductivity and resistivity tests, and thermal conductive inks disclosed in the prior art (controls 1 to 4) were used as controls, wherein the thermal conductive inks disclosed in the prior art and the preparation methods thereof are specifically shown in the preparation methods, test items and test results provided in reference documents in table 2, and are shown in table 3.
Table 2: control group and corresponding reference
Table 3: test results of examples 1 to 8 and control groups 1 to 4
As can be seen from Table 3, the thermal conductivity and the electrical resistivity of the amidated boron nitride-graphene oxide thermal conductive and insulating ink prepared by the invention are also obviously higher than those of the thermal conductive ink reported in the prior art under the condition of extremely low addition amount.
Therefore, the amidated boron nitride-graphene oxide heat conduction insulating ink provided by the application has the advantages that the amidated boron nitride-graphene oxide nano heat conduction insulating filler is added, so that the heat conduction and the insulation of the ink are greatly improved, the problem of poor heat conduction effect of the insulating ink for electronic devices is solved, the amidated boron nitride-graphene oxide nano heat conduction insulating filler is used for coating the surface of a circuit board to enhance the heat conduction and dissipation capacity of the circuit board, the working stability of the circuit is improved, the production cost is further reduced, and the preparation method is simple and suitable for industrial production; the boron nitride and the graphene oxide are connected through the amido bond, so that the compounding stability of the boron nitride and the graphene oxide is enhanced, the agglomeration effect of the boron nitride is reduced, the reactive functional group is introduced, the amido group on the aminated boron nitride and the carboxyl group on the graphene oxide form the amido bond to covalently combine the boron nitride and the graphene, and the preparation method is simple, convenient and fast and has strong operability.
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. The heat-conducting and insulating ink containing amidated boron nitride and graphene oxide is characterized in that: the composition consists of the following components: amidated boron nitride-graphene oxide nanofiller, a binder, a monomer, a photoinitiator and an auxiliary agent;
the preparation method of the amidated boron nitride-graphene oxide nanofiller comprises the following steps: s1, adding boron nitride crystals and amine substances into water, and performing ball milling for 4-24h; centrifuging for 10-60min after the ball milling is finished, collecting upper suspension, centrifuging the upper suspension for 30-60min, collecting lower precipitate, and drying for 1-2 h at the temperature of 50-100 ℃ to obtain the boron nitride amide;
s2, adding graphene oxide into water, uniformly stirring, and performing ultrasonic treatment at the temperature of 30-80 ℃ and with the power of 200-325W for 30-90min to obtain a graphene oxide dispersion liquid; and (2) adding the aminated boron nitride obtained in the step (S1) into the obtained graphene oxide dispersion liquid, adjusting the pH value in the system, adding a carboxyl activating agent, stirring for 4-20 hours at a stirring speed of 300-500r/min until the mixture is uniformly dispersed, carrying out suction filtration on the mixed liquid for 15-30 hours, and drying to obtain the graphene oxide dispersion liquid.
2. The amidated boron nitride-graphene oxide thermal conductive and insulating ink according to claim 1, wherein: the amine substance in the step S1 is one or a combination of urea, ammonium chloride and dopamine.
3. The amidated boron nitride-graphene oxide thermal conductive and insulating ink according to claim 1, wherein: in the step S1, the mass ratio of the boron nitride crystal to the amine substance is 1-50, and the solid content of the boron nitride crystal and the amine substance added into water is 10-50%.
4. The amidated boron nitride-graphene oxide thermal conductive and insulating ink according to claim 1, wherein: the mass ratio of the aminated boron nitride to the graphene oxide in the step S2 is 1-10.
5. The amidated boron nitride-graphene oxide thermal conductive and insulating ink according to claim 1, wherein: the carboxyl activating agent in the step S2 is a mixture of N-hydroxysuccinimide and amino 1-ethyl-3- (3-dimethylaminopropyl) carbodiimide; the ratio of the graphene oxide to the N-hydroxysuccinimide is 1; the graphene oxide and amino 1-ethyl-3- (3-dimethylaminopropyl) carbodiimide 1.
6. The amidated boron nitride-graphene oxide thermal conductive and insulating ink according to claim 1, wherein: the graphene oxide is prepared by a Hummers method or a modified Hummers method, and the concentration of the graphene oxide dispersion liquid in the step S2 is 0.08-10mg/ml.
7. The amidated boron nitride-graphene oxide thermal conductive and insulating ink according to claim 1, wherein: the proportion of the amidated boron nitride-graphene oxide nano filler in the heat-conducting insulating ink is 0.1-10%.
8. The amidated boron nitride-graphene oxide thermal conductive and insulating ink according to claim 1, consisting of the following components:
9. the preparation method of the amidated boron nitride-graphene oxide heat conduction and insulation ink according to any one of claims 1 to 8, characterized by comprising the following steps:
1) Stirring the urethane acrylate, the epoxy acrylate and the neopentyl glycol diacrylate at the stirring speed of 1200-2400r/min for 5-10min;
2) Adding amidated boron nitride-graphene oxide nanofiller, and stirring at the stirring speed of 3000-3500r/min for 10-15min;
3) Adding a defoaming agent, a dispersing agent and a wetting agent, finally slowly adding a photoinitiator and a flatting agent, and stirring at a stirring speed of 4000r/min for 30-40min to obtain a mixture;
4) And 3) crushing and grinding the mixture obtained in the step 3) for 1-6h, and filtering by using a 200-1000-mesh gauze to obtain the composite material.
10. Use of the amidated boron nitride-graphene oxide thermal conductive and insulating ink as claimed in any one of claims 1 to 9 in electronic and electrical printing and packaging.
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