CN115368736A - Heat-dissipation antibacterial resin for integrated circuit and preparation method thereof - Google Patents
Heat-dissipation antibacterial resin for integrated circuit and preparation method thereof Download PDFInfo
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- CN115368736A CN115368736A CN202110547903.1A CN202110547903A CN115368736A CN 115368736 A CN115368736 A CN 115368736A CN 202110547903 A CN202110547903 A CN 202110547903A CN 115368736 A CN115368736 A CN 115368736A
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- boron nitride
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- 239000011347 resin Substances 0.000 title claims abstract description 42
- 229920005989 resin Polymers 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims description 14
- 230000000844 anti-bacterial effect Effects 0.000 title abstract description 22
- 230000017525 heat dissipation Effects 0.000 title abstract description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 56
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000002071 nanotube Substances 0.000 claims abstract description 39
- 229910052582 BN Inorganic materials 0.000 claims abstract description 35
- 239000011787 zinc oxide Substances 0.000 claims abstract description 28
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 21
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 10
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 10
- 229920002545 silicone oil Polymers 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 9
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 9
- 239000004014 plasticizer Substances 0.000 claims abstract description 9
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 9
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 9
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 12
- 150000003751 zinc Chemical class 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- KJXSIXMJHKAJOD-LSDHHAIUSA-N (+)-dihydromyricetin Chemical compound C1([C@@H]2[C@H](C(C3=C(O)C=C(O)C=C3O2)=O)O)=CC(O)=C(O)C(O)=C1 KJXSIXMJHKAJOD-LSDHHAIUSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 7
- 239000003607 modifier Substances 0.000 claims description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000004246 zinc acetate Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims description 5
- HCOKJWUULRTBRS-UHFFFAOYSA-N propan-2-yloxysilane Chemical compound CC(C)O[SiH3] HCOKJWUULRTBRS-UHFFFAOYSA-N 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 4
- DSVRVHYFPPQFTI-UHFFFAOYSA-N bis(ethenyl)-methyl-trimethylsilyloxysilane;platinum Chemical compound [Pt].C[Si](C)(C)O[Si](C)(C=C)C=C DSVRVHYFPPQFTI-UHFFFAOYSA-N 0.000 claims description 4
- KQILIWXGGKGKNX-UHFFFAOYSA-N dihydromyricetin Natural products OC1C(=C(Oc2cc(O)cc(O)c12)c3cc(O)c(O)c(O)c3)O KQILIWXGGKGKNX-UHFFFAOYSA-N 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 3
- 150000005846 sugar alcohols Polymers 0.000 claims description 3
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 239000007822 coupling agent Substances 0.000 claims description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 2
- 239000002318 adhesion promoter Substances 0.000 claims 1
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 238000009413 insulation Methods 0.000 abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000945 filler Substances 0.000 abstract description 6
- 229910052710 silicon Inorganic materials 0.000 abstract description 6
- 239000010703 silicon Substances 0.000 abstract description 6
- 239000002105 nanoparticle Substances 0.000 abstract description 4
- 238000004806 packaging method and process Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 241000894006 Bacteria Species 0.000 description 4
- 230000005764 inhibitory process Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
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- 239000002041 carbon nanotube Substances 0.000 description 2
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- 239000001963 growth medium Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
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- 239000002086 nanomaterial Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 1
- 229920001817 Agar Polymers 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
- 239000008272 agar Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 150000004706 metal oxides Chemical class 0.000 description 1
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- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
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- 230000001737 promoting effect Effects 0.000 description 1
- 150000003222 pyridines Chemical class 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
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- 239000004332 silver Substances 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
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Images
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a resin for an integrated circuit, which comprises the following components in parts by weight: 10-20 parts of vinyl silicone oil, 50-60 parts of methyl-terminated polydimethylsiloxane, 10-20 parts of boron nitride nanotube-loaded zinc oxide, 2-5 parts of bonding auxiliary agent, 0.6-1.2 parts of cross-linking agent, 0.6-1.5 parts of catalyst and 4-6 parts of plasticizer. The boron nitride nanotube loaded zinc oxide nanoparticle hybrid filler is added into the resin for the integrated circuit, and the boron nitride nanotube loaded zinc oxide has high heat conduction, insulation and antibacterial properties, so that the organic silicon resin obtained by adding the boron nitride nanotube loaded zinc oxide filler into the organic silicon resin has good heat conduction, antibacterial property and electric insulation property. The organic silicon resin can be used for packaging integrated circuits and can improve excellent heat dissipation and antibacterial performance for the integrated circuits.
Description
Technical Field
The invention relates to a resin for an integrated circuit, in particular to a resin for an integrated circuit with heat dissipation and antibacterial properties.
Background
With the development of science and technology, electronic devices such as mobile phones, notebook computers, cameras, and wearable devices that have been gradually developed are closely related to the lives of people. Further, with the miniaturization, high power and high frequency of communication of electronic devices, resins for integrated circuits are required to have not only high thermal conductivity and insulation but also antibacterial performance as they are important to bacteria. Therefore, the resin for the integrated circuit of the portable electronic equipment is added with the material which has broad-spectrum antibacterial property and is nontoxic to human bodies, and meanwhile, the antibacterial material which can meet the packaging requirement of electronic products can be produced, and the produced portable equipment with antibacterial property is very important for meeting the requirements of people and promoting the technical development.
The antibacterial materials are various, and include organic matters such as quaternary ammonium salts, polyphenols and pyridines, natural antibacterial materials such as plant essential oil and chitosan, and inorganic materials such as metal ions, metal oxides and nano metal materials, and especially, the inorganic antibacterial materials are concerned with the advantages of stable chemical properties, good durability of antibacterial effect, safe use and the like. However, the nano material has large specific surface area and strong interaction force, is difficult to disperse and is easy to agglomerate. In order to improve the dispersibility of the nanomaterial. CN108147391A discloses a method for preparing a carbon nanotube carrying nano silver, which loads nano silver on the surface of the carbon nanotube to avoid the agglomeration of the nano silver. CN 110116216A discloses a preparation method of a boron nitride nanotube-silver hybrid particle material, which loads nano silver on the surface of nano boron nitride to avoid agglomeration.
However, the silver metal used in the above materials is conductive, which is not good for the insulation required by the electronic product package, and can not meet the requirement of high thermal conductivity.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the resin for the integrated circuit, which has high heat conductivity, insulation and antibiosis.
In order to achieve the purpose, the invention adopts the technical scheme that:
a resin for integrated circuits comprises the following components in parts by weight:
10-20 parts of vinyl silicone oil
50-60 parts of methyl-terminated polydimethylsiloxane
10-20 parts of boron nitride nanotube loaded zinc oxide
2-5 parts of bonding auxiliary agent
0.6 to 1.2 portions of cross-linking agent
0.6 to 1.5 portions of catalyst
4-6 parts of a plasticizer;
the preparation method of the boron nitride nanotube loaded zinc oxide comprises the following steps:
s1, ultrasonically dispersing a boron nitride nanotube in an ethanol solution to obtain an ethanol solution of the boron nitride nanotube, adding a modifier, stirring for 24-48h, filtering, washing with ethanol, and drying to obtain a modified boron nitride nanotube;
s2, dispersing the modified boron nitride nanotube obtained in the S1 into a zinc salt aqueous solution, adding alkali, and filtering to obtain filter residue;
s3, dispersing filter residues into polyhydric alcohol, reacting at 80 +/-2 ℃ for 20-30h, filtering, centrifuging, taking a solid, washing and drying to obtain the boron nitride nanotube-loaded nano zinc oxide material.
Preferably, the vinyl silicone oil has a viscosity of 1200cpa and the methyl terminated polydimethylsiloxane has a viscosity of 6000 to 12000cps.
Preferably, the bonding auxiliary agent is at least one of a borate compound and an isopropoxysilane coupling agent.
Preferably, the catalyst is at least one of a platinum (0) -divinyltetramethyldisiloxane complex and an alkoxy titanate.
Preferably, the cross-linking agent is at least one of methyl vinyl siloxane, methyl trimethoxysilane and methyl triethoxysilane.
Preferably, the plasticizer is at least one of dimethicone and octamethyltrisiloxane.
Preferably, the boron nitride nanotubes have an average length of 0.5 to 1.5 microns and an average diameter of 0.1 to 0.4 microns.
Preferably, the modifier is at least one of dihydromyricetin, KH570 and KH 550.
Preferably, in the step S1, the concentration of the boron nitride nanotubes in the ethanol solution of the boron nitride nanotubes is 0.5 to 2g/L; the mass ratio of the modifier to the boron nitride nanotube is 1-2:1.
preferably, in the step S2, the concentration of the boron nitride nanotube in the dispersed aqueous solution of zinc salt is 0.5-1g/L; the concentration of zinc ions in the aqueous solution of the zinc salt is 0.2-0.4g/L.
Preferably, the zinc salt is at least one of zinc acetate and zinc nitrate.
Preferably, the base is at least one of urea, ammonia and triethylamine.
Preferably, the amount of the base is 4~6 times the mass of the zinc salt.
Preferably, the polyol is at least one of ethylene glycol, propylene glycol, butylene glycol and glycerol.
Preferably, in step S3, the centrifugation is a fractional centrifugation: centrifuging at 1500-2500 rpm, collecting the upper layer liquid, and centrifuging at 4000-6000 rpm to collect the lower layer solid.
The preparation method of the resin for the integrated circuit comprises the following steps:
mixing the components in proportion, heating and stirring, vacuumizing for 4-6 hours, removing bubbles, mixing, placing in a mold, heating to 245-250 ℃, and curing and molding.
The invention has the beneficial effects that: the invention provides a resin for an integrated circuit, wherein a boron nitride nanotube loaded zinc oxide nanoparticle hybrid filler is added into the resin for the integrated circuit, and the boron nitride nanotube loaded zinc oxide has high heat conduction, insulation and antibacterial properties, so that the obtained organic silicon resin has good heat conduction, antibacterial property and electric insulation property by adding the boron nitride nanotube loaded zinc oxide filler into the organic silicon resin. The organic silicon resin can be used for packaging integrated circuits and can improve excellent heat dissipation and antibacterial performance for the integrated circuits.
Drawings
FIG. 1 is a scanning electron microscope image of a boron nitride nanotube loaded with zinc oxide nanoparticles.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
The resin for an integrated circuit described in this example contains the following components in parts by weight:
10 portions of vinyl silicone oil (the viscosity is 1200 cpa)
50 parts of methyl-terminated polydimethylsiloxane (viscosity 6000)
Boron nitride nanotube loaded zinc oxide 10 parts
Boric acid ester compound 2 parts
0.6 part of cross-linking agent methylvinylsiloxane
Catalyst platinum (0) -divinyltetramethyldisiloxane Complex 0.6 parts
4 parts of plasticizer dimethyl silicone oil;
the preparation method of the boron nitride nanotube loaded zinc oxide in the embodiment comprises the following steps:
s1, ultrasonically dispersing boron nitride nanotubes with the average length of 1 micron and the average diameter of 0.3 micron in an ethanol solution, wherein the concentration of the boron nitride nanotubes is 0.5g/L, and then adding a modifier, namely dihydromyricetin, wherein the mass ratio of the dihydromyricetin to the boron nitride nanotubes is 1:1, stirring for 24 hours at room temperature, filtering, washing with ethanol, and drying to obtain a modified boron nitride nanotube;
s2, dispersing the modified boron nitride nanotubes obtained in the S1 into an aqueous solution of zinc acetate, wherein the concentration of the boron nitride nanotubes is 0.5g/L, the concentration of the aqueous solution of the zinc acetate is 0.2g/L, adding ammonia water to precipitate the zinc acetate solution, wherein the adding amount of the ammonia water is 4 times that of the zinc acetate, and filtering to obtain a filter cake;
s3, dispersing the filter cake into ethylene glycol, reacting for 24 hours at 80 ℃, filtering, carrying out fractional centrifugation, firstly carrying out centrifugation at a rotating speed of 2000 rpm, collecting liquid at the upper layer, carrying out centrifugation at 5000 rpm, collecting solid at the lower layer, washing for 3 times, and then drying at 600 ℃ to obtain the boron nitride nanotube-loaded nano zinc oxide material.
FIG. 1 is a scanning electron microscope image of zinc oxide nanoparticles loaded on boron nitride nanotubes prepared by the method of this example; as can be seen from the figure, the nano zinc oxide is loaded on the surface of the boron nitride nanotube.
The preparation method of the resin for the integrated circuit in the embodiment comprises the following steps: the components are mixed according to a certain proportion, heated and stirred, the mixture is vacuumized for 4 hours, bubbles are removed, and then the mixture is placed in a mould and heated to 245 ℃ for curing and molding.
Example 2
The resin for an integrated circuit described in this example contains the following components in parts by weight:
20 portions of vinyl silicone oil (the viscosity is 1200 cpa)
60 portions of methyl-terminated polydimethylsiloxane (viscosity 12000)
Boron nitride nanotube loaded zinc oxide 20 parts
5 parts of bonding auxiliary agent namely isopropoxysilane
1.2 parts of crosslinking agent methyltrimethoxysilane
Catalyst alkoxy titanate 1.5 parts
Plasticizer octamethyltrisiloxane 6 parts
The preparation method of the boron nitride nanotube-loaded zinc oxide in this example is the same as that in example 1.
The preparation method of the resin for the integrated circuit in the embodiment comprises the following steps: the components are mixed according to a certain proportion, heated and stirred, the mixture is vacuumized for 6 hours, bubbles are removed, and then the mixture is placed in a mould and heated to 250 ℃ for curing and molding.
Example 3
The resin for an integrated circuit described in this example contains the following components in parts by weight:
20 portions of vinyl silicone oil (the viscosity is 1200 cpa)
60 portions of methyl-terminated polydimethylsiloxane (viscosity 12000)
Boron nitride nanotube loaded zinc oxide 10 parts
3 parts of bonding auxiliary agent namely isopropoxysilane
Cross-linking agent methylvinylsiloxane 1 part
Catalyst alkoxy titanate 1 part
4 parts of plasticizer octamethyltrisiloxane;
the preparation method of the boron nitride nanotube-loaded zinc oxide in this example is the same as that in example 1.
The preparation method of the resin for the integrated circuit in the embodiment comprises the following steps: the components are mixed according to a certain proportion, heated and stirred, the mixture is vacuumized for 6 hours, bubbles are removed, and then the mixture is placed in a mould and heated to 250 ℃ for curing and molding.
Example 4
The resin for an integrated circuit described in this example contains the following components in parts by weight:
20 portions of vinyl silicone oil (the viscosity is 1200 cpa)
60 portions of methyl end-capped polydimethylsiloxane (viscosity 8000)
Boron nitride nanotube loaded zinc oxide 15 parts
3 parts of bonding auxiliary agent namely isopropoxysilane
Cross-linking agent methylvinylsiloxane 1 part
Catalyst platinum (0) -divinyltetramethyldisiloxane Complex 1 part
Plasticizer octamethyltrisiloxane 4 parts
The preparation method of the boron nitride nanotube-loaded zinc oxide in this example is the same as that in example 1.
The preparation method of the resin for the integrated circuit in the embodiment comprises the following steps: the components are mixed according to a certain proportion, heated and stirred, the mixture is vacuumized for 6 hours, bubbles are removed, and then the mixture is placed in a mould and heated to 250 ℃ for curing and molding.
Comparative example 1
The resin for an integrated circuit described in this comparative example differs from example 1 only in that zinc oxide was supported without adding boron nitride nanotubes.
And (3) performance testing:
antibacterial property: the inhibition zones of the resins for integrated circuits described in example 1~4 and comparative example 1 were determined by the agar diffusion method. 0.1 ml of staphylococcus aureus liquid in logarithmic phase and escherichia coli (2X 10C FU/m L) are sucked and respectively placed on a culture medium suitable for growth of bacteria, and the bacteria liquid is uniformly coated by using a sterile coating rod. The material of examples 2 to 5 having a diameter of 3mm was cut out by a punch and placed in the center of the medium. The culture medium was placed in an oven at 37 ℃ and cultured in 24h and observed. The diameters (mm) of two vertical directions of each inhibition zone are respectively measured by a vernier caliper, the edge of the inhibition zone is the edge where bacteria can not obviously grow, and the antibacterial activity of different samples is evaluated. The above operations were repeated in parallel for 3 times, and the mean diameter of the zone of inhibition was calculated.
Thermal conductivity: the thermal conductivity of the resin for integrated circuits described in example 1~4 and comparative example 1 was measured by a laser flash method,
insulating property: the insulating properties of the resins for integrated circuits described in example 1~4 and comparative example 1 were characterized by dielectric strength.
Test results are shown in tables 1 and 2.
TABLE 1
| Antibacterial radius of staphylococcus aureus | Antibacterial radius of escherichia coli | |
| Example 1 | 0.26cm | 0.28cm |
| Example 2 | 0.37cm | 0.38cm |
| Example 3 | 0.22cm | 0.24cm |
| Example 4 | 0.32cm | 0.34cm |
| Comparative example 1 | 0 cm | 0 cm |
TABLE 2
| Thermal conductivity at 25 ℃ of lambda/(W/(m.K)) | Dielectric strength V/mum at 25 DEG C | |
| Example 1 | 1.29 | 53.6 |
| Example 2 | 1.61 | 51.1 |
| Example 3 | 1.07 | 54.1 |
| Example 4 | 1.42 | 52.3 |
| Comparative example 1 | 0.132 | 57.2 |
It can be seen from table 1 that the antibacterial performance of the organosilicon material added with the boron nitride nanotube-loaded zinc oxide filler is obviously better than that of the organosilicon resin, and from table 2, the heat-conducting performance of the organosilicon material added with the boron nitride nanotube-loaded zinc oxide filler is greatly improved, and the dielectric strength is reduced but the change is small.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The resin for the integrated circuit is characterized by comprising the following components in parts by weight:
10-20 parts of vinyl silicone oil
Methyl-terminated polydimethylsiloxane 50-60
Boron nitride nanotube loaded zinc oxide 10-20
2-5 parts of bonding auxiliary agent
0.6-1.2 parts of cross-linking agent
Catalyst 0.6-1.5
4-6 parts of a plasticizer;
the preparation method of the boron nitride nanotube loaded zinc oxide comprises the following steps:
s1, ultrasonically dispersing a boron nitride nanotube in an ethanol solution to obtain the ethanol solution of the boron nitride nanotube, adding a modifier, stirring for 24-48h, filtering, washing with ethanol, and drying to obtain a modified boron nitride nanotube;
s2, dispersing the modified boron nitride nanotube obtained in the S1 into a zinc salt aqueous solution, adding alkali, and filtering to obtain filter residue;
s3, dispersing filter residues into the polyhydric alcohol, reacting for 20-30h at the temperature of 80 +/-2 ℃, filtering, centrifuging, taking solid, washing and drying to obtain the boron nitride nanotube-loaded nano zinc oxide material.
2. The resin according to claim 1, wherein the vinyl silicone oil has a viscosity of 1200cpa and the methyl terminated polydimethylsiloxane has a viscosity of 6000 to 12000cps.
3. The resin for integrated circuits according to claim 1, wherein said adhesion promoter is at least one of a borate compound and an isopropoxysilane coupling agent.
4. The resin for integrated circuits according to claim 1, wherein the catalyst is at least one of a platinum (0) -divinyltetramethyldisiloxane complex and an alkoxy titanate.
5. The resin for integrated circuits of claim 1, wherein the crosslinking agent is at least one of methylvinylsiloxane, methyltrimethoxysilane, and methyltriethoxysilane.
6. The resin for integrated circuits according to claim 1, wherein the plasticizer is at least one of dimethylsilicone oil and octamethyltrisiloxane.
7. The resin for integrated circuits of claim 1, wherein said boron nitride nanotubes have an average length of 0.5 to 1.5 microns and an average diameter of 0.1 to 0.4 microns.
8. The resin for integrated circuits according to claim 1, wherein the modifier is at least one of dihydromyricetin, KH570 and KH 550.
9. The resin for integrated circuits according to claim 1, wherein in the step S1, the concentration of the boron nitride nanotubes in the ethanol solution of the boron nitride nanotubes is 0.5 to 2g/L; the mass ratio of the modifier to the boron nitride nanotube is 1-2:1.
10. the resin for integrated circuits according to claim 1, wherein at least one of the following (a) - (f):
(a) In the step S2, the concentration of the boron nitride nanotube in the dispersed zinc salt aqueous solution is 0.5-1g/L;
(b) In the zinc salt water solution, the concentration of zinc ions is 0.2-0.4g/L;
(c) The zinc salt is at least one of zinc acetate and zinc nitrate; the alkali is at least one of urea, ammonia water and triethylamine;
(d) The dosage of the alkali is 4-6 times of the mass of the zinc salt;
(e) The polyalcohol is at least one of ethylene glycol, propylene glycol, butanediol and glycerol;
(f) In step S3, the centrifugation is a fractional centrifugation: centrifuging at 1500-2500 rpm, collecting the upper layer liquid, and centrifuging at 4000-6000 rpm to collect the lower layer solid.
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| CN116218231A (en) * | 2023-02-28 | 2023-06-06 | 华南理工大学 | Chitosan and silane coupling agent modified silicone oil-based flexible heat-conducting composite material and preparation method thereof |
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