CN107033541B - A kind of nano silver/epoxy resin high-dielectric composite material and preparation method thereof - Google Patents
A kind of nano silver/epoxy resin high-dielectric composite material and preparation method thereof Download PDFInfo
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- CN107033541B CN107033541B CN201611224321.5A CN201611224321A CN107033541B CN 107033541 B CN107033541 B CN 107033541B CN 201611224321 A CN201611224321 A CN 201611224321A CN 107033541 B CN107033541 B CN 107033541B
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- 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
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- C08K3/08—Metals
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
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Abstract
The present invention relates to a kind of nano silver/epoxy resin high-dielectric composite materials and preparation method thereof, it is prepared by following methods: 1) complexing agent, silver salt, promotor, the reducing agent containing two aldehyde radicals and acid anhydride type curing agent being added sequentially in epoxy resin, are uniformly mixing to obtain mixed sols；2) mixed sols obtained by step 1) is poured into mold, it is placed in heater box, heated at constant temperature 2-6h at being 60-90 DEG C in temperature then heats to 100-130 DEG C of heated at constant temperature 2-6h, it is warming up to 150-180 DEG C of heated at constant temperature 2-4h again, obtains nano silver/epoxy resin high-dielectric composite material.The present invention by silver mirror reaction in-situ preparation there are the nano-Ag particles of good electric conductivity to solve the problems, such as that dielectric constant existing for tiny conducting particles/epoxy-resin systems is low or dielectric loss is high with good dispersibility.
Description
Technical field
The invention belongs to technical field of composite material manufacturing, are related to a kind of nano silver/epoxy resin high-dielectric composite material
And preparation method thereof.
Background technique
After epoxy resin cure have excellent mechanical property, adhesive property, corrosion resistance and its cure shrinkage and
Linear expansion coefficient is small, and dimensional stability and good manufacturability, comprehensive performance is good, is widely used in the production of buried capacitors.But
As power electronic equipment is towards large capacity, the development in high voltage direction, safety and operational reliability to capacitor are required more
What is added is stringent, and the requirement to epoxy resin dielectric properties is also higher and higher.
In general, the dielectric constant values of simple epoxy resin are lower.But according to coulomb blockade mechanism: when a metal is micro-
There are when electric insulation between grain and its surrounding medium, only electronics tunnelling could enter the gold from the outside under given conditions
Belong to particle.Therefore it is, in principle, that the dielectric constant for being added to the epoxy resin of nano-Ag particles is deserved under conductive percolation threshold
It is promoted to effective.
But this kind of epoxy matrix composite is in process, since nano-Ag particles are tiny, large specific surface area, easily produces
Raw reunion is hard to be uniformly dispersed in resin, and then leads to biggish dielectric loss.To meet power electronics industry to epoxy
The requirement of resin dielectric performance, while reducing dielectric loss, present invention application silver mirror reaction, i.e. supporting roller bush can be by aldehydes
It closes object and is reduced to silver, the in-situ preparation nano silver particles in epoxy-resin systems realize the evenly dispersed of nano-Ag particles, to ring
After oxygen resin solidification, it is prepared into the nano silver/epoxy resin composite materials of high-dielectric and low-loss.
Summary of the invention
The technical problem to be solved by the present invention is to aiming at the above shortcomings existing in the prior art, provide a kind of nanometer
The high dielectric composite wood of nano silver/epoxy resin is prepared in situ out in silver/epoxy resin high-dielectric composite material and preparation method thereof
Material, gained nano silver are uniformly dispersed in the epoxy, and gained epoxy matrix composite has high dielectric constant.
In order to solve the above technical problems, present invention provide the technical scheme that
A kind of nano silver/epoxy resin high-dielectric composite material is provided, it is prepared by following methods:
1) complexing agent, silver salt, promotor, the reducing agent containing two aldehyde radicals and acid anhydride type curing agent are added sequentially to epoxy
In resin, it is uniformly mixing to obtain mixed sols；
2) mixed sols obtained by step 1) is poured into mold, is placed in heater box, constant temperature adds at being 60-90 DEG C in temperature
Hot 2-6h then heats to 100-130 DEG C of heated at constant temperature 2-6h, then is warming up to 150-180 DEG C of heated at constant temperature 2-4h, obtains nanometer
Silver/epoxy resin high-dielectric composite material.
According to the above scheme, the step 1) silver salt is one of silver oxalate, silver nitrate, silver acetate or a variety of mixing
The mass ratio of object, the silver salt and epoxy resin is 0.1-0.5:1.
According to the above scheme, the step 1) complexing agent is N- (2- aminoethyl) -3- aminopropyl trimethoxysilane, N- (2-
Aminoethyl) -3- aminopropyl triethoxysilane, one of γ-mercaptopropyl trimethoxysilane or a variety of mixtures, it is described
The mass ratio of complexing agent and epoxy resin is 0.02-0.1:1.
According to the above scheme, the step 1) promotor be 2,4,6- tri- (dimethylamino methyl) phenol, tetraethylammonium bromide,
The mass ratio of one of 2-ethyl-4-methylimidazole or a variety of mixtures, the promotor and epoxy resin is 0.01-
0.05:1.
According to the above scheme, the step 1) reducing agent containing two aldehyde radicals is o-phthalaldehyde, m-terephthal aldehyde, to benzene two
The molar ratio of one of formaldehyde or a variety of mixtures, the reducing agent for containing two aldehyde radicals and the silver salt is 0.25-
0.5:1.
According to the above scheme, the step 1) acid anhydride type curing agent is phthalic anhydride, tetrabydrophthalic anhydride, methyl
One of hexahydrophthalic anhydride, methyl tetrahydro phthalic anhydride or in which several mixtures, the acid anhydride type curing agent and epoxy resin
Mass ratio is 0.8-0.9:1.
According to the above scheme, the step 1) epoxy resin is bisphenol A epoxide resin, bisphenol F epoxy resin, brominated bisphenol A
One of epoxy resin or in which several mixtures.
The present invention also provides the preparation methods of above-mentioned nano silver/epoxy resin high-dielectric composite material comprising following step
It is rapid:
1) complexing agent, silver salt, promotor, the reducing agent containing two aldehyde radicals and acid anhydride type curing agent are added sequentially to epoxy
In resin, it is uniformly mixing to obtain mixed sols；
2) mixed sols obtained by step 1) is poured into mold, is placed in heater box, constant temperature adds at being 60-90 DEG C in temperature
Hot 2-6h then heats to 100-130 DEG C of heated at constant temperature 2-6h, then is warming up to 150-180 DEG C of heated at constant temperature 2-4h, obtains nanometer
Silver/epoxy resin high-dielectric composite material.
The beneficial effects of the present invention are: the present invention makes argent-amine complex by silver mirror reaction in epoxy-resin systems
By containing there are two the reduction of the compound of aldehyde radical, in-situ preparation has the nano-Ag particles of good electric conductivity, with good point
Property is dissipated, solves the problems, such as that dielectric constant existing for tiny conducting particles/epoxy-resin systems is low or dielectric loss is high；This
The preparation method process that invention provides is short, technological operation is simple, and the stability in material manufacturing process can be improved, and is easy real
Existing mass production, reduces cost.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention makees the present invention below with reference to embodiment
It is described in further detail.
Embodiment 1
A kind of high dielectric compound resin is prepared, steps are as follows:
1) by 1g N- (2- aminoethyl) -3- aminopropyl triethoxysilane, 5g silver nitrate, tri- (diformazan of 0.5g 2,4,6-
Amino methyl) phenol, 1g o-phthalaldehyde, 8.5g methyl hexahydrophthalic anhydride be added sequentially in 10g E44 epoxy resin, high-speed stirring
It mixes and is uniformly dispersed to obtain mixed sols；
2) mixed sols obtained by step 1) is poured into iron mold, is placed into temperature-gradient method in air dry oven and solidifies,
Heated at constant temperature 6h at 60 DEG C then heats to 100 DEG C of heated at constant temperature 6h, then is warming up to 150 DEG C of heated at constant temperature 4h, obtains nanometer
Silver/epoxy resin high-dielectric composite material.
Measuring the dielectric constant of composite material manufactured in the present embodiment at 1 khz at room temperature is 8.2, and dielectric loss is
0.023。
Comparative example 1
A kind of dielectric compound resin is prepared, steps are as follows:
1) 0.5g 2,4,6- tri- (dimethylamino methyl) phenol, 8.5g methyl hexahydrophthalic anhydride are added sequentially to 10g E44
In epoxy resin, high-speed stirred is uniformly dispersed to obtain mixed sols；
2) mixed sols obtained by step 1) is poured into iron mold, is placed into temperature-gradient method in air dry oven and solidifies,
Heated at constant temperature 6h at 60 DEG C then heats to 100 DEG C of heated at constant temperature 6h, then is warming up to 150 DEG C of heated at constant temperature 4h, obtains nanometer
Silver/epoxy resin dielectric composite material.
Measuring the dielectric constant of composite material manufactured in the present embodiment at 1 khz at room temperature is 4.2, and dielectric loss is
0.008。
Embodiment 2
A kind of high dielectric compound resin is prepared, steps are as follows:
1) by 1g N- (2- aminoethyl) -3- aminopropyl trimethoxysilane, 5g silver oxalate, 0.2g tetraethylammonium bromide, 1g
M-terephthal aldehyde, 8.5g methyl tetrahydro phthalic anhydride are added sequentially in 10g E44 epoxy resin, and high-speed stirred, which is uniformly dispersed, is mixed
Close colloidal sol；
2) mixed sols obtained by step 1) is poured into iron mold, is placed into temperature-gradient method in air dry oven and solidifies,
Heated at constant temperature 4h at 60 DEG C then heats to 100 DEG C of heated at constant temperature 4h, then is warming up to 150 DEG C of heated at constant temperature 3h, obtains nanometer
Silver/epoxy resin high-dielectric composite material.
Measuring the dielectric constant of composite material manufactured in the present embodiment at 1 khz at room temperature is 8.7, and dielectric loss is
0.025。
Comparative example 2
A kind of dielectric compound resin is prepared, steps are as follows:
1) 0.2g tetraethylammonium bromide, 8.5g methyl tetrahydro phthalic anhydride are added sequentially in 10g E44 epoxy resin, high speed
It is dispersed with stirring and uniformly obtains mixed sols；
2) mixed sols obtained by step 1) is poured into iron mold, is placed into temperature-gradient method in air dry oven and solidifies,
Heated at constant temperature 4h at 60 DEG C then heats to 100 DEG C of heated at constant temperature 4h, then is warming up to 150 DEG C of heated at constant temperature 3h, obtains nanometer
Silver/epoxy resin dielectric composite material.
Measuring the dielectric constant of composite material manufactured in the present embodiment at 1 khz at room temperature is 4.6, and dielectric loss is
0.011。
Embodiment 3
A kind of high dielectric compound resin is prepared, steps are as follows:
1) by 0.2g N- (2- aminoethyl) -3- aminopropyl trimethoxysilane, 1g silver acetate, 0.3g 2- ethyl -4- first
Base imidazoles, 0.4g terephthalaldehyde, 8.5g methyl hexahydrophthalic anhydride are added sequentially in 10g E51 epoxy resin, high-speed stirred point
It dissipates and uniformly obtains mixed sols；
2) mixed sols obtained by step 1) is poured into iron mold, is placed into temperature-gradient method in air dry oven and solidifies,
Heated at constant temperature 2h at 60 DEG C then heats to 100 DEG C of heated at constant temperature 2h, then is warming up to 150 DEG C of heated at constant temperature 2h, obtains nanometer
Silver/epoxy resin high-dielectric composite material.
Measuring the dielectric constant of composite material manufactured in the present embodiment at 1 khz at room temperature is 5.7, and dielectric loss is
0.016。
Comparative example 3
A kind of dielectric compound resin is prepared, steps are as follows:
1) 0.3g 2-ethyl-4-methylimidazole, 8.5g methyl hexahydrophthalic anhydride are added sequentially to 10g E51 epoxy resin
In, high-speed stirred is uniformly dispersed to obtain mixed sols；
2) mixed sols obtained by step 1) is poured into iron mold, is placed into temperature-gradient method in air dry oven and solidifies,
Heated at constant temperature 2h at 60 DEG C then heats to 100 DEG C of heated at constant temperature 2h, then is warming up to 150 DEG C of heated at constant temperature 2h, obtains nanometer
Silver/epoxy resin dielectric composite material.
Measuring the dielectric constant of composite material manufactured in the present embodiment at 1 khz at room temperature is 4.3, and dielectric loss is
0.009。
Embodiment 4
A kind of high dielectric compound resin is prepared, steps are as follows:
1) by 0.6g γ-mercaptopropyl trimethoxysilane, 3g silver nitrate, 0.3g 2-ethyl-4-methylimidazole, 0.6g pairs
The mixture (mixing mass ratio 1:1) of phthalaldehyde and m-terephthal aldehyde, 8.5g methyl hexahydrophthalic anhydride are added sequentially to 10g E51
In epoxy resin, high-speed stirred is uniformly dispersed to obtain mixed sols；
2) mixed sols obtained by step 1) is poured into iron mold, is placed into temperature-gradient method in air dry oven and solidifies,
Heated at constant temperature 4h at 60 DEG C then heats to 100 DEG C of heated at constant temperature 4h, then is warming up to 150 DEG C of heated at constant temperature 3h, obtains nanometer
Silver/epoxy resin high-dielectric composite material.
Measuring the dielectric constant of composite material manufactured in the present embodiment at 1 khz at room temperature is 7.1, and dielectric loss is
0.021。
Comparative example 4
A kind of dielectric compound resin is prepared, steps are as follows:
1) by 0.3g 2-ethyl-4-methylimidazole, 8.5g methyl hexahydrophthalic anhydride is added sequentially to 10g E51 epoxy resin
In, high-speed stirred is uniformly dispersed to obtain mixed sols；
2) mixed sols obtained by step 1) is poured into iron mold, is placed into temperature-gradient method in air dry oven and solidifies,
Heated at constant temperature 4h at 60 DEG C then heats to 100 DEG C of heated at constant temperature 4h, then is warming up to 150 DEG C of heated at constant temperature 3h, obtains nanometer
Silver/epoxy resin dielectric composite material.
Measuring the dielectric constant of composite material manufactured in the present embodiment at 1 khz at room temperature is 4.7, and dielectric loss is
0.012。
Claims (6)
1. a kind of nano silver/epoxy resin high-dielectric composite material, which is characterized in that it is prepared by following methods:
1) complexing agent, silver salt, promotor, the reducing agent containing two aldehyde radicals and acid anhydride type curing agent are added sequentially to epoxy resin
In, it is uniformly mixing to obtain mixed sols；
2) mixed sols obtained by step 1) is poured into mold, is placed in heater box, heated at constant temperature 2- at being 60-90 DEG C in temperature
6h then heats to 100-130 DEG C of heated at constant temperature 2-6h, then is warming up to 150-180 DEG C of heated at constant temperature 2-4h, obtain nano silver/
Epoxy resin high-dielectric composite material；
Silver salt described in step 1) is one of silver oxalate, silver nitrate, silver acetate or a variety of mixtures, the silver salt and epoxy
The mass ratio of resin is 0.1-0.5:1；
Complexing agent described in step 1) is N- (2- aminoethyl) -3- aminopropyl trimethoxysilane, N- (2- aminoethyl) -3- aminopropyl
One of triethoxysilane, γ-mercaptopropyl trimethoxysilane or a variety of mixtures, the complexing agent and epoxy resin
Mass ratio be 0.02-0.1:1.
2. nano silver/epoxy resin high-dielectric composite material according to claim 1, it is characterised in that promote described in step 1)
It is one of 2,4,6- tri- (dimethylamino methyl) phenol, tetraethylammonium bromide, 2-ethyl-4-methylimidazole or a variety of into agent
Mixture, the mass ratio of the promotor and epoxy resin is 0.01-0.05:1.
3. nano silver/epoxy resin high-dielectric composite material according to claim 1, it is characterised in that contain described in step 1)
The reducing agent of two aldehyde radicals be one of o-phthalaldehyde, m-terephthal aldehyde, terephthalaldehyde or a variety of mixtures, it is described
The molar ratio of reducing agent and the silver salt containing two aldehyde radicals is 0.25-0.5:1.
4. nano silver/epoxy resin high-dielectric composite material according to claim 1, it is characterised in that acid described in step 1)
Anhydride curing agent be one of phthalic anhydride, tetrabydrophthalic anhydride, methyl hexahydrophthalic anhydride, methyl tetrahydro phthalic anhydride or
The mass ratio of wherein several mixture, the acid anhydride type curing agent and epoxy resin is 0.5-1:1.
5. nano silver/epoxy resin high-dielectric composite material according to claim 1, it is characterised in that ring described in step 1)
Oxygen resin is one of bisphenol A epoxide resin, bisphenol F epoxy resin, brominated bisphenol A epoxy resin or in which several mixing
Object.
6. a kind of preparation method of any nano silver/epoxy resin high-dielectric composite material of claim 1-5, feature
Be the following steps are included:
1) complexing agent, silver salt, promotor, the reducing agent containing two aldehyde radicals and acid anhydride type curing agent are added sequentially to epoxy resin
In, it is uniformly mixing to obtain mixed sols；
2) mixed sols obtained by step 1) is poured into mold, is placed in heater box, heated at constant temperature 2- at being 60-90 DEG C in temperature
6h then heats to 100-130 DEG C of heated at constant temperature 2-6h, then is warming up to 150-180 DEG C of heated at constant temperature 2-4h, obtain nano silver/
Epoxy resin high-dielectric composite material.
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| CN201611224321.5A CN107033541B (en) | 2016-12-27 | 2016-12-27 | A kind of nano silver/epoxy resin high-dielectric composite material and preparation method thereof |
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| CN110310760B (en) * | 2019-07-25 | 2021-02-23 | Oppo广东移动通信有限公司 | Antenna silver paste, preparation method, antenna for electronic equipment and electronic equipment |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781541A (en) * | 2010-02-02 | 2010-07-21 | 华南理工大学 | Situ preparation method of nano silver/epoxy conductive adhesive |
| CN105274505A (en) * | 2014-06-17 | 2016-01-27 | 中国科学院大连化学物理研究所 | Method for preparing nano-composite by controllable deposition of silver atoms on surface of nano-oxide |
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- 2016-12-27 CN CN201611224321.5A patent/CN107033541B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781541A (en) * | 2010-02-02 | 2010-07-21 | 华南理工大学 | Situ preparation method of nano silver/epoxy conductive adhesive |
| CN105274505A (en) * | 2014-06-17 | 2016-01-27 | 中国科学院大连化学物理研究所 | Method for preparing nano-composite by controllable deposition of silver atoms on surface of nano-oxide |
Non-Patent Citations (1)
| Title |
|---|
| 银纳米材料制备和应用进展;朱桂琴等;《科技导报》(第22期);第112-117页 * |
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