CN107936295A - A kind of modified Nano copper and Nanometer Copper epoxy resin composite material and preparation method thereof - Google Patents
A kind of modified Nano copper and Nanometer Copper epoxy resin composite material and preparation method thereof Download PDFInfo
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- CN107936295A CN107936295A CN201711192030.7A CN201711192030A CN107936295A CN 107936295 A CN107936295 A CN 107936295A CN 201711192030 A CN201711192030 A CN 201711192030A CN 107936295 A CN107936295 A CN 107936295A
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- copper
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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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
- C08K3/02—Elements
- 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
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a kind of modified Nano copper and Nanometer Copper epoxy resin composite material and preparation method thereof, aim to provide a kind of dielectric properties, stability and dispersed excellent modified Nano copper, specifically, the modified Nano copper is the Nanometer Copper that surface is coated with silicon oxide, meanwhile the present invention also provides Nanometer Copper epoxy resin composite material containing the modified Nano copper and preparation method thereof.
Description
Technical field
The present invention relates to high-dielectric composite material, is a kind of modified Nano copper and Nanometer Copper-epoxy resin specifically
Composite material, the invention further relates to the preparation method of the Nanometer Copper-epoxy resin composite material, belongs to field of material technology.
Background technology
In order to increase the performance of material, usually material is modified, 201310363280.8 epoxy resin of Chinese patent/
Hot interface composites of nano-copper/carbon nanotube and preparation method thereof, its scheme are kind of an Epoxy/nano copper/carbon nanotubes
Hot interface composites, it is characterised in that in parts by weight, its component composition is：100 parts of epoxy resin, 1~20 part of curing agent,
1~10 part of epoxy propane butyl ether diluent, 50~235 parts of nanometer copper particle, 0.5~25 part of the carbon nanotubes of carboxylated, its
In, curing agent is polyamide.The composite material purpose can realize carbon nanotubes in the epoxy fine dispersion at the same time with
Nanometer copper particle uniformly mixes the thermal conductivity for significantly improving epoxy resin composite material.It is that first the surface of carbon nanotubes is carried out
Carboxylated processing, is then total to molten and can uniformly divide with nanometer copper particle by it in epoxy resin base material under certain condition
Dissipate.
The content of the invention
For above-mentioned deficiency, it is excellent that of the invention first purpose is to provide a kind of dielectric properties, stability and dispersiveness
Modified Nano copper；
Second object of the present invention be to provide a kind of low-dielectric loss, controllable percolation threshold, good weatherability properties can
Nanometer Copper-epoxy resin composite material.
Third object of the present invention is to provide the preparation method of above-mentioned Nanometer Copper-epoxy resin composite material.
For this reason, first technical solution provided by the invention is such：
A kind of modified Nano copper, the modified Nano copper are the Nanometer Copper that surface is coated with silicon oxide.
In above-mentioned modified Nano copper, the specific method of the surface coated silica of the modified Nano copper is：
Surface modification is carried out to the surface of Nanometer Copper by tetramethoxysilance.
A kind of Nanometer Copper-epoxy resin composite material, is made of following components in parts by weight：Modified Nano copper particle 1~
10 parts, 90~98 parts of epoxy resin, 0.2~0.35 part of antioxidant, 0.2-0.4 parts of coupling agent.Further, above-mentioned nanometer
Copper-epoxy resin composite material, is made of following components in parts by weight：3~8 parts of modified Nano copper particle, epoxy resin 92~
96 parts, 0.25~0.30 part of antioxidant, 0.3 part of coupling agent.
Further, above-mentioned Nanometer Copper-epoxy resin composite material, the antioxidant are selected from four [β-(3,5- bis-
Tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (anti-1010), phosphite ester kind antioxidant be three [2,4- di-tert-butyls
Base] phosphite ester (anti-168), N, N'- be double-(3- (3,5- di-tert-butyl-hydroxy phenyls) propiono) hexamethylene diamine (anti-1098)；
One kind in β-(3,5- di-tert-butyl-hydroxy phenyls) propionic acid octadecanol ester (anti-1076).
Further, above-mentioned Nanometer Copper-epoxy resin composite material, the coupling agent are selected from silane coupling agent, such as
γ-aminopropyl triethoxysilane (A1100), three tert-butyl peroxide silane (Y-4310) of vinyl, diethylin are for methyl
One kind in triethoxysilane (ND22).
Second technical solution provided by the invention is the preparation method of above-mentioned Nanometer Copper-epoxy resin composite material,
Comprise the following steps successively：
1) under inert gas shielding, after tetramethoxysilance and copper nanoparticle are disperseed in ethanol, back flow reaction, room temperature
2~3h of mechanical agitation, makes it carry out surface modification to nanometer copper particle；
2) ethanol is made to volatilize in fume hood the alcohol suspension of the Nanometer Copper of modification, rear vacuum drying oven 60~80
DEG C drying, after block modified Nano copper is subjected to powder, obtain the modified Nano copper of dry refinement；
3) 90~98 parts of 1~10 part of the modified Nano copper and epoxy resin refined step 2) drying, antioxidant 0.2~
0.35 part, 0.2-0.4 parts of coupling agent, is uniformly mixed in low speed mixer, then is made at 230~240 DEG C by Single screw extrusion
Grain.
Further, the preparation method of above-mentioned Nanometer Copper-epoxy resin composite material, the low speed mixer rotating speed are
300~350r/min.
Compared with prior art, the stability of modified Nano copper of the invention and dispersiveness are excellent；
The shortcomings of Nanometer Copper-epoxy resin composite material of the present invention overcomes traditional compound material antioxygenic property poor,
With low-dielectric loss, controllable percolation threshold, good weatherability properties energy.
Embodiment
In order to become apparent from the purpose of the present invention, technical solution and advantageous effects, with reference to embodiments, to this
Invention is further elaborated.It should be appreciated that the embodiment described in this specification is just for the sake of this hair of explanation
It is bright, be not intended to limit the present invention, the parameter of embodiment, ratio etc. can adaptation to local conditions make a choice and substance had no to result
Influence.
Embodiment 1
A kind of Nanometer Copper-epoxy resin composite material provided by the invention, is made of the component of following mass numbers：Modification is received
Rice copper particle 9kg, epoxy resin 90.4kg, antioxidant 0.2kg, coupling agent 0.4kg.
Embodiment 2
A kind of Nanometer Copper-epoxy resin composite material provided by the invention, is made of the component of following mass numbers：Modification is received
Rice copper particle 1.45kg, epoxy resin 98kg, antioxidant 0.35kg, coupling agent 0.2kg.
Embodiment 3
A kind of Nanometer Copper-epoxy resin composite material provided by the invention, is made of the component of following mass numbers：Modification is received
Rice copper particle 3.4kg, epoxy resin 96kg, antioxidant 0.30kg, coupling agent 0.3kg.
Embodiment 4
A kind of Nanometer Copper-epoxy resin composite material provided by the invention, is made of the component of following mass numbers：Modification is received
Rice copper particle 5kg, epoxy resin 94.45kg, antioxidant 0.25kg, coupling agent 0.3kg.
Embodiment 5
A kind of Nanometer Copper-epoxy resin composite material provided by the invention, is made of the component of following mass numbers：Modification is received
Rice copper particle 7kg, epoxy resin 92.4kg, antioxidant 0.30kg, coupling agent 0.3kg.
The preparation method of embodiment 1 to 5 is specially：
Step 1：Under inert gas shielding, after tetramethoxysilance and copper nanoparticle are disperseed in ethanol, 20~50 take the photograph
When family name's degree temperature reflux reaction 0.5~2 is small, room temperature 2~3h of mechanical agitation, makes it carry out surface modification to nanometer copper particle；
The tetramethoxysilance and the mass ratio of copper nanoparticle are：1ml:2g.It should be noted that tetramethoxysilance with
Copper nanoparticle is not limited to 1ml:2g, more than the numerical value, is still what can effectively be modified.
Ethanol is set to volatilize in fume hood the alcohol suspension of the Nanometer Copper of modification, rear 60~80 DEG C of vacuum drying oven
Drying, after block modified Nano copper is subjected to powder, obtain the modified Nano copper of dry refinement；
By the modified Nano copper and epoxy resin of the dry refinement of step 2), antioxidant, coupling agent, in low speed mixer transfer
Speed is uniformly mixed for 300~350r/min, then is granulated at 230~240 DEG C by Single screw extrusion.
Any one Nanometer Copper-epoxy resin composite material in embodiment 1 to 5 is detected, dielectric loss≤
0.08tgδ；The ε r of dielectric constant >=160；Resistance to oxidation temperature >=200 DEG C.
Table 1 below gives the performance comparison result of the present embodiment and existing conventional product.
Table 1：The performance comparison result of the present embodiment 1 and existing conventional product
Data quoted from《Resistor-Capacitor Unit Materials Handbook》, P.606.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention and from above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of modified Nano copper, it is characterised in that the modified Nano copper is the Nanometer Copper that surface is coated with silicon oxide.
2. modified Nano copper according to claim 1, it is characterised in that the surface cladding dioxy of the modified Nano copper
The specific method of SiClx is：Surface modification is carried out to the surface of Nanometer Copper by tetramethoxysilance.
3. modified Nano copper according to claim 1, it is characterised in that the surface coated silica of the Nanometer Copper
Thickness is 4~400nm.
4. a kind of Nanometer Copper-epoxy resin composite material, it is characterised in that be made of following components in parts by weight：As right will
Ask any 1~10 part of the modified Nano copper particle of 1-3,90~98 parts of epoxy resin.
5. Nanometer Copper-epoxy resin composite material according to claim 4, it is characterised in that further include：Antioxidant 0.2
~0.35 part, 0.2-0.4 parts of coupling agent.
6. Nanometer Copper-epoxy resin composite material according to claim 4, it is characterised in that by the group of following weight parts
Divide and be made：3~8 parts of modified Nano copper particle as described in claim 1-3 is any, 92~96 parts of epoxy resin, antioxidant
0.25~0.30 part, 0.3 part of coupling agent.
7. Nanometer Copper-epoxy resin composite material according to claim 5, it is characterised in that the antioxidant is selected from
Four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters, phosphite ester kind antioxidant are three [2,4- bis- tertiary fourths
Base phenyl] phosphite ester, N, N'- be double-(3- (3,5- di-tert-butyl-hydroxy phenyls) propiono) hexamethylene diamine；β-(bis- uncles of 3,5-
Butyl -4- hydroxy phenyls) one kind in propionic acid octadecanol ester (anti-1076).
8. Nanometer Copper-epoxy resin composite material according to claim 5, it is characterised in that the coupling agent is selected from
Silane coupling agent is specially γ-aminopropyl triethoxysilane, three tert-butyl peroxide silane of vinyl, diethylin for first
One kind in ethyl triethoxy silicane alkane.
9. a kind of preparation method of Nanometer Copper-epoxy resin composite material as described in claim 4-8 is any, its feature exist
In comprising the following steps successively：
1) under inert gas shielding, after tetramethoxysilance and copper nanoparticle are disperseed in ethanol, back flow reaction, room temperature machinery
2~3h is stirred, it is carried out surface modification to nanometer copper particle；
2) ethanol is made to volatilize in fume hood the alcohol suspension of the Nanometer Copper of modification, rear 60~80 DEG C of bakings of vacuum drying oven
It is dry, after block modified Nano copper is subjected to powder, obtain the modified Nano copper of dry refinement；
3) by 90~98 parts of 1~10 part of the modified Nano copper and epoxy resin of the dry refinement of step 2), antioxidant 0.2~0.35
Part, 0.2-0.4 parts of coupling agent, is uniformly mixed in low speed mixer, then is granulated at 230~240 DEG C by Single screw extrusion.
10. the preparation method of Nanometer Copper-epoxy resin composite material according to claim 9, it is characterised in that described
Low speed mixer rotating speed is 300~350r/min.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711192030.7A CN107936295A (en) | 2017-11-24 | 2017-11-24 | A kind of modified Nano copper and Nanometer Copper epoxy resin composite material and preparation method thereof |
| PCT/CN2018/116301 WO2019101049A1 (en) | 2017-11-24 | 2018-11-20 | Modified nano-copper, and nano-copper-epoxy resin composite material and manufacturing method therefor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711192030.7A CN107936295A (en) | 2017-11-24 | 2017-11-24 | A kind of modified Nano copper and Nanometer Copper epoxy resin composite material and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN107936295A true CN107936295A (en) | 2018-04-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201711192030.7A Pending CN107936295A (en) | 2017-11-24 | 2017-11-24 | A kind of modified Nano copper and Nanometer Copper epoxy resin composite material and preparation method thereof |
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| CN (1) | CN107936295A (en) |
| WO (1) | WO2019101049A1 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019101049A1 (en) * | 2017-11-24 | 2019-05-31 | 广东聚航新材料研究院有限公司 | Modified nano-copper, and nano-copper-epoxy resin composite material and manufacturing method therefor |
| CN111269536A (en) * | 2020-04-16 | 2020-06-12 | 扬州金霞塑胶有限公司 | Nano cellulose/copper composite material modified resin and preparation method thereof |
| CN115353715A (en) * | 2022-01-25 | 2022-11-18 | 深圳基本半导体有限公司 | High-thermal-conductivity composite material for packaging power module and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103194165A (en) * | 2013-04-26 | 2013-07-10 | 中国电子科技集团公司第三十八研究所 | Method for preparing high-heat-conductivity conductive adhesive containing graphene |
| CN103381486A (en) * | 2013-05-20 | 2013-11-06 | 河南大学 | Method for preparing surface modified Cu@SiO2 nano particles adopting shell structures |
| CN103724938A (en) * | 2013-12-06 | 2014-04-16 | 黑龙江大学 | Method for preparing nano-copper/epoxy resin composite material |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107936295A (en) * | 2017-11-24 | 2018-04-20 | 广东聚航新材料研究院有限公司 | A kind of modified Nano copper and Nanometer Copper epoxy resin composite material and preparation method thereof |
-
2017
- 2017-11-24 CN CN201711192030.7A patent/CN107936295A/en active Pending
-
2018
- 2018-11-20 WO PCT/CN2018/116301 patent/WO2019101049A1/en active Application Filing
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103194165A (en) * | 2013-04-26 | 2013-07-10 | 中国电子科技集团公司第三十八研究所 | Method for preparing high-heat-conductivity conductive adhesive containing graphene |
| CN103381486A (en) * | 2013-05-20 | 2013-11-06 | 河南大学 | Method for preparing surface modified Cu@SiO2 nano particles adopting shell structures |
| CN103724938A (en) * | 2013-12-06 | 2014-04-16 | 黑龙江大学 | Method for preparing nano-copper/epoxy resin composite material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019101049A1 (en) * | 2017-11-24 | 2019-05-31 | 广东聚航新材料研究院有限公司 | Modified nano-copper, and nano-copper-epoxy resin composite material and manufacturing method therefor |
| CN111269536A (en) * | 2020-04-16 | 2020-06-12 | 扬州金霞塑胶有限公司 | Nano cellulose/copper composite material modified resin and preparation method thereof |
| CN115353715A (en) * | 2022-01-25 | 2022-11-18 | 深圳基本半导体有限公司 | High-thermal-conductivity composite material for packaging power module and preparation method thereof |
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| Publication number | Publication date |
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| WO2019101049A1 (en) | 2019-05-31 |
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