CN108219455A - A kind of polymer matrix composite - Google Patents
A kind of polymer matrix composite Download PDFInfo
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- CN108219455A CN108219455A CN201611161834.6A CN201611161834A CN108219455A CN 108219455 A CN108219455 A CN 108219455A CN 201611161834 A CN201611161834 A CN 201611161834A CN 108219455 A CN108219455 A CN 108219455A
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- Prior art keywords
- graphene oxide
- polymer matrix
- composite material
- matrix composite
- dielectric constant
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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
- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
- C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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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
- C08K3/04—Carbon
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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
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
Abstract
The present invention relates to a kind of dielectric material, more particularly to a kind of adjustable polymer matrix composite of dielectric constant.Doped with graphene oxide in the composite material.Graphene oxide is adulterated in the technical program in thermosetting resin, adjust the dielectric constant of composite material, since the dielectric constant of composite material is more sensitive to the doping of graphene oxide, so micro adjustment for the doping for passing through graphene oxide, the wider range adjustment of composite material dielectric constant can be realized, objectively compared with prior art, the density of composite material is reduced.Surface modification can be carried out to graphene oxide simultaneously, the binding force of graphene oxide and resin be improved, so as to improve the mechanical property of composite material.
Description
Technical field
The present invention relates to a kind of dielectric material, more particularly to a kind of adjustable polymer matrix composite of dielectric constant.
Background technology
High dielectric material has the function of good storage electric energy and uniform electric field, has in electronic motor cable industry
Very important application.With information, electronics, electric power, the fast development of nanometer technology and the upgrading of weaponry, to be situated between
Electric constant is adjustable, low-loss, and the polymer based nanocomposites of low-density become the hot spot of industry concern.
It is presently used in dielectric is adjustable, functional stuffings of low-loss polymer based composites mainly include metallic conductor,
Ferroelectric ceramics, organic semiconductor etc., metallic conductor is common Ag, Al, Ni etc., although these fillers are added to certain score,
The dielectric constant of polymer matrix composite can be greatly improved, but these conducting particles and polymer binding force are poor, very
Hardly possible forms homodisperse phase, eventually leads to the dielectric properties and mechanical property of the composite material.Ferroelectric ceramics common used material such as titanium
Sour barium (BT), barium strontium titanate (BST) with polymer is compound can prepare dielectric often adjustable composite material, but to reach very high
Dielectric constant, filling is general all very high, and dispersibility reduces, and the dielectric loss for leading to composite material is very high, poor processability, because
The shortcomings that this such material is limited there is dielectric constant, and adhesion strength is low and processing performance is low.In contrast, graphene density
It is small, electric conductivity number and at low cost and as seepage flow type dielectric composite material preferred material,.And with linear and platy particle
Its percolation threshold is relatively low for the composite material of filler for graphene, this is all very intentional for the loss of weight and reduction production cost of material
Justice.But graphene large specific surface area, surface can be high, thus be very easy to reunite in solvent and matrix, it is not easily dispersed in poly-
It closes in object, is difficult to control dielectric constant.
Invention content
The purpose of the present invention：A kind of adjustable dielectric constant, low-density, low-loss and gathering with excellent mechanical performance are provided
Close object based composites.
Technical scheme of the present invention：A kind of polymer matrix composite, it is characterized in that：In the composite material doped with
Graphene oxide.
Preferably, graphene oxide doped amount is bigger, and the dielectric constant of composite material is bigger.
Preferably, the degree of oxidation of graphene oxide is bigger, and the dielectric constant of composite material is bigger.
Preferably, the graphene oxide is the graphene oxide after silane treatment.
Preferably, the polymeric matrix is thermosetting resin.
Preferably, the carbon-to-oxygen ratio of the graphene oxide is 1-10, piece diameter 1nm-100nm.
A kind of preparation method of polymer matrix composite, it is characterized in that：Graphene oxide dispersion is ultrasonic in a solvent
The suspension of graphene oxide is made in 1-3h, is subsequently added into warmed-up 65-100 DEG C and in the diluted resin of solvent,
Ultrasound 1-2h at 25-100 DEG C；Then mixture heated, depressurized, stirred and make evaporation of the solvent；Then merging vacuum drying environment
In, de-bubbled 2h, further removes residual solvents at 80 DEG C；The curing agent of preheating is added in mixture while hot, is stirred
Uniformly；Mixture added with curing agent is cast in mold, is put into vacuum environment, de-bubbled cures, is cooled to room
Temperature demoulds to obtain polymer based nanocomposites.
Beneficial effects of the present invention：Graphene oxide is adulterated in the technical program in thermosetting resin, adjusts composite wood
The dielectric constant of material, since the dielectric constant of composite material is more sensitive to the doping of graphene oxide, so passing through oxidation
The micro adjustment of the doping of graphene, you can realize composite material dielectric constant wider range adjustment, objectively with it is existing
Technology is compared, and reduces the density of composite material.
Surface modification can be carried out to graphene oxide simultaneously, the binding force of graphene oxide and resin be improved, so as to carry
The high mechanical property of composite material.
Specific embodiment
Embodiment 1
(1) GO is dried into 3h, then dry GO is added in three-necked flask in 110 DEG C of baking ovens, the carbon-to-oxygen ratio of GO is
1.5.Then a certain amount of absolute ethyl alcohol is added in, is stirred evenly, coupling agent KH550 is added in and is stirred after 40~60 DEG C of water-bath high speeds
1.5h is mixed, is filtered, absolute ethyl alcohol washing is dried in vacuo 3h at 120 DEG C, and GO is modified up to the surface through coupling agent treatment.
(2) 0.3g is modified GO dispersions ultrasound 1h in acetone, the acetone suspension of GO is made, is subsequently added into warmed-up
65 DEG C and in the diluted 27g cyanates of acetone and 3g epoxy resin, the ultrasound 1h at 80 DEG C.Then mixture is placed in three mouthfuls
Heating decompression stirring evaporation solvent in flask.Then it is placed in vacuum drying chamber, the de-bubbled 2h at 70 DEG C is further removed residual
Deposit solvent.0.008g organotin catalysts are added in mixture, are stirred evenly.
(3) punching block for being coated with releasing agent is preheated, is then slowly cast to mixture in mold, pay attention to the process of casting
It is middle slowly to be poured into along wall, it avoids generating bubble in casting cycle, be subsequently placed into vacuum drying chamber, utilize residual temperature de-bubbled
0.5h first cures 2h at 150 DEG C, then cures 2h at 180 DEG C.
(4) it is cooled to room temperature, demoulding.
The dielectric constant and dielectric loss of the adjustable resin-base nano composite material of dielectric obtained by the implementation case are by waveguide
Short-circuit method measures, and bending strength is GB/T 1449 with modulus test standard, and basic performance see the table below.
| Test event | Performance |
| Density | 1.23 |
| Dielectric constant (10GHz) | 7.54 |
| Dielectric loss (10GHz) | 0.2 |
| Bending strength, MPa | 185 |
| Bending modulus, GPa | 3.3 |
Embodiment 2
(1) GO is dried into 3h, then dry GO is added in three-necked flask in 110 DEG C of baking ovens, the carbon-to-oxygen ratio of GO is
1.5.Then a certain amount of absolute ethyl alcohol is added in, is stirred evenly, coupling agent KH550 is added in and is stirred after 40~60 DEG C of water-bath high speeds
1.5h is mixed, is filtered, absolute ethyl alcohol washing is dried in vacuo 3h at 120 DEG C, and GO is modified up to the surface through coupling agent treatment.
(2) 1g is modified GO dispersions ultrasound 1h in acetone, the acetone suspension of GO is made, is subsequently added into warmed-up 65
DEG C and in the diluted 27g cyanates of acetone and 3g epoxy resin, the ultrasound 1h at 80 DEG C.Then mixture is placed in three mouthfuls of burnings
Heating decompression stirring evaporation solvent in bottle.Then it is placed in vacuum drying chamber, the de-bubbled 2h at 80 DEG C, further removal remaining
Solvent.0.008g organotin catalysts are added in mixture, are stirred evenly.
(3) punching block for being coated with releasing agent is preheated, is then slowly cast to mixture in mold, pay attention to the process of casting
It is middle slowly to be poured into along wall, it avoids generating bubble in casting cycle, be subsequently placed into vacuum drying chamber, utilize residual temperature de-bubbled
0.5h first cures 2h at 150 DEG C, then cures 2h at 180 DEG C.
(4) it is cooled to room temperature, demoulding.
The dielectric constant and dielectric loss of the adjustable resin-base nano composite material of dielectric obtained by the implementation case are by waveguide
Short-circuit method measures, and bending strength is GB/T 1449 with modulus test standard, and basic performance see the table below.
| Test event | Performance |
| Density | 1.22 |
| Dielectric constant (10GHz) | 78.4 |
| Dielectric loss (10GHz) | 0.3 |
| Bending strength, MPa | 188 |
| Bending modulus, GPa | 3.30 |
Embodiment 3
(1) GO is dried into 3h, then dry GO is added in three-necked flask in 110 DEG C of baking ovens, the carbon-to-oxygen ratio of GO is
1.5.Then a certain amount of absolute ethyl alcohol is added in, is stirred evenly, coupling agent is added in and is stirred after 40~60 DEG C of water-bath high speeds
1.5h is filtered, absolute ethyl alcohol washing, and 3h is dried in vacuo at 120 DEG C, and GO is modified up to the surface through coupling agent treatment.
(2) 1.5g is modified GO dispersions ultrasound 1h in acetone, the acetone suspension of GO is made, is subsequently added into warmed-up
65 DEG C and in the diluted 27g cyanates of acetone and 3g epoxy resin, the ultrasound 2h at 75 DEG C.Then mixture is placed in three mouthfuls
Heating decompression stirring evaporation solvent in flask.Then it is placed in vacuum drying chamber, the de-bubbled 2h at 70 DEG C is further removed residual
Deposit solvent.0.008g organotin catalysts are added in mixture, are stirred evenly.
(3) punching block for being coated with releasing agent is preheated, is then slowly cast to mixture in mold, pay attention to the process of casting
It is middle slowly to be poured into along wall, it avoids generating bubble in casting cycle, be subsequently placed into vacuum drying chamber, utilize residual temperature de-bubbled
0.5h first cures 2h at 150 DEG C, then cures 2h at 180 DEG C.
(4) it is cooled to room temperature, demoulding.
The dielectric constant and dielectric loss of the adjustable resin-base nano composite material of dielectric obtained by the implementation case are by waveguide
Short-circuit method measures, and bending strength is GB/T 1449 with modulus test standard, and basic performance see the table below.
| Test event | Performance |
| Density | 1.2 |
| Dielectric constant (10GHz) | 289 |
| Dielectric loss (10GHz) | 0.5 |
| Bending strength, MPa | 186 |
| Bending modulus, GPa | 3.30 |
Embodiment 4
(1) GO is dried into 3h, then dry GO is added in three-necked flask in 110 DEG C of baking ovens, the carbon-to-oxygen ratio of GO is
1.5.Then a certain amount of absolute ethyl alcohol is added in, is stirred evenly, coupling agent is added in and is stirred after 40~60 DEG C of water-bath high speeds
1.5h is filtered, absolute ethyl alcohol washing, and 3h is dried in vacuo at 120 DEG C, and GO is modified up to the surface through coupling agent treatment.
(2) 1g is modified GO dispersions ultrasound 1h in acetone, the acetone suspension of GO is made, is subsequently added into warmed-up 65
DEG C and in the diluted 100g epoxy resin of acetone, the ultrasound 2h at 75 DEG C.Then mixture is placed in three-necked flask and heated
Decompression stirring evaporation solvent.Then it is placed in vacuum drying chamber, de-bubbled 2h, further removes residual solvents at 70 DEG C.It will
10g dicyandiamide catalysts are added in mixture, are stirred evenly.
(3) punching block for being coated with releasing agent is preheated, is then slowly cast to mixture in mold, pay attention to the process of casting
It is middle slowly to be poured into along wall, it avoids generating bubble in casting cycle, be subsequently placed into vacuum drying chamber, utilize residual temperature de-bubbled
0.5h first cures 3h at 130 DEG C.
(4) it is cooled to room temperature, demoulding.
The dielectric constant and dielectric loss of the adjustable resin-base nano composite material of dielectric obtained by the implementation case are by waveguide
Short-circuit method measures, and bending strength is GB/T 1449 with modulus test standard, and basic performance see the table below.
| Test event | Performance |
| Density | 1.2 |
| Dielectric constant (10GHz) | 93 |
| Dielectric loss (10GHz) | 0.3 |
| Bending strength, MPa | 115 |
| Bending modulus, GPa | 3.50 |
Embodiment 5
(1) GO is dried into 3h, then dry GO is added in three-necked flask in 110 DEG C of baking ovens, the carbon-to-oxygen ratio of GO is 3.
Then a certain amount of absolute ethyl alcohol is added in, is stirred evenly, coupling agent KH550 is added in and is stirred after 40~60 DEG C of water-bath high speeds
1.5h is filtered, absolute ethyl alcohol washing, and 3h is dried in vacuo at 120 DEG C, and GO is modified up to the surface through coupling agent treatment.
(2) 0.3g is modified GO dispersions ultrasound 1h in acetone, the acetone suspension of GO is made, is subsequently added into warmed-up
65 DEG C and in the diluted 27g cyanates of acetone and 3g epoxy resin, the ultrasound 1h at 80 DEG C.Then mixture is placed in three mouthfuls
Heating decompression stirring evaporation solvent in flask.Then it is placed in vacuum drying chamber, the de-bubbled 2h at 70 DEG C is further removed residual
Deposit solvent.0.008g organotin catalysts are added in mixture, are stirred evenly.
(3) punching block for being coated with releasing agent is preheated, is then slowly cast to mixture in mold, pay attention to the process of casting
It is middle slowly to be poured into along wall, it avoids generating bubble in casting cycle, be subsequently placed into vacuum drying chamber, utilize residual temperature de-bubbled
0.5h first cures 2h at 150 DEG C, then cures 2h at 180 DEG C.
(4) it is cooled to room temperature, demoulding.
The dielectric constant and dielectric loss of the adjustable resin-base nano composite material of dielectric obtained by the implementation case are by waveguide
Short-circuit method measures, and bending strength is GB/T 1449 with modulus test standard, and basic performance see the table below.
| Test event | Performance |
| Density | 1.23 |
| Dielectric constant (10GHz) | 31 |
| Dielectric loss (10GHz) | 0.2 |
| Bending strength, MPa | 180 |
| Bending modulus, GPa | 3.3 |
Claims (7)
1. a kind of polymer matrix composite, it is characterized in that：Doped with graphene oxide in the composite material.
2. a kind of polymer matrix composite according to claim 1, it is characterized in that：Graphene oxide doped amount is bigger,
The dielectric constant of composite material is bigger.
3. a kind of polymer matrix composite according to claim 1, it is characterized in that：The degree of oxidation of graphene oxide is got over
Greatly, the dielectric constant of composite material is bigger.
4. a kind of polymer matrix composite according to claim 1, it is characterized in that：The graphene oxide is passes through
Graphene oxide after silane treatment.
5. a kind of polymer matrix composite according to claim 1, it is characterized in that：The polymeric matrix is thermosetting
Property resin.
6. a kind of polymer matrix composite according to claim 1, it is characterized in that：The carbon oxygen of the graphene oxide
Than for 1-10, piece diameter 1nm-100nm.
7. a kind of preparation method of polymer matrix composite according to claim 1, it is characterized in that：By graphene oxide
Ultrasound 1-3h, the suspension of obtained graphene oxide are subsequently added into warmed-up 65-100 DEG C and use solvent in a solvent for dispersion
In diluted resin, the ultrasound 1-2h at 25-100 DEG C；Then mixture heated, depressurized, stirred and make evaporation of the solvent；Then it puts
Enter to be dried in vacuo in environment, de-bubbled 2h, further removes residual solvents at 80 DEG C；The curing agent of preheating is added to while hot
In mixture, stir evenly；Mixture added with curing agent is cast in mold, is put into vacuum environment, de-bubbled is consolidated
Change, be cooled to room temperature, demould to obtain polymer based nanocomposites.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611161834.6A CN108219455A (en) | 2016-12-15 | 2016-12-15 | A kind of polymer matrix composite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611161834.6A CN108219455A (en) | 2016-12-15 | 2016-12-15 | A kind of polymer matrix composite |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286189A (en) * | 2011-06-24 | 2011-12-21 | 中国科学院理化技术研究所 | Method for preparing graphene oxide/epoxide resin nano composite material |
| CN102775786A (en) * | 2012-08-09 | 2012-11-14 | 西北工业大学 | Graphene oxide/cyanate ester composite material and preparation method thereof |
| CN103627139A (en) * | 2013-09-25 | 2014-03-12 | 杭州师范大学 | Preparation method of functionalized graphene oxide/epoxy resin nanocomposite |
-
2016
- 2016-12-15 CN CN201611161834.6A patent/CN108219455A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286189A (en) * | 2011-06-24 | 2011-12-21 | 中国科学院理化技术研究所 | Method for preparing graphene oxide/epoxide resin nano composite material |
| CN102775786A (en) * | 2012-08-09 | 2012-11-14 | 西北工业大学 | Graphene oxide/cyanate ester composite material and preparation method thereof |
| CN103627139A (en) * | 2013-09-25 | 2014-03-12 | 杭州师范大学 | Preparation method of functionalized graphene oxide/epoxy resin nanocomposite |
Non-Patent Citations (3)
| Title |
|---|
| DING, JUAN; HUANG, YING; HAN, TIAOZHENG: "Functional graphene nanoflakes/cyanate/epoxy nanocomposites: mechanical, dielectric and thermal properties", 《IRANIAN POLYMER JOURNAL》 * |
| REN, FANG; ZHU, GUANGMING; REN, PENGGANG; 等.: "In situ polymerization of graphene oxide and cyanate ester-epoxy with enhanced mechanical and thermal properties", 《APPLIED SURFACE SCIENCE》 * |
| 李金焕等: "石墨烯／氰酸酯一环氧树脂复合材料的制备和性能", 《复合材料学报》 * |
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Application publication date: 20180629 |
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