CN107793759A - A kind of preparation method and applications of modified graphite powder dielectric composite material - Google Patents
A kind of preparation method and applications of modified graphite powder dielectric composite material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L81/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen or carbon only; Compositions of polysulfones; Compositions of derivatives of such polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
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- C—CHEMISTRY; METALLURGY
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/32—Component parts, details or accessories; Auxiliary operations
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- B29C2043/5808—Measuring, controlling or regulating pressure or compressing force
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
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Abstract
The invention discloses a kind of preparation method and applications of modified graphite powder dielectric composite material, this method is used graphite powder and Kynoar, coupling agent reaction modifying, then mixed with polyphenylene sulfide, silicon tetrachloride, hydro-thermal reaction is carried out in autoclave, reaction product is added into N again, in N dimethylformamides, diglycidyl ether type epoxy resin is added after supersound process, then pass to inert gas, carry out insulation reaction, it is drying precipitated after centrifugation, finally mixture Screw Extrusion is granulated, hot pressing, obtains modified graphite powder dielectric composite material.The modified graphite powder dielectric composite material being prepared, its dielectric constant is high, dielectric loss is low, and bending strength is high, has preferable application prospect in electronic device product.
Description
Technical field
The present invention relates to this technical field of electronic material, is related specifically to a kind of modified graphite powder dielectric composite material
Preparation method and applications.
Background technology
Dielectric material is also known as dielectric, is the electric insulating materials that can be used for control storage electric charge and electric energy, in modern electricity
There is important strategic position in son and power system.Dielectric material mainly includes capacitors dielectrics and micro-wave dielectric material
Expect two big systems.Wherein it is used as the dielectric material of condenser dielectric, it is desirable to which the resistivity of material is high, and dielectric constant is big, whole
Occupy very big proportion in dielectric material.Dielectric material can also be divided into organic and inorganic two major class, and species is various.With modern electricity
The fast development of scarabaeidae skill, increasing application propose to the dielectric properties of electronic material and the miniaturization of electronic component
Higher requirement, there is an urgent need to high-k, low-loss while with higher force performance and processability by people
Dielectric material, the importance that this allows for high dielectric constant material is increasingly notable.Composite dielectric material is due to preferable
Mechanical performance, processing characteristics and insulating properties and receive the concern of scientific research personnel.
Graphite silty is soft, black gray expandable.Under the conditions of starvation, its fusing point is the mineral of most heatproof more than 3000 DEG C
One of.The chemical property of graphite powder is more stable under normal temperature, not soluble in water, diluted acid, diluted alkaline and organic solvent；Under different high temperature with
Oxygen reacts, and generates carbon dioxide or carbon monoxide；Only have fluorine directly to be reacted with simple substance carbon in halogen；Under heating, graphite
Powder is easier to by acid oxidase；At high temperature, moreover it is possible to many metal reactions, generate metal carbides, gold can be smelted at high temperature
Category.Graphite powder has superior electric conductivity and lubricating release.Machining graphite into graphite powder, there is excellent lubrication, conduction
Performance, the purity of graphite powder is higher, and electric conductivity is better.
The content of the invention
In order to improve the performance of existing dielectric material, the present invention provides a kind of modified graphite powder dielectric composite material
Preparation method, this method are used graphite powder and Kynoar, coupling agent reaction modifying, then with polyphenylene sulfide, four chlorinations
Silicon is mixed, and hydro-thermal reaction is carried out in autoclave, then reaction product is added in DMF, after supersound process
Diglycidyl ether type epoxy resin is added, then passes to inert gas, carries out insulation reaction, it is drying precipitated after centrifugation, finally will
Mixture Screw Extrusion is granulated, hot pressing, obtains modified graphite powder dielectric composite material.The modified graphite powder dielectric being prepared is answered
Condensation material, its dielectric constant is high, dielectric loss is low, and bending strength is high, before having preferably application in electronic device product
Scape.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of preparation method of modified graphite powder dielectric composite material, comprises the following steps：
（1）By graphite powder, 15 parts are added in the distilled water of 80 times of its weight, ultrasonic disperse 15 minutes, add Kynoar
3 parts, 90 DEG C are warming up to, insulated and stirred 15-20 minutes, 2 mol/L hydrochloric acid, which is then added dropwise, makes pH to 4.5, adds coupling agent 2
Part, stirring obtains mixed solution in 30 minutes, is finally dried in an oven under the conditions of 110 DEG C, all evaporates, obtain to moisture
Modified graphite powder；
（2）Modified graphite powder is mixed with polyphenylene sulfide 6-8 parts, silicon tetrachloride 4-5 parts, it is equal to add 120 parts of deionized water stirrings
It is even, inject in autoclave and carry out hydro-thermal reaction, be then cooled to normal temperature, obtain primary reaction mixture；
（3）Primary reaction mixture is added in the DMF of 10-17 times of its weight, is ultrasonically treated 25 points
Clock, 6 parts of diglycidyl ether type epoxy resin is then added, then passes to inert gas, the insulation reaction in 120 DEG C of oil bath
120-150 minutes, it will be deposited at 60 DEG C and be dried in vacuo 18 hours after centrifuging while hot, and obtain secondary reaction mixture；
（4）Secondary reaction mixture is put into screw extruder, comminutor is sent into after melting extrusion and is granulated, is then incited somebody to action
To granular material be placed on tablet press machine, temperature be 250-280 DEG C, pressure be 10 Mpa process conditions under, hot pressing 30
Minute, obtain dielectric composite material.
Preferably, the step（1）In coupling agent be silane coupler.
Preferably, the step（2）In the temperature of hydro-thermal reaction be 800-850 DEG C, pressure 2-5MPa, the reaction time is
50 minutes.
Preferably, the step（4）In extruder temperature be 320 DEG C, screw speed be 500 revs/min.
Further, the invention also discloses described modified graphite powder dielectric composite material in electronic device product
Using.
Compared with prior art, its advantage is the present invention：
（1）The preparation method of the modified graphite powder dielectric composite material of the present invention is used graphite powder and Kynoar, coupling
Agent reaction modifying, then mixed with polyphenylene sulfide, silicon tetrachloride, carry out hydro-thermal reaction in autoclave, then by reaction product
Add in DMF, diglycidyl ether type epoxy resin is added after supersound process, inert gas is then passed to, enters
Row insulation reaction, it is drying precipitated after centrifugation, finally mixture Screw Extrusion is granulated, hot pressing, obtains modified graphite powder dielectric and answer
Condensation material.The modified graphite powder dielectric composite material being prepared, its dielectric constant is high, dielectric loss is low, and bending strength is high,
There is preferable application prospect in electronic device product.
（2）The modified graphite powder dielectric composite material raw material of the present invention is easy to get, technique is simple, is transported suitable for heavy industrialization
With practical.
Embodiment
The technical scheme of invention is described in detail with reference to specific embodiment.
Embodiment 1
（1）By graphite powder, 15 parts are added in the distilled water of 80 times of its weight, ultrasonic disperse 15 minutes, add Kynoar
3 parts, 90 DEG C are warming up to, insulated and stirred 15 minutes, 2 mol/L hydrochloric acid, which is then added dropwise, makes pH to 4.5, adds silane coupler
2 parts, stirring obtains mixed solution in 30 minutes, finally dries under the conditions of 110 DEG C, is all evaporated to moisture in an oven,
Obtain modified graphite powder；
（2）Modified graphite powder is mixed with 6 parts of polyphenylene sulfide, 4 parts of silicon tetrachloride, 120 parts of deionized waters is added and stirs, note
Entering and hydro-thermal reaction is carried out in autoclave, the temperature of hydro-thermal reaction is 800 DEG C, the MPa of pressure 2, and the reaction time is 50 minutes,
Normal temperature then is cooled to, obtains primary reaction mixture；
（3）Primary reaction mixture is added in the DMF of 10 times of its weight, be ultrasonically treated 25 minutes, with
6 parts of diglycidyl ether type epoxy resin is added afterwards, then passes to inert gas, insulation reaction 120 is divided in 120 DEG C of oil bath
Clock, it will be deposited at 60 DEG C and be dried in vacuo 18 hours after centrifuging while hot, and obtain secondary reaction mixture；
（4）Secondary reaction mixture is put into screw extruder, extruder temperature is 320 DEG C, and screw speed is 500 revs/min
Clock, comminutor granulation is sent into after melting extrusion, then obtained granular material is placed on tablet press machine, be 250 in temperature
DEG C, pressure is under 10 Mpa process conditions, hot pressing 30 minutes, obtains dielectric composite material.
The performance test results of obtained modified graphite powder dielectric composite material are as shown in table 1.
Embodiment 2
（1）By graphite powder, 15 parts are added in the distilled water of 80 times of its weight, ultrasonic disperse 15 minutes, add Kynoar
3 parts, 90 DEG C are warming up to, insulated and stirred 17 minutes, 2 mol/L hydrochloric acid, which is then added dropwise, makes pH to 4.5, adds silane coupler
2 parts, stirring obtains mixed solution in 30 minutes, finally dries under the conditions of 110 DEG C, is all evaporated to moisture in an oven,
Obtain modified graphite powder；
（2）Modified graphite powder is mixed with 7 parts of polyphenylene sulfide, 5 parts of silicon tetrachloride, 120 parts of deionized waters is added and stirs, note
Enter and hydro-thermal reaction is carried out in autoclave, the temperature of hydro-thermal reaction is 825 DEG C, the MPa of pressure 3.5, and the reaction time is 50 points
Clock, normal temperature is then cooled to, obtains primary reaction mixture；
（3）Primary reaction mixture is added in the DMF of 14 times of its weight, be ultrasonically treated 25 minutes, with
6 parts of diglycidyl ether type epoxy resin is added afterwards, then passes to inert gas, insulation reaction 135 is divided in 120 DEG C of oil bath
Clock, it will be deposited at 60 DEG C and be dried in vacuo 18 hours after centrifuging while hot, and obtain secondary reaction mixture；
（4）Secondary reaction mixture is put into screw extruder, extruder temperature is 320 DEG C, and screw speed is 500 revs/min
Clock, comminutor granulation is sent into after melting extrusion, then obtained granular material is placed on tablet press machine, be 265 in temperature
DEG C, pressure is under 10 Mpa process conditions, hot pressing 30 minutes, obtains dielectric composite material.
The performance test results of obtained modified graphite powder dielectric composite material are as shown in table 1.
Embodiment 3
（1）By graphite powder, 15 parts are added in the distilled water of 80 times of its weight, ultrasonic disperse 15 minutes, add Kynoar
3 parts, 90 DEG C are warming up to, insulated and stirred 20 minutes, 2 mol/L hydrochloric acid, which is then added dropwise, makes pH to 4.5, adds silane coupler
2 parts, stirring obtains mixed solution in 30 minutes, finally dries under the conditions of 110 DEG C, is all evaporated to moisture in an oven,
Obtain modified graphite powder；
（2）Modified graphite powder is mixed with 8 parts of polyphenylene sulfide, 5 parts of silicon tetrachloride, 120 parts of deionized waters is added and stirs, note
Entering and hydro-thermal reaction is carried out in autoclave, the temperature of hydro-thermal reaction is 850 DEG C, the MPa of pressure 5, and the reaction time is 50 minutes,
Normal temperature then is cooled to, obtains primary reaction mixture；
（3）Primary reaction mixture is added in the DMF of 17 times of its weight, be ultrasonically treated 25 minutes, with
6 parts of diglycidyl ether type epoxy resin is added afterwards, then passes to inert gas, insulation reaction 150 is divided in 120 DEG C of oil bath
Clock, it will be deposited at 60 DEG C and be dried in vacuo 18 hours after centrifuging while hot, and obtain secondary reaction mixture；
（4）Secondary reaction mixture is put into screw extruder, extruder temperature is 320 DEG C, and screw speed is 500 revs/min
Clock, comminutor granulation is sent into after melting extrusion, then obtained granular material is placed on tablet press machine, be 280 in temperature
DEG C, pressure is under 10 Mpa process conditions, hot pressing 30 minutes, obtains dielectric composite material.
The performance test results of obtained modified graphite powder dielectric composite material are as shown in table 1.
Comparative example 1
（1）By graphite powder, 15 parts mix with 8 parts of polyphenylene sulfide, 5 parts of silicon tetrachloride, add 120 parts of deionized waters and stir, note
Entering and hydro-thermal reaction is carried out in autoclave, the temperature of hydro-thermal reaction is 850 DEG C, the MPa of pressure 5, and the reaction time is 50 minutes,
Normal temperature then is cooled to, obtains primary reaction mixture；
（2）Primary reaction mixture is added in the DMF of 17 times of its weight, be ultrasonically treated 25 minutes, with
6 parts of diglycidyl ether type epoxy resin is added afterwards, then passes to inert gas, insulation reaction 150 is divided in 120 DEG C of oil bath
Clock, it will be deposited at 60 DEG C and be dried in vacuo 18 hours after centrifuging while hot, and obtain secondary reaction mixture；
（3）Secondary reaction mixture is put into screw extruder, extruder temperature is 320 DEG C, and screw speed is 500 revs/min
Clock, comminutor granulation is sent into after melting extrusion, then obtained granular material is placed on tablet press machine, be 280 in temperature
DEG C, pressure is under 10 Mpa process conditions, hot pressing 30 minutes, obtains dielectric composite material.
The performance test results of obtained graphite powder dielectric composite material are as shown in table 1.
Comparative example 2
（1）By graphite powder, 15 parts are added in the distilled water of 80 times of its weight, ultrasonic disperse 15 minutes, add Kynoar
3 parts, 90 DEG C are warming up to, insulated and stirred 20 minutes, 2 mol/L hydrochloric acid, which is then added dropwise, makes pH to 4.5, adds silane coupler
2 parts, stirring obtains mixed solution in 30 minutes, finally dries under the conditions of 110 DEG C, is all evaporated to moisture in an oven,
Obtain modified graphite powder；
（2）Modified graphite powder is mixed for 8 parts with polyphenylene sulfide, 120 parts of deionized waters is added and stirs, inject autoclave
Middle carry out hydro-thermal reaction, the temperature of hydro-thermal reaction is 850 DEG C, the MPa of pressure 5, and the reaction time is 50 minutes, is then cooled to often
Temperature, obtain primary reaction mixture；
（3）Primary reaction mixture is added in the DMF of 17 times of its weight, be ultrasonically treated 25 minutes, with
6 parts of diglycidyl ether type epoxy resin is added afterwards, then passes to inert gas, insulation reaction 150 is divided in 120 DEG C of oil bath
Clock, it will be deposited at 60 DEG C and be dried in vacuo 18 hours after centrifuging while hot, and obtain secondary reaction mixture；
（4）Secondary reaction mixture is put into screw extruder, extruder temperature is 320 DEG C, and screw speed is 500 revs/min
Clock, comminutor granulation is sent into after melting extrusion, then obtained granular material is placed on tablet press machine, be 280 in temperature
DEG C, pressure is under 10 Mpa process conditions, hot pressing 30 minutes, obtains dielectric composite material.
The performance test results of obtained modified graphite powder dielectric composite material are as shown in table 1.
Comparative example 3
（1）By graphite powder, 15 parts are added in the distilled water of 80 times of its weight, ultrasonic disperse 15 minutes, add Kynoar
3 parts, 90 DEG C are warming up to, insulated and stirred 20 minutes, 2 mol/L hydrochloric acid, which is then added dropwise, makes pH to 4.5, adds silane coupler
2 parts, stirring obtains mixed solution in 30 minutes, finally dries under the conditions of 110 DEG C, is all evaporated to moisture in an oven,
Obtain modified graphite powder；
（2）Modified graphite powder is mixed with 8 parts of polyphenylene sulfide, 5 parts of silicon tetrachloride, 120 parts of deionized waters is added and stirs, note
Entering and hydro-thermal reaction is carried out in autoclave, the temperature of hydro-thermal reaction is 850 DEG C, the MPa of pressure 5, and the reaction time is 50 minutes,
Normal temperature then is cooled to, obtains primary reaction mixture；
（3）Primary reaction mixture is added in the DMF of 17 times of its weight, supersound process 25 minutes, so
After be passed through inert gas, insulation reaction 150 minutes in 120 DEG C of oil bath, will be deposited in vacuum at 60 DEG C after centrifuging while hot and do
Dry 18 hours, obtain secondary reaction mixture；
（4）Secondary reaction mixture is put into screw extruder, extruder temperature is 320 DEG C, and screw speed is 500 revs/min
Clock, comminutor granulation is sent into after melting extrusion, then obtained granular material is placed on tablet press machine, be 280 in temperature
DEG C, pressure is under 10 Mpa process conditions, hot pressing 30 minutes, obtains dielectric composite material.
The performance test results of obtained modified graphite powder dielectric composite material are as shown in table 1
Embodiment 1-3 and comparative example 1-3 obtained dielectric composite material are subjected to dielectric constant, dielectric loss, bending respectively
This several performance tests of intensity.
Table 1
| Dielectric constant | Dielectric loss（%） | Bending strength（MPa） | |
| Embodiment 1 | 68 | 0.04 | 125 |
| Embodiment 2 | 67 | 0.03 | 122 |
| Embodiment 3 | 65 | 0.03 | 131 |
| Comparative example 1 | 62 | 0.05 | 108 |
| Comparative example 2 | 60 | 0.07 | 113 |
| Comparative example 3 | 59 | 0.06 | 116 |
The preparation method of the modified graphite powder dielectric composite material of the present invention uses graphite powder and Kynoar, coupling agent is anti-
It should be modified, then be mixed with polyphenylene sulfide, silicon tetrachloride, hydro-thermal reaction be carried out in autoclave, then reaction product is added
In DMF, diglycidyl ether type epoxy resin is added after supersound process, inert gas is then passed to, is protected
Temperature reaction, it is drying precipitated after centrifugation, finally mixture Screw Extrusion is granulated, hot pressing, obtains modified graphite powder dielectric composite wood
Material.The modified graphite powder dielectric composite material being prepared, its dielectric constant is high, dielectric loss is low, and bending strength is high, has
Preferable application prospect.Meanwhile modified graphite powder dielectric composite material raw material of the invention is easy to get, technique is simple, suitable for big rule
Mould industrialization is used, practical.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair
The equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks
Domain, it is included within the scope of the present invention.
Claims (5)
1. a kind of preparation method of modified graphite powder dielectric composite material, it is characterised in that comprise the following steps：
（1）By graphite powder, 15 parts are added in the distilled water of 80 times of its weight, ultrasonic disperse 15 minutes, add Kynoar
3 parts, 90 DEG C are warming up to, insulated and stirred 15-20 minutes, 2 mol/L hydrochloric acid, which is then added dropwise, makes pH to 4.5, adds coupling agent 2
Part, stirring obtains mixed solution in 30 minutes, is finally dried in an oven under the conditions of 110 DEG C, all evaporates, obtain to moisture
Modified graphite powder；
（2）Modified graphite powder is mixed with polyphenylene sulfide 6-8 parts, silicon tetrachloride 4-5 parts, it is equal to add 120 parts of deionized water stirrings
It is even, inject in autoclave and carry out hydro-thermal reaction, be then cooled to normal temperature, obtain primary reaction mixture；
（3）Primary reaction mixture is added in the DMF of 10-17 times of its weight, is ultrasonically treated 25 points
Clock, 6 parts of diglycidyl ether type epoxy resin is then added, then passes to inert gas, the insulation reaction in 120 DEG C of oil bath
120-150 minutes, it will be deposited at 60 DEG C and be dried in vacuo 18 hours after centrifuging while hot, and obtain secondary reaction mixture；
（4）Secondary reaction mixture is put into screw extruder, comminutor is sent into after melting extrusion and is granulated, is then incited somebody to action
To granular material be placed on tablet press machine, temperature be 250-280 DEG C, pressure be 10 Mpa process conditions under, hot pressing 30
Minute, obtain dielectric composite material.
2. the preparation method of modified graphite powder dielectric composite material according to claim 1, it is characterised in that the step
（1）In coupling agent be silane coupler.
3. the preparation method of modified graphite powder dielectric composite material according to claim 1, it is characterised in that the step
（2）In hydro-thermal reaction temperature be 800-850 DEG C, pressure 2-5MPa, the reaction time be 50 minutes.
4. the preparation method of modified graphite powder dielectric composite material according to claim 1, it is characterised in that the step
（4）In extruder temperature be 320 DEG C, screw speed be 500 revs/min.
5. the answering in electronic device product of the modified graphite powder dielectric composite material according to claim any one of 1-4
With.
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Citations (4)
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| KR100777097B1 (en) * | 2006-12-05 | 2007-11-28 | 제일모직주식회사 | Composite of dielectric ceramic-polyphenylene sulfide |
| CN105949725A (en) * | 2016-07-18 | 2016-09-21 | 上海第二工业大学 | Epoxy-resin-based high-dielectric composite material and preparation method thereof |
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2017
- 2017-11-16 CN CN201711137562.0A patent/CN107793759A/en active Pending
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|---|---|---|---|---|
| KR100777097B1 (en) * | 2006-12-05 | 2007-11-28 | 제일모직주식회사 | Composite of dielectric ceramic-polyphenylene sulfide |
| CN106017748A (en) * | 2016-05-19 | 2016-10-12 | 北京印刷学院 | Capacitive flexible pressure sensor based on composite material dielectric layer and preparation method of capacitive flexible pressure sensor |
| CN105949725A (en) * | 2016-07-18 | 2016-09-21 | 上海第二工业大学 | Epoxy-resin-based high-dielectric composite material and preparation method thereof |
| CN106954380A (en) * | 2017-02-23 | 2017-07-14 | 云南联展科技有限公司 | A kind of many loss mechanisms inhale ripple shielding material and preparation method thereof |
Non-Patent Citations (2)
| Title |
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| 刘漫红等: "《纳米材料及其制备技术》", 31 August 2014, 冶金工业出版社 * |
| 谢宇: "《变化莫测的分子王国--化学工业》", 31 January 2010, 百花洲文艺出版社 * |
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