CN106189081B - A kind of skin covering of the surface and preparation method thereof with conductive characteristic - Google Patents
A kind of skin covering of the surface and preparation method thereof with conductive characteristic Download PDFInfo
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- CN106189081B CN106189081B CN201610537431.0A CN201610537431A CN106189081B CN 106189081 B CN106189081 B CN 106189081B CN 201610537431 A CN201610537431 A CN 201610537431A CN 106189081 B CN106189081 B CN 106189081B
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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
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2063/00—Use of EP, i.e. epoxy resins or derivatives thereof, as moulding material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2507/00—Use of elements other than metals as filler
- B29K2507/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
- C08J2471/10—Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
A kind of skin covering of the surface and preparation method thereof with conductive characteristic, it is related to the surface glued membrane of hot setting.The invention solves traditional conductivity meter facial masks can be corroded using metal for a long time, and resistance value changes, and stability is bad, and then influences the safety problem that aircraft flies in thundery sky.The skin covering of the surface with conductive characteristic of the present invention is made of epoxy resin, poly (arylene ether nitrile) ketone, Core-shell rubber particles, flow control additive, curing agent and conductive graphene.Preparation method:A small amount of graphene is adulterated in the epoxy, special toughening is carried out to resin, and being prepared by machinery calendering has conductive characteristic composite material surface film.Then press mold is cut out item, is put into multiple material plate groove, is compacted, cure under pressure.It finally measures and calculates resistivity when cured plate batten spacing is 50mm.The present invention has the characteristics that the skin covering of the surface film of conductive characteristic has excellent in mechanical performance, resistance value stability good, can be used for the manufacture of aircraft water conservancy diversion composite material structural member.
Description
Technical field
The present invention relates to conductive characteristic composite material surface film field, and in particular to epoxy resin (E51), poly- virtue
Ether nitrile ketone (PPENK), Core-shell rubber particles, flow control additive, curing agent and conductive graphene prepare conductive characteristic composite wood
Expect the method for skin covering of the surface.
Background technology
Recently as composite material being widely used in aerospace field, as the surface for improving multiple material surface quality
Film has also obtained quick development, and application amount is increasing, it can be such that the moulding process of multiple material greatly simplifies.As skin covering of the surface
One kind, be widely used in the anti-lightning strike field of aircraft with the composite material surface film of conductive characteristic.Traditional leads
Ammeter facial mask is exactly to realize conducting using conductive metal powder, but metal powder has many shortcomings compared with grapheme material:
(1) metallic is difficult to be uniformly dispersed than great in system, is being blended and may result in table in solidification process
Situations such as face and inconsistent bottom surface density, seriously affect the test of resistivity;And graphene is used as filling, in film preparation work
During skill, the problems such as will not settling.
(2) during high-speed flight, the components such as radome need to consider the Stealth Fighters such as wave transparent aircraft, to hidden
The requirement higher of body Stealth performance, this just proposes requirements at the higher level to material, can be to wave transparent using metallic filling
Performance etc. produces a very large impact, and uses grapheme material can be to avoid the generation of the problem.
(3) metallic is filled in resin system, under acid, alkali and hydrothermal aging, can accelerate to corrosion of metal and
Oxidation, especially coating metal, to be had an impact to the comprehensive performance of whole system;And use graphene system potting resin
Such risk would not be faced.
(4) a large amount of presence of metallic can reduce the mechanical property such as shear strength of membrane material, certainly will be to the material
Application range has an impact.
Invention content
The present invention is to solve it is existing there is conductive characteristic composite material surface film to be used for a long time resistance value is unstable asks
Topic, service life that is close and influencing material, makes aircraft in the normal flight of thundery sky by prodigious threat.The present invention is exactly to carry
It is prepared with conducting function and the controllable composite material surface film of resistance value for a kind of new method.
A kind of skin covering of the surface with conductive characteristic of the present invention, it is by 100phr epoxy resin, 6~14phr polyarylethers
Nitrile ketone, 4~8phr Core-shell rubber particles, 1~3phr flow control additives, 25~30phr curing agent and 5~15phr conduction stones
Black alkene is made.
A kind of preparation method of skin covering of the surface with conductive characteristic of the present invention, it is followed the steps below:
One, it adulterates:After epoxy resin and graphene are dissolved using solvent, by making the two fully mixed after ultrasonic vibration
It is even, mixture is then obtained by filtration;Mixture is dried to 5 hours removal solvents in an oven, it will finally by thin film evaporator
Remaining solvent removal is clean, obtains the epoxy resin adulterated with graphene;Wherein, epoxy resin addition is 100phr, institute
The graphene addition stated is 5phr~15phr;
Two, toughening:The epoxy resin adulterated with graphene that step 1 obtains is heated to 210 DEG C~230 DEG C, is then divided
Poly (arylene ether nitrile) ketone powder is added three times, is stirred continuously, keeps this temperature 25min~35min, wait for that poly (arylene ether nitrile) ketone powder is all molten
Cool the temperature to 130~170 DEG C after solution, Core-shell rubber particles be then added, be stirred continuously, it is to be mixed uniformly after by mixing liquid
It is poured on barrier paper for use;The poly (arylene ether nitrile) ketone addition be 6~14phr, Core-shell rubber particles addition be 4~
8phr;
Three, mechanical mixture:The hybrid resin that curing agent M-CDEA, flow control additive and antioxidant and step 2 are obtained
It is kneaded on the double roll mill, Bao Tongsan times;The curing agent addition is 25~30phr, mobility control
Agent addition is 1~3phr, and antioxidant is 0.1~0.3phr;
Four, the preparation of batten:The sizing material being kneaded is pressed into the glued membrane that thickness is 0.33~0.35mm thickness, is cut into 3mm wide,
The item of 30cm long is then placed in multiple material plate groove, and compacting, vacuum is cured, that is, completes the skin covering of the surface with conductive characteristic
It prepares.
The present invention includes following advantageous effect:
Then the present invention carries out special toughening to resin, passes through machine using a small amount of graphene is adulterated in matrix resin
Tool calendering prepares conducing composite material skin covering of the surface.Then it is pressed into the glued membrane of specific thickness, is cut into the item of corresponding size, is put into advance
In the multiple material plate groove prepared, compacting adds a vacuum cured, is measured finally by insulation tester and calculate cured plate
Resistivity when batten spacing is 50mm.
By the present invention in that with solvent method graphene dispersion in the epoxy, utmostly reduce the group of graphene
It is poly-, it is ensured that the uniformity and stability of resistance value;Combine in toughing ways and use poly (arylene ether nitrile) ketone and Core-shell rubber particles,
System is set to have both high temperature resistant, high tenacity;It is film material obtained by this experiment, has construction well special the application in future
Property.
Specific implementation mode
Specific implementation mode one:A kind of preparation method of skin covering of the surface with conductive characteristic of present embodiment, it be by
It is carried out according to following steps:
One, it adulterates:After epoxy resin and graphene are dissolved using solvent, by making the two fully mixed after ultrasonic vibration
It is even, mixture is then obtained by filtration;Mixture is dried to 5 hours removal solvents in an oven, it will finally by thin film evaporator
Remaining solvent removal is clean, obtains the epoxy resin adulterated with graphene;Wherein, epoxy resin addition is 100phr, institute
The graphene addition stated is 5phr~15phr;
Two, toughening:The epoxy resin adulterated with graphene that step 1 obtains is heated to 210 DEG C~230 DEG C, is then divided
Poly (arylene ether nitrile) ketone powder is added three times, is stirred continuously, keeps this temperature 25min~35min, wait for that poly (arylene ether nitrile) ketone powder is all molten
Cool the temperature to 130~170 DEG C after solution, Core-shell rubber particles be then added, be stirred continuously, it is to be mixed uniformly after by mixing liquid
It is poured on barrier paper for use;The poly (arylene ether nitrile) ketone addition be 6~14phr, Core-shell rubber particles addition be 4~
8phr;
Three, mechanical mixture:The hybrid resin that curing agent M-CDEA, flow control additive and antioxidant and step 2 are obtained
It is kneaded on the double roll mill, Bao Tongsan times;The curing agent addition is 25~30phr, mobility control
Agent addition is 1~3phr, and antioxidant is 0.1~0.3phr;
Four, the preparation of batten:The sizing material being kneaded is pressed into the glued membrane that thickness is 0.33~0.35mm thickness, is cut into 3mm wide,
The item of 30cm long is then placed in multiple material plate groove, and compacting, vacuum is cured, that is, completes the skin covering of the surface with conductive characteristic
It prepares.
Specific implementation mode two:The present embodiment is different from the first embodiment in that:The graphene of step 2 adulterates
Epoxy resin be heated to 210 DEG C~220 DEG C.It is other same as the specific embodiment one.
Specific implementation mode three:The present embodiment is different from the first embodiment in that:The poly (arylene ether nitrile) ketone of step 2
Addition is 8~14phr, and Core-shell rubber particles addition is 5~8phr.It is other same as the specific embodiment one.
Specific implementation mode four:The present embodiment is different from the first embodiment in that:The poly (arylene ether nitrile) ketone of step 2
Addition is 8~12phr, and Core-shell rubber particles addition is 6~8phr.It is other same as the specific embodiment one.
Specific implementation mode five:The present embodiment is different from the first embodiment in that:The poly (arylene ether nitrile) ketone of step 2
Addition is 10~12phr, and Core-shell rubber particles addition is 6~7phr.It is other same as the specific embodiment one.
Specific implementation mode six:The present embodiment is different from the first embodiment in that:Wait for that poly (arylene ether nitrile) ketone powder is complete
140~160 DEG C are cooled the temperature to after portion's dissolving.It is other same as the specific embodiment one.
Specific implementation mode seven:The present embodiment is different from the first embodiment in that:Wait for that poly (arylene ether nitrile) ketone powder is complete
150 DEG C are cooled the temperature to after portion's dissolving.It is other same as the specific embodiment one.
Specific implementation mode eight:The present embodiment is different from the first embodiment in that:Epoxy resin addition is
100phr, the graphene addition are 8phr~15phr.It is other same as the specific embodiment one.
Specific implementation mode nine:The present embodiment is different from the first embodiment in that:Epoxy resin addition is
100phr, the graphene addition are 8phr~12phr.It is other same as the specific embodiment one.
Specific implementation mode ten:The present embodiment is different from the first embodiment in that:The curing agent addition
For 25~28phr, flow control additive addition is 1~3phr, and antioxidant is 0.1~0.3phr.Other and specific embodiment party
Formula one is identical.
Specific implementation mode 11:The present embodiment is different from the first embodiment in that:The curing agent is added
Amount is 26~28phr, and flow control additive addition is 1~2phr, and antioxidant is 0.1~0.2phr.Other and specific implementation
Mode one is identical.
Specific implementation mode 12:The present embodiment is different from the first embodiment in that:The core shell rubbers grain
Son is MX-416.It is other same as the specific embodiment one.
Specific implementation mode 13:A kind of skin covering of the surface with conductive characteristic of present embodiment, it is by 100phr rings
Oxygen resin, 6~14phr poly (arylene ether nitrile)s ketone, 4~8phr Core-shell rubber particles, 1~3phr flow control additives, 25~30phr are solid
Agent and 5~15phr conductive graphenes are made.
Specific implementation mode 14:Present embodiment is unlike specific implementation mode 13:Curing agent is M-CDEA.
It is other identical as specific implementation mode 13.
The content of present invention is not limited only to the content of the respective embodiments described above, the group of one of them or several specific implementation modes
Contract sample can also realize the purpose of invention.
Beneficial effects of the present invention are verified by following embodiment:
Embodiment 1
A kind of preparation method of skin covering of the surface with conductive characteristic of the present embodiment, it is followed the steps below:
One, it adulterates:After epoxy resin and graphene are dissolved using solvent, by making the two adequately mixed after ultrasonic vibration
It closes, realizes the dispersion of reduced size, mixture is then obtained by filtration.By mixture, drying removes for 5 hours in baking oven (100 DEG C)
Remaining solvent is removed totally finally by thin film evaporator, it is for use to obtain the epoxy resin adulterated with graphene by solvent;With
Epoxy resin is 100phr, and the graphene addition is 10phr;
Two, toughening:The hybrid resin that step 1 obtains is heated to 220 DEG C, poly (arylene ether nitrile) ketone is then added in three times
(PPENK) powder is stirred continuously, and keeps this temperature 25min~35min, is cooled the temperature to after PPENK powder all dissolving
About 150 DEG C, then be added Core-shell rubber particles (MX-416), be stirred continuously, it is to be mixed uniformly after mixing liquid is poured over
It is for use on barrier paper;The PPENK additions are 8phr, and Core-shell rubber particles addition is 6phr;
Three, mechanical mixture:By curing agent M-CDEA (a kind of halogen-containing amine, Long Sha companies), flow control additive (gas
Phase method silica) and the hybrid resin that is obtained with step 2 of antioxidant be kneaded on the double roll mill, Bao Tongsan is all over i.e.
It can;The curing agent addition is 25phr, and flow control additive addition is 3phr, antioxidant 0.3phr;
Four, the preparation of batten:The sizing material being kneaded is pressed into the glued membrane that thickness is 0.33~0.35mm thickness, is cut into 3mm wide,
The item of 30cm long is then placed in multiple material plate groove well prepared in advance, and compacting adds a vacuum cured;
Five, the calculating of resistivity:It is measured by insulation tester and calculates resistance when cured plate batten spacing is 50mm
Rate;By controlling the dosage of graphene, the ranging from 2.7*10 of batten resistivity-4~3.5*105Ω.m。
In addition, setting up two control groups carries out contrast verification, control group 1 is to be operated according to the technical solution of embodiment 1, only
It is that the graphene in embodiment 1 is substituted for silver powder, other conditions are constant.Control group 2 is to be grasped according to the technical solution of embodiment 1
Make, the graphene in embodiment 1 is only substituted for copper powder, other conditions are constant.
The results are shown in Table 1.
Change in resistance after 1 130 DEG C/3h of table, two period heat ageings
As shown in Table 1:Adulterate the resistance after 130 DEG C/3h, two period heat ageings of the batten after the solidification of silver powder, copper powder
Rate both increases an order of magnitude, and the change in resistance of the batten of doped graphene is little, it can be said that bright pass through high temperature
The conductive network that graphene is formed after processing is still more stable, and the conductive network that silver powder and copper powder are formed is by high temperature
It is affected after reason, this is also that this experiment prepares the major reason with conductive characteristic skin covering of the surface using graphene.
The shear strength of 2 three kinds of membrane materials of table compares
As shown in Table 2:Skin covering of the surface with close conductivity, containing graphene is solid compared with the skin covering of the surface containing silver powder and copper powder
It may be the dispersity difference of graphene, silver powder with copper powder in resin to have preferable mechanical property, main cause after change
It is caused.
Claims (8)
1. a kind of skin covering of the surface with conductive characteristic, it is characterised in that it is by 100phr epoxy resin, 6~14phr polyarylethers
Nitrile ketone, 4~8phr Core-shell rubber particles, 1~3phr flow control additives, 25~30phr curing agent, 0.1~0.3phr antioxygens
Agent and 5~15phr conductive graphenes are made;Curing agent is M-CDEA;
Skin covering of the surface with conductive characteristic is prepared according to the following steps:
One, it adulterates:After epoxy resin and graphene are dissolved using solvent, by mixing well the two after ultrasonic vibration, so
After mixture is obtained by filtration;Mixture is dried to 5 hours removal solvents in an oven, it will be remaining finally by thin film evaporator
Solvent removal is clean, obtains the epoxy resin adulterated with graphene;Wherein, epoxy resin addition is 100phr, the stone
Black alkene addition is 5phr~15phr;
Two, toughening:The epoxy resin adulterated with graphene that step 1 obtains is heated to 210 DEG C~230 DEG C, then in three times
Poly (arylene ether nitrile) ketone powder is added, is stirred continuously, keeps this temperature 25min~35min, after poly (arylene ether nitrile) ketone powder all dissolving
Cool the temperature to 130~170 DEG C, Core-shell rubber particles be then added, be stirred continuously, it is to be mixed uniformly after mixing liquid is toppled over
It is for use on barrier paper;The poly (arylene ether nitrile) ketone addition is 6~14phr, and Core-shell rubber particles addition is 4~8phr;
Three, mechanical mixture:The hybrid resin that curing agent M-CDEA, flow control additive and antioxidant are obtained with step 2 is double
It is kneaded on roller open mill, Bao Tongsan times;The curing agent addition is 25~30phr, and flow control additive adds
It is 1~3phr to enter amount, and antioxidant is 0.1~0.3phr;
Four, the preparation of batten:The sizing material being kneaded is pressed into the glued membrane that thickness is 0.33~0.35mm thickness, is cut into 3mm wide, 30cm
Long item is then placed in multiple material plate groove, and compacting, vacuum is cured, that is, completes the preparation of the skin covering of the surface with conductive characteristic.
2. a kind of skin covering of the surface with conductive characteristic according to claim 1, it is characterised in that the graphene of step 2 is mixed
Miscellaneous epoxy resin is heated to 210 DEG C~220 DEG C.
3. a kind of skin covering of the surface with conductive characteristic according to claim 1, it is characterised in that the poly (arylene ether nitrile) of step 2
Ketone addition is 8~14phr, and Core-shell rubber particles addition is 5~8phr.
4. a kind of skin covering of the surface with conductive characteristic according to claim 1, it is characterised in that wait for poly (arylene ether nitrile) ketone powder
All 140~160 DEG C are cooled the temperature to after dissolving.
5. a kind of skin covering of the surface with conductive characteristic according to claim 3, it is characterised in that epoxy resin addition is
100phr, the graphene addition are 8phr~15phr.
6. a kind of skin covering of the surface with conductive characteristic according to claim 5, it is characterised in that epoxy resin addition is
100phr, the graphene addition are 8phr~12phr.
7. a kind of skin covering of the surface with conductive characteristic according to claim 1, it is characterised in that the curing agent is added
Amount is 25~28phr, and flow control additive addition is 1~3phr, and antioxidant is 0.1~0.3phr.
8. a kind of skin covering of the surface with conductive characteristic according to claim 7, it is characterised in that the curing agent is added
Amount is 26~28phr, and flow control additive addition is 1~2phr, and antioxidant is 0.1~0.2phr.
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