CN106167693A - A kind of preparation method of Graphene basement membrane product - Google Patents
A kind of preparation method of Graphene basement membrane product Download PDFInfo
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- CN106167693A CN106167693A CN201610451638.6A CN201610451638A CN106167693A CN 106167693 A CN106167693 A CN 106167693A CN 201610451638 A CN201610451638 A CN 201610451638A CN 106167693 A CN106167693 A CN 106167693A
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Abstract
The invention discloses the preparation method of a kind of Graphene basement membrane product, comprise the following steps: the preparation of (1) slurry；(2) it is coated with under magnetic field.The invention provides the preparation method of a kind of Graphene basement membrane product, it is possible to prepare the Graphene heat conducting film of high-efficiency heat conduction.The Graphene basement membrane product of the present invention is by selecting specific Graphene, heat conduction auxiliary agent, adhesive aid, binding agent and solvent to prepare slurry, and is coated slurry under the action of a magnetic field and is dried and prepared.Compared with the Graphene heat conducting film that traditional method prepares, the film product good heat conductivity of the present invention, cooling extent is at about 4.9 DEG C.It is coated under the action of a magnetic field and after drying, the film product film layer consistency of the present invention promotes, consistency increase about 30%～50%.The heat conducting film adhesion of the present invention is good, difficult drop-off, and water resistance is excellent.The preparation method of the present invention, processing step is simple, easily operates realization, and preparation condition is gentle, it is easy to control.
Description
Technical field
The present invention relates to the preparation method of a kind of Graphene basement membrane product, particularly belong to technical field of graphene.
Background technology
Graphene is the nano material that known world is the thinnest, the hardest, and it is almost fully transparent, only absorbs
The light of 2.3%；Heat conductivity is up to 5300W/m K, and higher than CNT and diamond, under room temperature, its electron mobility exceedes
15000cm2/ V s, again ratio CNT or silicon wafer height, and resistivity about 10-6Ω cm is lower than copper or silver, for generation
The material that upper resistivity is minimum.Because its resistivity is extremely low, the speed of electron transfer is exceedingly fast, and is therefore expected to can be used to develop more
Thin, conduction speed a new generation's electronic component or transistor faster.Due to a kind of transparent, good leading of Graphene
Body, also is adapted for for manufacturing transparent touch screen, tabula rasa, even solaode.
Graphene, owing to having heat conductivility, is often used as preparing heat conducting film.The preparation work of traditional Graphene heat conducting film
The heat conducting film that skill prepares, heat conductivility is the most excellent, and cooling extent is limited.Therefore, research one can prepare excellent
Good heat conductivility, promotes the preparation method of the Graphene heat conducting film of cooling extent, it appears particularly necessary.
Summary of the invention
For solving the deficiencies in the prior art, it is an object of the invention to provide the preparation side of a kind of Graphene basement membrane product
Method, it is possible to prepare the Graphene heat conducting film of high-efficiency heat conduction.
In order to realize above-mentioned target, the present invention adopts the following technical scheme that:
The preparation method of a kind of Graphene basement membrane product, comprises the following steps: the preparation of (1) slurry；(2) it is coated with under magnetic field
Cloth.
The preparation method of foregoing graphites thiazolinyl film product, specifically includes following steps:
(1) preparation of slurry: add Graphene, heat conduction auxiliary agent and bonding in the ball grinder being previously added ball milling pearl and help
Agent, then drip binding agent, it being subsequently added solvent, carry out ball milling, ball milling takes out slurry and removes bubble by stirring after terminating, standby
With；
(2) it is coated with under magnetic field: the base material after Ethanol Treatment is placed on magnetic field, by coating bar by step (1)
The slurry prepared is coated on base material, is dried subsequently and get final product in the presence of magnetic field.
The preparation method of foregoing graphites thiazolinyl film product, in step (2), magnetic field is arranged at distance base material 0～3cm, magnetic
The intensity of field is 10mT～1000mT.
The preparation method of foregoing graphites thiazolinyl film product, in step (1), described Graphene is water-soluble graphene or oil soluble
Property modified graphene, described heat conduction auxiliary agent is nano-ceramic particle, nano zine oxide, white carbon black, CNT or boron nitride, described
Adhesive aid is cellulose, cellulose derivative, polyvinyl alcohol or aerosil, and described binding agent is epoxy resin, poly-
Urethane resin or butadiene styrene resin, described solvent is water, ethanol, polyhydric alcohol, acetone, butanone or N-Methyl pyrrolidone.All right
In system, add surfactant, can fuse with promotion system.
The preparation method of foregoing graphites thiazolinyl film product, in step (1), according to mass ratio, Graphene heat conduction auxiliary agent glues
Knot auxiliary agent=30～60 200～500 40～120.
The preparation method of foregoing graphites thiazolinyl film product, in step (1), according to mass ratio, binding agent adhesive aid=1
～10 3～80.
The preparation method of foregoing graphites thiazolinyl film product, in step (1), according to mass volume ratio, the quality of Graphene is molten
The volume of agent=A g B mL, wherein 0 < A≤10,0 < B≤800.
The preparation method of foregoing graphites thiazolinyl film product, in step (1), during ball milling a length of 1～36h, the weight of ball milling pearl
For 0.5kg～5kg, the mass ratio of different-grain diameter ball milling pearl is: 1mm particle diameter ball milling pearl 5mm particle diameter ball milling pearl 10mm particle diameter ball
Mill pearl=1～20 1～10 1～8.The mass ratio of different-grain diameter ball milling pearl can be adjusted according to the size of ball mill, when adopting
During with little ball mill, it is preferred to use the mass ratio of different-grain diameter ball milling pearl is: 2mm particle diameter ball milling pearl 8mm particle diameter ball milling pearl=1
～15 1～6.
The preparation method of foregoing graphites thiazolinyl film product, in step (1), the rotating speed of stirring is 100～3000rpm, the time
It is 0.1～12h.
The preparation method of foregoing graphites thiazolinyl film product, in step (2), described base material is Copper Foil, aluminium foil or PET film,
The coating wet-film thickness of described coating bar is 10～250 microns, and described being dried is to be dried at 45 DEG C～150 DEG C.
In order to ensure the science, rationally of the inventive method, inventor has carried out a series of test.
The Graphene heat conducting film preparing the preparation method of Graphene basement membrane product of the present invention carries out heat conductivility survey
Examination.Take Graphene heat conducting film that the inventive method prepares and heat conducting film prepared by traditional method, pass through
Device in ZL2016202621805 carries out heat conductivility test.Test result shows, the heat conduction being prepared by the method for the present invention
Film is lowered the temperature about 4.9 DEG C, and heat conducting film cooling extent prepared by traditional method is less than 3.5 DEG C.Understand and be coated with under the action of a magnetic field,
Improve the performance of Graphene heat conducting film.
Heat conducting film is dried in the presence of magnetic field by the preparation method of the present invention, can effectively promote heat conducting film performance.
Understanding through heat conductivility test, heat conducting film is not directly dried under the existence condition of magnetic field, and its cooling extent is 3.5 DEG C of left sides
The right side, the heat conducting film prepared less than the inventive method.
The magnetic field set-up mode of the present invention preferably employs mode as shown in Figure 1.Magnetic field is arranged at the lower section of base material, deflector roll
Setting base material can persistently be moved, it is simple under magnetic field, slurry is coated on base material by continuous print.Preferably magnetic field is arranged
At distance base material 0～3cm, magnetic field intensity is 10mT～1000mT, it is possible to reach maximum cooling extent.Preparation method of the present invention
When magnetic field is arranged, the magnetic line of force is unsuitable overstocked, occurs that striated is advisable with graphene film.Preferably employ rubber magnetic sheet as magnetic field.
Coating when rubber magnetic sheet is arranged as magnetic field, heat conducting film occurs obvious zebra-stripe shape striped under moisture state, cooling
About 4.9 DEG C.May be relevant with rubber magnetic sheet special facture technique, because this lines and mode NSNSNSNS that magnetizes of rubber magnetic sheet
Zebra bar shaped about the same.And the coating when ferrite is arranged as magnetic field, owing to the magnetic line of force is overstocked, there is no obvious magnetic
Property striped occur, its cooling extent is about 3.5 DEG C.
Being prepared by the method for the present invention the Graphene heat conducting film obtained, compared with conventional pilot hotting mask, the consistency of film layer increases
Add 30%～50%.Testing the adhesion of product with method of testing in standard ISO2409-1992, result shows this
The adhesion of bright Graphene heat conducting film is good, difficult drop-off.Water resistant test is by directly dripping on the film layer of testing sample, and
Carry out with non-woven fabrics wiping.Water-fast test result indicate that, product prepared by the present invention without substantially fading, water-tolerant, along with
The increase of consumption of binder, water resistance the most gradually promotes.
The present invention select nano-ceramic particle, nano zine oxide, white carbon black, CNT or boron nitride help as heat conduction
Agent, prepares a series of Graphene heat conducting film by adding different heat conduction auxiliary agent, it is carried out heat conductivility test.Result such as table 1
Shown in.As shown in Table 1, selecting the heat conducting film that the heat conduction auxiliary agent of the present invention prepares, cooling extent is big, good heat conductivity.
Table 1
| Heat conduction auxiliary agent | Cooling extent (DEG C) |
| It is not added with heat conduction auxiliary agent | 3.6 |
| Nano-metal particle | 3.6 |
| Metal powder | 3.7 |
| Nano-ceramic powder | 4.7 |
| Nano zine oxide | 4.5 |
| CNT | 4.9 |
| White carbon black | 4.7 |
| Boron nitride | 4.4 |
The invention have benefit that: the invention provides the preparation method of a kind of Graphene basement membrane product, it is possible to system
The standby Graphene heat conducting film obtaining high-efficiency heat conduction.The Graphene heat conducting film of the present invention is by selecting specific Graphene, heat conduction
Auxiliary agent, adhesive aid, binding agent and solvent prepare slurry, and are coated slurry under the action of a magnetic field and are dried and make
?.Compared with the Graphene heat conducting film that traditional method prepares, the heat conducting film good heat conductivity of the present invention, cooling extent exists
About 4.9 DEG C.It is coated under the action of a magnetic field and after drying, the Graphene heat conducting film film layer consistency of the present invention promotes, cause
Density increase about 30%～50%.The heat conducting film adhesion of the present invention is good, difficult drop-off, and water resistance is excellent.The system of the present invention
Preparation Method, processing step is simple, easily operates realization, and preparation condition is gentle, it is easy to control.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the magnetic field setting of the present invention；
The implication of reference in figure: 1-base material, 2-deflector roll, 3-magnetic sheet.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further introduced.
In the present invention, agents useful for same is commercially available prod.
Embodiment 1
The preparation method of a kind of Graphene basement membrane product, comprises the following steps:
(1) preparation of slurry: in the ball grinder being previously added the ball milling pearl that weight is 0.5kg, adding mass ratio is 30
Water-soluble graphene, heat conduction auxiliary agent and the adhesive aid of 200 40, then drip binding agent, it is subsequently added solvent, carries out ball milling, ball
A length of 1h during mill, ball milling takes out slurry after terminating and removes bubble by stirring, and standby, the rotating speed of stirring is 100rpm, and the time is
12h.Wherein, the mass ratio of different-grain diameter ball milling pearl is: 1mm particle diameter ball milling pearl 5mm particle diameter ball milling pearl 10mm particle diameter ball milling pearl
=111；Described heat conduction auxiliary agent is nano-ceramic particle；Described adhesive aid is cellulose；Described binding agent is polyurethane tree
Fat；Described solvent is water；According to mass ratio, binding agent adhesive aid=1 3；According to mass volume ratio, the quality of Graphene
The volume of solvent=0.1g 10mL.
(2) being coated with under magnetic field: be placed on magnetic field by the base material after Ethanol Treatment, magnetic field is arranged on distance base material 3cm
Place, the intensity in magnetic field is 1000mT, is coated on base material by the slurry that step (1) prepares by coating bar, exists subsequently
Being dried in the presence of magnetic field, baking temperature is 150 DEG C, to obtain final product.Wherein, described base material is Copper Foil, the painting of described coating bar
Cloth wet-film thickness is 10 microns.
Embodiment 2
The preparation method of a kind of Graphene basement membrane product, comprises the following steps:
(1) preparation of slurry: in the ball grinder being previously added the ball milling pearl that weight is 5kg, adding mass ratio is 60
Water-soluble graphene, heat conduction auxiliary agent and the adhesive aid of 500 120, then drip binding agent, it is subsequently added solvent, carries out ball milling,
A length of 36h during ball milling, ball milling takes out slurry after terminating and removes bubble by stirring, and standby, the rotating speed of stirring is 3000rpm, time
Between be 0.1h.Wherein, the mass ratio of different-grain diameter ball milling pearl is: 1mm particle diameter ball milling pearl 5mm particle diameter ball milling pearl 10mm particle diameter ball
Mill pearl=20 10 8；Described heat conduction auxiliary agent is nano zine oxide；Described adhesive aid is polyvinyl alcohol；Described binding agent is fourth
Benzene resin；Described solvent is ethanol；According to mass ratio, binding agent adhesive aid=10 80；According to mass volume ratio, Graphene
The volume=10g 800mL of mass solvent.
(2) being coated with under magnetic field: be placed on magnetic field by the base material after Ethanol Treatment, magnetic field is arranged on distance base material 0cm
Place, the intensity in magnetic field is 10mT, is coated on base material, the slurry that step (1) prepares subsequently at magnetic by coating bar
Being dried in the presence of Chang, baking temperature is 45 DEG C, to obtain final product.Wherein, described base material is aluminium foil, and the coating of described coating bar is wet
Film thickness is 250 microns.
Embodiment 3
The preparation method of a kind of Graphene basement membrane product, comprises the following steps:
(1) preparation of slurry: in the ball grinder being previously added the ball milling pearl that weight is 4kg, adding mass ratio is 50
Water-soluble graphene, heat conduction auxiliary agent and the adhesive aid of 300 100, then drip binding agent, it is subsequently added solvent, carries out ball milling,
A length of 18h during ball milling, ball milling takes out slurry after terminating and removes bubble by stirring, and standby, the rotating speed of stirring is 2000rpm, time
Between be 6h.Wherein, the mass ratio of different-grain diameter ball milling pearl is: 1mm particle diameter ball milling pearl 5mm particle diameter ball milling pearl 10mm particle diameter ball milling
Pearl=10 54；Described heat conduction auxiliary agent is white carbon black；Described adhesive aid is aerosil；Described binding agent is butylbenzene tree
Fat；Described solvent is polyhydric alcohol；According to mass ratio, binding agent adhesive aid=5 40；According to mass volume ratio, Graphene
The volume of mass solvent=5g 300mL.
(2) being coated with under magnetic field: be placed on magnetic field by the base material after Ethanol Treatment, magnetic field is arranged on distance base material 20mm
Place, the intensity in magnetic field is 500mT, is coated on base material, the slurry that step (1) prepares subsequently at magnetic by coating bar
Being dried in the presence of Chang, baking temperature is 100 DEG C, to obtain final product.Wherein, described base material is PET film, the painting of described coating bar
Cloth wet-film thickness is 200 microns.
Embodiment 4
The preparation method of a kind of Graphene basement membrane product, comprises the following steps:
(1) preparation of slurry: in the ball grinder being previously added the ball milling pearl that weight is 3kg, adding mass ratio is 55
Oil-soluble modified graphene, heat conduction auxiliary agent and the adhesive aid of 400 60, then drip binding agent, it is subsequently added solvent, carries out ball
Mill, a length of 12h during ball milling, ball milling takes out slurry after terminating and removes bubble by stirring, and standby, the rotating speed of stirring is 1500rpm,
Time is 3h.Wherein, the mass ratio of different-grain diameter ball milling pearl is: 1mm particle diameter ball milling pearl 5mm particle diameter ball milling pearl 10mm particle diameter ball
Mill pearl=15 27；Described heat conduction auxiliary agent is CNT；Described adhesive aid is aerosil；Described binding agent is poly-
Urethane resin；Described solvent is acetone；According to mass ratio, binding agent adhesive aid=9 20；According to mass volume ratio, graphite
The volume of the mass solvent of alkene=2g 600mL.
(2) being coated with under magnetic field: be placed on magnetic field by the base material after Ethanol Treatment, magnetic field is arranged on distance base material 10mm
Place, the intensity in magnetic field is 800mT, is coated on base material, the slurry that step (1) prepares subsequently at magnetic by coating bar
Being dried in the presence of Chang, baking temperature is 120 DEG C, to obtain final product.Wherein, described base material is Copper Foil, the coating of described coating bar
Wet-film thickness is 50 microns.
Embodiment 5
The preparation method of a kind of Graphene basement membrane product, comprises the following steps:
(1) preparation of slurry: in the ball grinder being previously added the ball milling pearl that weight is 0.8kg, adding mass ratio is 35
Oil-soluble modified graphene, heat conduction auxiliary agent and the adhesive aid of 450 110, then drip binding agent, it is subsequently added solvent, carries out ball
Mill, a length of 24h during ball milling, ball milling takes out slurry after terminating and removes bubble by stirring, and standby, the rotating speed of stirring is 2500rpm,
Time is 9h.Wherein, the mass ratio of different-grain diameter ball milling pearl is: 1mm particle diameter ball milling pearl 5mm particle diameter ball milling pearl 10mm particle diameter ball
Mill pearl=6 92；Described heat conduction auxiliary agent is boron nitride；Described adhesive aid is cellulose derivative；Described binding agent is epoxy
Resin；Described solvent is butanone；According to mass ratio, binding agent adhesive aid=4 70；According to mass volume ratio, Graphene
The volume of mass solvent=8g 150mL.
(2) being coated with under magnetic field: be placed on magnetic field by the base material after Ethanol Treatment, magnetic field is arranged on distance base material 6mm
Place, the intensity in magnetic field is 100mT, is coated on base material, the slurry that step (1) prepares subsequently at magnetic by coating bar
Being dried in the presence of Chang, baking temperature is 80 DEG C, to obtain final product.Wherein, described base material is aluminium foil, and the coating of described coating bar is wet
Film thickness is 100 microns.
Embodiment 6
The preparation method of a kind of Graphene basement membrane product, comprises the following steps:
(1) preparation of slurry: in the ball grinder being previously added the ball milling pearl that weight is 3.5kg, adding mass ratio is 55
Oil-soluble modified graphene, heat conduction auxiliary agent and the adhesive aid of 200 45, then drip binding agent, it is subsequently added solvent, carries out ball
Mill, a length of 6h during ball milling, ball milling takes out slurry after terminating and removes bubble by stirring, and standby, the rotating speed of stirring is 500rpm, time
Between be 0.5h.Wherein, the mass ratio of different-grain diameter ball milling pearl is: 1mm particle diameter ball milling pearl 5mm particle diameter ball milling pearl 10mm particle diameter ball
Mill pearl=11 35；Described heat conduction auxiliary agent is CNT；Described adhesive aid is polyvinyl alcohol；Described binding agent is asphalt mixtures modified by epoxy resin
Fat；Described solvent is N-Methyl pyrrolidone；According to mass ratio, binding agent adhesive aid=2 16；According to mass volume ratio,
The volume of the mass solvent of Graphene=1g 120mL.
(2) being coated with under magnetic field: be placed on magnetic field by the base material after Ethanol Treatment, magnetic field is arranged on distance base material
At 1.5cm, the intensity in magnetic field is 400mT, is coated on base material by the slurry that step (1) prepares by coating bar, with
After be dried in the presence of magnetic field, baking temperature is 100 DEG C, to obtain final product.Wherein, described base material is PET film, described coating line
The coating wet-film thickness of rod is 30 microns.
Claims (10)
1. the preparation method of a Graphene basement membrane product, it is characterised in that: comprise the following steps: the preparation of (1) slurry；(2)
It is coated with under magnetic field.
The preparation method of Graphene basement membrane product the most according to claim 1, it is characterised in that: comprise the following steps:
(1) preparation of slurry: add Graphene, heat conduction auxiliary agent and adhesive aid in the ball grinder being previously added ball milling pearl, then
Dropping binding agent, is subsequently added solvent, carries out ball milling, and ball milling takes out slurry and removes bubble by stirring after terminating, standby；
(2) it is coated with under magnetic field: the base material after Ethanol Treatment is placed on magnetic field, by coating bar prepared by step (1)
The slurry obtained is coated on base material, is dried subsequently and get final product in the presence of magnetic field.
The preparation method of Graphene basement membrane product the most according to claim 2, it is characterised in that: in described step (2), magnetic
Field is arranged at distance base material 0～3cm, and the intensity in magnetic field is 10mT～1000mT.
The preparation method of Graphene basement membrane product the most according to claim 2, it is characterised in that: in step (1), described stone
Ink alkene is water-soluble graphene or oil-soluble modified graphene；Described heat conduction auxiliary agent is nano-ceramic particle, nano zine oxide, charcoal
Black, CNT or boron nitride；Described adhesive aid is cellulose, cellulose derivative, polyvinyl alcohol or aerosil,
Described binding agent is epoxy resin, polyurethane resin or butadiene styrene resin, and described solvent is water, ethanol, polyhydric alcohol, acetone, butanone
Or N-Methyl pyrrolidone.
The preparation method of Graphene basement membrane product the most according to claim 2, it is characterised in that: in described step (1), press
According to mass ratio, Graphene heat conduction auxiliary agent adhesive aid=30～60 200～500 40～120.
The preparation method of Graphene basement membrane product the most according to claim 2, it is characterised in that: in described step (1), press
According to mass ratio, binding agent adhesive aid=1～10 3～80.
The preparation method of Graphene basement membrane product the most according to claim 2, it is characterised in that: in described step (1), press
According to mass volume ratio, the volume of the mass solvent of Graphene=A g B mL, wherein 0 < A≤10,0 < B≤800.
The preparation method of Graphene basement membrane product the most according to claim 2, it is characterised in that: in described step (1), ball
During mill a length of 1～36h, the weight of ball milling pearl is 0.5kg～5kg, and the mass ratio of different-grain diameter ball milling pearl is: 1mm particle diameter ball milling
Pearl 5mm particle diameter ball milling pearl 10mm particle diameter ball milling pearl=1～20 1～10 1～8.
The preparation method of Graphene basement membrane product the most according to claim 2, it is characterised in that: in described step (1), stir
The rotating speed mixed is 100～3000rpm, and the time is 0.1～12h.
The preparation method of Graphene basement membrane product the most according to claim 2, it is characterised in that: in described step (2),
Base material is Copper Foil, aluminium foil or PET film, and the coating wet-film thickness of described coating bar is 10～250 microns, described be dried be
It is dried at 45 DEG C～150 DEG C.
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| CN108328938A (en) * | 2017-01-20 | 2018-07-27 | 株洲晨昕中高频设备有限公司 | A kind of conductive graphite piece and its production method |
| CN109536142A (en) * | 2019-01-15 | 2019-03-29 | 苏州世华新材料科技股份有限公司 | A kind of preparation method of graphene film Heat Conduction Material |
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| CN108328938A (en) * | 2017-01-20 | 2018-07-27 | 株洲晨昕中高频设备有限公司 | A kind of conductive graphite piece and its production method |
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| CN109679525A (en) * | 2018-12-29 | 2019-04-26 | 厦门十一维科技有限公司 | The preparation facilities of conductive tape and preparation method thereof based on graphene |
| CN109536142A (en) * | 2019-01-15 | 2019-03-29 | 苏州世华新材料科技股份有限公司 | A kind of preparation method of graphene film Heat Conduction Material |
| CN111037971A (en) * | 2019-11-25 | 2020-04-21 | 江苏鸿凌达科技有限公司 | Graphene heat-conducting thick film manufacturing process |
| CN112277435A (en) * | 2020-10-10 | 2021-01-29 | 山东华冠智能卡有限公司 | Production equipment and production method of graphene RFID tag antenna |
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