CN107937995A - A kind of grapheme conductive film and preparation method thereof - Google Patents
A kind of grapheme conductive film and preparation method thereof Download PDFInfo
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- CN107937995A CN107937995A CN201711171612.7A CN201711171612A CN107937995A CN 107937995 A CN107937995 A CN 107937995A CN 201711171612 A CN201711171612 A CN 201711171612A CN 107937995 A CN107937995 A CN 107937995A
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- sodium chloride
- graphene
- grapheme conductive
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 57
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 51
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 44
- 239000011780 sodium chloride Substances 0.000 claims abstract description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 16
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 12
- 238000010792 warming Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000012153 distilled water Substances 0.000 claims abstract description 9
- 238000005554 pickling Methods 0.000 claims abstract description 6
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 6
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 3
- 239000003292 glue Substances 0.000 claims description 5
- 239000003643 water by type Substances 0.000 claims description 5
- 238000005491 wire drawing Methods 0.000 claims description 5
- 238000000502 dialysis Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 24
- 239000012528 membrane Substances 0.000 abstract description 21
- 238000007731 hot pressing Methods 0.000 abstract description 7
- 238000012545 processing Methods 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 229910021642 ultra pure water Inorganic materials 0.000 abstract 1
- 239000012498 ultrapure water Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 15
- 238000000034 method Methods 0.000 description 11
- 238000012360 testing method Methods 0.000 description 8
- 239000007921 spray Substances 0.000 description 5
- 238000005452 bending Methods 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 238000005189 flocculation Methods 0.000 description 3
- 230000016615 flocculation Effects 0.000 description 3
- 239000000499 gel Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000007590 electrostatic spraying Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
- D01D5/0084—Coating by electro-spinning, i.e. the electro-spun fibres are not removed from the collecting device but remain integral with it, e.g. coating of prostheses
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Textile Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
A kind of grapheme conductive film and preparation method thereof, graphite powder and sodium chloride are mixed, then wash removing sodium chloride, then dry, be stirred overnight after adding the concentrated sulfuric acid, by potassium permanganate by the above-mentioned solution of addition, and keep temperature to be at this time no more than 20 DEG C, then, it is warming up to 40 DEG C, finally it is warming up to 90 DEG C, ultra-pure water is added, hydrogen peroxide is added, after hydrochloric acid solution pickling one time, dialyse in distilled water, obtain high concentration graphene oxide；By electrostatic spinning machine, flexible substrates are wrapped on grounded metal roller and collect EFI gained fine droplet as receiver, form grapheme conductive film.The present invention can be formed can arbitrarily curved flexible conductive film；By simple hot-pressing processing, graphene-based composite membrane can be made to be changed into the redox graphene composite membrane of high conductivity under conditions of nontoxic.
Description
Technical field
The invention belongs to the technology of preparing of nano material complex film, more particularly to a kind of grapheme conductive film and its preparation side
Method.
Background technology
Graphene is because of its very good intensity, flexible, conductive, heat conduction, optical characteristics, in physics, materialogy, electronics
The fields such as information, computer, aerospace are obtained for significant progress.In recent years, graphene is made to the conductive thin of two dimension
Film becomes the hot spot of the area research.Chemical vapour deposition technique is that (CVD) is production graphene film most efficient method at present.
The hair carries out the obtained graphene film that is vapor-deposited using carbon containing organic gas for raw material, and graphene prepared by this method has
The characteristics of area is greatly and quality is high, but cost is higher at this stage, and process conditions also need further perfect.By electrostatic spraying processes,
Graphene conductive film can be quickly prepared, meanwhile, its choice of the substrates wide scope, graphene film thickness, area, shape
Regulation and control.Therefore, which can become efficient, low cost prepares one of convenient method of diversity graphene conductive film.
The content of the invention
The technical problem of solution：The present invention is directed to above-mentioned technical problem, there is provided a kind of grapheme conductive film and its preparation side
Method, obtained flexible conductive film can arbitrarily bend, cut out.
Technical solution：A kind of preparation method of grapheme conductive film, preparation process are：In proportion, it is 10 by mass ratio:1-
30:1 graphite powder and sodium chloride mixing, then removing sodium chloride is washed, then dry, it is stirred after the addition 20-25mL concentrated sulfuric acids
At night, above-mentioned solution is added by potassium permanganate in the ratio that mass fraction is 20%-30%, and keeps temperature to be at this time no more than
20 DEG C, then, 40 DEG C of holding 30min are warming up to, 90 DEG C is finally warming up to and keeps 45min, adding 18M Ω ultra-pure waters makes sulfuric acid
Concentration dilution adds 150mL 5-10vol% hydrogen peroxide to 30-40vol% after 25min, after hydrochloric acid solution pickling one time,
Dialyse 3 days in distilled water, obtain high concentration graphene oxide；By NANON-01A electrostatic spinning machines, in voltage 10kV-20kV,
Distance is 12-15cm between metal needle and wire drawing device, and flow velocity 0.5-3mL/h, rotating speed of transferring shares is 500-3000rpm/min bars
Under part, flexible substrates are wrapped on grounded metal roller and collect EFI gained fine droplet as receiver, form graphene
Conducting film.
Preferably, the flexible substrates are the double glue A4 paper of 80g.
Preferably, the concentration of the hydrogen peroxide is 10vol.%, and the concentration of hydrochloric acid solution is 5wt.%.
Preferably, sodium chloride is added in the high concentration graphene oxide completed to dialysis, controls the mass concentration of sodium chloride
For 20%-50%.
Grapheme conductive film made from above-mentioned preparation method.
The present invention can be reduced rapidly by hot pressing (50-100 DEG C) to be obtained as redox graphene composite membrane, electric conductivity
To significantly being lifted.By four probe sheet resistance instrument, step instrument can test thickness and its electric conductivity.After bending 1000 times, still
So keep the 95% of initial conductivity.
Beneficial effect：By regulating and controlling flow velocity during electrostatic spray, distance, voltage, time, the viscosity of EFI solution with
And flexible substrates, different-thickness, the composite conductive film of different compositions can be obtained；Using electrostatic spray, can quickly, uniformly prepare conduction
Film；Using the interaction between the flexibility of substrate, graphene and substrate, (particularly A4 paper similar materials, are made by capillary
With can combine closely between graphene hydrogel) can be formed can arbitrarily curved flexible conductive film；At simple hot pressing
Reason, can make graphene-based composite membrane be changed into the redox graphene composite membrane of high conductivity under conditions of nontoxic.
Brief description of the drawings
Fig. 1 is the graphene film layer cross section SEM figures peeled off in redox graphene/A4 paper；
Fig. 2 is preparation process flow diagram.
Embodiment
Following embodiments only technical concepts and features to illustrate the invention, its object is to allow person skilled in the art
It is that can understand present disclosure and implement according to this, it is not intended to limit the scope of the present invention.It is all according to the present invention
The equivalent transformation or modification that Spirit Essence is done, should be covered by the protection scope of the present invention.
Embodiment 1：
A. graphene/A4 paper composite membranes are prepared using electrostatic spray：
First, high concentration graphene oxide is prepared by modified Hummers methods：1g graphite powders and 0.05g sodium chloride are mixed
Washing removes sodium chloride after conjunction, dry, and 22h is stirred after adding the 23mL concentrated sulfuric acids, 6g potassium permanganate is added above-mentioned solution, and protect
The temperature held at this time is no more than 20 DEG C, then, is warming up to 40 DEG C of holding 30min, is finally warming up to 90 DEG C and keeps 45min, add
Enter 46mL 18M Ω ultra-pure waters, 140mL distilled water and 10mL 30vol.% hydrogen peroxide are added after 25min, with the hydrochloric acid of 5wt.%
After solution pickling one time, dialyse 3 days in distilled water, obtain high concentration graphene oxide.
Secondly addition sodium chloride, the mass concentration for controlling sodium chloride is 30wt%, by flocculation, lifts graphene water
The viscosity of gel.
Using high viscosity graphene oxide as EFI solution, in voltage 10kV-20kV, the spacing of metal needle and wire drawing device
From for 12.5cm, flow velocity 0.5-3mL/h is double by flexible substrates such as 80g under the conditions of rotating speed of transferring shares is 500-3000rpm/min
Glue A4 paper bags are rolled on grounded metal roller collects fine droplet obtained by EFI as receiver, forms composite film material.
B. conducting performance test：
Using the sheet resistance R of the double electrical measurement four-point probe test graphene/A4 paper composite membranes of SDY-5 types.Using DEKTAK
150 type step instruments test the thickness d of graphene/A4 paper composite membranes.Graphene/A4 paper composite membranes are calculated by formula (1)
Electrical conductivity ρ be 1860S/m.
ρ=1/ (R × d) (1)
Embodiment 2：
A. graphene/A4 paper composite membranes are prepared using electrostatic spray：
First, high concentration graphene oxide is prepared by modified Hummers methods：1g graphite powders and 0.05g sodium chloride are mixed
Washing removes sodium chloride after conjunction, dry, and 22h is stirred after adding the 23mL concentrated sulfuric acids, 6g potassium permanganate is added above-mentioned solution, and protect
The temperature held at this time is no more than 20 DEG C, then, is warming up to 40 DEG C of holding 30min, is finally warming up to 90 DEG C and keeps 45min, add
Enter 46mL 18M Ω ultra-pure waters, 140mL distilled water and 10mL 30vol.% hydrogen peroxide are added after 25min, with the hydrochloric acid of 5wt.%
After solution pickling one time, dialyse 3 days in distilled water, obtain high concentration graphene oxide.
Secondly addition sodium chloride, the mass concentration for controlling sodium chloride is 30wt%, by flocculation, lifts graphene water
The viscosity of gel.
Using high viscosity graphene oxide as EFI solution, in voltage 10kV-20kV, the spacing of metal needle and wire drawing device
From for 12.5cm, flow velocity 0.5-3mL/h is double by flexible substrates such as 80g under the conditions of rotating speed of transferring shares is 500-3000rpm/min
Glue A4 paper bags are rolled on grounded metal roller collects fine droplet obtained by EFI as receiver, forms composite film material.
B. hot pressing reduces：
By hot-pressing processing, under the conditions of 100 DEG C, redox graphene/A4 paper composite membranes are prepared.
C. conducting performance test：
Using the sheet resistance R of the double electrical measurement four-point probe test graphene/A4 paper composite membranes of SDY-5 types.Using DEKTAK
150 type step instruments test the thickness d of graphene/A4 paper composite membranes.Graphene/A4 paper composite membranes are calculated by formula (1)
Electrical conductivity ρ be 3670S/m.
ρ=1/ (R × d) (1)
Embodiment 3：
A. graphene/A4 paper composite membranes are prepared using electrostatic spray：
First, high concentration graphene oxide is prepared by modified Hummers methods：1g graphite powders and 0.05g sodium chloride are mixed
Washing removes sodium chloride after conjunction, dry, and 22h is stirred after adding the 23mL concentrated sulfuric acids, 6g potassium permanganate is added above-mentioned solution, and protect
The temperature held at this time is no more than 20 DEG C, then, is warming up to 40 DEG C of holding 30min, is finally warming up to 90 DEG C and keeps 45min, add
Enter 46mL 18M Ω ultra-pure waters, 140mL distilled water and 10mL 30vol.% hydrogen peroxide are added after 25min, with the hydrochloric acid of 5wt.%
After solution pickling one time, dialyse 3 days in distilled water, obtain high concentration graphene oxide.
Secondly addition sodium chloride, the mass concentration for controlling sodium chloride is 30wt%, by flocculation, lifts graphene water
The viscosity of gel.
Using high viscosity graphene oxide as EFI solution, in voltage 10kV-20kV, the spacing of metal needle and wire drawing device
From for 12.5cm, flow velocity 0.5-3mL/h is double by flexible substrates such as 80g under the conditions of rotating speed of transferring shares is 500-3000rpm/min
Glue A4 paper bags are rolled on grounded metal roller collects fine droplet obtained by EFI as receiver, forms composite film material.
B. hot pressing reduces：
By hot-pressing processing, under the conditions of 100 DEG C, redox graphene/A4 paper composite membranes are prepared.
C. bending test
By redox graphene/A4 paper composite membrane bending 1000 times (bending angle is random).
D. conducting performance test：
Using the sheet resistance R of the double electrical measurement four-point probe test redox graphene/A4 paper composite membranes of SDY-5 types.Adopt
With the thickness d of 150 type step instruments of DEKTAK test redox graphene/A4 paper composite membranes.It is calculated by formula (1)
The electrical conductivity ρ of redox graphene/A4 paper composite membranes is 3487S/m.
ρ=1/ (R × d) (1)
1. graphenes of table/A4 paper membranes thickness, sheet resistance, electrical conductivity contrast form
Claims (5)
1. a kind of preparation method of grapheme conductive film, it is characterised in that preparation process is：In proportion, it is 10 by mass ratio:1-
30:1 graphite powder and sodium chloride mixing, then removing sodium chloride is washed, then dry, it is stirred after the addition 20-25 mL concentrated sulfuric acids
At night, above-mentioned solution is added by potassium permanganate in the ratio that mass fraction is 20%-30%, and keeps temperature to be at this time no more than 20
DEG C, then, 40 DEG C of 30 min of holding are warming up to, are finally warming up to 90 DEG C and keep 45 min, adding 18 M Ω ultra-pure waters makes
Sulfuric acid concentration is diluted to 30-40 vol%, 150mL 5-10 vol% hydrogen peroxide is added after 25 min, with hydrochloric acid solution pickling one time
Afterwards, dialyse 3 days in distilled water, obtain high concentration graphene oxide；By NANON-01A electrostatic spinning machines, in voltage 10
KV-20 kV, distance is 12-15 cm between metal needle and wire drawing device, and flow velocity is 0.5-3 mL/h, and rotating speed of transferring shares is 500-
Under the conditions of 3000 rpm/min, flexible substrates are wrapped on grounded metal roller and collect the small liquid of EFI gained as receiver
Drop, forms grapheme conductive film.
2. the preparation method of grapheme conductive film according to claim 1, it is characterised in that the flexible substrates are 80 g
Double glue A4 paper.
3. the preparation method of grapheme conductive film according to claim 1, it is characterised in that the concentration of the hydrogen peroxide is
10 vol.%, the concentration of hydrochloric acid solution is 5 wt.%.
4. the preparation method of grapheme conductive film according to claim 1, it is characterised in that the high concentration completed to dialysis
Sodium chloride is added in graphene oxide, the mass concentration for controlling sodium chloride is 20%-50%.
5. grapheme conductive film made from any preparation method of claim 1 ~ 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711171612.7A CN107937995B (en) | 2017-11-22 | 2017-11-22 | Graphene conductive film and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711171612.7A CN107937995B (en) | 2017-11-22 | 2017-11-22 | Graphene conductive film and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN107937995A true CN107937995A (en) | 2018-04-20 |
| CN107937995B CN107937995B (en) | 2020-04-21 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711171612.7A Expired - Fee Related CN107937995B (en) | 2017-11-22 | 2017-11-22 | Graphene conductive film and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111006800A (en) * | 2019-12-23 | 2020-04-14 | 浙江清华柔性电子技术研究院 | Flexible pressure sensor and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102658108A (en) * | 2012-05-04 | 2012-09-12 | 东南大学 | Method for preparing photocatalytic filtering membrane based on graphene/semiconductor by an electrospinning method |
| CN103628182A (en) * | 2013-11-29 | 2014-03-12 | 东南大学 | Preparation method of carbon-based nano fiber |
| KR20150142950A (en) * | 2014-06-12 | 2015-12-23 | 한국과학기술원 | Film capable of self-healing for electrical conductivy using light, fabrication method for the same, and application for the same |
| CN105752967A (en) * | 2016-01-29 | 2016-07-13 | 白德旭 | Preparation method of graphene conducting film |
| CN106757522A (en) * | 2016-11-10 | 2017-05-31 | 过冬 | A kind of method of graphene oxide modified titanium dioxide nanofiber |
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2017
- 2017-11-22 CN CN201711171612.7A patent/CN107937995B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102658108A (en) * | 2012-05-04 | 2012-09-12 | 东南大学 | Method for preparing photocatalytic filtering membrane based on graphene/semiconductor by an electrospinning method |
| CN103628182A (en) * | 2013-11-29 | 2014-03-12 | 东南大学 | Preparation method of carbon-based nano fiber |
| KR20150142950A (en) * | 2014-06-12 | 2015-12-23 | 한국과학기술원 | Film capable of self-healing for electrical conductivy using light, fabrication method for the same, and application for the same |
| CN105752967A (en) * | 2016-01-29 | 2016-07-13 | 白德旭 | Preparation method of graphene conducting film |
| CN106757522A (en) * | 2016-11-10 | 2017-05-31 | 过冬 | A kind of method of graphene oxide modified titanium dioxide nanofiber |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111006800A (en) * | 2019-12-23 | 2020-04-14 | 浙江清华柔性电子技术研究院 | Flexible pressure sensor and preparation method thereof |
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