CN104183702A - Flexible conductive graphene film and manufacturing method and application thereof - Google Patents
Flexible conductive graphene film and manufacturing method and application thereof Download PDFInfo
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Abstract
The invention provides a flexible conductive graphene film and a manufacturing method and application thereof. The flexible conductive graphene film comprises a metal substrate and an insulation layer and a conductive layer sequentially stacked on the metal substrate. Material of the metal substrate is stainless steel metal or copper. Material of the insulation layer is metal oxide or nitride. Material of the conductive layer is hybrid material of graphene and metal particles, wherein the metal particles are gold, platinum, silver or copper particles. The flexible conductive graphene film has high conductivity and light transmittance and good thermal conductivity. The flexible conductive graphene film manufacturing method comprises steps: the insulation layer is manufactured on the metal substrate, the graphene oxide, the metal particles and cellulose are dispersed in an organic solvent to prepare a hybrid dispersion liquid, the hybrid dispersion liquid coats the insulation layer to manufacture the conductive layer, a chemical reduction method is adopted for reducing the conductive layer, and the flexible conductive graphene film is manufactured.
Description
Technical field
The present invention relates to a kind of conductive film, be specifically related to a kind of compliant conductive graphene film and its preparation method and application.
Background technology
In Organic Light Emitting Diode (OLED) device or organic solar batteries device, conventionally use tin indium oxide (ITO) conductive film as anode, this is because ITO conductive film has good electric conductivity and higher light transmittance.But also there is many problems that is difficult to overcome in ITO conductive film in the application of OLED.The indium compound price comparison costliness that for example ITO conductive film adopts, in addition, in the process of preparation ITO conductive film, various elements are as wayward in the doping ratio composition of indium (In) and tin (Sn), cause pattern, charge carrier and the transmission performance of ITO conductive film to be difficult to control, therefore conductivity is also relatively difficult to control.
Accordingly, many researchers have developed graphene conductive film, and the cellular lattice structure of bidimensional (2D) cycle that Graphene is made up of carbon hexatomic ring, has very high specific area and remarkable mechanical property, be one the thinnest in known materials, and be the most firm hard one; Graphene has good electric property, and electron mobility has at room temperature reached 15000cm
2/ V.S; The special two-dimensional structure of Graphene is given its perfect quantum tunneling effect and the series of properties such as flexible, in photoelectricity device, has a wide range of applications.
Preparing at present graphene film conventionally adopts chemical vapour deposition (CVD) or reduces and make with graphite oxide, while carrying out chemical vapour deposition (CVD), due to the restriction of deposition chamber dimension, be difficult to prepare large-area graphene film, and the technique of chemical vapour deposition (CVD) is too complicated, and equipment cost is high.And the method that adopts graphite oxide to reduce needs high temperature to reduce conventionally, also more complicated of the control of reduction process, in addition, flexible base, board can not bear high temperature conventionally, therefore generally can not adopt the method for high temperature reduction to prepare graphene conductive film.
Summary of the invention
For addressing the above problem, the invention provides a kind of compliant conductive graphene film and its preparation method and application.Compliant conductive graphene film provided by the invention has higher conductance and light transmittance, and thermal conductivity is good, can be used for preparing the electrode of solar cell device and the electrode of organic light emitting diode device; In addition, compliant conductive method for preparing graphene membrane provided by the invention, technique is simple, with low cost.
First aspect, the invention provides a kind of compliant conductive graphene film, comprise metal substrate and successively lamination be arranged on insulating barrier and the conductive layer on described metal substrate, wherein, the material of described metal substrate is stainless steel metal or copper, the material of described insulating barrier is metal oxide or nitride, and the material of described conductive layer is the composite material of Graphene and metallic particles, and described metallic particles is gold, platinum, silver or copper; Wherein, the thickness of described metal substrate is 20～100 μ m, and the thickness of described insulating barrier is 1～5 μ m, and the thickness of described conductive layer is 20～100 μ m.
Preferably, described metal oxide is silicon dioxide (SiO
2), described nitride is silicon nitride (Si
3n
4).
Preferably, in described composite material, the quality of described metallic particles is 0.2～0.5 times of described Graphene quality, and the size of described metallic particles is 20～100nm.
Described compliant conductive graphene film comprises insulating barrier and is attached to respectively the double-edged metal substrate of insulating barrier and conductive layer, the material of described insulating barrier is metal oxide or nitride, the material of described metal substrate is stainless steel metal or copper, the material of described conductive layer is the composite material of Graphene and metallic particles, and described metallic particles is gold (Au), platinum (Pt), silver (Ag) or copper (Cu); Compared with graphene conductive layer, the hybrid conductive layer of Graphene and metallic particles, due to the metal of the high conduction performance that adulterated, can not only keep the original transmitance of Graphene, can also improve conductance; Metal oxide or nitride be as insulating barrier, and this insulating barrier not only can protective substrate, in case substrate is destroyed in the making of subsequent conductive layer, also helps raising thermal conductivity; Therefore, compliant conductive graphene film provided by the invention has higher conductance and light transmittance, and thermal conductivity is good.
Second aspect, the invention provides a kind of preparation method of compliant conductive graphene film, comprises the steps:
S10, getting metal substrate, to be placed in vacuum degree be 1.0 × 10
-5～1.0 × 10
-3in the vacuum film coating chamber of Pa, prepare insulating barrier in the upper sputter of described metal substrate, obtain having the metal substrate of insulating barrier, the material of described metal substrate is stainless steel or copper, and the material of described insulating barrier is metal oxide or nitride;
S20, graphene oxide, metallic particles and cellulose are scattered in organic solvent, the mixed dispersion liquid that the concentration that is mixed with graphene oxide is 0.05g/L～0.5g/L, the mass ratio of described metallic particles, described cellulose and described Graphene is 0.2～0.5:0.2～0.1:1;
S30, the metal substrate described in getting with insulating barrier are placed in the container of 50～100 DEG C, and mixed dispersion liquid prepared by S20 is sprayed on described insulating barrier, then vacuumize 1～5 hour at 80～150 DEG C;
S40, repetition S30 step 1～3 time form conductive layer precursor on described insulating barrier;
S50, will infiltrate in reducing agent through S40 metal substrate after treatment, in the airtight condition of 100～250 DEG C, reduce 5～20 hours subsequently, and make described conductive layer precursor be reduced to conductive layer, make compliant conductive graphene film.
Preferably, the thickness of described metal substrate is 20～100 μ m, and the thickness of described insulating barrier is 1～5 μ m, and the thickness of described conductive layer is 20～100 μ m.
Preferably, in described step S10, described metal oxide is silicon dioxide, and described nitride is silicon nitride.
Preferably, in described step S20, the material of described metallic particles is gold, platinum, silver and copper, and the size of described metallic particles is 20～100nm; Described cellulose is CMC or hydroxyethylcellulose; Described organic solvent is acetonitrile, ethanol, methyl alcohol or N ' N '-dimethyl formamide solution.
Preferably, described mixed dispersion liquid prepared by S20 is sprayed in the operation on described insulating barrier: the width of spray tip is 0.1～1mm, the distance of nozzle and described insulating barrier is 5～20cm, and spray pressure is 0.5～5MPa, and nozzle translational speed is 0.5～2cm/s.
Preferably, in described step S50, described reducing agent is anhydrous diamine, hydrazine hydrate or dimethyl trap.
The preparation method of compliant conductive graphene film provided by the invention, by introduce cellulose in the time that S20 step is prepared Graphene mixed liquor, is conducive to improve the adhesion of Graphene to insulating barrier; In addition, adopt the method for electronation to carry out redox graphene, the method for conventional high-temperature reduction is simpler relatively, and it can not only avoid high temperature to destroy flexible base, board, can also be cost-saving.
The third aspect, the invention provides the application in solar cell device or organic light emitting diode device of compliant conductive graphene film as described in first aspect.
Preferably, described compliant conductive graphene film is applicable to prepare the electrode of solar cell device.
Preferably, described compliant conductive graphene film is applicable to be prepared with the electrode of OLED (OLED) electrical equipment.
The invention provides a kind of compliant conductive graphene film and its preparation method and application, its beneficial effect is:
(1) compliant conductive graphene film provided by the invention comprise metal substrate and successively lamination be arranged on insulating barrier and the conductive layer on metal substrate; Wherein, the material of described conductive layer is the composite material of Graphene and metallic particles, described metallic particles is gold, platinum, silver or copper, compared with graphene conductive layer, the hybrid conductive layer of Graphene and metallic particles, due to the metal of the high conduction performance that adulterated, can not only keep the original transmitance of Graphene, can also improve conductance; The material of described insulating barrier is metal oxide or nitride, the material of described metal substrate is stainless steel metal or copper, metal oxide or nitride are as insulating barrier, this insulating barrier not only can protective substrate, in case substrate is destroyed in the making of subsequent conductive layer, also help raising thermal conductivity; Therefore, compliant conductive graphene film provided by the invention has higher conductance and light transmittance, and thermal conductivity is good;
(2) preparation method of compliant conductive graphene film provided by the invention, by introduce cellulose in the time configuring Graphene mixed liquor, is conducive to improve the adhesion of Graphene to insulating barrier; In addition, use the method for electronation, the method for conventional high-temperature reduction is simpler relatively, and it can not only avoid high temperature to destroy flexible base, board, can also be cost-saving;
(3) compliant conductive graphene film preparation provided by the invention is simple, can, for the preparation of the electrode of solar cell device, also be applicable to prepare the electrode of OLED device.
Brief description of the drawings
Fig. 1 is the schematic diagram of compliant conductive method for preparing graphene membrane provided by the invention.
Fig. 2 is the structural representation of the solar cell device that makes of the embodiment of the present invention 5.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
A preparation method for compliant conductive graphene film, comprises the steps:
(1) getting thickness is that the stainless steel substrate of 20 μ m is placed in vacuum film coating chamber, and the vacuum degree that coating chamber is set is 1.0 × 10
-5pa, on described stainless steel substrate, SiO is prepared in sputter
2layer, thickness is 1 μ m, obtains having SiO
2the stainless steel substrate of layer;
(2) in ethanol, add graphene oxide, nanometer Ag particle and hydroxyethylcellulose, after being uniformly dispersed, be configured to the dispersion liquid of graphene oxide, wherein, the concentration of graphene oxide is 0.05g/L, nanometer Ag particle is of a size of 100nm, and its quality accounts for 20% of graphene oxide quality, and the concentration of hydroxyethylcellulose is 0.05g/L;
(3) get the above-mentioned SiO of having
2the stainless steel substrate of layer is placed in the container of 50 DEG C, subsequently by the above-mentioned dispersion liquid configuring by spray gun spraying on described insulating barrier, the spray tip width adopting is 0.1mm, spray pressure is 0.5MPa, nozzle and substrate distance are 5cm, nozzle translational speed is 2cm/s, after spraying, this stainless steel substrate is placed in to the vacuum drying chamber of 80 DEG C, dry 5 hours, then repeat spraying and dry, repeat after 3 times, this stainless steel substrate is infiltrated with anhydrous diamine, with being placed in airtight condition, reductase 12 0 hour at 100 DEG C, make compliant conductive graphene film P1, the graphene film thickness forming is 100 μ m.
Embodiment 2
A preparation method for compliant conductive graphene film, comprises the steps:
(1) getting thickness is that the stainless steel substrate of 100 μ m is placed in vacuum film coating chamber, and the vacuum degree that coating chamber is set is 1.0 × 10
-3pa, on described stainless steel substrate, Si is prepared in sputter
3n
4layer, thickness is 5 μ m, obtains having Si
3n
4the stainless steel substrate of layer;
(2) in methyl alcohol, add graphene oxide, nanometer Au particle and hydroxyethylcellulose, after being uniformly dispersed, be configured to the dispersion liquid of graphene oxide, wherein, the concentration of graphene oxide is 0.5g/L, nanometer Au particle is of a size of 20nm, and its quality accounts for 20% of graphene oxide quality, and the concentration of CMC is 0.01g/L;
(3) get the above-mentioned Si of having
3n
4the stainless steel substrate that the stainless steel substrate of layer is got above-mentioned processing is placed in the container of 100 DEG C, subsequently by the above-mentioned dispersion liquid configuring by spray gun spraying on described insulating barrier, the spray tip width adopting is 0.1mm, spray pressure is 5MPa, nozzle and substrate distance are 20cm, nozzle translational speed is 0.5cm/s, after spraying, this stainless steel substrate is placed in to the vacuum drying chamber of 150 DEG C, dry 1 hour, then repeat spraying and dry, repeat after 1 time, this stainless steel substrate is infiltrated with hydrazine hydrate, with being placed in airtight condition, at 250 DEG C, reduce 5 hours, make compliant conductive graphene film P2, the graphene film thickness forming is 20 μ m.
Embodiment 3
A preparation method for compliant conductive graphene film, comprises the steps:
(1) getting thickness is that the copper sheet substrate of 50 μ m is placed in vacuum film coating chamber, and the vacuum degree that coating chamber is set is 1.0 × 10
-4pa, on described stainless steel substrate, Si is prepared in sputter
3n
4layer, thickness is 3 μ m, obtains having Si
3n
4the stainless steel substrate of layer;
(2) in acetonitrile, add graphene oxide, nanometer Pt particle and hydroxyethylcellulose, after being uniformly dispersed, be configured to the dispersion liquid of graphene oxide, wherein, the concentration of graphene oxide is 0.2g/L, nanometer Pt particle is of a size of 50nm, and its quality accounts for 30% of graphene oxide quality, and the concentration of CMC is 0.05g/L;
(3) get the above-mentioned Si of having
3n
4the stainless steel substrate of layer is placed in the container of 80 DEG C, subsequently by the above-mentioned dispersion liquid configuring by spray gun spraying on described insulating barrier, the spray tip width adopting is 0.5mm, spray pressure is 2MPa, nozzle and substrate distance are 10cm, nozzle translational speed is 1cm/s, after spraying, this stainless steel substrate is placed in to the vacuum drying chamber of 100 DEG C, dry 3 hours, then repeat spraying and dry, repeat after 2 times, this stainless steel substrate is infiltrated with dimethyl trap, with being placed in airtight condition, at 200 DEG C, reduce 10 hours, make compliant conductive graphene film P3, the graphene film thickness forming is 65 μ m.
Embodiment 4
A preparation method for compliant conductive graphene film, comprises the steps:
(1) getting thickness is that the stainless steel substrate of 50 μ m is placed in vacuum film coating chamber, and the vacuum degree that coating chamber is set is 1.0 × 10
-4pa, evaporation SiO on described stainless steel substrate
2layer, thickness is 2 μ m, obtains having SiO
2the stainless steel substrate of layer;
(2) at N ', in N '-dimethyl formamide, add graphene oxide, nanometer Cu particle and hydroxyethylcellulose, after being uniformly dispersed, be configured to the dispersion liquid of graphene oxide, wherein, the concentration of graphene oxide is 0.1g/L, and nanometer Cu particle is of a size of 50nm, its quality accounts for 20% of graphene oxide quality, and the concentration of CMC is 0.05g/L;
(3) get the above-mentioned SiO of having
2the stainless steel substrate of layer is placed in the container of 100 DEG C, subsequently by the above-mentioned dispersion liquid configuring by spray gun spraying on described insulating barrier, the spray tip width adopting is 1mm, spray pressure is 3MPa, nozzle and substrate distance are 15cm, nozzle translational speed is 1cm/s, after spraying, this stainless steel substrate is placed in to the vacuum drying chamber of 150 DEG C, dry 5 hours, then repeat spraying and dry, repeat after 3 times, this stainless steel substrate is infiltrated with dimethyl trap, with being placed in airtight condition, at 200 DEG C, reduce 3 hours, make compliant conductive graphene film P4, the graphene film thickness forming is 85 μ m.
For the beneficial effect of valid certificates compliant conductive graphene film provided by the invention and preparation method thereof, the present invention also provides the performance data of compliant conductive graphene film P1～P4 that above-described embodiment 1 to 3 makes, comprises the surperficial square resistance of compliant conductive graphene film P1～P4 at 380～780nm.Result is as shown in table 1:
The surperficial square resistance of table 1. compliant conductive graphene film
| ? | Square resistance Ω/ |
| P1 | 168.2 |
| P2 | 158.3 |
| P3 | 135.4 |
| P4 | 145.9 |
Data from table can be found out, the minimum 135.4 Ω/ that reached of square resistance of the compliant conductive graphene film P1～P4 of the embodiment of the present invention 1 to 4 preparation, and the electrode that can meet OLED and solar cell is prepared requirement.
Embodiment 5
The compliant conductive graphene film P1 that the present embodiment provides taking the embodiment of the present invention 1 is anode conducting substrate, prepare a kind of solar cell device, this solar cell device comprises the anode conducting substrate that lamination arranges successively, auxiliary layer, active layer and cathode layer, wherein, anode conducting substrate comprises basalis and conductive layer, described basalis comprises polyimide layer and cyclohexanone layer, and described conductive layer is graphene layer.
Concrete preparation process is: taking compliant conductive graphene film P1 as anode conducting substrate, auxiliary layer is prepared in surperficial spin coating at described anode conducting substrate, the material of described auxiliary layer is poly-3, the mixture of 4-dioxy ethene thiophene (PEDOT) and polyphenyl sulfonate (PSS), wherein the mass ratio of PEDOT and PSS is 3:1, and the thickness of described auxiliary layer is 60nm; Then adopt spin coating technique on auxiliary layer, to prepare active layer, the material of described active layer is the mixture of P3HT and PC61BM, wherein the mass ratio of P3HT and PC61BM is 1:2, the thickness of described active layer is 100nm, on described active layer, prepare cathode layer by vacuum evaporation technology, the material of described cathode layer is Ag, and thickness is 100nm, obtains solar cell device.
Fig. 2 is the structural representation of the solar cell device prepared of the embodiment of the present invention.As shown in Figure 1, this solar cell device comprises the anode conducting substrate 1 that lamination arranges successively, auxiliary layer 2, active layer 3 and negative electrode 4, wherein, anode conducting substrate 1, for the compliant conductive graphene film P1 that the embodiment of the present invention 1 provides, comprises metal substrate 11, insulating barrier 12 and conductive layer 13.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Claims (10)
1. a compliant conductive graphene film, it is characterized in that, comprise metal substrate and successively lamination be arranged on insulating barrier and the conductive layer on described metal substrate, wherein, the material of described metal substrate is stainless steel metal or copper, the material of described insulating barrier is metal oxide or nitride, and the material of described conductive layer is the composite material of Graphene and metallic particles, and described metallic particles is gold, platinum, silver or copper;
The thickness of described metal substrate is 20～100 μ m, and the thickness of described insulating barrier is 1～5 μ m, and the thickness of described conductive layer is 20～100 μ m.
2. compliant conductive graphene film as claimed in claim 1, is characterized in that, described metal oxide is silicon dioxide, and described nitride is silicon nitride.
3. compliant conductive graphene film as claimed in claim 2, is characterized in that, in described composite material, the quality of described metallic particles is 0.2～0.5 times of described Graphene quality, and the size of described metallic particles is 20～100nm.
4. a preparation method for compliant conductive graphene film, is characterized in that, comprises the steps:
S10, getting metal substrate, to be placed in vacuum degree be 1.0 × 10
-5～1.0 × 10
-3in the vacuum film coating chamber of Pa, prepare insulating barrier in the upper sputter of described metal substrate, obtain having the metal substrate of insulating barrier, the material of described metal substrate is stainless steel or copper, and the material of described insulating barrier is metal oxide or nitride;
S20, graphene oxide, metallic particles and cellulose are scattered in organic solvent, the mixed dispersion liquid that the concentration that is mixed with graphene oxide is 0.05g/L～0.5g/L, the mass ratio of described metallic particles, described cellulose and described Graphene is 0.2～0.5:0.2～0.1:1;
S30, the metal substrate described in getting with insulating barrier are placed in the container of 50～100 DEG C, and mixed dispersion liquid prepared by S20 is sprayed on described insulating barrier, then vacuumize 1～5 hour at 80～150 DEG C;
S40, repetition S30 step 1～3 time form conductive layer precursor on described insulating barrier;
S50, will infiltrate in reducing agent through S40 metal substrate after treatment, in the airtight condition of 100～250 DEG C, reduce 5～20 hours subsequently, and make described conductive layer precursor be reduced to conductive layer, make compliant conductive graphene film.
5. the preparation method of compliant conductive graphene film as claimed in claim 3, is characterized in that, the thickness of described metal substrate is 20～100 μ m, and the thickness of described insulating barrier is 1～5 μ m, and the thickness of described conductive layer is 20～100 μ m.
6. the preparation method of compliant conductive graphene film as claimed in claim 3, is characterized in that, in described step S10, described metal oxide is silicon dioxide, and described nitride is silicon nitride.
7. the preparation method of compliant conductive graphene film as claimed in claim 3, is characterized in that, in described step S20, the material of described metallic particles is gold, platinum, silver and copper, and the size of described metallic particles is 20～100nm; Described cellulose is CMC or hydroxyethylcellulose; Described organic solvent is acetonitrile, ethanol, methyl alcohol or N ' N '-dimethyl formamide solution.
8. the preparation method of compliant conductive graphene film as claimed in claim 3, it is characterized in that, described mixed dispersion liquid prepared by S20 is sprayed in the operation on described insulating barrier: the width of spray tip is 0.1～1mm, the distance of nozzle and described insulating barrier is 5～20cm, spray pressure is 0.5～5MPa, and nozzle translational speed is 0.5～2cm/s.
9. the preparation method of compliant conductive graphene film as claimed in claim 3, is characterized in that, in described step S50, described reducing agent is anhydrous diamine, hydrazine hydrate or dimethyl trap.
As claimed in claim 1 compliant conductive graphene film in the application of preparing in solar cell device or organic light emitting diode device.
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