CN104183699A - Flexible transparent conductive graphene film, preparation method thereof and application - Google Patents
Flexible transparent conductive graphene film, preparation method thereof and application Download PDFInfo
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Abstract
The invention provides a flexible transparent conductive graphene film, a preparation method thereof and application. The flexible transparent conductive graphene film comprises a graphene layer and a polyimides layer arranged on the grapheme layer. The conductive graphene film has high conductivity and light transmittance and good deflection. The preparation method of the flexible transparent conductive graphene film comprises: preparing a mold lubricant layer on a clean glass substrate through a method of electron beam evaporation, wherein the material of the mold lubricant layer is water-soluble halogen salt; then depositing the graphene layer on the mold lubricant layer through the method of vapour deposition; and then getting pyromellitic dianhydride(PMDA) and 4,4'-diaminodiphenyl ether with an evaporation velocity ratio 1:0.8-1.2 for co-evaporation in a vacuum plating chamber, forming the polyimides layer on the graphene layer; then dissolving the mold lubricant layer using water of 50-100 DEG C, enabling the graphene layer to disengage from the glass substrate, to prepare the flexible transparent conductive graphene film.
Description
Technical field
The present invention relates to a kind of conductive film, be specifically related to a kind of flexible and transparent conductive graphene membrane and its preparation method and application.
Background technology
In Organic Light Emitting Diode (OLED) device or solar cell 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.
At present, the application of flexible OLED and flexible solar battery is very extensive, but the graphene film of preparation at present, obtain higher conductance, conventionally need to adopt the preparation of the method such as chemical vapor deposition (CVD) and high-temperature oxydation film forming, these methods all require substrate can bear the temperature above up to 800 DEG C, for flexible electrode, conventionally thin polymer film all can not bear such temperature, and therefore developing flexible graphite alkene conductive film becomes the previous problem to be solved of order.
Summary of the invention
For addressing the above problem, the invention provides a kind of flexible and transparent conductive graphene membrane, this flexible and transparent conductive graphene membrane comprises graphene layer and is arranged on the polyimide layer on graphene layer, have higher conductance and light transmittance, and pliability is good.The present invention also provides the preparation method of this flexible and transparent conductive graphene membrane, and the method can be avoided directly on the thin polymer film substrate of non-refractory, preparing graphene layer and destroy substrate.In addition, the present invention also provides the application of this flexible and transparent conductive graphene membrane in solar cell device or organic light emitting diode device.
First aspect, the invention provides a kind of flexible and transparent conductive graphene membrane, described flexible and transparent conductive graphene membrane comprises graphene layer and is arranged on the polyimide layer on graphene layer, wherein, the thickness of described graphene layer is 100～2000nm, and the thickness of described polyimide layer is 500～1000nm.
Described flexible and transparent conductive graphene membrane comprises polyimide layer and graphene layer, and described polyimide layer is as substrate, and compared with glass substrate, the pliability of polyimide substrate is better; Described graphene layer is conductive layer, and Graphene not only has good electric property and transmitance, also has remarkable mechanical property, easily forms resistant to bending electrically conductive layer; Therefore, flexible and transparent conductive graphene membrane provided by the invention has higher conductance and transmitance, and pliability is good.
Second aspect, the invention provides a kind of preparation method of flexible and transparent conductive graphene membrane, comprises the steps:
S10, get clean glass substrate, adopt the method for electron beam evaporation to prepare releasing agent layer on described clean glass substrate, the material of described releasing agent layer is water-soluble halogen;
S20, will be placed in vapor deposition chamber through S10 glass substrate after treatment, pass into gaseous carbon source, the pressure maintaining in settling chamber is 10～1000Pa, at 600～1000 DEG C, on described releasing agent layer, deposit graphene layer, obtain having the glass substrate of graphene layer and parting-agent layer;
S30, S20 gained glass substrate is placed in to vacuum film coating chamber, it is 1.0 × 10 that indoor vacuum degree is set
-5pa～1.0 × 10
-3pa, gets pyromellitic acid anhydride and 4, and 4 '-diaminodiphenyl ether carries out common evaporation with the evaporation rate ratio of 1:0.8～1.2, makes to form on described graphene layer polyamic acid layer;
S40, will be placed in the vacuum heater of 180～300 DEG C through S30 glass substrate after treatment, processed 1～5 hour, makes described polyamic acid pull-up water form polyimide layer;
S50, will be placed in the water of 50～100 DEG C through S40 glass substrate after treatment, dissolve described releasing agent layer, described graphene layer is departed from from glass substrate, make flexible and transparent conductive graphene membrane, described flexible and transparent conductive graphene membrane comprises graphene layer and is arranged on the polyimide layer on graphene layer.
Preferably, the energy density of described electron beam evaporation is 10～100W/cm
2, evaporation rate is 0.1～1nm/s.
Preferably, the thickness of described parting-agent layer is 50～2000nm.
Preferably, in described step S10, described water-soluble halogen is sodium chloride, potassium chloride or magnesium chloride.
Preferably, in described step S20, described gaseous carbon source is one or more in methane, ethane and propane.
Preferably, the thickness of described graphene layer is 100～2000nm.
Preferably, the thickness of described polyimide layer is 500～1000nm.
The preparation method of flexible and transparent conductive graphene membrane provided by the invention is by introducing releasing agent layer, can avoid directly on the thin polymer film substrate of non-refractory, preparing graphene layer, thereby solve conventional high-temperature preparation and can damage the problem containing thin polymer film substrate, in addition, the material of the releasing agent layer of introducing in this method is halogen soluble in water, draw materials very simple, wherein, the also very environmental protection of process that graphene layer departs from from glass substrate.
The third aspect, the invention provides the application of a kind of flexible and transparent conductive graphene membrane as described in first aspect in solar cell device or organic light emitting diode device.
Preferably, described flexible and transparent conductive graphene membrane is applicable to prepare the electrode of solar cell device.
Preferably, described flexible and transparent conductive graphene membrane is applicable to be prepared with the electrode of OLED (OLED) electrical equipment, is particularly useful for the electrode of the OLED device of preparation top transmitting.
The invention provides a kind of flexible and transparent conductive graphene membrane and its preparation method and application, its beneficial effect is:
(1) flexible and transparent conductive graphene membrane provided by the invention comprises polyimide layer and graphene layer, and described polyimide layer is as substrate, and compared with glass substrate, the pliability of polyimide substrate is better; Described graphene layer is the conductive layer of film, and Graphene not only has good electric property and transmitance, also has remarkable mechanical property, easily forms resistant to bending electrically conductive layer; Therefore, flexible and transparent conductive graphene membrane provided by the invention has higher conductance and transmitance, and pliability is good;
(2) preparation method of flexible and transparent conductive graphene membrane provided by the invention is by introducing releasing agent layer, can avoid directly on the thin polymer film substrate of non-refractory, preparing graphene layer, can damage the problem containing thin polymer film substrate thereby solved conventional high-temperature preparation;
(3) in the preparation method of flexible and transparent conductive graphene membrane provided by the invention, the material of described releasing agent layer is halogen soluble in water, just can be dissolved and remove parting-agent layer by simple water treatment, this releasing agent layer is drawn materials simply, the comparatively environmental protection of the process of this dissolving parting-agent layer;
(4) flexible and transparent conductive graphene membrane 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, is particularly useful for the OLED device of preparation top transmitting.
Brief description of the drawings
Fig. 1 is the structural representation of the solar cell device that makes of the embodiment of the present invention 4.
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 flexible and transparent conductive graphene membrane, comprises the steps:
(1) getting glass substrate after cleaning, to be placed in vacuum degree be 1.0 × 10
-5in the vacuum film coating chamber of Pa, adopt the method for electron beam evaporation plating, on described glass substrate, prepare releasing agent layer, the material of remover is sodium chloride, and electron beam energy density is 10W/cm
2, evaporation rate is 0.1nm/s, the thickness that forms sodium chloride is 50nm; This glass substrate is transferred in vapor deposition chamber, and the temperature that settling chamber is set is 600 DEG C, passes into methane, deposits graphene layer on releasing agent layer, and the thickness of graphene layer is 100nm, makes the glass substrate with releasing agent layer and graphene layer;
(2) glass substrate with releasing agent layer and graphene layer is placed in to vacuum film coating chamber, then PMDA and two kinds of monomer materials of ODA is placed in respectively to two crucibles of vacuum film coating chamber, the vacuum degree that coating chamber is set is 1.0 × 10
-5pa, controls temperature, make PMDA and ODA with the speed of 1:0.8 than coevaporation and on graphene layer polymerization form polyamic acid layer, the thickness of polyamic acid layer is 1000nm;
(3) then the glass substrate that is prepared with polyamic acid layer is transferred in vacuum heater, be heated to 300 DEG C, processed 1 hour, polyamic acid pull-up water is formed after polyimide layer, transfer to temperature and be in the water of 100 DEG C, dissolve releasing agent layer, from glass substrate departs from, obtain flexible and transparent conductive graphene membrane P1 until graphene layer; Flexible and transparent conductive graphene membrane P1 is taken out and is dried from water.
Embodiment 2
A preparation method for flexible and transparent conductive graphene membrane, comprises the steps:
(1) getting glass substrate after cleaning, to be placed in vacuum degree be 1.0 × 10
-3in the vacuum film coating chamber of Pa, adopt the method for electron beam evaporation plating, on described glass substrate, prepare releasing agent layer, the material of remover is potassium chloride, and electron beam energy density is 100W/cm
2, evaporation rate is 1nm/s, the thickness that forms potassium chloride is 2000nm; This glass substrate is transferred in vapor deposition chamber, and the temperature that settling chamber is set is 1000 DEG C, passes into ethane, deposits graphene layer on releasing agent layer, and the thickness of graphene layer is 2000nm, makes the glass substrate with releasing agent layer and graphene layer;
(2) glass substrate with releasing agent layer and graphene layer is placed in to vacuum film coating chamber, then PMDA and two kinds of monomer materials of ODA is placed in respectively to two crucibles of vacuum film coating chamber, the vacuum degree that coating chamber is set is 1.0 × 10
-3pa, controls temperature, makes PMDA and ODA be total to and on graphene layer, form polyamic acid layer than evaporation with the speed of 1:1.2, and the thickness of polyamic acid layer is 500nm;
(3) then the glass substrate that is prepared with polyamic acid layer is transferred in vacuum heater, be heated to 180 DEG C, processed 5 hours, polyamic acid pull-up water is formed after polyimide layer, transfer to temperature and be in the water of 50 DEG C, dissolve releasing agent layer, from glass substrate departs from, obtain flexible and transparent conductive graphene membrane P2 until graphene layer; Flexible and transparent conductive graphene membrane P2 is taken out and is dried from water.
Embodiment 3
A preparation method for flexible and transparent conductive graphene membrane, comprises the steps:
(1) getting glass substrate after cleaning, to be placed in vacuum degree be 1.0 × 10
-4in the vacuum film coating chamber of Pa, adopt the method for electron beam evaporation plating, on described glass substrate, prepare releasing agent layer, the material of remover is magnesium chloride, and electron beam energy density is 50W/cm
2, evaporation rate is 0.5nm/s, the thickness that forms magnesium chloride is 1000nm; This glass substrate is transferred in vapor deposition chamber, and the temperature that settling chamber is set is 800 DEG C, passes into propane, deposits graphene layer on releasing agent layer, and the thickness of graphene layer is 1000nm, makes the glass substrate with releasing agent layer and graphene layer;
(2) glass substrate with releasing agent layer and graphene layer is placed in to vacuum film coating chamber, then PMDA and two kinds of monomer materials of ODA is placed in respectively to two crucibles of vacuum film coating chamber, the vacuum degree that coating chamber is set is 1.0 × 10
-4pa, controls temperature, makes PMDA and the ODA speed ratio coevaporation with 1:1, forms polyamic acid layer on graphene layer, and the thickness of polyamic acid layer is 800nm;
(3) then the glass substrate that is prepared with polyamic acid layer is transferred in vacuum heater, be heated to 250 DEG C, processed 2 hours, polyamic acid pull-up water is formed after polyimide layer, transfer to temperature and be in the water of 80 DEG C, dissolve releasing agent layer, from glass substrate departs from, obtain flexible and transparent conductive graphene membrane P3 until graphene layer; Flexible and transparent conductive graphene membrane P3 is taken out and is dried from water.
For the beneficial effect of valid certificates flexible and transparent conductive graphene membrane provided by the invention and preparation method thereof, the present invention also provides the performance data of the flexible and transparent conductive graphene membrane that above-described embodiment 1 to 3 makes, and comprises the square resistance of flexible and transparent conductive graphene membrane P1～P3 on the transmitance of 380～780nm and surface thereof.Result is as shown in table 1:
The performance data of table 1. flexible and transparent conductive graphene membrane
| ? | Transmitance | Square resistance Ω/ |
| P1 | 72.6% | 89.7 |
| P2 | 70.2% | 121.6 |
| P3 | 74.8% | 75.8 |
Data from table can be found out, the transmitance of the flexible and transparent conductive graphene membrane P1～P3 of the embodiment of the present invention 1 to 3 preparation in visible-range all exceeded 70%, substantially meet the requirement to transmitance in OLED application, and can be for the preparation of the OLED device of top transmitting; The minimum 75.8 Ω/ that reached of square resistance of flexible and transparent conductive graphene membrane provided by the invention, the electrode that can meet OLED and solar cell is prepared requirement.
Embodiment 4
The flexible and transparent conductive graphene membrane 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 polyimide layer and graphene layer.
Concrete preparation process is: taking flexible and transparent conductive graphene membrane P1 as anode conducting substrate, surface-coated at described anode conducting substrate is prepared auxiliary layer, 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 to prepare active layer on described auxiliary 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. 1 is the structural representation of the solar cell device prepared of the embodiment of the present invention 4.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 is the flexible and transparent conductive graphene membrane P1 that the embodiment of the present invention 1 provides, and comprises polyimide layer 11 and graphene layer 12.
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 (9)
1. a flexible and transparent conductive graphene membrane, is characterized in that, comprises graphene layer and is arranged on the polyimide layer on graphene layer, and wherein, the thickness of described graphene layer is 100～2000nm, and the thickness of described polyimide layer is 500～1000nm.
2. a preparation method for flexible and transparent conductive graphene membrane, is characterized in that, comprises the steps:
S10, get clean glass substrate, adopt the method for electron beam evaporation to prepare releasing agent layer on described clean glass substrate, the material of described releasing agent layer is water-soluble halogen;
S20, will be placed in vapor deposition chamber through S10 glass substrate after treatment, pass into gaseous carbon source, the pressure maintaining in settling chamber is 10～1000Pa, at 600～1000 DEG C, on described releasing agent layer, deposit graphene layer, obtain having the glass substrate of graphene layer and parting-agent layer;
S30, S20 gained glass substrate is placed in to vacuum film coating chamber, it is 1.0 × 10 that indoor vacuum degree is set
-5pa～1.0 × 10
-3pa, gets pyromellitic acid anhydride and 4, and 4 '-diaminodiphenyl ether carries out common evaporation with the evaporation rate ratio of 1:0.8～1.2, makes to form on described graphene layer polyamic acid layer;
S40, will be placed in the vacuum heater of 180～300 DEG C through S30 glass substrate after treatment, processed 1～5 hour, makes described polyamic acid pull-up water form polyimide layer;
S50, will be placed in the water of 50～100 DEG C through S40 glass substrate after treatment, dissolve described releasing agent layer, described graphene layer is departed from from glass substrate, make flexible and transparent conductive graphene membrane, described flexible and transparent conductive graphene membrane comprises graphene layer and is arranged on the polyimide layer on graphene layer.
3. the preparation method of flexible and transparent conductive graphene membrane as claimed in claim 2, is characterized in that, the energy density of described electron beam evaporation is 10～100W/cm
2, evaporation rate is 0.1～1nm/s.
4. the preparation method of flexible and transparent conductive graphene membrane as claimed in claim 2, is characterized in that, the thickness of described parting-agent layer is 50～2000nm.
5. the preparation method of flexible and transparent conductive graphene membrane as claimed in claim 2, is characterized in that, in described step S10, described water-soluble halogen is sodium chloride, potassium chloride or magnesium chloride.
6. the preparation method of flexible and transparent conductive graphene membrane as claimed in claim 2, is characterized in that, in described step S20, described gaseous carbon source is one or more in methane, ethane and propane.
7. the preparation method of flexible and transparent conductive graphene membrane as claimed in claim 2, is characterized in that, the thickness of described graphene layer is 100～2000nm.
8. the preparation method of flexible and transparent conductive graphene membrane as claimed in claim 2, is characterized in that, the thickness of described polyimide layer is 500～1000nm.
9. the application of flexible and transparent conductive graphene membrane as claimed in claim 1 in solar cell device or organic light emitting diode device.
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Application publication date: 20141203 |