CN103839608A - Method for manufacturing conductive graphene film through ink-jet printing - Google Patents
Method for manufacturing conductive graphene film through ink-jet printing Download PDFInfo
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Abstract
The invention relates to a method for manufacturing a conductive film, in particular to a method for manufacturing a conductive graphene film through ink-jet printing. Graphite or graphite derivatives are used as raw materials and ultrasonically separated in dispersant/ ethyl alcohol/dimethylformamide solvent to prepare graphene dispersion solution, and supernatant liquid is taken through centrifugation, and graphene powder is obtained after the supernatant liquid undergoes flocculation; the graphene powder is prepared into printing ink, the printing ink is injected into an ink box, and the printing ink is deposited on a preprocessed substrate according to a preset pattern through the ink-jet printing technology; the conductive graphene film is formed through thermal treatment at 200 DEG C to 350 DEG C. According to the method, the graphene is prepared through the liquid phase separation method, and the conductive graphene film is manufactured through the ink-jet printing technology. The manufactured film can be patterned and is high in electric conductivity and good in mechanical property. Equipment used for ink-jet printing is simple, operation does need to be performed according to an original template, complex patterns are easy to make, cost is low, and the method is expected to be used for replacing existing complex film coating and photoetching technologies under certain conditions.
Description
Technical field
The present invention relates to a kind of method of preparing conductive film, particularly relate to a kind of method that inkjet printing is prepared graphene conductive film.
Background technology
Flexible electronic is that organic/inorganic materials electronic device is produced on to the emerging electronic technology on flexibility/Drawability plastics or thin metal matrix plate, with flexibility/ductility and efficient, the low cost fabrication technique of its uniqueness, there is wide application prospect in fields such as information, the energy, medical treatment, national defence, as flexible electronic displays, Organic Light Emitting Diode OLED, printing RFID, thin-film solar cell panel, electronics surface stickup etc.Micro-patterning process technology is to realize the necessary means of flexible electronic device and integrated processing thereof, and traditional electronic fabrication processes exists apparatus expensive, complex process, the problem such as big for environment pollution as photoetching, sputter etc.Adopt printing technology such as ink jet printing, intaglio printing, silk screen printing etc. can make flexible electronic device, comprise the circuit, photovoltaic cell, flexible display of electronic tag etc., can realize large area, low cost, flexibility.
Ink-jet printing technology is shown one's talent in numerous electronic manufacturing technologies based on ink processing, it is that digital picture is directly delivered on patterned media by relevant device, do not need primary template, in thin film deposition, can realize again the graphical of film, be easy to prepare complex pattern, and can pointwise control composition, can realize efficiently the patterning of conductive film on flexible and large area substrate and process, good to the compatibility of substrate; And the equipment that ink jet printing adopts is simple, easy and simple to handle, and cost is low, be expected under a stable condition for replacing plated film, the photoetching process of existing complexity.Currently reported ink-jet printing technology is for the preparation of transistor, solar cell, light-emitting diode and sensor, although obtained these progress, but the low-resistance metallic electrode that obtains high resolution design is also a urgent need to solve the problem, particularly in the Circuits System of Highgrade integration.
Graphene owing to thering is unusual electric conductivity, exceed the intensity of iron and steel decades of times, fabulous light transmission and chemical stability, be to be hopeful to be most applied in printed electronic device technology as metallization composition.The preparation method of Graphene has chemical vapour deposition technique, oxidation-reduction method (Hummers method), liquid phase stripping method etc.Redox graphene is used for OTFT electrode, temperature and chemical sensor etc. by currently reported employing ink jet printing method, but because redox graphene can not recover the electronic structure of Graphene completely, conductivity obviously declines, and performance is not fully up to expectations.And liquid phase stripping method has low cost of material, can preparation in macroscopic quantity, low energy consumption, purity is high, the advantage of low defect, the Graphene of preparing has obvious advantage in the application aspect of electronic device.
Summary of the invention
The object of the present invention is to provide a kind of inkjet printing to prepare the method for graphene conductive film, the method adopts liquid phase stripping method to prepare Graphene, farthest keep the intrinsic electronic structure of Graphene not to be destroyed, utilize the printing high accuracy feature of inkjet technology, figure and the composition of the rete of pointwise control simply and easily, make pattern precision higher, sharpness of border, be evenly distributed, without plated film and etching.
The object of the invention is to be achieved through the following technical solutions:
Inkjet printing is prepared a method for graphene conductive film, and described method comprises and is prepared as follows step:
1) getting graphite or graphite derivative joins in dispersant/ethanol/dimethyl formamide organic solvent;
2) step (1) gained dispersion liquid is obtained to monolayer or multi-layer graphene solution through high density ul-trasonic irradiation, after high speed centrifugation, get supernatant liquid, after flocculation treatment, obtain graphene powder;
3) step (2) gained graphene powder is distributed in organic solvent, is made into ink-jet ink;
4) the described ink of step (3) is injected in print cartridge, adopts conventional inkjet technology to deposit to by predetermined pattern on the substrate of anticipating;
5) by described in step (4), deposit to on-chip conductive film dry in baking oven after, after heat treatment form graphene conductive film.
Described a kind of inkjet printing is prepared the method for graphene conductive film, the weight ratio of described graphite raw material and solvent is 1~10: 100, dispersant used is ethyl cellulose (EC), or dodecyl sodium sulfate (SDS) or polyvinyl alcohol (PVA) or wooden sodium sulfonate (SLS) or DNA or polyvinylpyrrolidone (PVP) plasma type or nonionic or high-molecular type dispersing agent, addition is 0.1~5% of weight of solvent, and ethanol and dimethyl formamide are prepared by different proportion.Described a kind of inkjet printing is prepared the method for graphene conductive film, and described employing ultrasonic cell disintegration instrument carries out ultrasonic processing to graphite dispersing solution, power 20~500W, 30~120 minutes time, 0~10 ℃ of temperature; Centrifugal revolution 10000,30~120 minutes time; Flocculant is the NaCl aqueous solution, concentration 0.05g/mL, and addition is 30~60% of graphene dispersing solution volume.
Described a kind of inkjet printing is prepared the method for graphene conductive film, and described configuration printing ink solvent is alcohols, ester class and ketones solvent, and control solution viscosity is that 10~30mPas, surface tension are 20~50mNm-1.
Described a kind of inkjet printing is prepared the method for graphene conductive film, and described substrate is polyimides (PI), and PETG (PET), or other printable base material are cleaned and dried up before base material uses.
Described a kind of inkjet printing is prepared the method for graphene conductive film, described air atmosphere, heat treatment temperature 200-400 ℃, 15~60 minutes time.
Described a kind of inkjet printing is prepared the method for graphene conductive film, and described graphene conductive film resistance adopts the film resistor of RTS-8 type four point probe tester test graphene film, and this graphene conductive film resistance is at 0.02~0.003 Ω cm.
Advantage of the present invention and effect are:
1. the present invention utilizes the printing high accuracy feature of inkjet technology, and figure and the composition of the rete of pointwise control simply and easily, make pattern precision higher, and sharpness of border, is evenly distributed, without plated film and etching and other complex processes.
2. the present invention adopts liquid phase stripping method to prepare Graphene, can farthest keep the intrinsic electronic structure of Graphene not to be destroyed, and gives full play to the advantage of Graphene high conduction performance, is more conducive to be applied in field of electronic devices.
3. the present invention makes conductive ink by oneself, adapts to the little requirement of nozzle bore, can on multiple flexible parent metal, prepare the conductive film of pattern complexity; Cycle is short, and cost is low, and technique is simple, can be widely used in the preparation process of electronic device.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
Measure respectively ethanol 50ml dimethyl formamide 50ml and mix, add 1g ethyl cellulose, get 3g graphite and join in ethyl cellulose (EC)/ethanol/dimethyl formamide organic solvent; Ultrasonic processing 60 minutes, power 100W, 4~6 ℃ of temperature; High speed centrifugation 10000 turns, and 40 minutes, get supernatant liquid, add the 25ml NaCl aqueous solution (0.05g/ml) flocculation, after filtration, obtain graphene powder; Graphene powder is distributed in organic solvent (ratio of cyclohexanone and terpinol is 60:40), is made into ink-jet ink, adjusting viscosity 10mPas, surface tension are 30mNm
-1; Ink is injected in print cartridge, adopts conventional inkjet technology to deposit to by predetermined pattern on the PI substrate of anticipating; To deposit to on-chip conductive film dry in baking oven after, after 20 minutes, form graphene conductive film through 300 ℃ of heat treatments.
The graphene conductive film that obtains in embodiment is carried out to resistivity measurement, and film resistor is 0.01 Ω cm, has good conductivity.
Embodiment 2
Measure respectively ethanol 30ml dimethyl formamide 70ml and mix, add 2g ethyl cellulose, get 5g graphite and join in ethyl cellulose (EC)/ethanol/dimethyl formamide organic solvent; Ultrasonic processing 80 minutes, power 200W, 4~6 ℃ of temperature; High speed centrifugation 10000 turns, and 90 minutes, get supernatant liquid, add the 50ml NaCl aqueous solution (0.05g/ml) flocculation, after filtration, obtain graphene powder; Graphene powder is distributed in organic solvent (ratio of cyclohexanone and terpinol is 70:30), is made into ink-jet ink, adjusting viscosity 15mPas, surface tension are 35mNm
-1; Ink is injected in print cartridge, adopts conventional inkjet technology to deposit to by predetermined pattern on the PI substrate of anticipating; To deposit to on-chip conductive film dry in baking oven after, after 30 minutes, form graphene conductive film through 250 ℃ of heat treatments.
The graphene conductive film that obtains in embodiment is carried out to resistivity measurement, and film resistor is 0.008 Ω cm, has good conductivity.
Embodiment 3
Measure respectively ethanol 80ml dimethyl formamide 20ml and mix, add 1.5g ethyl cellulose, get 4g graphite and join in ethyl cellulose (EC)/ethanol/dimethyl formamide organic solvent; Ultrasonic processing 80 minutes, power 150W, 4~6 ℃ of temperature; High speed centrifugation 10000 turns, and 60 minutes, get supernatant liquid, add the 40ml NaCl aqueous solution (0.05g/ml) flocculation, after filtration, obtain graphene powder; Graphene powder is distributed in organic solvent (ratio of cyclohexanone and terpinol is 85:15), is made into ink-jet ink, adjusting viscosity 12mPas, surface tension are 30mNm
-1; Ink is injected in print cartridge, adopts conventional inkjet technology to deposit to by predetermined pattern on the PET substrate of anticipating; To deposit to on-chip conductive film dry in baking oven after, after 30 minutes, form graphene conductive film through 200 ℃ of heat treatments.
The graphene conductive film that obtains in embodiment is carried out to resistivity measurement, and film resistor is 0.007 Ω cm, has good conductivity.
The above embodiment has only expressed several execution mode of the present invention, and it describes comparatively in detail concrete, but and can therefore be interpreted as the restriction to the scope of the claims of the present invention.Everyly do not depart from the present invention and conceive distortion and the improvement made, all belong to protection scope of the present invention.
Claims (7)
1. inkjet printing is prepared a method for graphene conductive film, it is characterized in that, described method comprises and is prepared as follows step:
1) getting graphite or graphite derivative joins in dispersant/ethanol/dimethyl formamide organic solvent;
2) step (1) gained dispersion liquid is obtained to monolayer or multi-layer graphene solution through high density ul-trasonic irradiation, after high speed centrifugation, get supernatant liquid, after flocculation treatment, obtain graphene powder;
3) step (2) gained graphene powder is distributed in organic solvent, is made into ink-jet ink;
4) the described ink of step (3) is injected in print cartridge, adopts conventional inkjet technology to deposit to by predetermined pattern on the substrate of anticipating;
5) by described in step (4), deposit to on-chip conductive film dry in baking oven after, after heat treatment form graphene conductive film.
2. a kind of inkjet printing according to claim 1 is prepared the method for graphene conductive film, it is characterized in that, the weight ratio of described graphite raw material and solvent is 1~10: 100, dispersant used is ethyl cellulose (EC), or dodecyl sodium sulfate (SDS) or polyvinyl alcohol (PVA) or wooden sodium sulfonate (SLS) or DNA or polyvinylpyrrolidone (PVP) plasma type or nonionic or high-molecular type dispersing agent, addition is 0.1~5% of weight of solvent, and ethanol and dimethyl formamide are prepared by different proportion.
3. a kind of inkjet printing according to claim 1 is prepared the method for graphene conductive film, it is characterized in that, described employing ultrasonic cell disintegration instrument carries out ultrasonic processing to graphite dispersing solution, power 20~500W, 30~120 minutes time, 0~10 ℃ of temperature; Centrifugal revolution 10000,30~120 minutes time; Flocculant is the NaCl aqueous solution, concentration 0.05g/mL, and addition is 30~60% of graphene dispersing solution volume.
4. a kind of inkjet printing according to claim 1 is prepared the method for graphene conductive film, it is characterized in that, described configuration printing ink solvent is alcohols, ester class and ketones solvent, and control solution viscosity is that 10~30mPas, surface tension are 20~50mNm
-1.
5. a kind of inkjet printing according to claim 1 is prepared the method for graphene conductive film, it is characterized in that, described substrate is polyimides (PI), and PETG (PET), or other printable base material are cleaned and dried up before base material uses.
6. a kind of inkjet printing according to claim 1 is prepared the method for graphene conductive film, it is characterized in that described air atmosphere, heat treatment temperature 200-400 ℃, 15~60 minutes time.
7. a kind of inkjet printing according to claim 1 is prepared the method for graphene conductive film, it is characterized in that, described graphene conductive film resistance adopts the film resistor of RTS-8 type four point probe tester test graphene film, and this graphene conductive film resistance is at 0.02~0.003 Ω cm.
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