CN102180463A - Method for reducing sheet resistance of graphene thin film - Google Patents
Method for reducing sheet resistance of graphene thin film Download PDFInfo
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- CN102180463A CN102180463A CN2011100417660A CN201110041766A CN102180463A CN 102180463 A CN102180463 A CN 102180463A CN 2011100417660 A CN2011100417660 A CN 2011100417660A CN 201110041766 A CN201110041766 A CN 201110041766A CN 102180463 A CN102180463 A CN 102180463A
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Abstract
The invention relates to a method for reducing sheet resistance of a graphene thin film, comprising the following step of soaking the graphene thin film and a substrate in a solution with an electron or hole donation capability for a certain time, wherein the solution in the step is one or mixed solution with an electron donation capability of low-valence solutions of heavy metal inorganic acid, organic alcohol and organic amine; or the solution in the step is one or mixed solution with a hole donation capability of a nonmetal inorganic acid solution and an organic alkane solution. The invention has the beneficial effects that: after the graphene thin film arranged on the substrate is soaked in a solution with the electron donation capability, the solution captures holes in the graphene thin film, thus the consistency of electrons in the graphene thin film is increased, and the sheet resistance of the graphene thin film is reduced.
Description
Technical field
The invention belongs to the electrode materials technical field, relate in particular to the graphene film technical field.
Background technology
Current, ITO (tin indium oxide), IZO (indium-zinc oxide) are modal inorganic, metal oxide membrane electrodes, yet scarcity day by day along with rare metal, price goes up day by day, and its fragility characteristics have further limited their large-scale application at photoelectricity, lighting field, particularly in the flexible electronic device field.So cost of development is cheap, abundant raw materials, stable high, flexible good conductive film is extremely urgent.
The Graphene (Graphene) that Univ Manchester UK's peace strong K sea nurse of moral (Andre K.Geim) etc. were found in 2004 is a kind of carbonaceous novel material by the tightly packed one-tenth bi-dimensional cellular of monolayer carbon atom shape structure.Theoretical investigation is found: Graphene has 200,000cm
2The mobility of/Vs, its electroconductibility can be compared with metallic copper, and optical transmittance can reach 97.7%, and far above conductive film, Graphene has high flexibility simultaneously.Under 6% strain, the resistance of Graphene side can not change, and under the similarity condition, ITO is just broken under 4% strain.Therefore, adopt graphene film, not only have the characteristic of low square resistance, but also have high optical transmittance, the advantage of high flexibility as conductive electrode.
Yet the precondition that realizes these potential application is to want to prepare on a large scale the graphene film of low cost, low square resistance.At present, the preparation method of graphene film mainly contains micromechanics and peels off method, liquid chemical method, SiC (silicon carbide) epitaxial graphite alkene membrane process, chemical vapor deposition (CVD) method etc.Not only area is little wherein to peel off method acquisition Graphene by micromechanics, and output is few, does not have industrial use value.Liquid chemical method is that the employing natural graphite is a raw material, by in the environment of strong acid, strong oxidizer Graphite Powder 99 oxidation, expansion being formed oxidized graphite flake, under reducing environment oxidized graphite flake is reduced into Graphene again; Though it is little to obtain the graphene film area by this method, output is big, can be by spin coating, and technology such as printing form graphene film on substrate.SiC epitaxial graphite alkene membrane process is to remove Si under hot conditions, makes the C on surface form graphene film.The CVD method is under hot conditions, and carbon source is fed in the CVD system, utilizes the catalytic of metal, and the catalytic decomposition carbon source forms graphene film on metal, adopts existing transfer techniques to obtain the big area graphene film.
Yet it is bigger to obtain its side's resistance of graphene film by liquid chemical method, SiC epitaxial graphite alkene membrane process, CVD method.Graphene film side's resistance that liquid chemical method obtains is about 5K Ω, and SiC epitaxial graphite alkene film side hinders about 10K Ω.And hinder about 1K Ω by the single-layer graphene film side that the CVD method obtains.After the graphene film stack multilayer that the CVD method obtains, can effectively reduce side's resistance of graphene film, but the stack multiwalled simultaneously, the optical transmittance of graphene film is also reducing.After four layers of the graphene film stacks that the CVD method obtains, its side resistance is also about 300 Ω, but this moment four layer graphene films optical transmittance be lower than 90%, be difficult to use in the technique of display field.How to obtain low square resistance, and the graphene film of keeping high optical transmittance becomes the technical bottleneck that Graphene is used for industrial circle.
Summary of the invention
The objective of the invention is therefore to have proposed a kind of method that reduces the resistance of graphene film side in order under the prerequisite that keeps the graphene film high-transmission rate, effectively to reduce side's resistance of graphene film.
To achieve these goals, technical scheme of the present invention is: a kind of method that reduces graphene film side resistance comprises the steps: graphene film and substrate be soaked in and has certain hour in the solution that gives electronics or give the hole ability.
Solution is the mixed solution of the acid of heavy metal mineral-type, organic alcohols and organic amine solution or aforementioned solution with low price of the electronic capability of giving in the above-mentioned steps.
The above-mentioned heavy metal mineral-type acid of stating the low price with the electronic capability of giving is hydrochloro-auric acid or Platinic chloride.
Above-mentioned organic alcohols with the electronic capability of giving is methyl alcohol or ethanol.
Above-mentioned organic amine with the electronic capability of giving is quadrol or N, the N dimethyl formamide.
Solution is to have the solution that gives the nonmetal inorganic acids of hole ability, organic alkanes or the mixed solution of aforementioned solution in the above-mentioned steps.
It is above-mentioned that to have the nonmetal inorganic acids that gives the hole ability be hydrochloric acid or nitric acid.
It is above-mentioned that to have the organic alkanes that gives the hole ability be Nitromethane 99Min. or nitroethane.
The invention has the beneficial effects as follows: after will being arranged in on-chip graphene film and being soaked in solution with the electronic capability of giving, this solution has been captured the hole in the graphene film, make the electron density in the graphene film increase, thereby make side's resistance of graphene film reduce.To be arranged in on-chip graphene film and be soaked in and have the solution that gives the hole ability, this solution is captured the electronics in the graphene film, makes that the hole concentration in the graphene film increases, thereby makes side's resistance of graphene film reduce.The graphene film owing to do not superpose in this process, the transmission change of the graphene film after therefore handling is also little.After adopting method of the present invention that Graphene is carried out surface treatment, can make the side resistance of graphene film reduce about 30～80%, and optical transmittance keeps suitable with the photoelectric properties of commercial ito thin film more than 90%, can be widely used in the technique of display field.
Embodiment
The invention will be further described below in conjunction with specific embodiment, but the present invention is not limited to embodiment.
Embodiment 1: a kind of method that reduces the resistance of graphene film side, and its concrete steps are as follows:
Step 1: preparation graphene film: in the chemical vapor deposition chamber body that is placed with 5 centimetres of metal copper foils of 5 cm x, feed 100Pa hydrogen, be warming up to 1000 ℃, kept 20 minutes, feed the methane of 100Pa again, kept 20 minutes, reduce to room temperature with 50 ℃/minute speed then, obtain to be positioned at the graphene film on the metal copper foil.
Step 2: graphene film is placed on the substrate: spin coating electronics etching glue on the product of step 1,100 nanometers, in the iron nitrate aqueous solution of 30% massfraction, corrode, be corroded fully until metal copper foil, salvage and in deionized water, clean twice, with PET (Polyethylene Terephthalate, polyethylene terephthalate) substrate is salvaged, toasted 10 minutes down in 60 ℃, then toasted 5 minutes down at 120 ℃, be soaked in the acetone, remove the electronics etching glue on graphene film surface, obtain to be positioned at the graphene film of the 5 centimetres of sizes of 5 cm x on the PET.The transmissivity that be positioned at the on-chip graphene film of PET this moment reaches 96.9%, and side's resistance of graphene film is 1000 Ω;
Step 3: graphene film and substrate are soaked in certain hour in the hydrochloric acid soln: the product of step 2 is soaked in the hydrochloric acid of 36% massfraction, after 30 minutes, take out, clean, obtain being positioned at the graphene film of on-chip high optical transmittance of PET and low square resistance with deionized water.This graphene film, transmissivity reaches 96.7% at visible region, and side's resistance of graphene film is 90 Ω.
Hydrochloric acid can replace with nonmetal inorganic acids such as nitric acid in the present embodiment.
Embodiment 2: a kind of method that reduces the resistance of graphene film side, and its concrete steps are as follows:
Step 1: preparation graphene film: in the chemical vapor deposition chamber body that is placed with 5 centimetres of metal copper foils of 5 cm x, feed 100Pa hydrogen, be warming up to 1000 ℃, kept 20 minutes, feed the methane of 100Pa again, kept 20 minutes, reduce to room temperature with 50 ℃/minute speed then, obtain to be positioned at the graphene film on the metal copper foil.
Step 2: graphene film is placed on the substrate: spin coating electronics etching glue on the product of step 1,100 nanometers, in the iron nitrate aqueous solution of 30% massfraction, corrode, be corroded fully until metal copper foil, salvage and in deionized water, clean twice, with PET (Polyethylene Terephthalate, polyethylene terephthalate) substrate is salvaged, toasted 10 minutes down in 60 ℃, then toasted 5 minutes down at 120 ℃, be soaked in the acetone, remove the electronics etching glue on graphene film surface, obtain to be positioned at the graphene film of the 5 centimetres of sizes of 5 cm x on the PET.The transmissivity that be positioned at the on-chip graphene film of PET this moment reaches 96.9%, and side's resistance of graphene film is 1000 Ω;
Step 3: graphene film and substrate are soaked in N, certain hour in the N dimethyl formamide solution: the N that the product of step 2 is soaked in 100% massfraction, in the N dimethyl formamide, after 30 minutes, take out, clean with deionized water, obtain being positioned at the graphene film of on-chip high optical transmittance of PET and low square resistance.
Step 4: repeating step 2 and step 3 twice obtain to be positioned at the on-chip three layer graphene films of PET
Obtain to be positioned at the on-chip graphene film of PET by this method, transmissivity reaches 93% at visible region, and side's resistance of graphene film is 10 Ω.
N in the present embodiment, the N dimethyl formamide can replace with organic amines such as quadrol.
Embodiment 3: a kind of method that reduces the resistance of graphene film side, and its concrete steps are as follows:
Step 1: preparation graphene film: in the chemical vapor deposition chamber body that is placed with 5 centimetres of metal copper foils of 5 cm x, feed 100Pa hydrogen, be warming up to 1000 ℃, kept 20 minutes, feed the methane of 100Pa again, kept 20 minutes, reduce to room temperature with 50 ℃/minute speed then, obtain to be positioned at the graphene film on the metal copper foil.
Step 2: graphene film is placed on the substrate: spin coating electronics etching glue on the product of step 1,100 nanometers, in the iron nitrate aqueous solution of 30% massfraction, corrode, be corroded fully until metal copper foil, salvage and in deionized water, clean twice, with PET (Polyethylene Terephthalate, polyethylene terephthalate) substrate is salvaged, toasted 10 minutes down in 60 ℃, then toasted 5 minutes down at 120 ℃, be soaked in the acetone, remove the electronics etching glue on graphene film surface, obtain to be positioned at the graphene film of the 5 centimetres of sizes of 5 cm x on the PET.
Step 3: repeating step 2 obtains being positioned at the on-chip three layer graphene films of PET twice, and the transmissivity that be positioned at three layer graphene films on the PET this moment reaches 90.4%, and it is 400 Ω that the side of graphene film hinders.
Step 4: graphene film and substrate are soaked in certain hour in the chlorauric acid solution: the product of step 2 is soaked in the hydrochloro-auric acid of 10% massfraction, after 30 minutes, take out, clean, obtain being positioned at the graphene film of on-chip high optical transmittance of PET and low square resistance with deionized water.Obtain to be positioned at the on-chip graphene film of PET by this method, transmissivity reaches 90% at visible region, and side's resistance of graphene film is 50 Ω.
Hydrochloro-auric acid can replace with the heavy metal mineral-type acid of low prices such as Platinic chloride in the present embodiment.
Embodiment 4: a kind of method that reduces the resistance of graphene film side, and its concrete steps are as follows:
Step 1: preparation graphene film: prepare the technology of Graphene by the SiC extension of standard, obtain to be positioned at the on-chip graphene film of SiC, this moment graphene film side's resistance 2000 Ω.
Step 2: will be arranged in the on-chip graphene film of SiC and be soaked in Nitromethane 99Min. solution; The product of step 1 is soaked in 100% Nitromethane 99Min., after 30 minutes, takes out, clean, obtain being positioned at the graphene film of the on-chip low square resistance of SiC with deionized water.The side's resistance that is positioned at the on-chip graphene film of SiC by this method acquisition is 200 Ω.
Nitromethane 99Min. can replace with organic alkanes such as nitroethane in the present embodiment.
Embodiment 5: a kind of method that reduces the resistance of graphene film side, and its concrete steps are as follows:
Step 1: preparation Graphene: utilize liquid chemical method to prepare graphene film, in the beaker that 1g natural graphite powder is housed, add 50 milliliters of vitriol oils and 5g SODIUMNITRATE and 5g Vanadium Pentoxide in FLAKES, stirred 3 hours, and cleaned, filter and obtain preoxidation graphite with deionized water; In the beaker that preoxidation graphite is housed, add 50 milliliters of vitriol oils and 5g potassium permanganate, stirred 3 hours, clean, filter and obtain graphite oxide with deionized water; Graphite oxide is distributed in the deionized water, adds the 5g sodium borohydride, stirred 1 hour, use washed with de-ionized water, filter and obtain Graphene;
Step 2: preparation graphene film: the Graphene that obtains in the step 1 is scattered in the ethanol, forms the concentration of 5 mg/ml, be spun on the PET substrate, oven dry obtains being positioned at the graphene film on the PET; Side's resistance of this graphene film is 5000 Ω, and transmission of visible light is 90%;
Step 3: the product (being arranged in the graphene film on the PET) of step 2 is soaked in 100% ethanol, after 30 minutes, takes out, clean with deionized water.Obtain to be positioned at the on-chip graphene film of PET by this method, transmissivity reaches 90% at visible region, and side's resistance of graphene film is 100 Ω.
Ethanol can replace with organic alcohols such as methyl alcohol in the present embodiment.
In the above-mentioned solution, the acid of heavy metal mineral-type as the golden chloric acid or the Platinic chloride of low price, organic alcohols such as methyl alcohol or ethanol, organic amine such as quadrol or N, the N dimethyl formamide has the electronic capability of giving, and after will being arranged in on-chip graphene film and being soaked in these solution with the electronic capability of giving, these solution have been captured the hole in the graphene film, make the electron density in the graphene film increase, thereby make side's resistance of graphene film reduce.
In the above-mentioned solution, nonmetal inorganic acids example hydrochloric acid or nitric acid, organic alkanes such as Nitromethane 99Min. or nitroethane have the hole of giving ability, to be arranged in on-chip graphene film is soaked in these and has the solution that gives the hole ability, these solution are captured the electronics in the graphene film, make the hole concentration in the graphene film increase, thereby make side's resistance of graphene film reduce.
By the graphene film after the aforesaid method processing, stable variation has taken place in physicochemical property, and the current carrier of graphene film (electronics or hole) concentration increases, and this concentration can keep stablizing in long-time.
Though the concrete restriction that in the foregoing description the concentration and the soak time of solution is provided; but those skilled in the art is to be appreciated that; the concentration of solution and soak time can reasonably be set according to the technical requirements of graphene film; might not be confined to the data that the foregoing description provides, so the variation of strength of solution and soak time can't break away from protection scope of the present invention.
Those of ordinary skill in the art will appreciate that embodiment described here is in order to help reader understanding's principle of the present invention, should to be understood that protection scope of the present invention is not limited to such special statement and embodiment.Those of ordinary skill in the art can make various other various concrete distortion and combinations that do not break away from essence of the present invention according to these technology enlightenments disclosed by the invention, and these distortion and combination are still in protection scope of the present invention.
Claims (8)
1. method that reduces graphene film side resistance comprises the steps: graphene film and substrate be soaked in and has certain hour in the solution that gives electronics or give the hole ability.
2. a kind of method that reduces the resistance of graphene film side according to claim 1, it is characterized in that solution is the mixed solution of the acid of heavy metal mineral-type, organic alcohols and organic amine solution or aforementioned solution with low price of the electronic capability of giving in the described step.
3. a kind of method that reduces the resistance of graphene film side according to claim 2 is characterized in that, described heavy metal mineral-type acid with low price of the electronic capability of giving is hydrochloro-auric acid or Platinic chloride.
4. a kind of method that reduces the resistance of graphene film side according to claim 2 is characterized in that described organic alcohols with the electronic capability of giving is methyl alcohol or ethanol.
5. a kind of method that reduces the resistance of graphene film side according to claim 2 is characterized in that described organic amine with the electronic capability of giving is quadrol or N, the N dimethyl formamide.
6. a kind of method that reduces graphene film side resistance according to claim 1 is characterized in that, solution is to have the solution that gives the nonmetal inorganic acids of hole ability, organic alkanes or the mixed solution of aforementioned solution in the described step.
7. a kind of method that reduces graphene film side resistance according to claim 6 is characterized in that, described to have the nonmetal inorganic acids that gives the hole ability be hydrochloric acid or nitric acid.
8. a kind of method that reduces graphene film side resistance according to claim 6 is characterized in that, described to have the organic alkanes that gives the hole ability be Nitromethane 99Min. or nitroethane.
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Cited By (6)
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| CN103011150A (en) * | 2012-12-27 | 2013-04-03 | 上海交通大学 | Flexible graphene composite film and preparation method thereof |
| CN103373721A (en) * | 2012-04-12 | 2013-10-30 | 国家纳米科学中心 | Method for treating graphene on inert base |
| CN103996458A (en) * | 2014-05-30 | 2014-08-20 | 重庆墨希科技有限公司 | Method for improving conductivity of grapheme film |
| CN104998857A (en) * | 2014-04-15 | 2015-10-28 | 宁波宝新不锈钢有限公司 | Dipping repair method of slide way of ABB shape meter slide ring |
| CN104332390B (en) * | 2014-08-28 | 2017-07-28 | 京东方科技集团股份有限公司 | A kind of patterned Graphene preparation method, array base palte and display device |
| CN107376006A (en) * | 2017-07-28 | 2017-11-24 | 浙江理工大学 | A kind of preparation method of porous artificial skin receptor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103373721A (en) * | 2012-04-12 | 2013-10-30 | 国家纳米科学中心 | Method for treating graphene on inert base |
| CN103011150A (en) * | 2012-12-27 | 2013-04-03 | 上海交通大学 | Flexible graphene composite film and preparation method thereof |
| CN103011150B (en) * | 2012-12-27 | 2015-06-17 | 上海交通大学 | Flexible graphene composite film and preparation method thereof |
| CN104998857A (en) * | 2014-04-15 | 2015-10-28 | 宁波宝新不锈钢有限公司 | Dipping repair method of slide way of ABB shape meter slide ring |
| CN103996458A (en) * | 2014-05-30 | 2014-08-20 | 重庆墨希科技有限公司 | Method for improving conductivity of grapheme film |
| CN103996458B (en) * | 2014-05-30 | 2017-03-29 | 重庆墨希科技有限公司 | A kind of method for lifting graphene film electric conductivity |
| CN104332390B (en) * | 2014-08-28 | 2017-07-28 | 京东方科技集团股份有限公司 | A kind of patterned Graphene preparation method, array base palte and display device |
| CN107376006A (en) * | 2017-07-28 | 2017-11-24 | 浙江理工大学 | A kind of preparation method of porous artificial skin receptor |
| CN107376006B (en) * | 2017-07-28 | 2020-08-18 | 浙江理工大学 | Preparation method of porous artificial skin receptor |
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Application publication date: 20110914 |