CN115246949B - Reduced graphene oxide flexible conductive film and three-step moderate reduction preparation process thereof - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 24
- 229920000139 polyethylene terephthalate Polymers 0.000 claims abstract description 20
- 239000005020 polyethylene terephthalate Substances 0.000 claims abstract description 20
- 239000000758 substrate Substances 0.000 claims abstract description 16
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 12
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 12
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000011248 coating agent Substances 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000002834 transmittance Methods 0.000 claims abstract description 7
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 6
- -1 polyethylene terephthalate Polymers 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000012153 distilled water Substances 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000003638 chemical reducing agent Substances 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 4
- 238000007738 vacuum evaporation Methods 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000010345 tape casting Methods 0.000 claims description 2
- 238000007606 doctor blade method Methods 0.000 claims 1
- 239000011259 mixed solution Substances 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 238000001771 vacuum deposition Methods 0.000 claims 1
- 238000004804 winding Methods 0.000 abstract description 5
- 238000002791 soaking Methods 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract 1
- 238000002386 leaching Methods 0.000 abstract 1
- 238000006722 reduction reaction Methods 0.000 description 23
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229920002799 BoPET Polymers 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012279 sodium borohydride Substances 0.000 description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000002508 contact lithography Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000001883 metal evaporation Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
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- C08J7/06—Coating with compositions not containing macromolecular substances
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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Abstract
The invention discloses a reduced graphene oxide flexible conductive film and a preparation process of three-step moderate reduction, which are characterized in that: the flexible conductive film with excellent performance is prepared by adopting graphene oxide, ascorbic acid, polyethylene terephthalate (PET) film and the like through wire winding rod coating and three-step moderate reduction. The method mainly comprises the following steps: (1) Ultrasonic soaking is carried out on the PET flexible substrate to remove surface impurities, so that the surface contact property is improved; (2) Adding a certain proportion of ascorbic acid into the graphene oxide solution, and stirring at constant temperature for reaction to obtain a primarily reduced graphene oxide solution; (3) uniformly coating the solution on PET, and curing to form a film; (4) Carrying out surface reduction by adopting an ascorbic acid solution under heating; (5) Vacuum aluminum is deposited on the surface of the film, and acid leaching treatment is carried out, so that the flexible conductive film with stable structure and low surface resistance can be prepared. The preparation process is safe, the operation is simple, the film has excellent electrical property, and when the light transmittance is 54.0%, the area resistance is only 6.23kΩ/sq, and the film can be produced in a large scale.
Description
Technical Field
The invention belongs to the technical field of flexible conductive film preparation, and particularly relates to a clean, efficient and low-cost chemical reduction method preparation process of a rod-coated graphene oxide film.
Background
The conductive material is always a research hot spot in the field of materials, the conductive material with flexibility has great advantages in mechanical properties, the flexible conductive film can be applied to the fields of flexible film sensors, flexible film electrodes, antistatic films and the like, and the preparation cost and the use performance of the flexible conductive film are of great concern. Graphene is an emerging two-dimensional carbon material with excellent electron transport performance and electron mobility exceeding 15000cm 2 V.s, good mechanical properties and excellent optical properties, and is widely usedIn the fields of electronics, energy sources, biology, medicine and the like. Therefore, graphene becomes an excellent raw material for preparing the flexible conductive film, but the preparation method of graphene such as micro-mechanical stripping, epitaxial growth, chemical vapor deposition and the like is high in cost and is not suitable for large-scale production and application because graphene sheets are transferred onto a transparent substrate through physical contact printing or chemical etching process to prepare the flexible conductive film of graphene. The preparation of the flexible conductive film by a chemical oxidation-reduction method with low cost and simple operation is the main research direction in the field at present.
Graphene oxide is currently generally prepared by a modified Hummers method. Graphene oxide contains a large amount of oxygen-containing functional groups, which is beneficial to dispersing in a solvent, but greatly reduces the conductivity of the graphene oxide, so that reduction of the graphene oxide to restore the conductive structure of the graphene oxide is an important subject. The reduction process mainly comprises two methods of thermal reduction and chemical reduction, and the thermal reduction method has higher requirements on the substrate and has limitation in comparison. The reducing agent hydrazine or hydrazine hydrate commonly selected by the chemical reduction method has high toxicity and explosiveness, and potential safety hazards exist in the use process; sodium borohydride has a good reducing ability, but is easy to hydrolyze, and a stable sodium borohydride aqueous solution is difficult to obtain. The choice of green and safe reducing agents is therefore critical for the preparation of flexible conductive films.
Disclosure of Invention
The invention aims to overcome the defects in the background art, and provides a preparation process of a reduced graphene oxide flexible conductive film, and the prepared film has low surface resistance, good mechanical properties and good application value in the fields of flexible film electrodes and the like.
The technical scheme of the invention is as follows: firstly, soaking a polyethylene terephthalate (PET) flexible substrate film by using acetone in an ultrasonic manner, cleaning the film by using distilled water, and then drying the film; weighing a certain amount of reducing substances, adding the reducing substances into a Graphene Oxide (GO) solution with a certain concentration, and placing the Graphene Oxide (GO) solution into a constant-temperature water bath heating stirrer to react for a period of time to prepare primarily reduced graphene oxide (I-rGO); uniformly coating the I-rGO solution on the treated PET substrate by a wire winding rod knife coating method at a certain temperature, and curing to form a film; carrying out surface reduction on the GO film for a period of time by adopting a prepared reduction solution with a certain concentration in an environment higher than room temperature, and repeating the reduction operation once to obtain a surface reduced graphene oxide film (S-rGO); and (3) covering the surface of the S-rGO film by adopting a vacuum evaporation technology to prepare an Al-rGO film, immersing the Al-rGO film in acid for a period of time, and repeatedly cleaning and drying the Al-rGO film to prepare the flexible conductive film with stable structure and low surface resistance.
The main innovation points of the invention are as follows: the reduced graphene oxide (rGO) flexible conductive film with excellent conductive performance is prepared by a three-step reduction method. The graphene oxide solution is reduced integrally by preliminary solid reduction, and meanwhile, good dispersibility of the graphene oxide solution is ensured, so that a uniform film is formed; the surface of the film-formed graphene oxide is reduced by the two-step solution surface reduction, and the thickness of the film is in the micron level, so that the solution method can reduce the whole film to a great extent and does not damage the uniformity of the film; the three-step metal evaporation reduction further effectively reduces the film, and the graphene oxide is reduced by utilizing electrons and primary hydrogen generated by the action of metal and acid. The preparation process is simple, safe and low in cost; the selected reducing reagent is ascorbic acid, so that the safety and the reducibility are strong; the vacuum evaporation metal reduction method is simple, quick and safe.
The method for preparing the I-rGO film by the preliminary solid reduction method comprises the following steps: the ascorbic acid powder with the mass fraction of 0.1-0.5% is weighed and added into the graphene oxide solution prepared by the improved Hummers method to react in a constant-temperature water bath at 15-85 ℃ while stirring for 0.5-2.5 hours. The prepared I-rGO solution is coated on a transparent flexible substrate PET by adopting winding rods of different types to obtain I-rGO films with the thickness of 20-30 mu m, 35-45 mu m and 50-60 mu m respectively.
The method for preparing the S-rGO film by the two-step solution surface reduction method comprises the following steps: an ascorbic acid solution with a concentration of 3.5-4.5 mg/mL is prepared, and the pH of the solution is adjusted to be about 9-11. And (3) carrying out surface reduction of the I-rGO film on a heating plate at 80-90 ℃ for 10-15 minutes, washing and drying, and then carrying out secondary solution surface reduction, washing with distilled water and drying to obtain the S-rGO film.
The method for preparing the Al-rGO film by the three-step metal reduction method comprises the following steps: evaporating metal aluminum on the surface of the S-rGO film by adopting a vacuum film plating instrument to form a compact Al-rGO film, wherein the thickness of the Al film is 0.5-100 nm, immersing the Al film in 8-12 mol/L acid for 10-20 minutes, and repeatedly cleaning and drying the Al film.
Reagents and materials used in the invention: graphene oxide solution, ascorbic acid, ammonia water, acetone, polyethylene terephthalate, ethanol, water, metallic aluminum, hydrochloric acid and the like.
In the invention, X-ray photoelectron spectroscopy (XPS) and the like are adopted to characterize the reduction condition of the prepared reduced graphene oxide flexible conductive film.
Drawings
Fig. 1 is a process flow diagram of a preparation process of a reduced graphene oxide flexible conductive film.
FIG. 2 is the sheet resistance of a reduced graphene oxide flexible conductive film prepared using a solution having a concentration of 1.5 mg/mL.
FIG. 3 is the sheet resistance of a reduced graphene oxide flexible conductive film prepared using a solution having a concentration of 2.0 mg/mL.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1:
first, a polyethylene terephthalate (PET) flexible substrate film was subjected to ultrasonic immersion treatment with acetone for 20 minutes, and washed with distilled water and dried. Taking Graphene Oxide (GO) solution with the concentration of 6.8mg/mL as a raw material, weighing 1.10mL, adding 3.34mL of distilled water and 0.56mL of ethanol, and preparing 5mL of GO solution with the concentration of 1.5 mg/mL. 0.015mg of ascorbic acid was weighed into GO solution and reacted in a 45℃thermostatted water bath magnetic stirrer for 1.8 hours. And (3) placing the treated PET film substrate on a heating table at 140 ℃, and coating by using a winding rod of RDS12 model. 0.0807g of ascorbic acid was weighed and added to 20mL of distilled water to prepare a solution of 4.035mg/mL, and the pH of the solution was adjusted to about 10 by using ammonia water. And (3) carrying out two-step solution surface reduction of the I-rGO film on a heating plate at the temperature of 85 ℃ for 15 minutes, and cleaning and drying to obtain the S-rGO film. And evaporating aluminum to the surface of the S-rGO film by adopting a vacuum film plating instrument to form a compact Al-rGO film, wherein the thickness of the Al film is 30nm. And (3) placing the Al-rGO film in a 10mol/L hydrochloric acid solution, soaking for 15 minutes, washing with distilled water, and drying to obtain the reduced graphene oxide flexible conductive film with stable structure, high light transmittance and low surface resistance, wherein when the light transmittance of the film is 84.0%, the surface resistance is 214.7kΩ/sq.
Example 2:
first, a polyethylene terephthalate (PET) flexible substrate film was subjected to ultrasonic immersion treatment with acetone for 20 minutes, and washed with distilled water and dried. Taking Graphene Oxide (GO) solution with the concentration of 6.8mg/mL as a raw material, weighing 1.47mL, adding 3.02mL of distilled water and 0.51mL of ethanol, and preparing 5mL of GO solution with the concentration of 2.0 mg/mL. 0.020mg of ascorbic acid was weighed into GO solution and reacted in a 45℃constant temperature water bath magnetic stirrer for 2 hours. And (3) placing the treated PET film substrate on a heating table at 130 ℃, and coating by using a winding rod of RDS24 model. 0.0807g of ascorbic acid was weighed and added to 20mL of distilled water to prepare a solution of 4.035mg/mL, and the pH of the solution was adjusted to about 10 by using ammonia water. And (3) carrying out two-step solution surface reduction of the I-rGO film on a heating plate at 80 ℃ for 10 minutes, and cleaning and drying to obtain the S-rGO film. And evaporating aluminum to the surface of the S-rGO film by adopting a vacuum film plating instrument to form a compact Al-rGO film, wherein the thickness of the Al film is 50nm. And (3) placing the Al-rGO film in a 10mol/L hydrochloric acid solution, soaking for 20 minutes, washing with distilled water, and drying to obtain the reduced graphene oxide flexible conductive film with stable structure, high light transmittance and low surface resistance, wherein when the light transmittance of the film is 54.0%, the surface resistance is 6.23kΩ/sq.
Claims (6)
1. The preparation process of the reduced graphene oxide flexible conductive film mainly comprises the steps of firstly ultrasonically cleaning a polyethylene terephthalate (PET) flexible substrate film by distilled water and acetone, and then drying to obtain a PET substrate; weighing a certain amount of reducing substances, adding the reducing substances into a graphene oxide GO solution with a certain concentration, and placing the graphene oxide GO solution into a constant-temperature water bath heating stirrer to react for a period of time to prepare primarily reduced graphene oxide I-rGO; uniformly coating the I-rGO solution on a PET substrate by a doctor blade method at a certain temperature, and curing to form a film; carrying out surface reduction on the graphene oxide film for a period of time by adopting a prepared reducing solution with a certain concentration in an environment higher than room temperature, and repeating the reduction operation once to prepare a surface reduced graphene oxide S-rGO film; then, a vacuum evaporation technology is adopted to cover a metal aluminum coating on the surface of the S-rGO film to prepare an Al-rGO film, the Al-rGO film is immersed into acid for treatment for a period of time, and the Al-rGO film is repeatedly cleaned and dried to prepare a reduced graphene oxide flexible conductive film with stable structure and low surface resistance, wherein the film can be used as a film electrode, an antistatic film and a film sensor; the preparation process is safe, the operation is simple, the film has excellent electrical property, and when the light transmittance is 54.0%, the surface resistance is only 6.23k ohm/sq, so that the film can be produced in a large scale;
the reducing substance is ascorbic acid, the mass fraction of the reducing substance is 0.1% -0.5%, the temperature of the constant-temperature water bath is 15-85 ℃, and the stirring time is 0.5-2.5 hours;
when the Al-rGO film is soaked in the acid solution for treatment, the acid solution is hydrochloric acid solution with the concentration of 8-12 mol/L, and the generated electrons and primary hydrogen are utilized to reduce graphene oxide for 10-20 minutes;
the prepared reduction solution is ascorbic acid solution with the concentration of 3.5-4.5 mg/mL, and the pH value of the solution is adjusted to 9-11;
and (3) carrying out two-step solution surface reduction of the I-rGO film on a heating plate at 80-90 ℃ for 10-15 minutes, and repeating the two-step solution surface reduction step of the I-rGO film after washing and drying once, and washing and drying with distilled water.
2. The preparation process of claim 1, wherein the graphene oxide GO solution with a certain concentration is prepared from graphene oxide prepared by controlling oxidation and ultrasonic processes by a Hummers method, the sheet diameter is 20-100 μm, the solvent is a mixed solution of water and ethanol with a certain proportion, and the concentration of the obtained graphene oxide solution is 0.5-3.5 mg/mL.
3. The preparation process according to claim 1, wherein the PET flexible substrate film is immersed in acetone and washed with distilled water for 10 to 30 minutes.
4. The process according to claim 1, characterized in that the step of applying the I-rGO solution to the PET substrate is: and (3) placing the PET substrate on a heating plate at 130-140 ℃, and coating by adopting a Meyer rod with three types of RDS12, RDS18 and RDS24, wherein the thickness of the doctor-blading film is respectively 20-30 mu m, 35-45 mu m and 50-60 mu m.
5. The preparation process according to claim 1, wherein a vacuum coating instrument is used to evaporate aluminum onto the surface of the S-rGO film to form a dense Al-rGO film, and the thickness of the Al film is 0.5-100 nm.
6. The preparation process according to claim 1, wherein the prepared reduced graphene oxide conductive film has good flexibility, and the area resistance is only 6.23k Ω/sq when the light transmittance is 54.0%.
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