CN112216808A - Preparation of reduced graphene oxide-TiO by one-step reduction method2Electrode for electrochemical cell - Google Patents
Preparation of reduced graphene oxide-TiO by one-step reduction method2Electrode for electrochemical cell Download PDFInfo
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- CN112216808A CN112216808A CN201910622340.0A CN201910622340A CN112216808A CN 112216808 A CN112216808 A CN 112216808A CN 201910622340 A CN201910622340 A CN 201910622340A CN 112216808 A CN112216808 A CN 112216808A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 44
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 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 26
- 238000000034 method Methods 0.000 claims abstract description 25
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 22
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 16
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 16
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 16
- 239000000661 sodium alginate Substances 0.000 claims abstract description 16
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 13
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 12
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 20
- 239000011268 mixed slurry Substances 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 7
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 abstract description 6
- 239000000853 adhesive Substances 0.000 abstract description 4
- 230000001070 adhesive effect Effects 0.000 abstract description 4
- 238000007600 charging Methods 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 4
- 238000004132 cross linking Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 15
- 239000006260 foam Substances 0.000 description 10
- 239000007772 electrode material Substances 0.000 description 9
- 239000011149 active material Substances 0.000 description 6
- 238000005265 energy consumption Methods 0.000 description 5
- -1 polytetrafluoroethylene Polymers 0.000 description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 description 5
- 238000007599 discharging Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000002028 Biomass Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 239000003431 cross linking reagent Substances 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000006258 conductive agent Substances 0.000 description 2
- 238000010277 constant-current charging Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000012279 sodium borohydride Substances 0.000 description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 description 2
- 238000001075 voltammogram Methods 0.000 description 2
- 235000000069 L-ascorbic acid Nutrition 0.000 description 1
- 239000002211 L-ascorbic acid Substances 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/049—Manufacturing of an active layer by chemical means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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Abstract
The invention discloses a one-step reduction method with simple operation, which is used for preparing reduced graphene oxide-TiO2And measuring the electrochemical performance of the electrode. Namely sodium alginate adhesive, graphene oxide and TiO2Physically crosslinking, coating a film on the foamed nickel, and drying at constant temperature. Then directly placing the coated film electrode in an ascorbic acid hot solvent for one-step reduction to obtain reduced graphene oxide-TiO2And an electrode. The preparation method is simple to operate, low in cost and environment-friendly. The electrode obtained by the method avoids the electrode in the process of charging and dischargingThe material falls off, the system structure is stable, and the electrochemical performance is good.
Description
Technical Field
The invention relates to an electrode, in particular to reduced graphene oxide-TiO2The preparation method of the electrode and the electrochemical performance measurement thereof.
Background
In recent years, with the rapid development of science and technology, the application field of batteries is more and more extensive, and the demand is increasing, so that the manufacture of batteries with faster charging and larger electric energy storage becomes a hot spot of research of people. The electrode is an important component of the battery, and is receiving more and more attention from researchers.
The adhesive with good performance can prevent the electrode material from separating from the surface of the electrode and entering into electrolyte solution, and the stability of the electrode structure is kept. A binder commonly used in recent research is polytetrafluoroethylene, which is relatively stable in an electrolyte. However, the polytetrafluoroethylene has a weak interaction force with the active material, and the mechanical strength of the electrode obtained by bonding the polytetrafluoroethylene to the active material is insufficient, so that it is difficult to suppress the detachment of the active electrode material from the electrode surface, and the structural stability of the electrode cannot be effectively maintained. In addition, polyvinylidene fluoride is dissolved only in a specific solvent such as methyl pyrrolidone, which increases the manufacturing cost of the electrode, and the solvent volatilized during the manufacturing process is harmful to human body. The electrode prepared by the novel adhesive sodium alginate has higher mechanical strength, can effectively inhibit the structural damage of the active material in the charging and discharging process of the battery, has stronger adhesive force to the active material, makes the active material more difficult to separate from a current collector, and has good biocompatibility, no toxicity and no harm, and can not cause pollution. Therefore, sodium alginate is more suitable for being used as a novel electrode material binder with high energy density compared with polytetrafluoroethylene.
Metal oxides such as ZnO, MnO, CuO and TiO2And the like, has good physical and chemical properties, excellent electrochemical activity and high conductivity, and is a novel electrode material. Wherein the TiO is2The material is an inorganic semiconductor material with stable property, has good photocatalytic and electrocatalytic activity, is widely applied in the field of photocatalysis, and has wide application prospect in the aspect of electrode materials. However, as an electrode material, the conductivity is not ideal enough, which limits the application of the electrode material.
Reduced graphene oxide has a large specific surface area, excellent electrical conductivity, good mechanical strength, and a two-dimensional open structure, and has received much attention as a good conductive agent in the electrochemical field. Most of reduced graphene oxide reported in the current research is obtained by reducing graphene oxide, and a common reduction method is sodium borohydride reductionThe original method, the strong base reduction method, the hydrothermal reduction method and the like. However, the methods have large operation risk, strict experimental condition requirements and large energy consumption. Ascorbic acid is gradually used for reducing graphene oxide as a soft reducing agent, but most of the existing researches are used for reducing a single graphene oxide solution, the obtained reduced graphene oxide is easy to agglomerate, redundant ascorbic acid solution is easy to remain, and the washing process is difficult. The invention uses a one-step reduction method to directly oxidize the graphene oxide-TiO2The electrode is placed in an ascorbic acid hot solution for reduction, the reduction process is simple, the energy consumption is low, and the operation process is safe and has no risk, so the method is a novel efficient reduction method.
Therefore, the invention takes the biomass material sodium alginate as a cross-linking agent, the reduced graphene oxide as a conductive agent and TiO2Is used as an electrode material and combines physical crosslinking and a one-step reduction method to prepare reduced graphene oxide-TiO2And an electrode. The one-step reduction method is simple to operate, low in energy consumption, safe, free of risks, environment-friendly, low in cost of the prepared electrode and good in electrochemical performance.
Disclosure of Invention
The invention aims to provide a one-step reduction method which is simple to operate, low in energy consumption, safe, risk-free and environment-friendly and is used for preparing reduced graphene oxide-TiO2And an electrode.
The method comprises the following specific steps:
(1) sodium alginate, graphene oxide and TiO in a certain mass ratio2And (3) mixing the powder, mechanically stirring for 0.5-1 h at the normal temperature at the rotating speed of 200-300 rpm, and performing ultrasonic dispersion for 30min after uniformly stirring to obtain mixed slurry.
(2) Uniformly coating the mixed slurry in a 1cm multiplied by 1cm area at one end of a 1cm multiplied by 2cm foamed nickel sheet, and drying in a drying oven at constant temperature for 8-12 h to obtain foamed nickel/graphene oxide/TiO2A sheet.
(3) The foamed nickel/graphene oxide/TiO is mixed2The sheet is placed in 100mL of ascorbic acid solution with a certain mass concentration, reduced for a certain time in a water bath at the temperature of 60-90 ℃, washed for 8-10 times by deionized water, soaked in the deionized water for 12 hours and thenDrying the graphene oxide in an oven at the temperature of between 40 and 60 ℃ for 12 hours to obtain the reduced graphene oxide-TiO2And an electrode.
The invention aims at obtaining the reduced graphene oxide-TiO2The composite material is subjected to X-ray photoelectron spectroscopy. The result shows that the graphene oxide is successfully reduced after one-step reduction by an ascorbic acid hot solvent method.
The invention aims at obtaining the reduced graphene oxide/TiO2And (3) measuring the electrochemical performance of the electrode, wherein the potential window of the cyclic voltammetry is as follows: -1V; the current density tested by the constant current charging and discharging curve is 1A/g-10A/g; and the electrochemical impedance and the cycle curve of the electrode are tested and analyzed.
Drawings
FIG. 1 shows reduced graphene oxide-TiO with different mass ratios2The voltammogram of the composite material was scanned at a rate of 100 mV/s.
FIG. 2 is TiO2Electrode and reduced graphene oxide-TiO2Impedance curves of the electrodes are compared.
Detailed Description
These examples are only illustrative of the present invention, but the present invention is not limited to these examples.
Example 1
Mixing 0.05g of sodium alginate and 0.225g of TiO2Mixing the powder with 22.5ml and 0.01g/ml graphene oxide solution, mechanically stirring at the normal temperature for 0.5h at the rotating speed of 200rpm, uniformly stirring, and performing ultrasonic dispersion for 30min to obtain mixed slurry; uniformly coating the mixed slurry in a 1cm multiplied by 1cm area at one end of a 1cm multiplied by 2cm foam nickel sheet, and drying for 8 hours in a drying oven at constant temperature to obtain foam nickel/graphene oxide/TiO2A sheet; the foamed nickel/graphene oxide/TiO is mixed2The thin slice is put into 100mL of ascorbic acid solution with the concentration of 1g/L, reduced for 15min in water bath with the temperature of 60 ℃, washed for 8 times by deionized water, soaked in deionized water for 12h, and dried in an oven at the temperature of 40 ℃ for 12h to obtain the reduced graphene oxide-TiO2And an electrode.
Example 2
Mixing 0.1g sodium alginate and 0.27g TiO2Mixing the powder with 13ml and 0.01g/ml graphene oxide solution, mechanically stirring at the normal temperature for 45min at the rotating speed of 250rpm, uniformly stirring, and ultrasonically dispersing for 30min to obtain mixed slurry; uniformly coating the mixed slurry in a 1cm multiplied by 1cm area at one end of a 1cm multiplied by 2cm foam nickel sheet, and drying in a drying oven at constant temperature for 10 hours to obtain foam nickel/graphene oxide/TiO2A sheet; the foamed nickel/graphene oxide/TiO is mixed2The thin sheet is placed in 100mL of ascorbic acid solution with the concentration of 5g/L, reduced for 30min in a water bath with the temperature of 70 ℃, washed for 9 times by deionized water, soaked in deionized water for 12h, and dried in a drying oven at the temperature of 50 ℃ for 12h to obtain the reduced graphene oxide-TiO2And an electrode.
Example 3
Mixing 0.2g sodium alginate and 0.225g TiO2Mixing the powder with 7.5ml and 0.01g/ml graphene oxide solution, mechanically stirring at the normal temperature for 1h at the rotating speed of 300rpm, uniformly stirring, and performing ultrasonic dispersion for 30min to obtain mixed slurry; uniformly coating the mixed slurry in a 1cm multiplied by 1cm area at one end of a 1cm multiplied by 2cm foam nickel sheet, and drying in a drying oven at constant temperature for 10 hours to obtain foam nickel/graphene oxide/TiO2A sheet; the foamed nickel/graphene oxide/TiO is mixed2The thin slice is put into 100mL of 10g/L ascorbic acid solution, reduced for 45min in a water bath at the temperature of 80 ℃, washed for 10 times by deionized water, soaked in the deionized water for 12h, and dried in an oven at the temperature of 60 ℃ for 12h to obtain the reduced graphene oxide-TiO2And an electrode.
Example 4
Mixing 0.25g sodium alginate and 0.21g TiO2Mixing the powder with 4.2ml and 0.01g/ml graphene oxide solution, mechanically stirring at the normal temperature for 1h at the rotating speed of 300rpm, uniformly stirring, and performing ultrasonic dispersion for 30min to obtain mixed slurry; uniformly coating the mixed slurry in a 1cm multiplied by 1cm area at one end of a 1cm multiplied by 2cm foam nickel sheet, and drying in a drying oven at constant temperature for 12 hours to obtain foam nickel/graphene oxide/TiO2A sheet; the foamed nickel/graphene oxide/TiO is mixed2The slices are put into 100mL of ascorbic acid solution with the concentration of 15g/L, reduced for 60min in a water bath with the temperature of 90 ℃, then washed 10 times by deionized water, soaked in deionized water for 12h, and then put into an ovenDrying at 60 ℃ for 12h to obtain the reduced graphene oxide-TiO2And an electrode.
Example 5
Mixing 0.2g sodium alginate and 0.3g TiO2Placing the powder in 10ml of deionized water, mechanically stirring for 1h at normal temperature at the rotating speed of 300rpm, and performing ultrasonic dispersion for 30min after uniformly stirring to obtain mixed slurry; uniformly coating the mixed slurry in a 1cm multiplied by 1cm area at one end of a 1cm multiplied by 2cm foam nickel sheet, and drying in a drying oven at constant temperature for 12 hours to obtain foam nickel/graphene oxide/TiO2A sheet; the foamed nickel/graphene oxide/TiO is mixed2The thin slice is put into 100mL of ascorbic acid solution with the concentration of 20g/L, reduced for 60min in water bath with the temperature of 90 ℃, washed for 10 times by deionized water, soaked in deionized water for 12h, and dried in an oven at the temperature of 60 ℃ for 12h to obtain TiO2And an electrode.
Compared with hydrothermal reduction, sodium borohydride reduction and strong base reduction methods, the one-step reduction method adopted by the invention is safer to operate and low in energy consumption, and the problems that graphene products are easy to agglomerate and reducing agents are not easy to remove in single graphene oxide solution reduction are solved. In addition, reduced graphene oxide/TiO is prepared by using biomass material sodium alginate as a cross-linking agent2The electrode is different from the electrode which is prepared by taking polytetrafluoroethylene as a cross-linking agent in most documents, the biomass material sodium alginate has good biocompatibility, is nontoxic and harmless, cannot cause pollution, and is reduced graphene oxide-TiO prepared by taking the sodium alginate as a novel binder2The electrode has high mechanical strength, can effectively inhibit the structural damage of the active material in the charging and discharging process of the battery, and prevents the electrode material from falling off.
Reduced graphene oxide-TiO2The electrode exhibits better conductivity and cycling stability. When the current density is 5A/g, the capacity retention rate can still reach 68.4 percent after the constant current charging and discharging is carried out for 350 times. The specific capacitance calculated from the voltammograms at a scan rate of 10mV/s was 106F/g; when the current density was 0.5A/g, the specific capacitance calculated from the constant-current charge-discharge curve was 222F/g. The TiO can be known from the electrochemical impedance diagram2Electrode and reduced graphene oxide-TiO2The charge transfer resistances (Rct) of the electrodes were 0.201 Ω and 0.080 Ω respectively,the equivalent series resistances (Rcp) are 2.13 Ω and 1.14 Ω, respectively.
The invention is not limited to the examples, and any equivalent changes to the technical solution of the invention by a person skilled in the art after reading the description of the invention are covered by the claims of the invention.
Claims (5)
1. Preparation of reduced graphene oxide-TiO by one-step reduction method2The electrode is characterized by comprising the following specific steps:
(1) sodium alginate, graphene oxide and TiO in a certain mass ratio2And (3) mixing the powder, mechanically stirring for 0.5-1 h at the normal temperature at the rotating speed of 200-300 rpm, and performing ultrasonic dispersion for 30min after uniformly stirring to obtain mixed slurry.
(2) Uniformly coating the mixed slurry in a 1cm multiplied by 1cm area at one end of a 1cm multiplied by 2cm foamed nickel sheet, and drying in a drying oven at constant temperature for 8-12 h to obtain foamed nickel/graphene oxide/TiO2A sheet.
(3) The foamed nickel/graphene oxide/TiO is mixed2The thin slice is placed in 100mL of ascorbic acid solution with certain mass concentration, reduced for a certain time in a water bath at the temperature of 60-90 ℃, washed 8-10 times by deionized water, soaked in the deionized water for 12 hours, and dried in an oven at the temperature of 40-60 ℃ for 12 hours to obtain the reduced graphene oxide-TiO2And an electrode.
2. The one-step reduction method for preparing reduced graphene oxide-TiO according to claim 12The electrode is characterized in that TiO in the mixed slurry in the step (1)2The mass ratio of the graphene oxide to the graphene oxide is 1: 2-5: 1;
3. the one-step reduction method for preparing reduced graphene oxide-TiO according to claim 12The electrode is characterized in that the mass of sodium alginate in the mixed slurry in the step (1) accounts for TiO2And the total mass of the graphene oxide and the sodium alginate is 10-50%.
4. The one-step reduction of claim 1Method for preparing reduced graphene oxide-TiO2The electrode is characterized in that the mass concentration of the ascorbic acid solution in the step (3) is 1-20 g/L.
5. The one-step reduction method for preparing reduced graphene oxide-TiO according to claim 12The electrode is characterized in that the reduction time in the step (3) is 15-60 min.
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CN116386928A (en) * | 2023-06-02 | 2023-07-04 | 山东科技大学 | Sodium alginate/titanium dioxide composite porous electrode material and preparation method thereof |
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CN103839696A (en) * | 2012-11-23 | 2014-06-04 | 海洋王照明科技股份有限公司 | Graphene electrode plate, and preparation method and application thereof |
JP2014209472A (en) * | 2013-03-28 | 2014-11-06 | 株式会社半導体エネルギー研究所 | Method of manufacturing electrode for accumulator battery |
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CN103839696A (en) * | 2012-11-23 | 2014-06-04 | 海洋王照明科技股份有限公司 | Graphene electrode plate, and preparation method and application thereof |
JP2014209472A (en) * | 2013-03-28 | 2014-11-06 | 株式会社半導体エネルギー研究所 | Method of manufacturing electrode for accumulator battery |
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CN116386928A (en) * | 2023-06-02 | 2023-07-04 | 山东科技大学 | Sodium alginate/titanium dioxide composite porous electrode material and preparation method thereof |
CN116386928B (en) * | 2023-06-02 | 2023-08-04 | 山东科技大学 | Sodium alginate/titanium dioxide composite porous electrode material and preparation method thereof |
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Application publication date: 20210112 |