CN113652699B - Method for improving electrocatalytic hydrogen production activity of graphene - Google Patents
Method for improving electrocatalytic hydrogen production activity of graphene Download PDFInfo
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- CN113652699B CN113652699B CN202110759471.0A CN202110759471A CN113652699B CN 113652699 B CN113652699 B CN 113652699B CN 202110759471 A CN202110759471 A CN 202110759471A CN 113652699 B CN113652699 B CN 113652699B
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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Abstract
The invention discloses a method for improving the electrocatalytic hydrogen production activity of graphene, which comprises the following steps: s1, preparing graphene oxide by using graphite as a raw material through a chemical oxidation method; s2, preparing reduced graphene oxide from the graphene oxide prepared in the step S1 through a chemical reduction method; and S3, treating the reduced graphene oxide prepared in the step S2 by adopting a plurality of times of linear voltammetry scanning methods. According to the invention, graphene is not subjected to any chemical modification and modification, and is only activated through multiple linear volt-ampere scans, so that the electrocatalytic hydrogen evolution current of graphene is greatly improved, and the graphene can replace a noble metal Pt/C catalyst to prepare hydrogen through electrocatalytic hydrolysis.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to a method for improving the electrocatalytic hydrogen production activity of graphene.
Background
In order to solve the increasingly serious energy crisis and environmental problems, developing clean and efficient hydrogen energy is a sustainable and promising method. The graphene has excellent properties such as high theoretical specific surface area, excellent mechanical strength, good flexibility, high conductivity and the like due to a single-layer flaky special structure formed by carbon atoms, and has exciting application prospects in photocatalytic and electrocatalytic hydrogen production.
The hydrogen production catalyst is needed for water electrolysis, photocatalysis and photoelectrocatalysis to decompose water to produce hydrogen. The best hydrogen production catalyst at present is metallic platinum, but platinum is expensive, and the content of platinum in the crust is rare, which tends to limit industrialized hydrogen production. Therefore, the search for efficient and inexpensive alternatives is of great importance for practical industrialization.
Graphene oxide is an important low-cost way to prepare graphene, and the obtained graphene is used for electrocatalytic hydrogen production. Yanuang Li et alJournal ofAmerican Chemistry Society,133, 7296, 2011 reports that reduced graphene oxide was modified on a glassy carbon electrode at 0.5mol/L H 2 SO 4 Linear voltammetric scans were performed and showed that the hydrogen evolution current was very small even at very negative voltages. Therefore, few documents report modification of graphene. Yao Zheng et al, nature Communication,4, 4783, 2014 report that N-doped graphene has a current density of 10mA/cm at an overvoltage of-0.56V vs RHE 2 . Bhaskar R.Sathe et al Catalysis Science&In Technology,4, 2023, 2014, it is reported that B-doped graphene is modified on a glassy carbon electrode at 0.5mol/L H 2 SO 4 Linear voltammetric scans in solution showed a current density of 10mA/cm 2 At the time of hydrogen evolution, the overvoltage was-0.46V vs RHE. Yuanfu Chen et al, international Journal of Hydrogen Energy,42, 2017 reported that treatment with Ar plasma and co-doping of N, S gave graphene foam with a greater degree of improvement in electrocatalytic hydrogen evolution activity than undoped graphene foam, at 10mA/cm2, hydrogen evolution overpotential was-0.30V vs RHE. Although the doped modified graphene has a certain improvement on electrocatalytic hydrogen production compared with unmodified graphene, the activity is still lower, and the activity is very different from the catalytic activity of the conventional noble metal Pt/C. The invention does not carry out any chemical modification and modification on the graphene, but only carries out the electrochemical method: multiple linear volt-ampere scanning treatments greatly reduce the electro-catalytic hydrogen evolution overpotential of graphene at 10mA/cm 2 At current density, the hydrogen evolution overpotential is approximately-110 mV.
Disclosure of Invention
Aiming at the defects and the problems in the prior art, the invention aims to provide a method for improving the electrocatalytic hydrogen production activity of graphene.
The invention is realized by the following technical scheme:
a method for improving the electrocatalytic hydrogen production activity of graphene, comprising the following steps:
s1, preparing graphene oxide by using graphite as a raw material through a chemical oxidation method;
s2, preparing reduced graphene oxide from the graphene oxide prepared in the step S1 through a chemical reduction method;
and S3, treating the reduced graphene oxide prepared in the step S2 by adopting a plurality of times of linear voltammetry scanning methods.
The chemical reduction method of the step S2 adopts sodium borohydride or hydrazine hydrate as a reducing agent; the chemical reduction method is any one of a hydrothermal method, a solvothermal method, a hydrogen heat assisted reduction method and a heat stripping method.
The step S3 specifically comprises the following steps:
s31, dispersing the reduced graphene oxide obtained in the step S2 in a dispersing agent to form reduced graphene oxide dispersion liquid, wherein the solubility is 0.5-10 mg/mL, and the dispersing agent is 0.025-0.15 wt% of Nafion aqueous solution;
s32, dispersing and dripping reduced graphene oxide on the working electrode, wherein the loaded graphene is 0.01-1.0 mg/cm 2 The working electrode is a glassy carbon electrode;
s33, reducing the working electrode loaded with the reduced graphene oxide to N 2 Carrying out multiple linear voltammetric scans in saturated sulfuric acid solution; the counter electrode is a platinum wire (disk or net) electrode, and the reference electrode can be a saturated calomel electrode or an Ag/AgCl electrode; the initial voltage of the linear volt-ampere scanning is-1.2 to-0.7V, the end voltage is 0 to 0.6V, the scanning speed is 5 to 100mV/s, and the scanning times are 400 to 2000 times.
After the linear volt-ampere scanning is finished, when the hydrogen evolution current density is 10mA/cm 2 When the overvoltage is about-0.1V, the electrocatalytic hydrogen production performance of the graphene is greatly improved.
Compared with the prior art, the method does not carry out any chemical modification and modification on the graphene, only activates the graphene through multiple linear volt-ampere scans, greatly improves the electrocatalytic hydrogen evolution current of the graphene, and can replace a noble metal Pt/C catalyst to carry out electrocatalytic hydrolysis hydrogen production.
Drawings
FIG. 1 is a linear voltammetric scan of graphene before and after activation in example 1 of the present invention;
FIG. 2 is a linear voltammetric scan of a Pt/C catalyst according to example 1 of the present invention;
FIG. 3 is a linear voltammetric scan of graphene before and after activation in example 2 of the present invention;
FIG. 4 is a linear voltammetric scan of graphene before and after activation in example 3 of the present invention;
FIG. 5 is a linear voltammetric scan of graphene before and after activation in example 4 of the present invention;
fig. 6 is a linear voltammetric scan of graphene before and after activation in example 5 of the present invention.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
Example 1
The technical route is as follows: the method comprises the steps of (1) graphite, (2) graphite oxide, (3) graphene oxide, (4) hydrazine hydrate reduction graphene oxide into graphene, (5) a graphene working electrode, (6) multiple times of linear voltammetric scanning activation graphene.
(1) Graphite: purity of 99.9%
(2) Graphite oxide: 12g of graphite with the purity of 99.9% in the step (1) is weighed, 10g of potassium peroxodisulfate (analytically pure), 10g of phosphorus pentoxide (analytically pure) and 48mL of concentrated sulfuric acid (mass fraction 98%) are added into a round-bottom flask, the mixture is stirred in a water bath at 80 ℃ for reaction for 4.5 hours, 500mL of deionized water is added after the reaction is finished, the mixture is filtered and washed to be neutral by suction, and the mixture is dried at 60 ℃ to obtain the preoxidized graphite. Weighing 2g of the preoxidized graphite, adding 1g of sodium nitrate (analytically pure), 46mL of concentrated sulfuric acid, stirring for 30min in an ice bath, slowly adding 6g of potassium permanganate (analytically pure), and reacting for 45min in the ice bath; then the mixture is heated to 35 ℃, stirred and reacted for 2 hours, and then 90mL of deionized water is slowly added dropwise; the mixture was heated rapidly to 95℃and stirred for 15min. And finally, 144mL of deionized water is added for dilution, 30mL of hydrogen peroxide (mass fraction is 30%), stirring is carried out for 30min, centrifugal washing is carried out on the mixture until the pH value is 6, and drying is carried out at 80 ℃ for 48h, thus obtaining the graphite oxide sheet.
(3) And ultrasonically dispersing the graphite oxide into graphene oxide in water, wherein the concentration is 1mg/mL.
(4) 200mL of graphene oxide in the step (3) is taken, 0.2mL of hydrazine hydrate (80 wt%) is added, the mixture is stirred in a water bath at 90 ℃ for reaction for 2h, filtered, washed with water for several times, and dried at 80 ℃.
(5) Adding 5mg of graphene obtained in the step (4) into 2mL of Nafion solution (0.075 wt%) for ultrasonic dispersion for 2h, dripping 6 mu L of graphene suspension onto a clean glassy carbon electrode, and naturally drying.
(6) N of the working electrode prepared in the step (5) at 0.5mol/L 2 Saturated H 2 SO 4 In the solution, the counter electrode is a Pt wire electrode, the reference electrode is a saturated calomel electrode, the initial voltage is-0.8V, the termination voltage is 0.4V, the scanning speed is 50mV/s, and the scanning times are 600 times for activation.
Fig. 1 is a linear voltammetric scan of graphene before and after activation in this example, and fig. 2 is a linear voltammetric scan of Pt/C in this example. From FIGS. 1 and 2, it can be seen that the electrocatalytic hydrogen evolution current of the activated graphene is greatly increased, and the current density is 10mA/cm 2 At an overvoltage of-0.117V, whereas the conventional noble metal catalyst Pt/C is at 10mA/cm 2 At current density, the overvoltage is-0.1V.
Example 2
The technical route is as follows: the method comprises the steps of (1) graphite, (2) graphite oxide, (3) graphene oxide, (4) reduction of graphene oxide by sodium borohydride into graphene, (5) graphene working electrode, (6) multiple times of linear voltammetric scanning to activate the graphene.
(1) Same as in example 1
(2) Same as in example 1
(3) Same as in example 1
(4) 200mL of graphene oxide in the step (3) is taken, added with sodium borohydride, stirred in a water bath at 80 ℃ and reacted for 10h. Filtering, washing with water several times, and drying at 80deg.C.
(5) Same as in example 1
(6) N of the working electrode prepared in the step (5) at 0.5mol/L 2 Saturated H 2 SO 4 In the solution, the counter electrode is a Pt wire electrode, the reference electrode is a saturated calomel electrode, the initial voltage is-0.8V, the termination voltage is 0.4V, the scanning speed is 50mV/s, and the scanning times are 500 times for activation.
FIG. 3 is a linear voltammetric scan of graphene before and after activation in this example, and as can be seen from FIG. 3, the current density of graphene after activation is 10mA/cm 2 The overvoltage was-0.116V.
Example 3
The technical route is as follows: the method comprises the steps of (1) graphite, (2) graphite oxide, (3) graphene oxide, (4) reduction of graphene oxide into graphene by a hydrothermal method, (5) graphene working electrode, (6) multiple times of linear voltammetric scanning activation of graphene.
(1) Same as in example 1
(2) Same as in example 1
(3) Same as in example 1
(4) And (3) adding 80mL of graphene oxide in the step (3) into a reaction kettle of 100mL of polytetrafluoroethylene, reacting for 12h at 160 ℃, filtering, washing for several times, and drying at 80 ℃.
(5) Same as in example 1
(6) N of the working electrode prepared in the step (5) at 0.5mol/L 2 Saturated H 2 SO 4 In the solution, the counter electrode is a Pt wire electrode, the reference electrode is a saturated calomel electrode, the initial voltage is-0.8V, the termination voltage is 0.4V, the scanning speed is 50mV/s, and the scanning times are 800 times for activation.
FIG. 4 is a linear voltammetric scan of graphene before and after activation in this example, and it can be seen from FIG. 4 that the current density of graphene after activation is 10mA/cm 2 The overvoltage was-0.125V.
Example 4
The technical route is as follows: the method comprises the steps of (1) graphite, (2) graphite oxide, (3) graphene oxide, (4) reduction of graphene oxide into graphene by a solvothermal method, (5) graphene working electrode, (6) multiple times of linear voltammetric scanning activation of graphene.
(1) Same as in example 1
(2) Same as in example 1
(3) Taking 80mg of graphite oxide in the step (2), adding the graphite oxide into 80mL of dimethyl sulfoxide, and performing ultrasonic dispersion for 2h
(4) Adding the graphene oxide in the step (3) into a reaction kettle of 100mL polytetrafluoroethylene, reacting for 12h at 180 ℃, filtering ethanol, washing for several times, and drying at 80 ℃.
(5) Same as in example 1
(6) N of the working electrode prepared in the step (5) at 0.5mol/L 2 Saturated H 2 SO 4 In the solution, the counter electrode is a Pt wire electrode, the reference electrode is a saturated calomel electrode, the initial voltage is-0.8V, the termination voltage is 0.4V, the scanning speed is 50mV/s, and the scanning times are 600 times for activation.
FIG. 5 is a linear voltammetric scan of graphene before and after activation in this example, and it can be seen from FIG. 5 that the current density of graphene after activation is 10mA/cm 2 The overvoltage was-0.119V.
Example 5
The technical route is as follows: the method comprises the steps of (1) graphite, (2) graphite oxide, (3) hydrogen-assisted thermal reduction of graphite oxide into graphene, (4) a graphene working electrode, and (5) multiple linear voltammetric scanning activation of graphene.
(1) Same as in example 1
(2) Same as in example 1
(3) And (3) heating the graphite oxide to 500 ℃ at a heating rate of 15 ℃/min in a nitrogen-hydrogen mixed gas flow with the volume concentration of hydrogen of 5% and the flow rate of 60mL/min, maintaining for 2h, and finally cooling to room temperature in the nitrogen-hydrogen mixed gas (flow rate of 60 mL/min) to obtain the graphene.
(4) The obtained graphene is 5mg, added into 2mL of Nafion solution (0.075 wt%) and dispersed for 2h by ultrasonic, 6 mu L of graphene suspension is taken and dripped on a clean glassy carbon electrode, and the solution is naturally dried.
(5) The prepared working electrode is 0.5mol/L N 2 Saturated H 2 SO 4 In the solution, the counter electrode is a Pt wire electrode, the reference electrode is a saturated calomel electrode, the initial voltage is-0.8V, the termination voltage is 0.4V, the scanning speed is 50mV/s, and the scanning times are 900 times for activation.
FIG. 6 is a linear voltammetric scan of graphene before and after activation in this example, and it can be seen from FIG. 6 that the current density of graphene after activation is 10mA/cm 2 The overvoltage was-0.115V.
The foregoing description of the preferred embodiments of the present invention has been presented only in terms of those specific and detailed descriptions, and is not, therefore, to be construed as limiting the scope of the invention. It should be noted that modifications, improvements and substitutions can be made by those skilled in the art without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (4)
1. A method for improving the electrocatalytic hydrogen production activity of graphene, which is characterized by comprising the following steps:
s1, preparing graphene oxide by using graphite as a raw material through a chemical oxidation method;
s2, preparing reduced graphene oxide from the graphene oxide prepared in the step S1 through a chemical reduction method;
s3, treating the reduced graphene oxide prepared in the step S2 by adopting a multiple linear voltammetry scanning method; the method specifically comprises the following steps:
s31, dispersing the reduced graphene oxide obtained in the step S2 in a dispersing agent to form reduced graphene oxide dispersion liquid;
s32, the reduced graphene oxide dispersion is dripped on a working electrode;
s33, reducing the working electrode loaded with the reduced graphene oxide to N 2 Performing multiple linear volt-ampere scans in saturated sulfuric acid solution, wherein the initial voltage of the linear volt-ampere scans is-1.2 to-0.7V, the end voltage of the linear volt-ampere scans is 0-0.6V, the scanning speed is 50-100 mV/s, and the scanning times are 400-2000.
2. The method for improving the electrocatalytic hydrogen production activity of graphene according to claim 1, wherein the method comprises the following steps: the chemical reduction method of the step S2 adopts sodium borohydride or hydrazine hydrate as a reducing agent; the chemical reduction method is any one of a hydrothermal method, a solvothermal method, a hydrogen heat assisted reduction method and a heat stripping method.
3. The method for improving the electrocatalytic hydrogen production activity of graphene according to claim 1, wherein the method comprises the following steps: the solubility of the reduced graphene oxide in the dispersion liquid prepared in the step S31 is 0.5-10 mg/mL; the dispersing agent is Nafion aqueous solution with the concentration of 0.025-0.15 and wt percent.
4. The method for improving the electrocatalytic hydrogen production activity of graphene according to claim 1, wherein the method comprises the following steps: the graphene amount loaded on the working electrode in the step S32 is 0.01-1.0 mg/cm 2 The working electrode is made of glassy carbonAnd (5) a pole.
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| CN102192936A (en) * | 2011-02-19 | 2011-09-21 | 中国科学院海洋研究所 | Glassy carbon electrode modified by reduction-state graphene, and preparation and application of glassy carbon electrode |
| CN108425128A (en) * | 2018-03-12 | 2018-08-21 | 华南理工大学 | A kind of porous amino functional graphene catalysis material and preparation and application |
| CN110526235A (en) * | 2018-05-23 | 2019-12-03 | 浙江大学 | A method of oxygen doping three-dimensional grapheme in situ is prepared by electrochemical stripping |
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| CN102192936A (en) * | 2011-02-19 | 2011-09-21 | 中国科学院海洋研究所 | Glassy carbon electrode modified by reduction-state graphene, and preparation and application of glassy carbon electrode |
| CN108425128A (en) * | 2018-03-12 | 2018-08-21 | 华南理工大学 | A kind of porous amino functional graphene catalysis material and preparation and application |
| CN110526235A (en) * | 2018-05-23 | 2019-12-03 | 浙江大学 | A method of oxygen doping three-dimensional grapheme in situ is prepared by electrochemical stripping |
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