CN104056630A - Preparation method of carbon-coated cobalt oxygen evolution reaction electro-catalyst - Google Patents
Preparation method of carbon-coated cobalt oxygen evolution reaction electro-catalyst Download PDFInfo
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- CN104056630A CN104056630A CN201410305400.3A CN201410305400A CN104056630A CN 104056630 A CN104056630 A CN 104056630A CN 201410305400 A CN201410305400 A CN 201410305400A CN 104056630 A CN104056630 A CN 104056630A
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Abstract
The invention relates to a preparation method of a carbon-coated cobalt oxygen evolution reaction electro-catalyst and belongs to the preparation field of electrochemical catalysts. The preparation method includes the steps that firstly, a carbon source and cobalt salts in proportion are placed into water for dissolving and mixing, and then evaporation to dryness is performed at the water bath condition at the temperature of 50 DEG C-80 DEG C to obtain powder evenly mixed; then the powder is heated to 400 DEG C-1000 DEG C under the shielding gas condition and then calcinated for 30 minutes-120 minutes to obtain a carbon-coated cobalt elementary substance; finally, an electrochemical pretreatment method is used for obtaining a nano-particle of carbon layer-cobaltic oxide-elementary substance cobalt, wherein the nano-particle is of an electric conduction core-shell structure. The method is simple in process, convenient to implement and low in requirement for preparation equipment and improves safety in the experiment process. The carbon layer-cobaltic oxide-elementary substance cobalt prepared through the method is even in diameter and good in electric conduction and has good electro-catalysis water oxidation performance.
Description
Technical field
The present invention relates to a kind of preparation method of oxygen evolution reaction eelctro-catalyst of carbon coating cobalt, belong to the preparation field of electrochemical catalyst.
Background technology
Brine electrolysis generates hydrogen and oxygen is storage solar energy, and the intermittent energy source such as wind energy provide a kind of possible mode.But due to oxygen evolution reaction dynamic process slowly, brine electrolysis required voltage is much higher than the thermodynamics electromotive force of water decomposition.The highest at present active oxygen evolution reaction catalysts is RuO
2and IrO
2but these noble metals are very rare, can not use on a large scale.Therefore, the non-precious metal oxygen evolution reaction eelctro-catalyst of development high catalytic activity is most important.
In recent years, especially the oxide of cobalt is because of its aboundresources for transition metal oxide, and catalytic performance is good and paid close attention to widely.But with RuO
2and IrO
2comparing, still there is the problems such as catalytic current density is low, and overpotential is higher, poor stability in these catalyst, and the synthetic method of catalyst is often also more complicated.
Summary of the invention
The object of the invention is to have in order to solve existing catalyst that catalytic current density is low, overpotential is higher, poor stability problem, a kind of preparation method of oxygen evolution reaction eelctro-catalyst of carbon coating cobalt is provided.
The object of the invention is to be achieved through the following technical solutions.
An oxygen evolution reaction eelctro-catalyst for carbon coating cobalt, the nano composite material being formed by the oxide of graphite and cobalt.
A preparation method for the oxygen evolution reaction eelctro-catalyst of carbon coating cobalt, concrete steps are as follows:
Step 1, by cobalt salt and carbon source, in molar ratio 1:(100～500) proportionate relationship put into deionized water dissolve mix; Then water bath method, obtains powder;
Step 2, by the powder of step 1 gained, under inert gas shielding, be heated to 400 DEG C～1000 DEG C, constant temperature keep 30min～120min obtain carbon coating cobalt simple substance;
Step 3, by the carbon coating cobalt simple substance of step 2 gained, be dissolved in the mixed solution of organic solvent and naphthols; The mixed volume of organic solvent and naphthols is than being (965～995): (35～5); Then be coated in rotating disk electrode (r.d.e), under the constant voltage condition of 0.5V～1.2V, carry out electroxidation pretreatment, obtain oxygen evolution reaction eelctro-catalyst;
Described cobalt salt is cobalt nitrate, cobalt chloride, cobaltous sulfate;
Described carbon source is urea, glucose, sucrose;
Described inert gas is nitrogen or argon gas;
Organic solvent comprises methyl alcohol, ethanol, isopropyl alcohol, dimethyl sulfoxide (DMSO), dimethyl formamide.
Beneficial effect
1, the oxygen evolution reaction eelctro-catalyst of a kind of carbon coating cobalt of the present invention, has good catalytic performance, is the good catalyst of oxygen evolution reaction (OER), and when overpotential is 320mV, current density is 10mAcm
-2, Tafel slope reaches 58mV/dec, and stability is better than IrO
2, can substitute RuO
2and IrO
2be applied in electro-catalysis water decomposition.
2, the preparation method of the oxygen evolution reaction eelctro-catalyst of a kind of carbon coating cobalt of the present invention, adopt a step high-temperature calcination, then the liquid deposition of sample is carried out on electrode to in-situ oxidation, step is simple, easy to operate, adopt solid-state carbon source, improve the security in experimentation; Cobalt source is common cobalt salt, and cost is low.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of the spherical carbon coating cobalt simple substance prepared of embodiment 1 under amplifying 50000 times;
Fig. 2 is the scanning electron microscope (SEM) photograph (SEM) of the spherical carbon coating cobalt simple substance prepared of embodiment 1 under amplifying 240000 times;
Fig. 3 is the high power transmission electron microscope picture (TEM) of the spherical carbon coating cobalt simple substance prepared of embodiment 1;
Fig. 4 is the oxygen evolution reaction catalysts of the spherical carbon coating cobalt prepared of embodiment 1 scanning electron microscope (SEM) photograph (SEM) under amplifying 10000 times;
Fig. 5 is the transmission electron microscope picture (TEM) of the oxygen evolution reaction catalysts of the spherical carbon coating cobalt prepared of embodiment 1;
Fig. 6 is the oxygen evolution reaction catalysts high power transmission electron microscope picture (HRTEM) of the spherical carbon coating cobalt prepared of embodiment 1;
Fig. 7 is the x-ray photoelectron energy spectrogram (XPS) of the oxygen evolution reaction catalysts of the spherical carbon coating cobalt prepared of embodiment 1;
Fig. 8 is the impedance diagram that the cobalt powder after oxygen evolution reaction catalysts and the electrochemical treatments of the spherical carbon coating cobalt prepared of embodiment 1 relatively obtains;
Fig. 9 is oxygen evolution reaction catalysts and the RuO of the spherical carbon coating cobalt prepared of embodiment 1
2and IrO
2oxygen evolution reaction performance comparison diagram;
Figure 10 is oxygen evolution reaction catalysts and the RuO of the spherical carbon coating cobalt prepared of embodiment 1
2and IrO
2tafel slope of curve comparison diagram;
Figure 11 is oxygen evolution reaction catalysts and the RuO of the spherical carbon coating cobalt prepared of embodiment 1
2and IrO
2, be 10mAcm in current density
-2galvanostatic conditions under stability comparison diagram;
Figure 12 is the scanning electron microscope (SEM) photograph (SEM) of carbon-cobalt oxygen evolution reaction catalysts of preparing of embodiment 2 under amplifying 5000 times;
Figure 13 is the oxygen evolution reaction polarization curve of carbon-cobalt oxygen evolution reaction catalysts of preparing of embodiment 2.
Figure 14 is the oxygen evolution reaction polarization curve of carbon-cobalt oxygen evolution reaction catalysts of preparing of embodiment 3.
Detailed description of the invention
Below in conjunction with drawings and Examples, content of the present invention is elaborated.
Embodiment 1
The oxygen evolution reaction eelctro-catalyst of carbon coating cobalt, the composite being formed by the oxide of the cobalt of the good graphite of electric conductivity and high catalytic activity.
The preparation method of the oxygen evolution reaction catalysts of a kind of carbon coating cobalt of the present invention, concrete preparation process is as follows:
1) 0.29g cabaltous nitrate hexahydrate and 6.006g urea (mol ratio is 1:100) are dissolved in deionized water to the solution that ultrasonic dispersion is uniformly mixed; Mixed solution heating water bath evaporate to dryness, obtains powder;
2) by the 1st) obtain powder after step heating evaporate to dryness, under argon shield condition, be heated to 900 DEG C, and constant temperature keeps 1h, after naturally lowering the temperature, obtain carbon coating cobalt simple substance black powder;
3) by the 2nd) black powder that obtains, be dissolved in the mixed solution of ethanol and naphthols; The mixed volume of ethanol and naphthols is than being 985:15; Liquid deposition is upper in rotating disk electrode (r.d.e) (RDE), under 0.8Vvs.Ag/AgCl constant voltage condition, carry out electroxidation pretreatment, obtain carbon bag cobalt oxygen evolution reaction eelctro-catalyst.
As shown in Figure 1, 2, the SEM of the spherical carbon coating cobalt simple substance that embodiment 1 prepares, can find out that products therefrom is spherical, and the diameter of bead is even.
As shown in Figure 3, prove that the bead that embodiment 1 prepares is the coated cobalt simple substance of carbon-coating.
As Fig. 4, shown in 5, after electroxidation is processed, obtain carbon coating cobalt oxygen evolution reaction catalysts, can find out that a lot of nano particles appear in bead surface.
As shown in Figure 6, can see that by high power TEM collection of illustrative plates the surface of spherical carbon coating cobalt oxygen evolution reaction catalysts is carbon-coating and cobaltosic oxide.
As shown in Figure 7, by XPS collection of illustrative plates, further prove that cobaltosic oxide is contained on the surface of spherical carbon coating cobalt oxygen evolution reaction catalysts;
As shown in Figure 8, curve 1 is the impedance behavior test curve of spherical carbon coating cobalt oxygen evolution reaction catalysts, and curve 2 is the impedance behavior test curve of cobalt powder after electroxidation is processed, and the resistance of curve 1 is 10 ohm, the resistance of curve 2 is 125 ohm, has proved that the former electric conductivity is better than the latter;
As shown in Figure 9, abscissa represents the variation of current potential in OER process, and what ordinate represented is the current density that course of reaction produces.Curve 1 is the oxygen evolution reaction polarization curve of spherical carbon coating cobalt oxygen evolution reaction catalysts, and curve 2 is IrO
2oxygen evolution reaction polarization curve, curve 3 is RuO
2oxygen evolution reaction polarization curve.The take-off potential of oxygen evolution reaction occurs curve 1 and the oxygen evolution reaction take-off potential of curve 2 and curve is～1.45V, and overpotential is lower; The water oxidation current density that curve 1 reaches is greater than curve 2 and curve 3, has proved that the catalytic performance of the oxygen evolution reaction catalysts of spherical carbon bag cobalt prepared by embodiment 1 is better than IrO
2and RuO
2; These advantages are conducive to the present invention and substitute noble metal catalyst large-scale application in oxygen evolution reaction electro-catalysis.
As shown in figure 10, what abscissa represented is the logarithm value of the current density of course of reaction generation, and ordinate represents the variation of current potential in OER process.Curve 1 is the Tafel curve of spherical carbon coating cobalt oxygen evolution reaction catalysts, and curve 2 is IrO
2tafel curve, curve 3 is RuO
2tafel curve.Wherein, the slope of curve 1 is 58mV/dec, and the slope of curve 2 is 67mV/dec, and the slope of curve 3 is 87mV/dec, has further proved that the oxygen evolution reaction catalytic performance of spherical carbon bag cobalt oxygen evolution reaction catalysts prepared by embodiment 1 is better than IrO
2and RuO
2.
As shown in figure 11, what abscissa represented is the variation of current potential in oxygen evolution reaction process, and ordinate represents the reaction time.Curve 1 is that spherical carbon coating cobalt oxygen evolution reaction catalysts is 10mAcm in current density
-2constant current conditions under stability curve, curve 2 is IrO
2be 10mAcm in current density
-2constant current conditions under stability curve.In curve 1, voltage did not change substantially with the reaction time, and in curve 2, voltage increased gradually with the reaction time, had proved that the stability of spherical carbon coating cobalt oxygen evolution reaction catalysts is better than IrO
2.
Embodiment 2
The oxygen evolution reaction eelctro-catalyst of carbon coating cobalt, the composite being formed by the oxide of the cobalt of the good graphite of electric conductivity and high catalytic activity.
The preparation method of a kind of carbon-cobalt oxygen evolution reaction catalysts of the present invention, concrete preparation process is as follows:
1) 0.29g cabaltous nitrate hexahydrate and 15.015g urea (mol ratio is 1:250) are dissolved in deionized water to the solution that ultrasonic dispersion is uniformly mixed; By mixed solution heating water bath evaporate to dryness;
2) by the 1st) powder that obtains after step heating evaporate to dryness, under argon shield condition, be heated to 900 DEG C, and constant temperature keeps 1h, after naturally lowering the temperature, obtain carbon-cobalt black powder;
3) by the 2nd) black powder that obtains, be dissolved in the mixed solution of ethanol and naphthols; The mixed volume of ethanol and naphthols is than being 970:30; And liquid deposition is upper in rotating disk electrode (r.d.e) (RDE), under 0.8Vvs.Ag/AgCl constant-pressure conditions, carry out electroxidation pretreatment, obtain carbon-cobalt oxygen evolution reaction catalysts;
As shown in figure 12, nanotube-shaped carbon-cobalt oxygen evolution reaction catalysts that embodiment 2 prepares, diameter is 50-200nm, long is 1-2 μ m;
As shown in figure 13, abscissa represents the variation of current potential in catalytic process, and what ordinate represented is the current density that course of reaction produces.Curve represents the polarization curve of carbon-cobalt oxygen evolution reaction catalysts that embodiment 2 prepares, and the take-off potential of catalytic reaction is 1.5V, and when voltage is 1.7V, catalytic current density reaches 10mAcm
-2.
Embodiment 3
The oxygen evolution reaction eelctro-catalyst of carbon coating cobalt, the composite being formed by the oxide of the cobalt of the good graphite of electric conductivity and high catalytic activity.
The preparation method of a kind of carbon-cobalt oxygen evolution reaction catalysts of the present invention, concrete preparation process is as follows:
1) 0.29g cabaltous nitrate hexahydrate and 30.03g urea (mol ratio is (1:500)) are dissolved in deionized water to the solution that ultrasonic dispersion is uniformly mixed; By mixed solution heating water bath evaporate to dryness;
2) by the 1st) powder that obtains after step heating evaporate to dryness, under argon shield condition, be heated to 900 DEG C, and constant temperature keeps 1h, after naturally lowering the temperature, obtain carbon-cobalt black powder;
3) by the 2nd) black powder that obtains, be dissolved in the mixed solution of ethanol and naphthols; The mixed volume of ethanol and naphthols is than being 985:20; And liquid deposition is upper in rotating disk electrode (r.d.e) (RDE), under 0.6Vvs.Ag/AgCl constant-pressure conditions, carry out electroxidation pretreatment, obtain carbon-cobalt oxygen evolution reaction catalysts;
As shown in figure 14, abscissa represents the variation of current potential in catalytic process, and what ordinate represented is the current density that course of reaction produces.Curve represents the catalytic performance curve of carbon-cobalt oxygen evolution reaction catalysts that embodiment 3 prepares, and the take-off potential of catalytic reaction is 1.52V, and when voltage is 1.9V, catalytic current density reaches 10mAcm
-2.
Embodiment 4
The oxygen evolution reaction eelctro-catalyst of carbon coating cobalt, the composite being formed by the oxide of the cobalt of the good graphite of electric conductivity and high catalytic activity.
The preparation method of a kind of carbon-cobalt oxygen evolution reaction catalysts of the present invention, concrete preparation process is as follows:
1) 0.24g cobalt chloride hexahydrate and 18.02g glucose (mol ratio is 1:100) are dissolved in deionized water to the solution that ultrasonic dispersion is uniformly mixed; By mixed solution heating water bath evaporate to dryness;
2) by the 1st) powder that obtains after step heating evaporate to dryness, under argon shield condition, be heated to 900 DEG C, and constant temperature keeps 1h, after naturally lowering the temperature, obtain carbon-cobalt black powder;
3) by the 2nd) black powder that obtains, be dissolved in the mixed solution of ethanol and naphthols; The mixed volume of methyl alcohol and naphthols is than being 995:5; And liquid deposition is upper in rotating disk electrode (r.d.e) (RDE), under 0.6Vvs.Ag/AgCl constant-pressure conditions, carry out electroxidation pretreatment, obtain carbon-cobalt oxygen evolution reaction catalysts;
Embodiment 5
The oxygen evolution reaction eelctro-catalyst of carbon coating cobalt, the composite being formed by the oxide of the cobalt of the good graphite of electric conductivity and high catalytic activity.
The preparation method of a kind of carbon-cobalt oxygen evolution reaction catalysts of the present invention, concrete preparation process is as follows:
1) 0.24g cobalt chloride hexahydrate and 45.04g (mol ratio is 1:250) glucose are dissolved in deionized water to the solution that ultrasonic dispersion is uniformly mixed; By mixed solution heating water bath evaporate to dryness;
2) by the 1st) powder that obtains after step heating evaporate to dryness, under argon shield condition, be heated to 900 DEG C, and constant temperature keeps 1h, after naturally lowering the temperature, obtain carbon-cobalt black powder;
3) by the 2nd) black powder that obtains, be dissolved in the mixed solution of ethanol and naphthols; The mixed volume of isopropyl alcohol and naphthols is than being 978:22; And liquid deposition is upper in rotating disk electrode (r.d.e) (RDE), under 0.7Vvs.Ag/AgCl constant-pressure conditions, carry out electroxidation pretreatment, obtain carbon-cobalt oxygen evolution reaction catalysts.
Claims (6)
1. an oxygen evolution reaction eelctro-catalyst for carbon coating cobalt, is characterized in that: the nano composite material being made up of the oxide of graphite and cobalt.
2. a preparation method for the oxygen evolution reaction eelctro-catalyst of carbon coating cobalt, is characterized in that: concrete steps are as follows:
Step 1, by cobalt salt and carbon source, in molar ratio 1:(100～500) proportionate relationship put into deionized water dissolve mix; Then water bath method, obtains powder;
Step 2, by the powder of step 1 gained, under inert gas shielding, be heated to 400 DEG C～1000 DEG C, constant temperature keep 30min～120min obtain carbon coating cobalt simple substance;
Step 3, by the carbon coating cobalt simple substance of step 2 gained, be dissolved in the mixed solution of organic solvent and naphthols; The mixed volume of organic solvent and naphthols is than being (965～995): (35～5); Then be coated in rotating disk electrode (r.d.e), under the constant voltage condition of 0.5V～1.2V, carry out electroxidation pretreatment, obtain oxygen evolution reaction eelctro-catalyst.
3. the preparation method of the oxygen evolution reaction eelctro-catalyst of a kind of carbon coating cobalt as claimed in claim 2, is characterized in that: described cobalt salt is cobalt nitrate, cobalt chloride, cobaltous sulfate.
4. the preparation method of the oxygen evolution reaction eelctro-catalyst of a kind of carbon coating cobalt as claimed in claim 2, is characterized in that: described carbon source is urea, glucose, sucrose.
5. the preparation method of the oxygen evolution reaction eelctro-catalyst of a kind of carbon coating cobalt as claimed in claim 2, is characterized in that: described inert gas is nitrogen or argon gas.
6. the preparation method of the oxygen evolution reaction eelctro-catalyst of a kind of carbon coating cobalt as claimed in claim 2, is characterized in that: organic solvent comprises methyl alcohol, ethanol, isopropyl alcohol, dimethyl sulfoxide (DMSO), dimethyl formamide.
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| CN110193347B (en) * | 2019-06-06 | 2021-05-28 | 华南农业大学 | Nano carbon-coated cobaltous oxide and preparation method and application thereof |
| CN110193347A (en) * | 2019-06-06 | 2019-09-03 | 华南农业大学 | A kind of nano-sized carbon packet cobalt protoxide and its preparation method and application |
| CN110404577A (en) * | 2019-08-30 | 2019-11-05 | 安徽理工大学 | A kind of carbon-based phosphating sludge nano particle Electrocatalytic Activity for Hydrogen Evolution Reaction agent, preparation method and application |
| CN113088988A (en) * | 2021-03-23 | 2021-07-09 | 武汉理工大学 | Cobalt-doped foam carbon pyrolysis derived carbon material and preparation method thereof |
| CN113088988B (en) * | 2021-03-23 | 2024-01-23 | 武汉理工大学 | Cobalt-doped foam carbon pyrolysis derived carbon material and preparation method thereof |
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