CN104056630B - A kind of preparation method of oxygen evolution reaction eelctro-catalyst of carbon coating cobalt - Google Patents
A kind of preparation method of oxygen evolution reaction eelctro-catalyst of carbon coating cobalt Download PDFInfo
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- CN104056630B CN104056630B CN201410305400.3A CN201410305400A CN104056630B CN 104056630 B CN104056630 B CN 104056630B CN 201410305400 A CN201410305400 A CN 201410305400A CN 104056630 B CN104056630 B CN 104056630B
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- oxygen evolution
- evolution reaction
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Abstract
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.Preparation method of the present invention: after first carbon source and cobalt salt being put in proportion water dissolving mixing, evaporate to dryness under the water bath condition of 50 DEG C ~ 80 DEG C, the powder be uniformly mixed; It carried out being heated to 400 DEG C ~ 1000 DEG C under protective gas condition, calcining 30min ~ 120min obtains carbon coating cobalt simple substance again; Finally use the method for electrochemical pre-treatment, obtain the nano particle with the oxide-simple substance cobalt of the carbon-coating-cobalt of conductive core shell structure.Method step of the present invention is simple, easy to operate, requires low, improve the security in experimentation to Preparation equipment.Adopt the oxide of carbon-coating-cobalt of preparing of the inventive method-simple substance cobalt uniform diameter, good conductivity, and there is good electro-catalysis Water oxidize 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 thermodynamic electric potential of water decomposition.The oxygen evolution reaction catalysts that current activity is the highest 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 developing high catalytic activity is most important.
In recent years, the oxide of transition metal oxide especially cobalt is because of its aboundresources, and catalytic performance is excellent and paid close attention to widely.But with RuO
2and IrO
2compare, it is low still to there is catalytic current density in these catalyst, the problems such as overpotential is higher, poor stability, and the synthetic method of catalyst is often also more complicated.
Summary of the invention
The object of the invention is have that catalytic current density is low, overpotential is higher, poor stability problem to solve existing catalyst, 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 be made up of 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 one, by cobalt salt and carbon source, in molar ratio 1:(100 ~ 500) proportionate relationship put into deionized water dissolve mixing; Then water bath method, obtains powder;
Step 2, by the powder of step one gained, be heated to 400 DEG C ~ 1000 DEG C under inert gas shielding, constant temperature keeps 30min ~ 120min to 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 catalyst that oxygen evolution reaction (OER) is good, and when overpotential is 320mV, current density is 10mAcm
-2, Tafel slope reaches 58mV/dec, and stability is better than IrO
2, can RuO be substituted
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 in-situ oxidation on electrode, 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.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of spherical carbon coating cobalt simple substance under amplification 50000 times prepared by embodiment 1;
Fig. 2 is the scanning electron microscope (SEM) photograph (SEM) of spherical carbon coating cobalt simple substance under amplification 240000 times prepared by embodiment 1;
Fig. 3 is the high power transmission electron microscope picture (TEM) of spherical carbon coating cobalt simple substance prepared by embodiment 1;
Fig. 4 is the scanning electron microscope (SEM) photograph (SEM) of oxygen evolution reaction catalysts under amplification 10000 times of spherical carbon coating cobalt prepared by embodiment 1;
Fig. 5 is the transmission electron microscope picture (TEM) of the oxygen evolution reaction catalysts of spherical carbon coating cobalt prepared by embodiment 1;
Fig. 6 is the oxygen evolution reaction catalysts high power transmission electron microscope picture (HRTEM) of spherical carbon coating cobalt prepared by embodiment 1;
Fig. 7 is the x-ray photoelectron energy spectrogram (XPS) of the oxygen evolution reaction catalysts of spherical carbon coating cobalt prepared by embodiment 1;
Fig. 8 is that the oxygen evolution reaction catalysts of spherical carbon coating cobalt prepared by embodiment 1 compares with the cobalt powder after electrochemical treatments the impedance diagram obtained;
Fig. 9 is oxygen evolution reaction catalysts and the RuO of spherical carbon coating cobalt prepared by embodiment 1
2and IrO
2oxygen evolution reaction Performance comparision figure;
Figure 10 is oxygen evolution reaction catalysts and the RuO of spherical carbon coating cobalt prepared by embodiment 1
2and IrO
2tafel slope of curve comparison diagram;
Figure 11 is oxygen evolution reaction catalysts and the RuO of spherical carbon coating cobalt prepared by 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 under amplification 5000 times that embodiment 2 prepares;
Figure 13 is the oxygen evolution reaction polarization curve of carbon-cobalt oxygen evolution reaction catalysts that embodiment 2 prepares.
Figure 14 is the oxygen evolution reaction polarization curve of carbon-cobalt oxygen evolution reaction catalysts that embodiment 3 prepares.
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 that the oxide of the graphite good by electric conductivity and the cobalt of high catalytic activity forms.
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, the solution that ultrasonic disperse is uniformly mixed; Mixed solution heating water bath evaporate to dryness, obtains powder;
2) by the 1st) step heating evaporate to dryness after obtain powder, under argon shield condition, be heated to 900 DEG C, and constant temperature keep 1h, obtain carbon coating cobalt simple substance black powder after Temperature fall;
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; By liquid deposition 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 uniform diameter of bead.
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 process, obtain carbon coating cobalt oxygen evolution reaction catalysts, can find out that a lot of nano particle appears in bead surface.
As shown in Figure 6, can see that the surface of spherical carbon coating cobalt oxygen evolution reaction catalysts is carbon-coating and cobaltosic oxide by high power TEM collection of illustrative plates.
As shown in Figure 7, by XPS collection of illustrative plates, prove that cobaltosic oxide is contained on the surface of spherical carbon coating cobalt oxygen evolution reaction catalysts further;
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 process, and the resistance of curve 1 is 10 ohm, the resistance of curve 2 is 125 ohm, and the electric conductivity demonstrating the former is better than the latter;
As shown in Figure 9, abscissa represents the change 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 oxidize current density that curve 1 reaches is greater than curve 2 and curve 3, and the catalytic performance demonstrating 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, the logarithm value of the current density that course of reaction that what abscissa represented is produces, ordinate represents the change 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, and the oxygen evolution reaction catalytic performance further demonstrating spherical carbon bag cobalt oxygen evolution reaction catalysts prepared by embodiment 1 is better than IrO
2and RuO
2.
As shown in figure 11, the change of what abscissa represented is current potential in oxygen evolution reaction process, ordinate represents the reaction time.Curve 1 is 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, and the stability demonstrating 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 that the oxide of the graphite good by electric conductivity and the cobalt of high catalytic activity forms.
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, the solution that ultrasonic disperse 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, obtains carbon-cobalt black powder after Temperature fall;
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 by liquid deposition 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, and long is 1-2 μm;
As shown in figure 13, abscissa represents the change 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 that the oxide of the graphite good by electric conductivity and the cobalt of high catalytic activity forms.
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, the solution that ultrasonic disperse 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, obtains carbon-cobalt black powder after Temperature fall;
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 by liquid deposition 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 change 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 that the oxide of the graphite good by electric conductivity and the cobalt of high catalytic activity forms.
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, the solution that ultrasonic disperse 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, obtains carbon-cobalt black powder after Temperature fall;
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 by liquid deposition 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 that the oxide of the graphite good by electric conductivity and the cobalt of high catalytic activity forms.
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, the solution that ultrasonic disperse 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, obtains carbon-cobalt black powder after Temperature fall;
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 by liquid deposition 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 (4)
1. a preparation method for the oxygen evolution reaction eelctro-catalyst of carbon coating cobalt, is characterized in that: concrete steps are as follows:
Step one, by cobalt salt and carbon source, in molar ratio 1:(100 ~ 500) proportionate relationship put into deionized water dissolve mixing; Then water bath method, obtains powder;
Step 2, by the powder of step one gained, be heated to 400 DEG C ~ 1000 DEG C under inert gas shielding, constant temperature keeps 30min ~ 120min to 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.
2. the preparation method of the oxygen evolution reaction eelctro-catalyst of a kind of carbon coating cobalt as claimed in claim 1, is characterized in that: described cobalt salt is cobalt nitrate, cobalt chloride, cobaltous sulfate.
3. the preparation method of the oxygen evolution reaction eelctro-catalyst of a kind of carbon coating cobalt as claimed in claim 1, is characterized in that: described carbon source is urea, glucose, sucrose.
4. the preparation method of the oxygen evolution reaction eelctro-catalyst of a kind of carbon coating cobalt as claimed in claim 1, is characterized in that: organic solvent comprises methyl alcohol, ethanol, isopropyl alcohol, dimethyl sulfoxide (DMSO), dimethyl formamide.
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| CN105552393B (en) * | 2016-01-22 | 2018-03-30 | 中南大学 | A kind of alkaline water system metal-air batteries bifunctional catalyst and preparation method thereof |
| CN109072458A (en) | 2016-04-18 | 2018-12-21 | 沙特基础工业全球技术公司 | The analysis oxygen elctro-catalyst of cobalt (II, III) oxide skin(coating) containing carbon coating |
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| CN108262048B (en) * | 2018-01-25 | 2020-04-28 | 北京化工大学 | Carbon-coated cobalt tungstate composite material and application thereof in electrocatalytic oxygen evolution reaction |
| CN109004239B (en) * | 2018-08-10 | 2019-05-14 | 南京晓庄学院 | A kind of Co of P doping3S4Nanometer sheet and its preparation method and application |
| CN109513442B (en) * | 2018-09-28 | 2022-01-07 | 中国林业科学研究院林产化学工业研究所 | NaBH4Hydrogen production catalyst Co-CoOx@ C-rGO and preparation method thereof |
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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 |
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