CN117210854A - Preparation method of carbon cloth in-situ growth cobalt oxide nanosheets - Google Patents
Preparation method of carbon cloth in-situ growth cobalt oxide nanosheets Download PDFInfo
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- CN117210854A CN117210854A CN202311176325.0A CN202311176325A CN117210854A CN 117210854 A CN117210854 A CN 117210854A CN 202311176325 A CN202311176325 A CN 202311176325A CN 117210854 A CN117210854 A CN 117210854A
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 26
- 239000004744 fabric Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910000428 cobalt oxide Inorganic materials 0.000 title claims abstract description 8
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 8
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 title claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- 150000001868 cobalt Chemical class 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 4
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 claims description 2
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000012300 argon atmosphere Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 30
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 21
- 239000001257 hydrogen Substances 0.000 abstract description 21
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 21
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 230000008569 process Effects 0.000 abstract description 9
- 238000005868 electrolysis reaction Methods 0.000 abstract description 8
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 239000007772 electrode material Substances 0.000 abstract description 5
- 230000005540 biological transmission Effects 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 239000010411 electrocatalyst Substances 0.000 abstract description 4
- 239000002243 precursor Substances 0.000 abstract description 4
- 238000009792 diffusion process Methods 0.000 abstract description 2
- 238000012546 transfer Methods 0.000 abstract description 2
- 239000002064 nanoplatelet Substances 0.000 description 14
- 238000001000 micrograph Methods 0.000 description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- DSVGQVZAZSZEEX-UHFFFAOYSA-N [C].[Pt] Chemical compound [C].[Pt] DSVGQVZAZSZEEX-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 210000002969 egg yolk Anatomy 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000000703 high-speed centrifugation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000012430 stability testing Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- -1 transition metal cobalt oxide Chemical class 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000004832 voltammetry Methods 0.000 description 1
- 238000001075 voltammogram Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention belongs to the technical field of hydrogen production electrocatalysts by water electrolysis, and discloses a preparation method of a carbon cloth in-situ growth cobalt oxide nano-sheet. The invention is used for preparing Co (OH) 2 The conditions used in the CC precursor process are mild, which is beneficial to reducing the preparation cost of the material; co (OH) is used in preparing CoO/CC nano-sheets 2 CC is a precursor, and CO (OH) can be realized through heat treatment 2 Complete conversion to CoO; the material is loaded on the carbon cloth, so that the electron transmission speed of CoO can be improved, and the electron transmission path can be shortened, thereby accelerating the charge transfer of the material in the hydrogen electrolysis process of waterAnd ion diffusion rate; in the heat treatment process, the material maintains the original three-dimensional reticular structure, and the CoO/CC nano electrode material of the structure has large specific surface area and more active sites, thereby being beneficial to improving the HER activity of the material; the three-dimensional network structure of the material ensures that the material has good stability in the process of electrolyzing water to produce hydrogen.
Description
Technical Field
The invention belongs to the technical field of hydrogen production electrocatalysts by water electrolysis, and particularly relates to a preparation method of a three-dimensional netlike transition metal cobalt oxide electrocatalyst formed by nano sheets in situ grown on a carbon cloth substrate.
Background
In recent years, with the widespread use of fossil fuels, serious energy and environmental crisis have arisen, forcing people to seek alternative energy sources. The hydrogen energy is widely focused by a plurality of scientific researchers because of the advantages of high combustion value, green pollution-free property and the like, and the hydrogen production process equipment for electrolyzing water is simply considered as the hydrogen production technology with the most application prospect. Currently, platinum-based materials are the best catalysts for water electrolysis hydrogen production due to their low overpotential and high current density, however the high cost and scarcity of such materials limit their practical application. Therefore, there is a need to develop and design green, efficient and inexpensive catalysts for producing hydrogen by electrolysis of water.
Recently, the transition metal cobalt-based nano material is found to be an efficient electrocatalyst for hydrogen evolution reaction, and has wide application prospect in the fields of super capacitors, lithium ion batteries and the like. However, cobalt-based nanomaterials have the disadvantage of poor conductivity and unstable structure during hydrogen evolution. Research shows that constructing special shapes such as spheres, yolk shells, lines and the like is an effective means for improving the hydrogen production performance of the electrode material by water electrolysis (Sci.Adv., 2019,5, eaav 6009). Wherein the two-dimensional structure can increase the specific surface area of the material, increase the catalytic active site and improve the catalytic activity of the material (ACS appl. Mater. Interfaces,2018,10,25409-25414). However, the nanomaterial size of the lamellar structure is difficult to control and stacking occurs easily to reduce the electrochemical activity of the material. In addition, conventional electrode materials often require the use of binders in the fabrication of the electrode, resulting in a reduction in the active sites of the material. Therefore, the material is loaded on the conductive substrate, so that not only can the conductivity of the material be increased, but also the material can be directly used as an electrode material.
Disclosure of Invention
Aiming at the problems, a preparation method for preparing the carbon cloth supported two-dimensional cobalt oxide (CoO/CC) nanosheets by combining a hydrothermal method with a heat treatment process at a lower temperature is developed. The preparation method has the advantages of low cost, simplicity, convenience, rapidness, mild conditions, good product morphology reproducibility and stable structure. Meanwhile, the prepared material is a three-dimensional network structure formed by crosslinking nano sheets, and the structure can increase the specific surface area of the material, so that more active sites are exposed, and the stability of the material is greatly improved while the activity of the material is improved. Electrochemical test results show that the hydrogen production performance of the cobalt oxide nano-sheet in-situ grown on the carbon cloth substrate is improved, and the hydrogen production performance of the prepared catalyst is superior to that of commercial Pt/C. The prepared material is expected to be widely applied to the fields of electrochemical energy storage, photocatalysis, water electrolysis and the like.
The technical scheme of the invention is as follows:
the preparation method of the carbon cloth in-situ growth cobalt oxide nano sheet comprises the following steps:
by HNO respectively 3 Absolute alcohol and deionized carbon cloth; then, cobalt salt and hexamethylenetetramine are dissolved in deionized water, and uniform mixed solution is obtained after stirring for 20-50 min; immersing the treated carbon cloth into the mixed solution, and carrying out hydrothermal reaction at the temperature of 80-100 ℃ for 8-12h; taking out carbon cloth, cleaning, oven drying at 50-80deg.C to obtain cobalt hydroxide nanosheets (Co (OH) 2 CC); co (OH) 2 placing/CC in a tube furnace, and treating at 450-750deg.C for 0.5-2.5 hr at a heating rate of 3.5-6.5 deg.C/min under argon gas at a flow rate of 35-55sccm to obtain CoO/CC nanosheets.
The molar ratio of the cobalt salt to the hexamethylenetetramine is 1:2, and the concentration of the cobalt salt in the mixed solution is 0.167mol L -1 。
The invention has the beneficial effects that: the invention is used for preparing Co (OH) 2 The conditions used in the CC precursor process are mild, which is beneficial to reducing the preparation cost of the material; co (OH) is used in preparing CoO/CC nano-sheets 2 CC is a precursor, viaThe heat treatment can realize CO (OH) 2 Complete conversion to CoO; after the material is loaded on the carbon cloth, the electron transmission speed of CoO can be improved, and the electron transmission path can be shortened, so that the charge transfer and ion diffusion rate of the material in the hydrogen electrolysis process of water can be accelerated; in the heat treatment process, the material maintains the original three-dimensional reticular structure, and the CoO/CC nano electrode material of the structure has large specific surface area and more active sites, thereby being beneficial to improving the HER activity of the material; the three-dimensional network structure of the material ensures that the material has good stability in the process of electrolyzing water to produce hydrogen.
Drawings
FIG. 1 is Co (OH) 2 XRD patterns of/CC and CoO/CC nanoplatelets.
FIG. 2 is Co (OH) 2 Scanning electron microscope image of CC nanosheets, a at 5 μm size, b at 2 μm size.
FIG. 3 is a scanning electron microscope image of CoO/CC nanoplatelets, a at a size of 5 μm and b at a size of 500 nm.
FIG. 4 is a scanning electron microscope image of CoO nanoplatelets, a at a size of 1 μm and b at a size of 500 nm.
FIG. 5 is CC, co (OH) 2 LSV polarization curves of/CC, coO (aq.)/CC, coO/CC and Pt/CC in 0.5M sulfuric acid.
FIG. 6 is Co (OH) 2 Impedance diagrams of/CC, coO (aq.)/CC and CoO/CC from 0.01Hz to 100 KHz.
FIG. 7 is a stability curve of CoO/CC nanoplatelets.
FIG. 8 is a scanning electron microscope image of the CoO/CC nanoplatelets after stability testing.
Detailed Description
The following describes the embodiments of the present invention further with reference to the drawings and technical schemes.
Co(OH) 2 Preparation of CC nanosheets: 1X 1cm -2 Before using, pre-treating with concentrated nitric acid (95 vol.%), immersing overnight, sequentially ultrasonic cleaning with absolute ethyl alcohol and deionized water for 3 times, and drying in a vacuum drying oven at 60 ℃ for 10h. 5mmol Co (NO) was stirred 3 ) 2 ·6H 2 O and 10mmol HMT were dissolved in 30mL deionized water in sequenceTransferring the solution to a reaction kettle after 30min, adding the treated carbon cloth, performing hydrothermal reaction at 100 ℃ for 10h, cooling to room temperature, taking out the carbon cloth, cleaning the carbon cloth with ethanol and deionized water respectively, and drying in a vacuum oven at 60 ℃ overnight. Finally, co (OH) is obtained 2 CC nanoplatelets.
Preparation of CoO/CC nanosheets: co (OH) 2 Placing the/CC nano-sheets in a tubular furnace, treating for 1h at 600 ℃ under the protection of argon, heating at a rate of 5 ℃/min, cooling, respectively flushing the carbon cloth with absolute ethyl alcohol and secondary water, and drying in a vacuum oven at 60 ℃ for 8h to obtain the CoO/CC nano-sheets.
Preparation of CoO nanoplatelets: in order to study the influence of carbon cloth on material performance, the method is adopted to prepare the CoO nano-sheet. Carbon cloth is not added in the hydrothermal process, and Co (OH) is obtained by adopting a high-speed centrifugation method after the hydrothermal reaction is completed 2 A nano-sheet. The solvent in the centrifugation process is absolute ethanol and secondary water, and the rotating speed is 7000r min -1 The centrifugation time was 5min each time. Drying the solid sample in a vacuum oven at 60 ℃ overnight after centrifugation to finally obtain Co (OH) 2 A nano-sheet. Carrying out high-temperature treatment on the dried solid sample, carrying out high-temperature treatment for 1h at 600 ℃ under the protection of argon, wherein the heating rate is 5 ℃/min, and after cooling, respectively centrifugally washing the sample with absolute ethyl alcohol and secondary water at the rotating speed of 7000r min -1 And (3) centrifuging for 5min each time, and drying the centrifuged solid sample in a vacuum oven at 60 ℃ for 8h to obtain the CoO nano-sheets.
For testing electrochemical hydrogen production performance
The hydrogen production performance test method comprises the following steps: three-electrode system, saturated calomel electrode (reference electrode), graphite rod (counter electrode), coO/CC (working electrode), electrolyte of 0.5. 0.5M H 2 SO 4 A solution. Introducing nitrogen for 30min to remove oxygen before testing, wherein the test method comprises linear voltammetry and sweep speed of 2mV/s; electrochemical impedance method with frequency range of 0.1Hz-10 5 Hz, amplitude of 5mV; timing current curve method, current density 10mA/cm -2 . The test voltage was corrected to the hydrogen electrode formula: e (vs. rhe) =e (vs. sce) +0.242V. Preparation of CoO nanoplatelet working electrode: the material was dispersed in a water/ethanol mixture containing 950uL 1:1 (v: v) and 50uL5 wt%And (3) dripping a certain amount of solution into the Nafion solution on the pretreated carbon cloth, and drying at room temperature to obtain the electrode.
As can be seen from XRD patterns of the samples (FIG. 1), co (OH) can be prepared in one step by using a hydrothermal method 2 CC nanosheets, co (OH) 2 the/CC nano-sheets can be completely converted into CoO/CC nano-sheets by heat treatment. Co (OH) obtained by hydrothermal method 2 The CC nanoplatelets are uniform two-dimensional platelet structures (fig. 2), the nanoplatelets are about 35nm thick, and the two-dimensional nanoplatelets are connected together to form a three-dimensional network structure. The CoO/CC nanoplatelets (FIG. 3) still maintain the original three-dimensional network structure after heat treatment. The CoO nanoplatelets (fig. 4) obtained without adding carbon cloth have uneven microstructures such as thickness, size and the like, and the nanoplatelets are piled together and do not form a net structure.
Fig. 5 is a linear voltammogram of the prepared sample and bare carbon cloth. As can be seen from the graph, the CoO nano-sheets grown in situ on the carbon cloth show optimal hydrogen production activity, and the current density is 10mAcm -2 When the overvoltage of the CoO/CC nano-sheet is only 22mV, which is lower than the overvoltage (26 mV) of the commercial platinum carbon. From the impedance plot of the sample, coO/CC has more excellent conductivity at the same voltage. FIG. 7 is a graph of sample stability with no significant change in current density after 18 hours. The scanning electron microscope image (figure 8) of the sample after the stability test shows that the morphology of the sample is not changed obviously, which indicates that the prepared sample has good hydrogen production stability.
Claims (5)
1. The preparation method of the carbon cloth in-situ growth cobalt oxide nano-sheet is characterized by comprising the following steps:
by HNO respectively 3 Absolute alcohol and deionized carbon cloth; then, cobalt salt and hexamethylenetetramine are dissolved in deionized water, and uniform mixed solution is obtained after stirring for 20-50 min; immersing the treated carbon cloth into the mixed solution, and carrying out hydrothermal reaction at the temperature of 80-100 ℃ for 8-12h; taking out the carbon cloth, cleaning, and drying to obtain cobalt hydroxide nanosheets Co (OH) 2 CC; co (OH) 2 placing/CC in a tube furnace, and treating at 450-750deg.C for 0.5-2.5 hr under argon atmosphere to obtain CoO/CC nanosheets.
2. The method according to claim 1, wherein the heating rate of the tube furnace is 3.5-6.5 ℃/min.
3. The method according to claim 1, wherein the drying temperature is 50-80 ℃.
4. The method of claim 1, wherein the argon gas has a flow rate of 35-55sccm.
5. The preparation method according to claim 1, wherein the molar ratio of cobalt salt to hexamethylenetetramine is 1:2, and the concentration of cobalt salt in the mixed solution is 0.167mol L -1 。
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311176325.0A CN117210854A (en) | 2023-09-13 | 2023-09-13 | Preparation method of carbon cloth in-situ growth cobalt oxide nanosheets |
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