CN114232015A - Tubular MoO2Preparation and application of/C composite material - Google Patents
Tubular MoO2Preparation and application of/C composite material Download PDFInfo
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- CN114232015A CN114232015A CN202210021461.1A CN202210021461A CN114232015A CN 114232015 A CN114232015 A CN 114232015A CN 202210021461 A CN202210021461 A CN 202210021461A CN 114232015 A CN114232015 A CN 114232015A
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- 239000002131 composite material Substances 0.000 title claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000000243 solution Substances 0.000 claims abstract description 40
- 238000003756 stirring Methods 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 239000008367 deionised water Substances 0.000 claims abstract description 21
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 21
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- QXYJCZRRLLQGCR-UHFFFAOYSA-N molybdenum(IV) oxide Inorganic materials O=[Mo]=O QXYJCZRRLLQGCR-UHFFFAOYSA-N 0.000 claims abstract description 13
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 11
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 11
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 11
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 11
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 11
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 11
- 229960001149 dopamine hydrochloride Drugs 0.000 claims abstract description 11
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 10
- 239000000725 suspension Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000007772 electrode material Substances 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims description 12
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 238000007664 blowing Methods 0.000 claims description 2
- 239000002073 nanorod Substances 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims 1
- 238000003760 magnetic stirring Methods 0.000 abstract description 14
- RFHAOTPXVQNOHP-UHFFFAOYSA-N fluconazole Chemical compound C1=NC=NN1CC(C=1C(=CC(F)=CC=1)F)(O)CN1C=NC=N1 RFHAOTPXVQNOHP-UHFFFAOYSA-N 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- 239000001257 hydrogen Substances 0.000 description 10
- 229910052739 hydrogen Inorganic materials 0.000 description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 9
- 238000002484 cyclic voltammetry Methods 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 7
- 239000010411 electrocatalyst Substances 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000007605 air drying Methods 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229910020647 Co-O Inorganic materials 0.000 description 2
- 229910020704 Co—O Inorganic materials 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- 230000003442 weekly effect Effects 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 229910003178 Mo2C Inorganic materials 0.000 description 1
- 244000183331 Nephelium lappaceum Species 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001588 bifunctional effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- IUYLTEAJCNAMJK-UHFFFAOYSA-N cobalt(2+);oxygen(2-) Chemical compound [O-2].[Co+2] IUYLTEAJCNAMJK-UHFFFAOYSA-N 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(II) oxide Inorganic materials [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- SXTLQDJHRPXDSB-UHFFFAOYSA-N copper;dinitrate;trihydrate Chemical compound O.O.O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O SXTLQDJHRPXDSB-UHFFFAOYSA-N 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- QZRHHEURPZONJU-UHFFFAOYSA-N iron(2+) dinitrate nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QZRHHEURPZONJU-UHFFFAOYSA-N 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- FYFFGSSZFBZTAH-UHFFFAOYSA-N methylaminomethanetriol Chemical compound CNC(O)(O)O FYFFGSSZFBZTAH-UHFFFAOYSA-N 0.000 description 1
- 239000011325 microbead Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000002074 nanoribbon Substances 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 235000007861 rambutan Nutrition 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention relates to a tubular MoO2Preparation and application of the/C composite material. The preparation method comprises the following steps: firstly, 65% of HNO is measured3 2 mL，H2Preparing O9.5 mL into a mixed solution, adding 0.5 g of ammonium molybdate, stirring until the solution is transparent, carrying out hydrothermal reaction at the reaction temperature of 200 ℃ for 20 hours, and then carrying out centrifugal drying. Then putting 0.1 g of the obtained product into a small beaker, adding 20 mL of deionized water, carrying out ultrasonic treatment, adding 0.05 g of dopamine hydrochloride, stirring to obtain an orange red suspension, adding 40 mL of ethanol, carrying out magnetic stirring for 5 min, adding 0.3 mL of ammonia water, carrying out magnetic stirring for 2 h, and carrying out centrifugal drying on the obtained solution. And finally, heating to 750 ℃ under Ar condition, and preserving heat for 4 h to obtain a final sample. The preparation method is simple in preparation process, high in yield and controllable; prepared tubular MoO2the/C composite material has the advantages of stable structure, excellent electrochemical performance, low overpotential and the like, and is very suitable forCan be used as an electrode material in the field of electrocatalysis.
Description
Technical Field
The invention belongs to the technical field of new energy electronic materials, and relates to a tubular MoO2Preparation and application of the/C composite material.
Background
With the exhaustion of fossil fuels and the growing environmental problem, the development of renewable and sustainable alternative energy sources has led to extensive research by researchers. Hydrogen is an important green energy source, has the characteristics of reproducibility, abundant resources, no pollution and the like, and therefore becomes a research hotspot in the field of clean energy. At present, among many methods for preparing hydrogen, hydrogen production by water electrolysis is a hydrogen production method with great development prospect, and is widely used due to the advantages of high efficiency, zero emission and the like. At present, inThe catalyst with the best performance in the hydrogen production reaction by water electrolysis is noble metal Pt, but the application of the catalyst in the hydrogen production direction by water electrolysis is limited due to the defects of high scarcity and cost and the like. Compared with noble metal catalysts, non-noble metal materials represented by transition metal oxides are cheap and easily available, and are beneficial to realizing large-scale application of the transition metal oxides. At present, molybdenum dioxide hydrogen evolution catalyst is considered to be one of catalysts with better development prospect, MoO2The adsorption free energy of hydrogen atoms at the edge is very close to that of metal Pt, which is MoO2Provides the possibility of being an effective hydrogen evolution electrocatalyst which shows good catalytic activity in catalyzing the HER reaction. Weekly et al have synthesized the CoP @ Mo-Co-O hollow microsphere similar to rambutan as a HER electrocatalyst, and have shown strong long-term stability and excellent cycling stability thanks to the unique three-dimensional space structure and interface effect between Mo-Co-O. (Zhouwen, Wumamom, Ligaoren rambutan-Douginose shaped cobalt phosphide @ molybdenum cobaltous oxide hollow micro beads for basic electrocatalytic hydrogen evolution [ J]Catalytic school, 2020(4). Mo prepared by Fan et al2The C Nanocrystals (NCs) are immobilized on vertically aligned graphene nanoribbons (VA-GNR) and exhibit high activity and long-lasting electrocatalytic properties for Hydrogen Evolution Reactions (HER) and Oxygen Reduction Reactions (ORR). (Nanotechnology; Reports from Rice University Advance Knowledge in Nanotechnology (Atomic H-Induced Mo2C Hybrid as an Active and Stable Bifunctional Electron analysis) [ J]. Nanotechnology Weekly,2017,11(1):384-394）。
Chinese patent document CN111359611A discloses a preparation method of FeCu/C electrocatalyst, which comprises the following steps: soaking a piece of foam nickel into hydrochloric acid with the mass fraction of 5% for 10 minutes, then taking out the foam nickel, carrying out ultrasonic treatment in acetone for 15 minutes, and then respectively washing with deionized water and ethanol once; weighing 0.5 mmol of iron nitrate nonahydrate, 0.5 mmol of copper nitrate trihydrate, 10 mmol of urea and 4 mmol of ammonium fluoride in 30 mL of water to form a yellow solution; then transferring the solution into a reaction kettle with the volume of 50 mL, and soaking the treated foamed nickel into the solution; reacting the reaction kettle at 140 ℃ for 24 hours; naturally cooling to room temperature, taking out the foamed nickel, respectively washing with deionized water and ethanol once, and drying at 60 ℃ for 24 hours to obtain a precursor a; preparing a trihydroxymethyl aminomethane solution with the pH value of 8.5, and weighing polypyrrole according to the concentration of 3 mg/mL to dissolve in the solution; placing the precursor a in the solution for 10 minutes to obtain a precursor b; and sintering the precursor b for 24 hours at 700 ℃ in an argon atmosphere to obtain the FeCu/C electrocatalyst, wherein the FeCu/C electrocatalyst is attached to the surface of the foamed nickel. But the electrocatalytic performance of the electrode material prepared by the method has larger promotion space.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a tubular MoO with low overpotential2A preparation method of the/C composite material.
According to the invention, a tubular MoO2The preparation method of the/C composite material comprises the following steps:
(1) measuring 65% of HNO3 1~3 mL，H2Preparing a mixed solution by using 9.5 mL of O;
(2) adding 0.2-0.5 g of ammonium molybdate into the mixed solution obtained in the step (1), and stirring until the solution is transparent;
(3) transferring the solution obtained in the step (2) to a 20 mL hydrothermal reaction kettle, putting the hydrothermal reaction kettle into an oven, heating to 200 ℃, and keeping the temperature for 20 hours;
(4) centrifuging the solution obtained in the step (3), washing for 3 times by deionized water and ethanol at the rotating speed of 5000-6000 r/min;
(5) blowing and drying the product obtained in the step (4) at 70 ℃ to obtain MoO2A nanorod;
(6) putting 0.1 g of the product obtained in the step (5) into a small beaker, adding 20 mL of deionized water, and carrying out ultrasonic treatment for 15 min;
(7) dissolving 0.02-0.08 g of dopamine hydrochloride in the solution obtained in the step (6), and stirring to obtain an orange-red suspension;
(8) adding 40 mL of ethanol into the solution obtained in the step (7), and magnetically stirring for 5 min;
(9) quickly adding 0.1-0.5 mL of ammonia water into the solution obtained in the step (8), and magnetically stirring for 2 hours;
(10) centrifuging the solution obtained in the step (9) at the speed of 800 r/min, and then washing with deionized water or ethanol;
(11) putting the product obtained in the step (10) into a vacuum drying oven, and drying for 12 hours;
(12) and (3) heating the product obtained in the step (11) to 700-900 ℃ under Ar condition, preserving the heat for 4-6 h, and increasing the temperature at a rate of 5 ℃/min to obtain a final sample.
According to the invention, it is preferred that 65% of the HNO is taken in step (1)3 2 mL。
According to the present invention, it is preferable that the mass of ammonium molybdate added in step (2) is 0.5 g.
According to the present invention, it is preferable that the mass of dopamine hydrochloride added in the step (7) is 0.05 g.
According to the present invention, it is preferred that the volume of the aqueous ammonia added in step (10) is 0.3 mL.
According to the present invention, it is preferable that the reaction temperature in the step (12) is 750oC。
According to the present invention, it is preferred that the incubation time in step (12) is 4 hours.
Tubular MoO2Application of the/C composite material to electrocatalytic electrode materials.
The technical advantages of the invention are as follows:
(1) the preparation method is simple in preparation process, easy to operate and short in time consumption.
(2) The gelatin fiber prepared by the invention has excellent electrochemical performance and stable structure, and has the current density of 10 mA cm-2The overpotential is only 350 mV, which is superior to the reported carbon-based metal-free electrocatalyst.
Drawings
FIG. 1 is a tubular MoO made in example 1 of the present invention2Transmission electron micrograph of the/C composite.
FIG. 2 is a tubular MoO made in example 1 of the present invention2Linear cyclic voltammogram of the/C composite.
Detailed Description
The present invention will be further described with reference to the following embodiments and drawings, but is not limited thereto.
Meanwhile, the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1:
firstly, 65% of HNO is measured3 2 mL，H2O9.5 mL, resulting in 65% HNO3And H2The volume ratio of O is 1: 5, preparing a mixed solution, adding 0.5 g of ammonium molybdate into the mixed solution, stirring until the solution is transparent, transferring the solution into a 20 mL hydrothermal reaction kettle, putting the hydrothermal reaction kettle into an oven, heating to 200 ℃, keeping the temperature for 20 hours, centrifuging, washing for 3 times by using deionized water and ethanol, and carrying out forced air drying on the obtained product at 70 ℃.
Then putting 0.1 g of the obtained product into a small beaker, adding 20 mL of deionized water, carrying out ultrasonic treatment for 15 min, adding 0.05 g of dopamine hydrochloride, stirring to obtain an orange red suspension, adding 40 mL of ethanol, carrying out magnetic stirring for 5 min, adding 0.3 mL of ammonia water, rapidly stirring for 2 min, and then carrying out magnetic stirring for 2 h. The obtained solution is centrifuged at the speed of 800 r/min, then washed by ethanol, and the obtained product is put into a vacuum drying oven and dried for 12 hours. And finally, heating to 750 ℃ under Ar condition, preserving the heat for 4 h, and obtaining the final sample, wherein the heating rate is 5 ℃/min.
Adopting a three-electrode system, in 1 mol/L KOH electrolyte, the sweep rate is 2 mV s-1Linear cyclic voltammetry tests were performed under conditions.
Tubular MoO made in this example2The transmission electron microscope image of the/C composite material is shown in FIG. 1, and the catalyst grows more uniformly as can be seen from FIG. 1.
Tubular MoO made in this example2The linear cyclic voltammogram of the/C composite is shown in FIG. 2, and it can be seen from FIG. 2 that the current density is 10 mA cm-2The overpotential is only 350 mV, which shows that the catalyst in this example has excellent performance.
Example 2:
firstly, 65% of HNO is measured3 1 mL，H2O9.5 mL, preparing a mixed solution, mixing 0.5 gAdding ammonium molybdate into the mixed solution, stirring until the solution is transparent, transferring the solution into a 20 mL hydrothermal reaction kettle, putting the hydrothermal reaction kettle into an oven, heating to 200 ℃, keeping the temperature for 20 hours, centrifuging, washing for 3 times by using deionized water and ethanol, and carrying out air-blast drying on the obtained product at 70 ℃.
Then putting 0.1 g of the obtained product into a small beaker, adding 20 mL of deionized water, carrying out ultrasonic treatment for 15 min, adding 0.05 g of dopamine hydrochloride, stirring to obtain an orange red suspension, adding 40 mL of ethanol, carrying out magnetic stirring for 5 min, adding 0.3 mL of ammonia water, rapidly stirring for 2 min, and then carrying out magnetic stirring for 2 h. The obtained solution is centrifuged at the speed of 800 r/min, then washed by ethanol, and the obtained product is put into a vacuum drying oven and dried for 12 hours. And finally, heating to 750 ℃ under Ar condition, preserving the heat for 4 h, and obtaining the final sample, wherein the heating rate is 5 ℃/min.
Adopting a three-electrode system, in 1 mol/L KOH electrolyte, the sweep rate is 2 mV s-1Linear cyclic voltammetry tests were performed under conditions.
Example 3:
firstly, 65% of HNO is measured3 2 mL，H2O9.5 mL, resulting in 65% HNO3And H2The volume ratio of O is 1: 5, preparing a mixed solution, adding 0.2 g of ammonium molybdate into the mixed solution, stirring until the solution is transparent, transferring the solution into a 20 mL hydrothermal reaction kettle, putting the hydrothermal reaction kettle into an oven, heating to 200 ℃, keeping the temperature for 20 hours, centrifuging, washing for 3 times by using deionized water and ethanol, and carrying out forced air drying on the obtained product at 70 ℃.
Then putting 0.1 g of the obtained product into a small beaker, adding 20 mL of deionized water, carrying out ultrasonic treatment for 15 min, adding 0.05 g of dopamine hydrochloride, stirring to obtain an orange red suspension, adding 40 mL of ethanol, carrying out magnetic stirring for 5 min, adding 0.3 mL of ammonia water, rapidly stirring for 2 min, and then carrying out magnetic stirring for 2 h. The obtained solution is centrifuged at the speed of 800 r/min, then washed by ethanol, and the obtained product is put into a vacuum drying oven and dried for 12 hours. And finally, heating to 750 ℃ under Ar condition, preserving the heat for 4 h, and obtaining the final sample, wherein the heating rate is 5 ℃/min.
Adopting a three-electrode system, in 1 mol/L KOH electrolyte, the sweep rate is 2 mV s-1Linear cyclic voltammetry tests were performed under conditions.
Example 4:
firstly, 65% of HNO is measured3 2 mL，H2O9.5 mL, resulting in 65% HNO3And H2The volume ratio of O is 1: 5, preparing a mixed solution, adding 0.5 g of ammonium molybdate into the mixed solution, stirring until the solution is transparent, transferring the solution into a 20 mL hydrothermal reaction kettle, putting the hydrothermal reaction kettle into an oven, heating to 200 ℃, keeping the temperature for 20 hours, centrifuging, washing for 3 times by using deionized water and ethanol, and carrying out forced air drying on the obtained product at 70 ℃.
Then putting 0.1 g of the obtained product into a small beaker, adding 20 mL of deionized water, carrying out ultrasonic treatment for 15 min, adding 0.07 g of dopamine hydrochloride, stirring to obtain an orange red suspension, adding 40 mL of ethanol, carrying out magnetic stirring for 5 min, adding 0.3 mL of ammonia water, rapidly stirring for 2 min, and then carrying out magnetic stirring for 2 h. The obtained solution is centrifuged at the speed of 800 r/min, then washed by ethanol, and the obtained product is put into a vacuum drying oven and dried for 12 hours. And finally, heating to 750 ℃ under Ar condition, preserving the heat for 4 h, and obtaining the final sample, wherein the heating rate is 5 ℃/min.
Adopting a three-electrode system, in 1 mol/L KOH electrolyte, the sweep rate is 2 mV s-1Linear cyclic voltammetry tests were performed under conditions.
Example 5:
firstly, 65% of HNO is measured3 2 mL，H2O9.5 mL, resulting in 65% HNO3And H2The volume ratio of O is 1: 5, preparing a mixed solution, adding 0.5 g of ammonium molybdate into the mixed solution, stirring until the solution is transparent, transferring the solution into a 20 mL hydrothermal reaction kettle, putting the hydrothermal reaction kettle into an oven, heating to 200 ℃, keeping the temperature for 20 hours, centrifuging, washing for 3 times by using deionized water and ethanol, and carrying out forced air drying on the obtained product at 70 ℃.
Then putting 0.1 g of the obtained product into a small beaker, adding 20 mL of deionized water, carrying out ultrasonic treatment for 15 min, adding 0.05 g of dopamine hydrochloride, stirring to obtain an orange red suspension, adding 40 mL of ethanol, carrying out magnetic stirring for 5 min, adding 0.5 mL of ammonia water, rapidly stirring for 2 min, and then carrying out magnetic stirring for 2 h. The obtained solution is centrifuged at the speed of 800 r/min, then washed by ethanol, and the obtained product is put into a vacuum drying oven and dried for 12 hours. And finally, heating to 750 ℃ under Ar condition, preserving the heat for 4 h, and obtaining the final sample, wherein the heating rate is 5 ℃/min.
Adopting a three-electrode system, in 1 mol/L KOH electrolyte, the sweep rate is 2 mV s-1Linear cyclic voltammetry tests were performed under conditions.
Example 6:
firstly, 65% of HNO is measured3 1.9 mL，H2O9.5 mL, resulting in 65% HNO3And H2The volume ratio of O is 1: 5, preparing a mixed solution, adding 0.4 g of ammonium molybdate into the mixed solution, stirring until the solution is transparent, transferring the solution into a 20 mL hydrothermal reaction kettle, putting the hydrothermal reaction kettle into an oven, heating to 200 ℃, keeping the temperature for 20 hours, centrifuging, washing for 3 times by using deionized water and ethanol, and carrying out forced air drying on the obtained product at 70 ℃.
Then putting 0.1 g of the obtained product into a small beaker, adding 20 mL of deionized water, carrying out ultrasonic treatment for 15 min, adding 0.05 g of dopamine hydrochloride, stirring to obtain an orange red suspension, adding 40 mL of ethanol, carrying out magnetic stirring for 5 min, adding 0.5 mL of ammonia water, rapidly stirring for 2 min, and then carrying out magnetic stirring for 2 h. The obtained solution is centrifuged at the speed of 800 r/min, then washed by ethanol, and the obtained product is put into a vacuum drying oven and dried for 12 hours. And finally, heating to 800 ℃ under Ar condition, preserving the heat for 6 h, and obtaining the final sample, wherein the heating rate is 5 ℃/min.
Adopting a three-electrode system, in 1 mol/L KOH electrolyte, the sweep rate is 2 mV s-1Linear cyclic voltammetry tests were performed under conditions.
Claims (8)
1. Tubular MoO2The preparation method of the/C composite material comprises the following steps:
(1) measuring 65% of HNO3 1~3 mL，H2Preparing a mixed solution by using 9.5 mL of O;
(2) adding 0.2-0.5 g of ammonium molybdate into the mixed solution obtained in the step (1), and stirring until the solution is transparent;
(3) transferring the solution obtained in the step (2) to a 20 mL hydrothermal reaction kettle, putting the hydrothermal reaction kettle into an oven, heating to 200 ℃, and keeping the temperature for 20 hours;
(4) centrifuging the solution obtained in the step (3), washing for 3 times by deionized water and ethanol at the rotating speed of 5000-6000 r/min;
(5) blowing and drying the product obtained in the step (4) at 70 ℃ to obtain MoO2A nanorod;
(6) putting 0.1 g of the product obtained in the step (5) into a small beaker, adding 20 mL of deionized water, and carrying out ultrasonic treatment for 15 min;
(7) dissolving 0.02-0.08 g of dopamine hydrochloride in the solution obtained in the step (6), and stirring to obtain an orange-red suspension;
(8) adding 40 mL of ethanol into the solution obtained in the step (7), and magnetically stirring for 5 min;
(9) quickly adding 0.1-0.5 mL of ammonia water into the solution obtained in the step (8), and magnetically stirring for 2 hours;
(10) centrifuging the solution obtained in the step (9) at the speed of 800 r/min, and then washing with deionized water or ethanol;
(11) putting the product obtained in the step (10) into a vacuum drying oven, and drying for 12 hours;
(12) and (3) heating the product obtained in the step (11) to 700-900 ℃ under Ar condition, preserving the heat for 4-6 h, and increasing the temperature at a rate of 5 ℃/min to obtain a final sample.
2. The tubular MoO of claim 12The preparation method of the/C composite material is characterized in that 65 percent of HNO in the step (1)3The addition amount is 2 mL, H2The amount of O added was 9.5 mL.
3. The tubular MoO of claim 12The preparation method of the/C composite material is characterized in that the mass of the ammonium molybdate added in the step (2) is 0.5 g.
4. The tubular MoO of claim 12The preparation method of the/C composite material is characterized in that the mass of the dopamine hydrochloride added in the step (7) is 0.05 g.
5. The tubular MoO of claim 12The preparation method of the/C composite material is characterized in that the volume of the ammonia water added in the step (10) is 0.3 mL.
6. The tubular MoO of claim 12The method for preparing the/C composite material is characterized in that the reaction temperature in the step (12) is 750oC。
7. The tubular MoO of claim 12The preparation method of the/C composite material is characterized in that the heat preservation time in the step (12) is 4 hours.
8. Tubular MoO2Application of the/C composite material in an electrode material for electrocatalytic oxygen evolution.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115477374A (en) * | 2022-07-21 | 2022-12-16 | 贵州大学 | MoO (MoO) 2 Preparation and application methods of @ NHCS hollow structure material |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108971509A (en) * | 2018-07-31 | 2018-12-11 | 上海工程技术大学 | A kind of preparation method of the iron-nickel alloy nano material of controllable grain size |
| CN109037664A (en) * | 2018-07-05 | 2018-12-18 | 华南理工大学 | A kind of carbon-coated Mo of N doping2The preparation method of C/C functional composite material and its application in lithium-sulfur cell |
| CN109399722A (en) * | 2018-12-27 | 2019-03-01 | 陕西科技大学 | A kind of preparation method of porous rodlike molybdenum dioxide/carbon composite |
| CN109967107A (en) * | 2019-05-06 | 2019-07-05 | 曾婉艺 | A kind of porous structure Mo2C/C composite material and preparation method |
-
2022
- 2022-01-10 CN CN202210021461.1A patent/CN114232015A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109037664A (en) * | 2018-07-05 | 2018-12-18 | 华南理工大学 | A kind of carbon-coated Mo of N doping2The preparation method of C/C functional composite material and its application in lithium-sulfur cell |
| CN108971509A (en) * | 2018-07-31 | 2018-12-11 | 上海工程技术大学 | A kind of preparation method of the iron-nickel alloy nano material of controllable grain size |
| CN109399722A (en) * | 2018-12-27 | 2019-03-01 | 陕西科技大学 | A kind of preparation method of porous rodlike molybdenum dioxide/carbon composite |
| CN109967107A (en) * | 2019-05-06 | 2019-07-05 | 曾婉艺 | A kind of porous structure Mo2C/C composite material and preparation method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115477374A (en) * | 2022-07-21 | 2022-12-16 | 贵州大学 | MoO (MoO) 2 Preparation and application methods of @ NHCS hollow structure material |
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