CN108620110A - A kind of vanadium carbide/graphene nanometer sheet composite material, preparation method and its application in terms of hydrogen is produced in water-splitting - Google Patents
A kind of vanadium carbide/graphene nanometer sheet composite material, preparation method and its application in terms of hydrogen is produced in water-splitting Download PDFInfo
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- CN108620110A CN108620110A CN201810435342.4A CN201810435342A CN108620110A CN 108620110 A CN108620110 A CN 108620110A CN 201810435342 A CN201810435342 A CN 201810435342A CN 108620110 A CN108620110 A CN 108620110A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 42
- INZDTEICWPZYJM-UHFFFAOYSA-N 1-(chloromethyl)-4-[4-(chloromethyl)phenyl]benzene Chemical compound C1=CC(CCl)=CC=C1C1=CC=C(CCl)C=C1 INZDTEICWPZYJM-UHFFFAOYSA-N 0.000 title claims abstract description 33
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 239000001257 hydrogen Substances 0.000 title claims abstract description 20
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000013067 intermediate product Substances 0.000 claims abstract description 21
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 15
- 239000012298 atmosphere Substances 0.000 claims abstract description 12
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims abstract 2
- 229910021641 deionized water Inorganic materials 0.000 claims abstract 2
- 239000007864 aqueous solution Substances 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 229910052573 porcelain Inorganic materials 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 239000003643 water by type Substances 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 3
- 229930006000 Sucrose Natural products 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 239000007791 liquid phase Substances 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 26
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 230000003197 catalytic effect Effects 0.000 abstract description 7
- 239000002245 particle Substances 0.000 abstract description 6
- 238000006555 catalytic reaction Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 239000003792 electrolyte Substances 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 7
- 150000001336 alkenes Chemical class 0.000 description 5
- 239000004575 stone Substances 0.000 description 5
- 238000005336 cracking Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- -1 transition metal carbides Chemical class 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 description 1
- 229910039444 MoC Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
-
- B01J35/33—
-
- 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
-
- 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
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
-
- 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 discloses a kind of preparation methods of vanadium carbide/graphene nanometer sheet composite material, including：Prepare the presoma mixed liquor comprising graphene nanometer sheet, carbon source, ammonium metavanadate and deionized water；Hydro-thermal reaction is carried out to presoma mixed liquor, obtains powder intermediate product；It is fully ground intermediate product, is heat-treated in 700 1200 DEG C under atmosphere protection, vanadium carbide/graphene nanometer sheet composite material is obtained.The invention also discloses the application of this vanadium carbide/graphene nanometer sheet composite material and the material in terms of hydrogen is produced in water-splitting.Carrier graphene nanometer sheet in the present invention not only substantially increases the conductive capability of catalyst, while having disperseed vanadium carbide particle, to improve the catalytic activity of VC/GNS；Graphene in structure protects vanadium carbide particle, protects it from the corrosion of electrolyte, therefore can be used for the full pH value production hydrogen elctro-catalyst of the water-splitting in electro-catalysis field.
Description
Technical field
The present invention relates to the synthesis of catalyst and applied technical fields, and in particular to a kind of vanadium carbide/graphene nanometer sheet
Composite material, preparation method and its application in terms of cracking aquatic products hydrogen catalyst as electro-catalysis.
Background technology
The one kind of vanadium carbide material as transition metal carbide, the general characteristic with transition metal carbides, together
When there is good conduction, heat conduction, catalytic performance has a wide range of applications in physics, chemistry, Material Field.Conventional method（Such as
Carbothermic method, precursor process）Prepared vanadium carbide particle size is larger, mainly due in single-phase vanadium carbide sintering process
It is easy to happen agglomeration, is applied in ceramic industry field.And carbide（Molybdenum carbide, tungsten carbide etc.）Due to having similar platinum family
Metal electron structure is studied as splitting water catalyst extensively, and with excellent catalytic performance and good steady
It is qualitative.And pertinent literature of the vanadium carbide in electro-catalysis field only has several, therefore, it is necessary to explore and study vanadium carbide
Preparation method carries out structure regulating to single-phase vanadium carbide, to improve it as the performance of cracking aquatic products hydrogen catalyst.
According to document report in recent years, the structure regulating of carbide, mainly there is following means at present：(1) grain
Sub extra smallization；(2) heteroatomic modification；(3) various carrier design (calculated) load type catalyst are utilized, dispersibility and active table are improved
Face.In order to improve the catalytic activity and stability of vanadium carbide, vanadium carbide is carried on the surface of graphene nanometer sheet, stone by this work
Black alkene nanometer sheet is a kind of one-dimensional c-based nanomaterial, the physical and chemical performance that it has carbon nanomaterial excellent, such as highly conductive
Property, excellent mechanical property and good chemical stability etc..The growth in situ of vanadium carbide nano-particle can be supported, carbon is inhibited
Change the reunion of vanadium particle so that catalyst exposes more active sites, to improve the catalytic activity of composite material.
Invention content
The purpose of the present invention is to provide a kind of vanadium carbide/graphene nanometer sheets（VC/GNS）Composite material, preparation method
And its application in terms of cracking aquatic products hydrogen catalyst as electro-catalysis.
In order to achieve the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of VC/CNTs productions hydrogen elctro-catalyst, includes the following steps：
Step 1：Prepare the graphene nanometer sheet aqueous solution of the concentration 5mg/mL of enough volumes；
Step 2：Carbon source, ammonium metavanadate are weighed, mass ratio is（1-3）：1, it is placed in beaker, 20ml deionized waters is added, instill
Graphene nanometer sheet aqueous solution in the step of certain volume one, obtains presoma mixed liquor；
Step 3：The mixed liquor is placed in 50mL reaction kettles, and 160 DEG C of -200 DEG C of hydro-thermal reaction 12-24h are incited somebody to action after being cooled to room temperature
To powder centrifugation, washing alcohol wash alternately six times, vacuum drying, obtain intermediate product；
Step 4：Intermediate product is fully ground 20~50min, is placed in porcelain boat, is reacted in tube furnace under certain atmosphere, temperature
Ranging from 700-1200 DEG C, soaking time 2-5h of degree, heating rate are 10 DEG C/min, obtain VC/GNS production hydrogen elctro-catalysts.
Carbon source in above-mentioned steps two refers to one kind in citric acid, glucose, urea, sucrose；
Certain atmosphere in above-mentioned steps four refers to any one in argon gas, nitrogen, vacuum.
And a kind of VC/GNS prepared by the above method produces hydrogen elctro-catalyst, VC/GNS production hydrogen electricity prepared by the present invention
Catalyst, sample topography is uniform, and catalytic activity is high, and stability is good.
Compared with prior art, the present invention has technique effect beneficial below：
1）The synthesis strategy of VC/GNS of the present invention, the design for carbide elctro-catalyst provide thinking；
2）Carrier graphene nanometer sheet in the present invention not only substantially increases the conductive capability of catalyst, while having disperseed carbonization
Vanadium particle, to improve the catalytic activity of VC/GNS；
3）The full pH value production hydrogen of water-splitting that VC/GNS production hydrogen elctro-catalysts prepared by this method can be applied in electro-catalysis field
Elctro-catalyst protects it from the corrosion of electrolyte this is because the graphene in structure protects vanadium carbide particle.
Description of the drawings
Fig. 1 is the XRD diagram of the VC/GNS prepared in embodiment 1；
The TEM figures that Fig. 2 is the VC/GNS prepared in embodiment 4.
Specific implementation mode
Below in conjunction with the accompanying drawings and embodiment invention is further described in detail, it should be appreciated that these embodiments are only used
In illustrating rather than limit the scope of the invention.Here it will be understood that this field after having read the content of the invention authorized
Technical staff can make the present invention any change or modification, these equivalences equally fall within the application the appended claims and limited
Fixed range.
Embodiment 1
Step 1：Prepare the graphene nanometer sheet aqueous solution of 5mL concentration 5mg/mL；
Step 2：Citric acid 0.6g is weighed, ammonium metavanadate 0.3g is placed in beaker, and 20ml deionized waters are added, and instills 5mL stones
Black alkene nanometer sheet aqueous solution, obtains presoma mixed liquor；
Step 3：The mixed liquor is placed in 50mL reaction kettles, 160 DEG C of hydro-thermal reaction 12h, after being cooled to room temperature by obtained powder from
The heart, washing alcohol are washed alternately six times, and vacuum drying obtains intermediate product；
Step 4：Intermediate product is fully ground 20min, is placed in porcelain boat, is reacted in tube furnace under argon gas atmosphere, temperature model
It is 700 DEG C, soaking time 5h to enclose, and heating rate is 10 DEG C/min, obtains VC/GNS production hydrogen elctro-catalysts.
Fig. 1 is the XRD spectrum of the VC/GNS elctro-catalysts prepared by the present embodiment, and as can be seen from the figure sample is corresponding
VC standard PDF card numbers are 65-8819, and four diffraction maximums correspond to crystal face respectively（111）、（200）、（220）With（311）, diffraction
Peak is sharp, and intensity is high, illustrates that the vanadium carbide crystallinity that the embodiment obtains is fine.
Embodiment 2
Step 1：Prepare the graphene nanometer sheet aqueous solution of 10mL concentration 5mg/mL；
Step 2：Glucose 0.9g is weighed, ammonium metavanadate 0.3g is placed in beaker, and 20ml deionized waters are added, and instills 10mL stones
Black alkene nanometer sheet aqueous solution, obtains presoma mixed liquor；
Step 3：The mixed liquor is placed in 50mL reaction kettles, 180 DEG C of hydro-thermal reaction 18h, after being cooled to room temperature by obtained powder from
The heart, washing alcohol are washed alternately six times, and vacuum drying obtains intermediate product；
Step 4：Intermediate product is fully ground 40min, is placed in porcelain boat, is reacted in tube furnace under argon gas atmosphere, temperature model
It is 800 DEG C, soaking time 4h to enclose, and heating rate is 10 DEG C/min, obtains VC/GNS production hydrogen elctro-catalysts.
Embodiment 3
Step 1：Prepare the graphene nanometer sheet aqueous solution of 15mL concentration 5mg/mL；
Step 2：Urea 0.3g is weighed, ammonium metavanadate 0.3g is placed in beaker, and 20ml deionized waters are added, and instills 15mL graphite
Alkene nanometer sheet aqueous solution, obtains presoma mixed liquor；
Step 3：The mixed liquor is placed in 50mL reaction kettles, 200 DEG C of hydro-thermal reactions for 24 hours, after being cooled to room temperature by obtained powder from
The heart, washing alcohol are washed alternately six times, and vacuum drying obtains intermediate product；
Step 4：Intermediate product is fully ground 30min, is placed in porcelain boat, is reacted in tube furnace under nitrogen atmosphere, temperature model
It is 900 DEG C, soaking time 3h to enclose, and heating rate is 10 DEG C/min, obtains VC/GNS production hydrogen elctro-catalysts.
Embodiment 4
Step 1：Prepare the graphene nanometer sheet aqueous solution of 5mL concentration 5mg/mL；
Step 2：Sucrose 0.6g is weighed, ammonium metavanadate 0.3g is placed in beaker, and 20ml deionized waters are added, and instills 5mL graphite
Alkene nanometer sheet aqueous solution, obtains presoma mixed liquor；
Step 3：The mixed liquor is placed in 50mL reaction kettles, 160 DEG C of hydro-thermal reaction 12h, after being cooled to room temperature by obtained powder from
The heart, washing alcohol are washed alternately six times, and vacuum drying obtains intermediate product；
Step 4：Intermediate product is fully ground 50min, is placed in porcelain boat, is reacted in tube furnace under argon gas atmosphere, temperature model
It is 1000 DEG C, soaking time 2h to enclose, and heating rate is 10 DEG C/min, obtains VC/GNS production hydrogen elctro-catalysts.
Fig. 2 is the TEM collection of illustrative plates of the VC/GNS elctro-catalysts prepared by the present embodiment, as can be seen from the figure graphene sheet
Structure retains, and vanadium carbide nano-particle is dispersed on graphene film, and the electronics transfer that is combined into of the two provides channel, association
Same-action promotes the activity of catalyst.
Embodiment 5
Step 1：Prepare the graphene nanometer sheet aqueous solution of 10mL concentration 5mg/mL；
Step 2：Citric acid 0.9g is weighed, ammonium metavanadate 0.3g is placed in beaker, and 20ml deionized waters are added, and instills 10mL stones
Black alkene nanometer sheet aqueous solution, obtains presoma mixed liquor；
Step 3：The mixed liquor is placed in 50mL reaction kettles, 180 DEG C of hydro-thermal reactions for 24 hours, after being cooled to room temperature by obtained powder from
The heart, washing alcohol are washed alternately six times, and vacuum drying obtains intermediate product；
Step 4：Intermediate product is fully ground 20min, is placed in porcelain boat, is reacted in tube furnace under argon gas atmosphere, temperature model
It is 1100 DEG C, soaking time 2h to enclose, and heating rate is 10 DEG C/min, obtains VC/GNS production hydrogen elctro-catalysts.
Embodiment 6
Step 1：Prepare the graphene nanometer sheet aqueous solution of 15mL concentration 5mg/mL；
Step 2：Glucose 0.3g is weighed, ammonium metavanadate 0.3g is placed in beaker, and 20ml deionized waters are added, and instills 15mL stones
Black alkene nanometer sheet aqueous solution, obtains presoma mixed liquor；
Step 3：The mixed liquor is placed in 50mL reaction kettles, 200 DEG C of hydro-thermal reaction 18h, after being cooled to room temperature by obtained powder from
The heart, washing alcohol are washed alternately six times, and vacuum drying obtains intermediate product；
Step 4：Intermediate product is fully ground 30min, is placed in porcelain boat, is reacted in tube furnace under argon gas atmosphere, temperature model
It is 1200 DEG C, soaking time 1h to enclose, and heating rate is 10 DEG C/min, obtains VC/GNS production hydrogen elctro-catalysts.
Claims (10)
1. a kind of preparation method of vanadium carbide/graphene nanometer sheet composite material, which is characterized in that include the following steps：
Prepare the presoma mixed liquor comprising graphene nanometer sheet, carbon source, ammonium metavanadate and deionized water；Presoma is mixed
Liquid carries out hydro-thermal reaction, obtains powder intermediate product；It is fully ground intermediate product, is carried out in 700-1200 DEG C under atmosphere protection hot
Processing, obtains vanadium carbide/graphene nanometer sheet composite material.
2. a kind of preparation method of vanadium carbide/graphene nanometer sheet composite material according to claim 1, feature exist
In：The carbon source is one or more of citric acid, glucose, urea, sucrose.
3. a kind of preparation method of vanadium carbide/graphene nanometer sheet composite material according to claim 1, feature exist
In：The presoma mixed liquor is the mixture for including following components：
Graphene is not more than 1 mass parts
Carbon source 4-12 mass parts
4 mass parts of ammonium metavanadate
Water is enough.
4. a kind of preparation method of vanadium carbide/graphene nanometer sheet composite material according to claim 1 or 2 or 3, special
Sign is：The presoma mixed liquor is obtained by method comprising the following steps：
Prepare graphene nanometer sheet aqueous solution；And
By the proportioning of carbon source in formula and ammonium metavanadate, the mixed liquor for including carbon source and ammonium metavanadate is prepared；And
By the proportioning of graphene in formula and ammonium metavanadate, by graphene nanometer sheet aqueous solution and include carbon source and ammonium metavanadate
Blended liquid phase mixing, obtain presoma mixed liquor.
5. a kind of preparation method of vanadium carbide/graphene nanometer sheet composite material according to claim 1, feature exist
In：The condition that presoma mixed liquor carries out hydro-thermal reaction is, in 160 DEG C of -200 DEG C of hydro-thermal reaction 12-24h.
6. a kind of preparation method of vanadium carbide/graphene nanometer sheet composite material according to claim 1, feature exist
In：The time that intermediate product is heat-treated under atmosphere protection is 2-5h.
7. a kind of preparation method of vanadium carbide/graphene nanometer sheet composite material according to claim 1, feature exist
In：Used atmosphere protection is one kind in argon gas, nitrogen, vacuum when heat treatment.
8. a kind of preparation method of vanadium carbide/graphene nanometer sheet composite material according to claim 1, feature exist
In specific steps include：
Step 1：Prepare the graphene nanometer sheet aqueous solution of the concentration 5mg/mL of enough volumes；
Step 2：In mass ratio（1-3）：1 weighs carbon source and ammonium metavanadate, is dissolved in enough ionized waters, and with step
Graphene nanometer sheet aqueous solution in rapid one mixes, and obtains presoma mixed liquor；
Step 3：By presoma mixed liquor in 160 DEG C of -200 DEG C of hydro-thermal reaction 12-24h, the powder that will be obtained after being cooled to room temperature
Centrifugation, washing alcohol are washed alternately six times, and vacuum drying obtains intermediate product；
Step 4：Intermediate product is fully ground, is placed in porcelain boat, is reacted in tube furnace under certain atmosphere, temperature range is
700-1200 DEG C, soaking time 2-5h, heating rate is 10 DEG C/min, obtains vanadium carbide/graphene nanometer sheet composite material.
9. vanadium carbide/graphene nanometer sheet composite material prepared by any one of claim 1-8 methods.
10. application of the vanadium carbide/graphene nanometer sheet composite material in terms of hydrogen is produced in water-splitting described in claim 9.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113578358A (en) * | 2021-05-26 | 2021-11-02 | 东莞理工学院 | Pt/NVC-g-C3N4Photocatalytic material and preparation method and application thereof |
| CN114042467A (en) * | 2020-07-23 | 2022-02-15 | 陕西科技大学 | Ultrathin carbon layer composite material modified by nano nickel cluster and vanadium carbide particles and preparation method and application thereof |
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