CN109280934A - A kind of carbon-coated vanadium nitride elctro-catalyst, preparation method and application - Google Patents
A kind of carbon-coated vanadium nitride elctro-catalyst, preparation method and application Download PDFInfo
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- CN109280934A CN109280934A CN201811139985.0A CN201811139985A CN109280934A CN 109280934 A CN109280934 A CN 109280934A CN 201811139985 A CN201811139985 A CN 201811139985A CN 109280934 A CN109280934 A CN 109280934A
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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
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The present invention provides a kind of carbon-coated vanadium nitride elctro-catalysts, using rich carbon organic matter as carbon source, using metal vanadic salts as vanadium source, with urea, carbonic acid ammonia, ammonium hydrogen carbonate etc. for nitrogen source, passes through one-step calcination after mixing by Mechanical Method and obtain carbon-coated VN nanoparticle.Raw material of the present invention is cheap, and synthetic method is simple, and controllability is high.Gained VN is nano particle, and is coated by amorphous carbon layer, and the conductive capability of the material is improved.The carbon-coated VN nano material chemical composition of this method preparation is uniform, and purity and crystallinity are all higher, shows certain production hydrogen catalysis activity.
Description
Technical field
The invention belongs to be electrolysed aquatic products hydrogen catalyst technical field, and in particular to a kind of carbon-coated vanadium nitride electro-catalysis
Agent, preparation method and application.
Background technique
Since the shortage of the today's society energy, environmental pollution are sharply serious, hydrogen can store as one kind, is pollution-free, can
Regenerated high-grade energy carrier has been subjected to widely researching and developing.Water electrolysis hydrogen production method be a kind of easy to operate, technology at
Ripe large-scale hydrogen production process；But there is currently greatest problem be that power consumption is big, produce most effective needed for hydrogen urge
The noble metals such as agent Pt, Pd and its alloy price are high, and some non-precious metal catalysts include nickel or nickel-base material, metal vulcanization
Object, selenides, carbide, nitride, phosphide etc. are developed.Therefore cheap, rich content, catalytic activity are developed
High catalyst substitutes noble metal by extensive concern.
The advantages that vanadium nitride (VN) mechanical strength with higher, electron-transport rate, corrosion resistance, in chemistry, battery etc.
Field has a wide range of applications, colleague and very promising electrocatalysis material, therefore the carbon-coated vanadium nitride powder-body prepared
Is produced from hydrogen field in electro-catalysis to have great importance.
Application No. is the Chinese patent of CN101717076A " a kind of preparation method of vanadium nitride " by vanadium-containing compound with have
The mixing of machine nitride, calcines in nitrogenous gas, obtains vanadium nitride.The process of this method raw material preparation is more complex, preparation process
The parameter for needing to control is more, is applied to super capacitor material preparation field.
Application No. is the Chinese patent of CN107381515A " a kind of preparation of vanadium nitride elctro-catalyst and product " by urea,
Ammonium metavanadate and six nitric hydrates mix in proportion, are placed in tube furnace after being fully ground and are calcined to obtain a kind of powder nitridation
Vanadium product.
This work has prepared a kind of carbon-coated VN material by one-step calcination method, is mainly used in electro-catalysis and produces hydrogen neck
Domain.
Summary of the invention
The invention discloses a kind of preparation method of carbon-coated VN nanometer particle electrocatalyst and its as electro-catalysis
Crack the application in terms of aquatic products hydrogen catalyst.For the present invention using rich carbon organic matter as carbon source, metal vanadic salts is vanadium source, and rich nitrogen salt is nitrogen
Source, passed through after mixing by Mechanical Method one-step calcination obtain carbon-coated VN nanoparticle, materials chemistry composition it is uniform,
There is the production hydrogen elctro-catalyst of electro catalytic activity in acid and alkaline electrolyte.
In order to achieve the above object, the present invention adopts the following technical scheme:
Step 1: metal vanadic salts, rich carbon organic matter and nitrogen source are mixed to be placed in mortar and is ground first, is uniformly mixed
Close object；
Step 2: the air-tightness of tube furnace is checked；Obtained mixture, which is put into tube-type atmosphere furnace, to be calcined, and temperature range is
600-900 DEG C, soaking time 2-3h obtains black powder.
Compared with the prior art, the present invention at least has following beneficial effect:
1) synthesis material is cheap, and synthetic method is simple, and controllability is high；
2) gained VN is nano particle, and is coated by amorphous carbon layer, and the conductive capability of the material is improved；
3) this method prepares that carbon-coated VN nano material chemical composition is uniform, and purity and crystallinity are all higher；
4) it is a kind of novel water-splitting production hydrogen elctro-catalyst that this method, which prepares carbon-coated VN, shows certain production hydrogen catalysis
Activity.
Detailed description of the invention
Fig. 1 is X-ray diffraction (XRD) map of carbon coating VN prepared by the embodiment of the present invention 1；
Fig. 2 is scanning electron microscope (SEM) picture of carbon coating VN prepared by the embodiment of the present invention 2；
Fig. 3 is transmission electron microscope (TEM) picture of carbon coating VN prepared by the embodiment of the present invention 2；
Fig. 4 is production hydrogen LSV test chart of the carbon coating VN of the preparation of the embodiment of the present invention 3 under PH=0；
Fig. 5 is production hydrogen LSV test chart of the carbon coating VN of the preparation of the embodiment of the present invention 3 under PH=14.
Specific embodiment
With reference to the accompanying drawing and embodiment invention is further described in detail, it should be appreciated that below these examples only
Illustrate and not limit the scope of the present invention.Here it will be understood that the ability after having read the content of the invention authorized
Field technique personnel can make any change or modification to the present invention, these equivalences equally fall within the application the appended claims institute
The range of restriction.
Embodiment 1
Step 1: 400mg trithiocyanuric acid, 54mg vanadium trichloride and 0.5g urea are placed in mortar and are ground, raw material is made
Uniformly mixing, gained mixture is put into porcelain boat, porcelain boat is placed in tube-type atmosphere furnace, and in two furnaces of pipe both ends each side
Plug.
Step 2: being passed through inert gas into pipe, then carries out 8 pumping tonifying Qi, drains inner air tube, and last time is taken out
No longer tonifying Qi after gas, control intraductal atmospheric pressure are -1 ~ 0MPa；When air pressure is -1 ~ 0MPa, with the heating rate of 10 DEG C/min
700 DEG C are risen to, and keeps the temperature 3h；After heat preservation, air valve is opened immediately, inert gas is passed through with 700 ~ 800sccm air-flow, is discharged
The gas generated in insulating process will guarantee that cooling carries out under argon gas stream later.
Fig. 1 is X-ray diffraction (XRD) map of carbon coating vanadium nitride manufactured in the present embodiment；It can be seen that sample spreads out
Penetrate characteristic peak can index VN, diffraction maximum is sharp, and intensity is high, almost has no other impurity peaks appearance, illustrates its purity is high, knot
Crystalline substance is good.
Embodiment 2
Step 1: 377mg trithiocyanuric acid, 54mg vanadium trichloride and 0.5g urea are placed in mortar and are ground, mortar is made
Middle raw material uniformly mixes, and gained mixture is put into porcelain boat, porcelain boat is placed in tube-type atmosphere furnace, and in pipe both ends each side two
A furnace plug.
Step 2: being passed through inert gas into pipe, then carries out 5 pumping tonifying Qi, drains inner air tube, and last time is taken out
No longer tonifying Qi after gas, control intraductal atmospheric pressure are -1 ~ 0MPa；When air pressure is -1 ~ 0MPa, with the heating rate of 5 DEG C/min
800 DEG C are risen to, and keeps the temperature 2h；After heat preservation, air valve is opened immediately, inert gas is passed through with 700 ~ 800sccm air-flow, is discharged
The gas generated in insulating process will guarantee that cooling carries out under argon gas stream later.
Fig. 2 is scanning electron microscope (SEM) map of carbon coating VN manufactured in the present embodiment；It can be seen that sample is graininess.
Fig. 3 is transmission electron microscope (TEM) map of carbon coating VN manufactured in the present embodiment；It can be seen that sample is wrapped in nothing
In setting carbon.
Embodiment 3
Step 1: 400mg trithiocyanuric acid, 107mg ammonium metavanadate and 0.3g ammonium carbonate are placed in mortar and are ground, makes to grind
Raw material uniformly mixes in alms bowl, and gained mixture is put into porcelain boat, porcelain boat is placed in tube-type atmosphere furnace, and in pipe both ends each side
Two furnace plugs.
Step 2: being passed through inert gas into pipe, then carries out 8 pumping tonifying Qi, drains inner air tube, and last time is taken out
No longer tonifying Qi after gas, control intraductal atmospheric pressure are -1 ~ 0MPa；When air pressure is -1 ~ 0MPa, with the heating rate of 10 DEG C/min
600 DEG C are risen to, and keeps the temperature 3h；After heat preservation, air valve is opened immediately, inert gas is passed through with 700 ~ 800sccm air-flow, is discharged
The gas generated in insulating process will guarantee that cooling carries out under argon gas stream later.
Fig. 4 is production hydrogen test chart (LSV) map of carbon coating VN manufactured in the present embodiment in an acidic solution；It can be seen that
Carbon coating VN prepared by the present embodiment, under the test condition of pH=0, when current density is 10mA/cm2, sweep speed 5
When mV/s, which is 400mV, there is certain production hydrogen catalysis activity.
Fig. 5 is production hydrogen test chart (LSV) map of carbon coating VN manufactured in the present embodiment in alkaline solution；It can be seen that
Carbon coating VN prepared by the present embodiment, under the test condition of pH=14, when current density is 10mA/cm2, sweep speed 5
When mV/s, which is 310mV, there is certain production hydrogen catalysis activity.
Embodiment 4
Step 1: 400.8mg trithiocyanuric acid, the vanadium acetylacetonate of 118mg and 0.5g ammonium hydrogen carbonate are placed in mortar and carried out
Grinding, mixes raw material in mortar uniformly, gained mixture is put into porcelain boat, porcelain boat is placed in tube-type atmosphere furnace, and
Two furnace plugs of pipe both ends each side.
Step 2: being passed through inert gas into pipe, then carries out 8 pumping tonifying Qi, drains inner air tube, and last time is taken out
No longer tonifying Qi after gas, control intraductal atmospheric pressure are -1 ~ 0MPa；When air pressure is -1 ~ 0MPa, with the heating rate of 5 DEG C/min
900 DEG C are risen to, and keeps the temperature 2h；After heat preservation, air valve is opened immediately, inert gas is passed through with 700 ~ 800sccm air-flow, is discharged
The gas generated in insulating process will guarantee that cooling carries out under argon gas stream later.
Claims (9)
1. a kind of preparation method of carbon coating vanadium nitride elctro-catalyst, which comprises the following steps: by metal vanadic salts,
Rich carbon organic matter and nitrogen source are uniformly mixed by Mechanical Method, 600~900 DEG C of calcinings 2 under inert atmosphere protection of gained mixture
Carbon-coated vanadium nitride can be obtained in~3h.
2. a kind of preparation method of carbon-coated vanadium nitride elctro-catalyst according to claim 1, which is characterized in that described
Metal vanadic salts be one of vanadium trichloride, ammonium metavanadate, vanadium acetylacetonate or a variety of.
3. a kind of preparation method of carbon-coated vanadium nitride elctro-catalyst according to claim 1, which is characterized in that described
Rich carbon organic matter is trithiocyanuric acid.
4. a kind of preparation method of carbon-coated vanadium nitride elctro-catalyst according to claim 1, which is characterized in that nitrogen source
For one of urea, ammonium carbonate, ammonium hydrogen carbonate or a variety of.
5. a kind of preparation method of carbon-coated vanadium nitride elctro-catalyst according to claim 1, which is characterized in that mixing
Before object is calcined under inert atmosphere protection, guarantee the air-tightness of calcination environment by the following method: before calcining, into reaction vessel
It is passed through inert gas, then carries out 3 ~ 10 pumping tonifying Qi, drains the air in reaction vessel, last time is no longer mended after being evacuated
Gas, control intraductal atmospheric pressure are -1 ~ 0MPa.
6. a kind of preparation method of carbon-coated vanadium nitride elctro-catalyst according to claim 1, which is characterized in that calcining
When heating rate be 2 ~ 10 DEG C/min.
7. a kind of preparation method of carbon-coated vanadium nitride elctro-catalyst according to claim 1, which is characterized in that calcining
After, air valve is opened immediately, and inert gas is passed through with 500 ~ 1500sccm air-flow, the gas generated in insulating process is discharged,
To guarantee that cooling carries out under inert atmosphere stream later.
8. passing through a kind of carbon-coated vanadium nitride elctro-catalyst of any one of claim 1 ~ 7 the method preparation.
9. a kind of application of the carbon-coated vanadium nitride elctro-catalyst according to any one of claims 8 as electrolysis aquatic products hydrogen catalyst.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110681409A (en) * | 2019-10-23 | 2020-01-14 | 陕西科技大学 | Carbon tube supported ultra-small VN hydrogen production electrocatalyst, synthesis method and application |
| CN112919429A (en) * | 2019-12-06 | 2021-06-08 | 中国科学院过程工程研究所 | Preparation method of vanadium nitride, vanadium nitride prepared by preparation method and application of vanadium nitride |
| CN113135553A (en) * | 2021-04-22 | 2021-07-20 | 陕西科技大学 | Tungsten nitride coated vanadium nitride powder and preparation method and application thereof |
| CN113215614A (en) * | 2021-04-26 | 2021-08-06 | 陕西科技大学 | Carbon-layer-loaded tungsten-doped vanadium nitride nanoparticle composite electrocatalyst and preparation method and application thereof |
| CN113235129A (en) * | 2021-04-26 | 2021-08-10 | 陕西科技大学 | Vanadium nitride/tungsten carbide composite electrocatalyst and preparation method and application thereof |
| CN114635154A (en) * | 2020-12-15 | 2022-06-17 | 陕西科技大学 | Vanadium nitride/vanadium trioxide composite electro-catalytic material, preparation method and application thereof in aspect of hydrogen production by water cracking |
| CN114645283A (en) * | 2020-12-15 | 2022-06-21 | 陕西科技大学 | High-efficiency vanadium nitride/molybdenum carbide heterojunction hydrogen production electrocatalyst and preparation method and application thereof |
| CN114645284A (en) * | 2020-12-15 | 2022-06-21 | 陕西科技大学 | Three-phase system vanadium trioxide/vanadium nitride/molybdenum carbide nano electrode material and preparation method and application thereof |
| CN115010502A (en) * | 2022-05-25 | 2022-09-06 | 松山湖材料实验室 | Method for rapidly preparing nano vanadium nitride coated carbon fiber composite ceramic powder, product and application thereof |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110681409A (en) * | 2019-10-23 | 2020-01-14 | 陕西科技大学 | Carbon tube supported ultra-small VN hydrogen production electrocatalyst, synthesis method and application |
| CN112919429A (en) * | 2019-12-06 | 2021-06-08 | 中国科学院过程工程研究所 | Preparation method of vanadium nitride, vanadium nitride prepared by preparation method and application of vanadium nitride |
| CN114645283B (en) * | 2020-12-15 | 2024-02-09 | 陕西科技大学 | High-efficiency vanadium nitride/molybdenum carbide heterojunction hydrogen-producing electrocatalyst and preparation method and application thereof |
| CN114635154B (en) * | 2020-12-15 | 2023-12-19 | 陕西科技大学 | Vanadium nitride/vanadium trioxide composite electrocatalytic material, preparation method and application thereof in hydrogen production by water splitting |
| CN114645284B (en) * | 2020-12-15 | 2023-11-24 | 陕西科技大学 | Three-phase system vanadium trioxide/vanadium nitride/molybdenum carbide nano electrode material and preparation method and application thereof |
| CN114635154A (en) * | 2020-12-15 | 2022-06-17 | 陕西科技大学 | Vanadium nitride/vanadium trioxide composite electro-catalytic material, preparation method and application thereof in aspect of hydrogen production by water cracking |
| CN114645283A (en) * | 2020-12-15 | 2022-06-21 | 陕西科技大学 | High-efficiency vanadium nitride/molybdenum carbide heterojunction hydrogen production electrocatalyst and preparation method and application thereof |
| CN114645284A (en) * | 2020-12-15 | 2022-06-21 | 陕西科技大学 | Three-phase system vanadium trioxide/vanadium nitride/molybdenum carbide nano electrode material and preparation method and application thereof |
| CN113135553B (en) * | 2021-04-22 | 2022-11-04 | 陕西科技大学 | Tungsten nitride coated vanadium nitride powder and preparation method and application thereof |
| CN113135553A (en) * | 2021-04-22 | 2021-07-20 | 陕西科技大学 | Tungsten nitride coated vanadium nitride powder and preparation method and application thereof |
| CN113215614A (en) * | 2021-04-26 | 2021-08-06 | 陕西科技大学 | Carbon-layer-loaded tungsten-doped vanadium nitride nanoparticle composite electrocatalyst and preparation method and application thereof |
| CN113215614B (en) * | 2021-04-26 | 2022-02-11 | 陕西科技大学 | Carbon-layer-loaded tungsten-doped vanadium nitride nanoparticle composite electrocatalyst and preparation method and application thereof |
| CN113235129B (en) * | 2021-04-26 | 2022-02-11 | 陕西科技大学 | Vanadium nitride/tungsten carbide composite electrocatalyst and preparation method and application thereof |
| CN113235129A (en) * | 2021-04-26 | 2021-08-10 | 陕西科技大学 | Vanadium nitride/tungsten carbide composite electrocatalyst and preparation method and application thereof |
| CN115010502A (en) * | 2022-05-25 | 2022-09-06 | 松山湖材料实验室 | Method for rapidly preparing nano vanadium nitride coated carbon fiber composite ceramic powder, product and application thereof |
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