CN107416834A - A kind of method that gas template prepares hollow molybdenum carbide nanosphere - Google Patents
A kind of method that gas template prepares hollow molybdenum carbide nanosphere Download PDFInfo
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- CN107416834A CN107416834A CN201710764462.4A CN201710764462A CN107416834A CN 107416834 A CN107416834 A CN 107416834A CN 201710764462 A CN201710764462 A CN 201710764462A CN 107416834 A CN107416834 A CN 107416834A
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- deionized water
- ethyl alcohol
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of method that gas template prepares hollow molybdenum carbide nanosphere, including：According to following quality proportionings, solution is prepared：The mass ratio of four hydration ammonium paramolybdates and dopamine hydrochloride is 1：(0.25~2) is dissolved in deionized water, obtains solution A, the concentration of four hydration ammonium paramolybdates is 1g/mL；The preparation of the ethanol solution of certain gas saturation, obtains solution B；B solution is poured into step solution A, and stirred；To mixed solution and dripping 100~400uL concentrated ammonia liquors, 2~24h is reacted under room temperature and atmospheric pressure；Resulting solution centrifuges, and is washed with deionized water and absolute ethyl alcohol and be dried in vacuo again, obtains Red-brown powder.
Description
Technical field
The invention belongs to material preparation and energy field, and in particular to a kind of hollow Mo2C nano ball preparation method.
Background technology
In recent years, the nano material of hollow structure has been widely used in every field, such as medicament transport, wastewater treatment
And some other fields.Relative to other structures, the advantage of hollow structure is high specific surface area, adjustable porosity and infiltration
Property it is high.The method of synthesis hollow structure mainly has three kinds：(1) hard template method (2) soft template method (3) self-template method.Wherein, soft mode
Plate method not only avoid the step of removing template, and can design its inside and outside structure, while the production cost reduced.
According to the difference of template, soft template method includes emulsion template method, Micellar Gel method and hydrogen bubble template again.Bubble template is used in
Caused bubble is soft template to synthesize hollow nanostructures in liquid phase, building-up process include bubble generation and little particle in gas
The deposition on surface is steeped, further grows to form shell structurre by particle.
Mo2C is a kind of important transition metal carbonaceous, is a kind of high performance HER due to its electronic structure and platinum class seemingly
Catalyst, therefore widely studied by people.People have also prepared the Mo of various structures2C, such as medicine ball, tubulose, porous eight
Face body and nano wire etc..
The content of the invention
It is an object of the invention to provide the hollow Mo being made up of nanoscale twins2The simple and cost of C nano ball is cheap
Preparation method.This method is prepared hollow using four hydration ammonium paramolybdates, dopamine hydrochloride as raw material in alcohol-water mixed solution
Mo2C nano ball.The technical scheme that the present invention solves the technical problem is to provide the hollow Mo being made up of nanoscale twins2C nano
The preparation method of ball.
A kind of method that gas template prepares hollow molybdenum carbide nanosphere, comprises the following steps：
(1) according to following quality proportionings, solution is prepared：Four hydration ammonium paramolybdates and the mass ratio of dopamine hydrochloride are
1：(0.25~2) is dissolved in deionized water, obtains solution A, the concentration of four hydration ammonium paramolybdates is 1g/mL；
(2) preparation of the ethanol solution of certain gas saturation：In at room temperature and atmospheric pressure by H2、He、N2、O2, Ar or CO2
In a kind of gas be passed through in absolute ethyl alcohol, it is such a to obtain the ethanol solution of gas saturation, referred to as solution B；
(3) it is 1 according to the ratio between volume：The proportioning of (1~2.5), B solution is poured into step solution A, and stirred；
(4) to mixed solution and dripping 100~400uL concentrated ammonia liquors of step (3), reaction 2 under room temperature and atmospheric pressure~
24h；
(5) step (4) resulting solution is centrifuged, and is washed with deionized water and absolute ethyl alcohol and be dried in vacuo again, obtained red
Brown powder；
(6) by Red-brown powder in tube furnace H2700-800 DEG C of carbonization in/Ar mixed gas.
Compared with prior art, beneficial effect of the present invention is：
1) bubble is produced when the two is mixed using different solubility of the gas in alcohol and water, it is not necessary to add template
And template removal processes, technique is simple, cost is cheap.
2) the hollow Mo being made up of in preparation nanoscale twins2During C, by the species, the alcohol water that change saturated gas
Than and raw material proportioning can control hollow ball size.
Brief description of the drawings
Fig. 1-4 is that the present invention prepares hollow Mo respectively2C nano ball embodiment 1-4 SEM figures and TEM figures, left figure SEM
Figure, right figure are schemed for TEM.
Embodiment
Clear, complete description will be carried out to the technical scheme in the embodiment of the present invention below, it is clear that described implementation
Example is the part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the common skill in this area
The every other embodiment that art personnel are obtained on the premise of creative work is not made, belong to the model that the present invention protects
Enclose.
Embodiment 1
(1) according to following quality proportionings, solution is prepared：Four hydration ammonium paramolybdate 0.3g, dopamine hydrochloride 0.3g, go
Ionized water 30mL；
(2) preparation of the ethanol solution of certain gas saturation：In at room temperature and atmospheric pressure by CO2Gas is passed through absolute ethyl alcohol
In, bubbling 30min；
(3) absolute ethyl alcohol of step (2) is poured into the solution of step (1), and stirred, the volume of solution A and B solution
The ratio between volume is 1：2, the ratio between the volume of solution A and the volume of B solution are 1：2；
(4) to the mixed solution and dripping 300uL concentrated ammonia liquors of step (3), 3h is reacted under room temperature and atmospheric pressure；
(5) resulting solution is centrifuged, and washed with deionized water and absolute ethyl alcohol, 50 DEG C of vacuum drying, obtain bronzing
Powder；
(6) by the Red-brown powder obtained by step (5) in tube furnace H2750 DEG C of carbonization 120min in/Ar mixed gas.
After tested, hollow Mo2The size of C nano ball is 600-800nm.
Embodiment 2
(1) according to following quality proportionings, solution is prepared：Four hydration ammonium paramolybdate 0.3g, dopamine hydrochloride 0.3g, go
Ionized water 30mL；
(2) preparation of the ethanol solution of certain gas saturation：Ar gases are passed through absolute ethyl alcohol at room temperature and atmospheric pressure
In, bubbling 30min；
(3) absolute ethyl alcohol of step (2) is poured into the solution of step (1), and stirred；
(4) to the mixed solution and dripping 300uL concentrated ammonia liquors of step (3), 3h is reacted under room temperature and atmospheric pressure；
(5) resulting solution is centrifuged, and washed with deionized water and absolute ethyl alcohol, 50 DEG C of vacuum drying, obtain bronzing
Powder；
(6) by the Red-brown powder obtained by step (5) in tube furnace H2750 DEG C of carbonization 120min in/Ar mixed gas.
After tested, hollow Mo2The size of C nano ball is 200-300nm.
Embodiment 3
(1) according to following quality proportionings, solution is prepared：Four hydration ammonium paramolybdate 0.3g, dopamine hydrochloride 0.3g, go
Ionized water 30mL；
(2) preparation of the ethanol solution of certain gas saturation：In at room temperature and atmospheric pressure by O2Gas is passed through absolute ethyl alcohol
In, bubbling 30min；
(3) absolute ethyl alcohol of step (2) is poured into the solution of step (1), and stirred, the volume of solution A and B solution
The ratio between volume is 1：2；
(4) to the mixed solution and dripping 300uL concentrated ammonia liquors of step (3), 3h is reacted under room temperature and atmospheric pressure；
(5) resulting solution is centrifuged, and washed with deionized water and absolute ethyl alcohol, 50 DEG C of vacuum drying, obtain bronzing
Powder；
(6) by the Red-brown powder obtained by step (5) in tube furnace H2750 DEG C of carbonization 120min in/Ar mixed gas.
After tested, hollow Mo2The size of C nano ball is 500-600nm.
Embodiment 4
((1) prepares solution according to following quality proportionings：Four hydration ammonium paramolybdate 0.3g, dopamine hydrochloride 0.3g,
Deionized water 30mL；
(2) preparation of the ethanol solution of certain gas saturation：In at room temperature and atmospheric pressure by N2Gas is passed through absolute ethyl alcohol
In, bubbling 30min；
(3) absolute ethyl alcohol of step (2) is poured into the solution of step (1), and stirred, the volume of solution A and B solution
The ratio between volume is 1：2；
(4) to the mixed solution and dripping 300uL concentrated ammonia liquors of step (3), 3h is reacted under room temperature and atmospheric pressure；
(5) resulting solution is centrifuged, and washed with deionized water and absolute ethyl alcohol, 50 DEG C of vacuum drying, obtain bronzing
Powder；
(6) by the Red-brown powder obtained by step (5) in tube furnace H2750 DEG C of carbonization 120min in/Ar mixed gas.
After tested, hollow Mo2The size of C nano ball is 300-400nm.
The present invention does not address part and is applied to prior art.
Claims (1)
1. a kind of method that gas template prepares hollow molybdenum carbide nanosphere, comprises the following steps：
(1) according to following quality proportionings, solution is prepared：The mass ratio of four hydration ammonium paramolybdates and dopamine hydrochloride is 1：
(0.25~2) is dissolved in deionized water, obtains solution A, the concentration of four hydration ammonium paramolybdates is 1g/mL.
(2) preparation of the ethanol solution of certain gas saturation：In at room temperature and atmospheric pressure by H2、He、N2、O2, Ar or CO2In one
Kind gas is passed through in absolute ethyl alcohol, such a to obtain the ethanol solution of gas saturation, referred to as solution B；
(3) it is 1 according to the ratio between volume：The proportioning of (1~2.5), B solution is poured into step solution A, and stirred；
(4) to mixed solution and dripping 100~400uL concentrated ammonia liquors of step (3), 2~24h is reacted under room temperature and atmospheric pressure；
(5) step (4) resulting solution is centrifuged, and is washed with deionized water and absolute ethyl alcohol and be dried in vacuo again, obtain bronzing
Powder；
(6) by Red-brown powder in tube furnace H2700-800 DEG C of carbonization in/Ar mixed gas.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109921044A (en) * | 2019-03-22 | 2019-06-21 | 南方科技大学 | Fuel cell anode catalyst and preparation method thereof and proton exchange membrane fuel cell |
| CN110759328A (en) * | 2019-10-22 | 2020-02-07 | 济南大学 | Preparation method of hollow carbon micro-flower-loaded superfine molybdenum carbide material and application of hollow carbon micro-flower-loaded superfine molybdenum carbide material in lithium-sulfur battery |
| CN110918109A (en) * | 2019-12-19 | 2020-03-27 | 吉林大学 | Carbon/molybdenum carbide coated titanium dioxide composite photocatalytic water decomposition hydrogen production catalyst and preparation method thereof |
| CN113249735A (en) * | 2021-04-19 | 2021-08-13 | 北京化工大学 | Preparation method of efficient molybdenum carbide hydrogen evolution catalyst |
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| CN102070143A (en) * | 2010-02-11 | 2011-05-25 | 浙江工业大学 | Preparation method of mesoporous hollow sphere-shaped tungsten carbide |
| CN105016341A (en) * | 2015-07-15 | 2015-11-04 | 浙江大学 | Hollow carbide nanosphere with high specific surface area and preparation method thereof |
| CN105731463A (en) * | 2016-03-31 | 2016-07-06 | 华南理工大学 | Preparation method and application of molybdenum carbide microspheres |
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2017
- 2017-08-30 CN CN201710764462.4A patent/CN107416834B/en not_active Expired - Fee Related
Patent Citations (3)
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|---|---|---|---|---|
| CN102070143A (en) * | 2010-02-11 | 2011-05-25 | 浙江工业大学 | Preparation method of mesoporous hollow sphere-shaped tungsten carbide |
| CN105016341A (en) * | 2015-07-15 | 2015-11-04 | 浙江大学 | Hollow carbide nanosphere with high specific surface area and preparation method thereof |
| CN105731463A (en) * | 2016-03-31 | 2016-07-06 | 华南理工大学 | Preparation method and application of molybdenum carbide microspheres |
Non-Patent Citations (1)
| Title |
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| CHUNLI WANG ET AL.: "Formation of Mo–Polydopamine Hollow Spheres and Their Conversions to MoO2/C and Mo2C/C for Efficient Electrochemical Energy Storage and Catalyst", 《SMALL》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109921044A (en) * | 2019-03-22 | 2019-06-21 | 南方科技大学 | Fuel cell anode catalyst and preparation method thereof and proton exchange membrane fuel cell |
| CN109921044B (en) * | 2019-03-22 | 2021-09-24 | 南方科技大学 | Fuel cell anode catalyst and preparation method thereof and proton exchange membrane fuel cell |
| CN110759328A (en) * | 2019-10-22 | 2020-02-07 | 济南大学 | Preparation method of hollow carbon micro-flower-loaded superfine molybdenum carbide material and application of hollow carbon micro-flower-loaded superfine molybdenum carbide material in lithium-sulfur battery |
| CN110759328B (en) * | 2019-10-22 | 2022-05-27 | 济南大学 | Preparation method of hollow carbon micro-flower-loaded superfine molybdenum carbide material and application of hollow carbon micro-flower-loaded superfine molybdenum carbide material in lithium-sulfur battery |
| CN110918109A (en) * | 2019-12-19 | 2020-03-27 | 吉林大学 | Carbon/molybdenum carbide coated titanium dioxide composite photocatalytic water decomposition hydrogen production catalyst and preparation method thereof |
| CN110918109B (en) * | 2019-12-19 | 2021-08-13 | 吉林大学 | Carbon/molybdenum carbide coated titanium dioxide composite photocatalytic water decomposition hydrogen production catalyst and preparation method thereof |
| CN113249735A (en) * | 2021-04-19 | 2021-08-13 | 北京化工大学 | Preparation method of efficient molybdenum carbide hydrogen evolution catalyst |
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