CN110228797A - A kind of method that low cost prepares two-dimentional molybdenum nitride or tungsten nitride nanometer sheet - Google Patents
A kind of method that low cost prepares two-dimentional molybdenum nitride or tungsten nitride nanometer sheet Download PDFInfo
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- CN110228797A CN110228797A CN201810826139.XA CN201810826139A CN110228797A CN 110228797 A CN110228797 A CN 110228797A CN 201810826139 A CN201810826139 A CN 201810826139A CN 110228797 A CN110228797 A CN 110228797A
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- molybdenum
- tungsten
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
- C01B21/062—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with chromium, molybdenum or tungsten
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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
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
Abstract
The invention discloses a kind of methods that low cost prepares two-dimentional molybdenum nitride or tungsten nitride nanometer sheet, belong to field of nano material preparation.The present invention is primary raw material using molybdenum concentrate (molybdenum disulfide) or tungsten disulfide, and a certain amount of sodium carbonate is added, nitridation reaction is carried out between in high temperature furnace 600-900 DEG C of ammonia atmosphere.Then by product washing, filtering and the drying after reaction, two-dimentional molybdenum nitride or tungsten nitride nanometer sheet are obtained.The lower molybdenum concentrate of use cost (molybdenum disulfide) of the present invention or tungsten disulfide and sodium carbonate are primary raw material, can reduce production cost.This method high production efficiency, simple process are suitble to that two-dimentional molybdenum nitride or tungsten nitride nanometer sheet is mass produced.
Description
Technical field
The invention belongs to field of nano material preparation, discloses a kind of low cost and prepare two-dimentional molybdenum nitride or tungsten nitride nanometer
The method of piece.
Background technique
Molybdenum nitride and tungsten nitride have very unique physics and a chemical characteristic, such as the hardness, excellent of high-melting-point, superelevation
Corrosion resistance, excellent conductivity it is magnetic, excellent heterogeneity and catalytic activity.Two-dimentional molybdenum nitride and tungsten nitride nanometer sheet,
Its thickness is less than 100nm, due to making it have higher ion diffusion speed with big electrochemistry and catalytic activation surface area
Rate, chemical property and catalytic activity.Therefore, in energy storage, electrode material, electrochemistry is urged for two-dimentional molybdenum nitride and tungsten nitride nanometer sheet
Change, hydrogenation catalyst, superconductor and electromagnetic interference shield etc. have important purposes.
But the method for the two-dimentional molybdenum nitride of preparation being currently known and tungsten nitride nanometer sheet is less, there is salt mould in document
Plate synthetic method, chemical liquid deposition and hydrothermal synthesis ammonia nitriding again, but these method higher costs, production efficiency
It is low, be not suitable for large-scale production.It the low cost of two-dimentional molybdenum nitride and tungsten nitride nanometer sheet, high efficiency and is prepared on a large scale and is still
A problem, this significantly limits it in the application of every field.
Summary of the invention
The purpose of the present invention solves the problems, such as that two-dimentional molybdenum nitride at present and the preparation of tungsten nitride nanometer sheet are difficult, provides a kind of new
Low cost, simple process, efficiently, be suitable for large-scale industrial production the two-dimentional molybdenum nitride of preparation or the side of tungsten nitride nanometer sheet
Method.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of method that low cost prepares two-dimentional molybdenum nitride or tungsten nitride nanometer sheet, it is characterised in that the following steps are included:
(1) molybdenum concentrate or tungsten disulfide and sodium carbonate are uniformly mixed by certain stoichiometric ratio, the ammonia in high temperature furnace
Nitridation reaction is carried out under atmosphere；
(2) product obtained in step (1) washed, filtered, being dried to obtain two-dimentional molybdenum nitride nanometer sheet or two dimension nitridation
Tungsten nanometer sheet.
Further, the charge ratio of molybdenum concentrate described in step (1) and sodium carbonate is the reality of molybdenum disulfide in molybdenum concentrate
Border content and sodium carbonate molar ratio 1:1.5-1:4；The charge ratio of the tungsten disulfide and sodium carbonate is molar ratio 1:1.5-1:
4；The nitridation reaction temperature is 600-900 DEG C；Washing methods described in step (2) is washing and pickling.
Further, the molybdenum concentrate can be replaced with molybdenum disulfide and molybdenum disulfide raw material as main component；Institute
The tungsten disulfide stated can use tungsten disulfide raw material substitution as main component；The sodium carbonate can use sodium hydroxide, carbon
Sour potassium, potassium hydroxide, lithium carbonate, lithium hydroxide, calcium carbonate, calcium oxide, calcium hydroxide, magnesium carbonate, magnesia or magnesium hydroxide
Instead of.
Compared with prior art, the present invention having the advantage that
1. the present invention uses molybdenum concentrate, tungsten disulfide and sodium carbonate for primary raw material, cost of material is low.
2. present invention process is simple, high production efficiency, production cost is low, is suitble to industrialization large-scale production two dimension molybdenum nitride
With tungsten nitride nanometer sheet.
3. two-dimentional molybdenum nitride and tungsten nitride nanometer sheet that present invention process is prepared, purity is high, thickness are thin.
Specific embodiment
To further appreciate that the contents of the present invention.Further statement is made to the present invention below with reference to example.
Embodiment one:
By molybdenum concentrate (wherein molybdenum disulfide mass fraction is 95%) and sodium carbonate by practical molybdenum disulfide in molybdenum concentrate
Content and sodium carbonate molar ratio 1:2.5 ingredient are simultaneously uniformly mixed.The raw material of mixing is roasted under ammonia atmosphere to 2 at 800 DEG C
Hour.Then it washes, pickling will be precipitated after filtering, refilter and two-dimentional molybdenum nitride nanometer sheet will be obtained after precipitating drying.
Embodiment two:
Molybdenum disulfide (purity 99%) and sodium carbonate 1:2 ingredient and are uniformly mixed in molar ratio.By the raw material of mixing
3 hours are roasted under ammonia atmosphere at 750 DEG C.Then it washes, filter and obtain two-dimentional molybdenum nitride nanometer sheet after dry.
Embodiment three:
Tungsten disulfide (purity 99%) and sodium carbonate 1:3 ingredient and are uniformly mixed in molar ratio.By the raw material of mixing
5 hours are roasted under ammonia atmosphere at 750 DEG C.Then it washes, filter and obtain two-dimentional tungsten nitride nanometer sheet after dry.
Claims (3)
1. a kind of method that low cost prepares two-dimentional molybdenum nitride or tungsten nitride nanometer sheet, it is characterised in that the following steps are included:
(1) molybdenum concentrate or tungsten disulfide and sodium carbonate are uniformly mixed by certain stoichiometric ratio, the ammonia atmosphere in high temperature furnace
Lower carry out nitridation reaction；
(2) product obtained in step (1) washed, filtered, being dried to obtain two-dimentional molybdenum nitride nanometer sheet or two-dimentional tungsten nitride is received
Rice piece.
2. the method that a kind of low cost according to claim 1 prepares two-dimentional molybdenum nitride or tungsten nitride nanometer sheet, feature
It is, the charge ratio of molybdenum concentrate described in step (1) and sodium carbonate is the actual content and carbonic acid of molybdenum disulfide in molybdenum concentrate
Sodium molar ratio 1:1.5-1:4；The charge ratio of the tungsten disulfide and sodium carbonate is molar ratio 1:1.5-1:4；The nitridation
Reaction temperature is 600-900 DEG C；Washing methods described in step (2) is washing and pickling.
3. a kind of method that low cost prepares two-dimentional molybdenum nitride or tungsten nitride nanometer sheet according to right 1, which is characterized in that
The molybdenum concentrate can be replaced with molybdenum disulfide and molybdenum disulfide raw material as main component；The tungsten disulfide can use two
Tungsten sulfide raw material substitution as main component；The sodium carbonate can use sodium hydroxide, potassium carbonate, potassium hydroxide, lithium carbonate, hydrogen
Lithia, calcium carbonate, calcium oxide, calcium hydroxide, magnesium carbonate, magnesia or magnesium hydroxide replace.
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| CN201810826139.XA CN110228797B (en) | 2018-07-25 | 2018-07-25 | Method for preparing two-dimensional molybdenum nitride or tungsten nitride nanosheets at low cost |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110721717A (en) * | 2019-09-30 | 2020-01-24 | 南方科技大学 | Porous flaky tungsten nitride/carbon composite material and preparation method and application thereof |
| CN112830459A (en) * | 2021-01-21 | 2021-05-25 | 华中科技大学 | Method for preparing two-dimensional transition metal nitride with assistance of decomposable alkali metal compound |
| CN113089099A (en) * | 2021-03-11 | 2021-07-09 | 中国检验检疫科学研究院 | Synthesis method and application of monocrystalline porous square flaky tungsten nitride nanoparticles |
| CN113373441A (en) * | 2020-03-09 | 2021-09-10 | 中国科学院大连化学物理研究所 | Preparation method of tungsten single crystal surface step confinement two-dimensional tungsten nitride |
| CN113479855A (en) * | 2021-07-26 | 2021-10-08 | 武汉科技大学 | Method for preparing non-lamellar two-dimensional transition metal compound by using bulk phase lamellar transition metal sulfide |
| CN113735173A (en) * | 2021-09-08 | 2021-12-03 | 北京航空航天大学 | Molybdenum sulfide-molybdenum nitride composite material and preparation method and application thereof |
| CN114937561A (en) * | 2022-06-01 | 2022-08-23 | 河北工业大学 | Tungsten nitride/molybdenum nitride composite material with layered staggered structure and preparation method and application thereof |
| CN115744840A (en) * | 2022-10-18 | 2023-03-07 | 南昌航空大学 | Carbon nanosheet packaged atomic-level amorphous tungsten-nitrogen cluster sodium storage material and forming method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104627996A (en) * | 2015-02-13 | 2015-05-20 | 山东大学 | Method for preparing two-dimensional nano material employing recrystallization |
| CN104743529A (en) * | 2015-03-23 | 2015-07-01 | 北京科技大学 | Synthesis method of tungsten nitride with high catalytic performance |
| CN106672921A (en) * | 2016-12-26 | 2017-05-17 | 华中科技大学 | Preparation method of two-dimensional metal compound material |
-
2018
- 2018-07-25 CN CN201810826139.XA patent/CN110228797B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104627996A (en) * | 2015-02-13 | 2015-05-20 | 山东大学 | Method for preparing two-dimensional nano material employing recrystallization |
| CN104743529A (en) * | 2015-03-23 | 2015-07-01 | 北京科技大学 | Synthesis method of tungsten nitride with high catalytic performance |
| CN106672921A (en) * | 2016-12-26 | 2017-05-17 | 华中科技大学 | Preparation method of two-dimensional metal compound material |
Non-Patent Citations (2)
| Title |
|---|
| GUO-DONG SUN ET AL.: "Synthesis of molybdenum nitrides nanosheets by nitriding 2H-MoS2 with ammonia", 《JOURNAL OF AMERICAN CERAMIC SOCIETY》 * |
| XU XIAO ET AL.: "Salt-Templated Synthesis of 2D Metallic MoN and Other Nitrides", 《ACS NANO》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110721717A (en) * | 2019-09-30 | 2020-01-24 | 南方科技大学 | Porous flaky tungsten nitride/carbon composite material and preparation method and application thereof |
| CN113373441A (en) * | 2020-03-09 | 2021-09-10 | 中国科学院大连化学物理研究所 | Preparation method of tungsten single crystal surface step confinement two-dimensional tungsten nitride |
| CN113373441B (en) * | 2020-03-09 | 2022-06-10 | 中国科学院大连化学物理研究所 | Preparation method of tungsten single crystal surface step confinement two-dimensional tungsten nitride |
| CN112830459A (en) * | 2021-01-21 | 2021-05-25 | 华中科技大学 | Method for preparing two-dimensional transition metal nitride with assistance of decomposable alkali metal compound |
| CN113089099A (en) * | 2021-03-11 | 2021-07-09 | 中国检验检疫科学研究院 | Synthesis method and application of monocrystalline porous square flaky tungsten nitride nanoparticles |
| CN113479855A (en) * | 2021-07-26 | 2021-10-08 | 武汉科技大学 | Method for preparing non-lamellar two-dimensional transition metal compound by using bulk phase lamellar transition metal sulfide |
| CN113735173A (en) * | 2021-09-08 | 2021-12-03 | 北京航空航天大学 | Molybdenum sulfide-molybdenum nitride composite material and preparation method and application thereof |
| CN114937561A (en) * | 2022-06-01 | 2022-08-23 | 河北工业大学 | Tungsten nitride/molybdenum nitride composite material with layered staggered structure and preparation method and application thereof |
| CN114937561B (en) * | 2022-06-01 | 2024-02-20 | 河北工业大学 | Tungsten nitride/molybdenum nitride composite material with layered staggered structure and preparation method and application thereof |
| CN115744840A (en) * | 2022-10-18 | 2023-03-07 | 南昌航空大学 | Carbon nanosheet packaged atomic-level amorphous tungsten-nitrogen cluster sodium storage material and forming method and application thereof |
| CN115744840B (en) * | 2022-10-18 | 2024-02-09 | 南昌航空大学 | Carbon nano-sheet encapsulated atomic-level amorphous tungsten-nitrogen cluster sodium storage material, and forming method and application thereof |
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