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 PDF

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Publication number
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
nitride
nanometer sheet
dimentional
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CN110228797B (en
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张国华
孙国栋
常贺强
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Henan Tianqu New Material Technology Co.,Ltd.
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University of Science and Technology Beijing USTB
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/06Binary 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
    • C01B21/0615Binary 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
    • C01B21/062Binary 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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/20Particle morphology extending in two dimensions, e.g. plate-like
    • C01P2004/24Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer

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  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
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  • Manufacture And Refinement Of Metals (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

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

A kind of method that low cost prepares two-dimentional molybdenum nitride or tungsten nitride nanometer sheet
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.
CN201810826139.XA 2018-07-25 2018-07-25 Method for preparing two-dimensional molybdenum nitride or tungsten nitride nanosheets at low cost Active CN110228797B (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
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

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CN106672921A (en) * 2016-12-26 2017-05-17 华中科技大学 Preparation method of two-dimensional metal compound material

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Cited By (11)

* Cited by examiner, † Cited by third party
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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