CN105753053A - Preparation method of nano-micro structure MoS2 spheres - Google Patents

Preparation method of nano-micro structure MoS2 spheres Download PDF

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Publication number
CN105753053A
CN105753053A CN201610212039.9A CN201610212039A CN105753053A CN 105753053 A CN105753053 A CN 105753053A CN 201610212039 A CN201610212039 A CN 201610212039A CN 105753053 A CN105753053 A CN 105753053A
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China
Prior art keywords
nano
preparation
micro structure
ball
structure mos
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Pending
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CN201610212039.9A
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Chinese (zh)
Inventor
李亚峰
魏明灯
车宗洲
柳宇彬
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Fuzhou University
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Fuzhou University
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Priority to CN201610212039.9A priority Critical patent/CN105753053A/en
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/06—Sulfides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention belongs to the field of preparation of nano materials and in particular relates to a preparation method of nano-micro structure MoS2 spheres. The preparation method comprises the following steps: by taking thiourea and ammonium molybdate as precursors, dropwise adding hydrazine hydrate solution in presence of a surfactant polyvinylpyrrolidone, and carrying out one-step hydrothermal synthesis, so that the nano-micro structure MoS2 spheres are obtained. The preparation method provided by the invention is simple, inexpensive in raw materials, good in repeatability and beneficial to mass production and has potential application value.

Description

A kind of nano-micro structure MoS2The preparation method of ball
Technical field
The invention belongs to the preparation field of nano material, be specifically related to a kind of nano-micro structure MoS2The preparation method of ball.
Background technology
MoS2It is the Layered dual compound of a kind of graphite-like structure, has a wide range of applications in lubrication, catalysis and energy storage and conversion etc. and enjoy the concern of people.Recent studies have shown that ultra-thin MoS2The more common MoS of nanometer sheet2There is higher electron mobility, more avtive spot and bigger specific surface area, thus show more excellent performance.Yet with bigger specific surface area and interlayer Van der Waals force, it is made to be susceptible in actual applications reunite thus hindering its application in many aspects, substantial amounts of research shows the nanometer sheet of two-dimensional structure is assembled into three-dimensional graded structure material, single nanometer sheet performance can not only be kept, and be prevented from the reunion of material, thus show more excellent performance.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that a kind of nano-micro structure MoS2The preparation method of ball.The method is simple, cheaper starting materials, reproducible, be conducive to large-scale production, there is potential using value.
For achieving the above object, the present invention adopts the following technical scheme that
A kind of nano-micro structure MoS2The preparation method of ball: with thiourea, ammonium molybdate for presoma, when surfactant polyvinylpyrrolidone, drips hydrazine hydrate solution, a step Hydrothermal Synthesis nano-micro structure MoS2Ball.
The amount ratio of thiourea, ammonium molybdate, polyvinylpyrrolidone and hydrazine hydrate is 0.9g:0.525g:1.5g:4.5ml.
Described nano-micro structure MoS2The preparation method of ball, more specifically, thiourea and polyvinylpyrrolidone are dissolved in water/alcohol mixed solvent, it is stirring evenly and then adding into ammonium molybdate, after continuing stirring 0.5h, drip hydrazine hydrate solution, through hydro-thermal reaction 24h after continuation stirring 15min, centrifugal, washing after cooling, dry, by the product obtained high-temperature calcination under an inert atmosphere and get final product.
The temperature of hydro-thermal reaction is 220 DEG C；Described calcining be under an ar atmosphere 800 DEG C calcining 2h.
The nano-micro structure MoS that a kind of preparation method as above prepares2Ball.
The beneficial effects of the present invention is:
1) present invention is by the MoS of two-dimensional structure2Nanometer sheet is assembled into three-dimensional graded structure material, can not only keep single nanometer sheet performance, and is prevented from the reunion of material, thus shows more excellent performance；
2) preparation method of the present invention is simple, cheaper starting materials, reproducible, be conducive to large-scale production, there is potential using value.
Accompanying drawing explanation
Fig. 1 nano-micro structure MoS2The XRD spectra of ball；
Fig. 2 (a), Fig. 2 (b) are nano-micro structure MoS2The scanning electron microscope (SEM) photograph of ball；
Fig. 2 (c), Fig. 2 (d), Fig. 2 (e) are nano-micro structure MoS2The transmission electron microscope picture of ball；
Fig. 2 (f) is nano-micro structure MoS2The high-resolution projection Electronic Speculum figure of ball, wherein the illustration in (f) is electronogram.
Detailed description of the invention
Present invention the following example further illustrates the present invention, but protection scope of the present invention is not limited to the following example.
Embodiment 1
0.9g thiourea and 1.5g polyvinylpyrrolidone are dissolved in water/alcohol mixed solvent, it is stirring evenly and then adding into 0.525g ammonium molybdate, after continuing stirring 0.5h, dropping 4.5ml hydrazine hydrate solution, through 220 DEG C of hydro-thermal reaction 24h after continuation stirring 15min, centrifugal, washing after cooling, dry, by the product obtained 800 DEG C of calcining 2h under an ar atmosphere and get final product.
The foregoing is only presently preferred embodiments of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to the covering scope of the present invention.

Claims (5)

1. a nano-micro structure MoS2The preparation method of ball, it is characterised in that: with thiourea, ammonium molybdate for presoma, when surfactant polyvinylpyrrolidone, drip hydrazine hydrate solution, a step Hydrothermal Synthesis nano-micro structure MoS2Ball.
2. nano-micro structure MoS according to claim 12The preparation method of ball, it is characterised in that: the amount ratio of thiourea, ammonium molybdate, polyvinylpyrrolidone and hydrazine hydrate is 0.9g:0.525g:1.5g:4.5ml.
3. nano-micro structure MoS according to claim 12The preparation method of ball, it is characterized in that: thiourea and polyvinylpyrrolidone are dissolved in water/alcohol mixed solvent, it is stirring evenly and then adding into ammonium molybdate, after continuing stirring 0.5h, dropping hydrazine hydrate solution, continue hydro-thermal reaction 24h after stirring 15min, centrifugal, washing after cooling, dry, by the product obtained high-temperature calcination under an inert atmosphere and get final product.
4. nano-micro structure MoS according to claim 32The preparation method of ball, it is characterised in that: the temperature of hydro-thermal reaction is 220 DEG C；Described high-temperature calcination is 800 DEG C of calcining 2h under Ar gas atmosphere.
5. the nano-micro structure MoS that the preparation method as described in any one of claim 1-4 prepares2Ball.
CN201610212039.9A 2016-04-07 2016-04-07 Preparation method of nano-micro structure MoS2 spheres Pending CN105753053A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610212039.9A CN105753053A (en) 2016-04-07 2016-04-07 Preparation method of nano-micro structure MoS2 spheres

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610212039.9A CN105753053A (en) 2016-04-07 2016-04-07 Preparation method of nano-micro structure MoS2 spheres

Publications (1)

Publication Number Publication Date
CN105753053A true CN105753053A (en) 2016-07-13

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106179406A (en) * 2016-07-11 2016-12-07 福州大学 A kind of single layer structure MnSb2s4the preparation method of catalysis material
CN106379939A (en) * 2016-08-30 2017-02-08 青岛科技大学 Morphology-adjustable molybdenum disulfide preparation method
CN107579248A (en) * 2017-08-23 2018-01-12 江汉大学 The preparation method and applications of negative electrode of lithium ion battery molybdenum disulfide
CN109734132A (en) * 2019-03-12 2019-05-10 中国矿业大学 A method of controlling synthesis of carbon/molybdenum disulfide particle in mixed solvent system
CN110491991A (en) * 2019-08-20 2019-11-22 西安工业大学 It is a kind of to prepare hydro-thermal method MoS2The method of multistage resistance-variable storing device
WO2021059325A1 (en) * 2019-09-24 2021-04-01 Dic株式会社 Molybdenum sulfide powder and method for producing same
WO2022202738A1 (en) * 2021-03-24 2022-09-29 Dic株式会社 Noble metal adsorbent, noble metal recovery method, and noble metal adsorbent recyling method
WO2022201610A1 (en) * 2021-03-24 2022-09-29 Dic株式会社 Molybdenum disulfide particles and lubricating composition

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CN104393294A (en) * 2014-11-27 2015-03-04 江苏理工学院 Preparation method of flower-shaped molybdenum disulfide microspheres
CN104591286A (en) * 2014-12-25 2015-05-06 江苏大学 Preparation method of molybdenum disulfide microspheres
CN105226277A (en) * 2015-09-10 2016-01-06 中国科学院上海硅酸盐研究所 A kind of high-performance transition metal dichalcogenide nanometer sheet radial direction assembling micro-sphere material and preparation method thereof

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CN104393294A (en) * 2014-11-27 2015-03-04 江苏理工学院 Preparation method of flower-shaped molybdenum disulfide microspheres
CN104591286A (en) * 2014-12-25 2015-05-06 江苏大学 Preparation method of molybdenum disulfide microspheres
CN105226277A (en) * 2015-09-10 2016-01-06 中国科学院上海硅酸盐研究所 A kind of high-performance transition metal dichalcogenide nanometer sheet radial direction assembling micro-sphere material and preparation method thereof

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106179406A (en) * 2016-07-11 2016-12-07 福州大学 A kind of single layer structure MnSb2s4the preparation method of catalysis material
CN106179406B (en) * 2016-07-11 2018-06-15 福州大学 A kind of single layer structure MnSb2S4The preparation method of catalysis material
CN106379939A (en) * 2016-08-30 2017-02-08 青岛科技大学 Morphology-adjustable molybdenum disulfide preparation method
CN107579248A (en) * 2017-08-23 2018-01-12 江汉大学 The preparation method and applications of negative electrode of lithium ion battery molybdenum disulfide
CN109734132A (en) * 2019-03-12 2019-05-10 中国矿业大学 A method of controlling synthesis of carbon/molybdenum disulfide particle in mixed solvent system
CN110491991A (en) * 2019-08-20 2019-11-22 西安工业大学 It is a kind of to prepare hydro-thermal method MoS2The method of multistage resistance-variable storing device
WO2021059325A1 (en) * 2019-09-24 2021-04-01 Dic株式会社 Molybdenum sulfide powder and method for producing same
JPWO2021060377A1 (en) * 2019-09-24 2021-04-01
WO2021060377A1 (en) * 2019-09-24 2021-04-01 Dic株式会社 Molybdenum sulfide powder and method for manufacturing same, heavy-metal adsorbent, photothermal conversion material, distillation method, oxygen reduction catalyst, and catalyst ink
JP7060170B2 (en) 2019-09-24 2022-04-26 Dic株式会社 Molybdenum sulfide powder and its manufacturing method, heavy metal adsorbent, photoheat conversion material, distillation method, oxygen reduction catalyst, and catalyst ink
TWI815041B (en) * 2019-09-24 2023-09-11 日商迪愛生股份有限公司 Molybdenum sulfide powder and its manufacturing method, heavy metal adsorbent, photothermal conversion material, distillation method, oxygen reduction catalyst and catalyst ink
WO2022202738A1 (en) * 2021-03-24 2022-09-29 Dic株式会社 Noble metal adsorbent, noble metal recovery method, and noble metal adsorbent recyling method
WO2022201610A1 (en) * 2021-03-24 2022-09-29 Dic株式会社 Molybdenum disulfide particles and lubricating composition
JPWO2022202738A1 (en) * 2021-03-24 2022-09-29
JP7460015B2 (en) 2021-03-24 2024-04-02 Dic株式会社 Precious metal adsorbent, precious metal recovery method, and precious metal adsorbent regeneration method

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Application publication date: 20160713