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A kind of preparation method of 2h phase monolayer molybdenum disulfide nanosheet

A technology of single-layer molybdenum disulfide and nanosheets, which is applied in the manufacture of hybrid/electric double-layer capacitors, electrical components, battery electrodes, etc., can solve the problems of complex process, difficulty in preparation, cumbersome operation, etc., and achieve simple process operation, The effect of mild reaction conditions and low cost

Inactive Publication Date: 2018-03-06
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is difficult to prepare MoS with a pure single-layer structure by general chemical and physical methods. 2 Nanomaterials, especially monolayer molybdenum sulfide exfoliation preparation in different phases
Monolayer MoS is currently prepared 2 Nanomaterials mainly include micromechanical force stripping method, chemical vapor deposition method, lithium ion intercalation method, and liquid phase ultrasonic method. 2 The yield is extremely low, most of which are low-layer MoS with a thickness of 1-100nm 2 Nanosheets, not true single-layer MoS 2
In addition to the difficulty of exfoliating monolayer MoS with high efficiency 2 Outside of nanosheets, MoS 2 Nanosheets can only be peeled off and preserved in high-boiling organic solvents such as dimethylformamide and N-methylpyrrolidone. These organic solvents have high viscosity and high boiling point. MoS 2 reassembled into multilayer MoS 2 nanosheets, thereby confining monolayer MoS 2 Exploration and application of nanosheets in some scientific research or industrial fields

Method used

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  • A kind of preparation method of 2h phase monolayer molybdenum disulfide nanosheet
  • A kind of preparation method of 2h phase monolayer molybdenum disulfide nanosheet

Examples

Experimental program
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Embodiment 1

[0022] Weigh 0.008 mol of lithium hydroxide and 0.004 mol of ammonium thiomolybdate, mix and grind them in an agate mortar for 1 hour, place the ground mixture in a corundum crucible, place it in a tube furnace, and protect it with argon. , the temperature was programmed to 400°C, kept for 1 hour, and then continued to pass argon to cool down to room temperature naturally to obtain lithium-intercalated 2H-phase molybdenum sulfide (Li 2 MoS 4 ) block; place the lithium-inserted molybdenum sulfide block in a container filled with 100mL deionized water, and disperse it ultrasonically for 10 minutes. The suspension was washed three times with water and ethanol in a centrifuge at a speed of 4000r / min to remove Li 2 For soluble impurities such as S, ultrasonically disperse the washed precipitate in 200mL deionized water, in which the 2H phase monolayer MoS 2 The concentration is about 0.8mg / mL, and its thickness is 0.66nm detected by atomic force microscope, and X-photoelectron sp...

Embodiment 2

[0024] Weigh 0.008mol of lithium acetate and 0.004mol of ammonium thiomolybdate, mix and grind in an agate mortar for 1 hour, place the ground mixture in a corundum crucible, place it in a tube furnace, and protect it with argon. The temperature was raised to 200°C by program, kept for 10 hours, and then continued to flow argon to cool down to room temperature naturally to obtain lithium-intercalated 2H phase molybdenum sulfide (Li 2 MoS 4 ) blocks; place lithium-inserted molybdenum sulfide blocks in a container filled with 200mL of deionized water, ultrasonically disperse for 10 minutes, and the dispersed suspension is centrifuged and precipitated on a centrifuge at a speed of 1000r / min; after removing the precipitate The suspension was washed 3 times with water and ethanol in a centrifuge with a rotational speed of 10000r / min to remove Li 2 For soluble impurities such as S, ultrasonically disperse the washed precipitate in 200mL absolute ethanol, in which the 2H phase monol...

Embodiment 3

[0026] Weigh 0.008 mol of lithium nitrate and 0.004 mol of ammonium thiomolybdate, mix and grind in an agate mortar for 1 hour, place the ground mixture in a corundum crucible, place it in a tube furnace, and protect it with argon. The temperature was raised to 300°C by program, kept for 5 hours, and then the temperature was naturally cooled to room temperature with argon gas to obtain lithium-intercalated 2H phase molybdenum sulfide (Li 2 MoS 4) block; place the lithium-inserted molybdenum sulfide block in a container filled with 100mL deionized water, and disperse it ultrasonically for 5 minutes. The suspension was washed 3 times with water and ethanol in a centrifuge with a speed of 15000r / min to remove Li 2 For soluble impurities such as S, ultrasonically disperse the washed precipitate in 200mL isopropanol, in which the 2H phase monolayer MoS 2 The concentration is about 1.3mg / mL, and its thickness is 0.62nm detected by atomic force microscope, and X-photoelectron spect...

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Abstract

The invention discloses a preparation method of 2H-phase single-layer molybdenum disulfide nanosheets. The specific steps are: mixing and grinding ammonium thiomolybdate and lithium salt compound according to the molar ratio of 1:2, and the ground mixture is protected by an inert gas. Insulate at 200-400°C for 1-10h, cool to room temperature to obtain lithium-intercalated 2H-phase molybdenum sulfide block; place lithium-intercalated 2H-phase molybdenum sulfide block in deionized water, assist ultrasonic hydrolysis for 5-30min, and then The resulting suspension was placed in a centrifuge, and the unstripped precipitate was removed by centrifugation to obtain a 2H phase monolayer MoS2 nanosheet suspension; the 2H phase monolayer MoS2 nanosheet suspension was centrifuged with water and ethanol on a centrifuge, respectively. The soluble impurities are removed by washing, and finally the precipitated 2H-phase single-layer MoS2 nanosheets are dispersed in a small molecule solvent for storage, and the thickness of the 2H-phase single-layer MoS2 nanosheets is less than 1 nm. The process of the invention is simple in operation, mild in reaction conditions, low in price in reagents, and environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of synthesis of molybdenum disulfide nanomaterials, and in particular relates to a preparation method of a 2H phase single-layer molybdenum disulfide nanosheet. Background technique [0002] Molybdenum disulfide has a typical sandwich layered structure. Due to the relatively weak van der Waals force between layers, it can also be exfoliated into single-layer or few-layer nanosheets. It is considered to be another very important two-dimensional nanosheet material. Has unique physical, chemical and electrical properties. Tests by Radisavljevic et al. show that single-layer MoS 2 The conductivity of bulk MoS is higher than that of bulk MoS 2 The improvement of 100 orders of magnitude makes it have superior performance in electronic devices and electronic sensors (Nat.Nanotechnol.2011,6,147); Mak et al. showed that MoS 2 From the bulk to the monolayer, due to the quantum confinement effect, its forbidden band...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01G11/30H01G11/86H01M4/58H01M4/139
CPCH01G11/30H01G11/86H01M4/139H01M4/5815Y02E60/10
Inventor 常焜常照荣李苞汤宏伟上官恩波
Owner HENAN NORMAL UNIV