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Preparation method for molybdenum disulfide nanometer nuclear shell nano-structure

A nano-core-shell and nano-structure technology, applied in the field of nanomaterials, can solve the problems of harsh reaction conditions, difficult to control morphology, and high cost, and achieve the effects of high product difference rate, simple and easy-to-control production process, and low cost.

Inactive Publication Date: 2013-03-27
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003]The commonly used methods for synthesizing nano-core-shell composite materials include high-temperature solid-phase method, sol-gel method, hydrothermal method, etc.; among them, the reaction of high-temperature solid-phase method The conditions are harsh, the operation is cumbersome, the product is uneven and the shape is irregular; the steps of the sol-gel method are cumbersome, the cost is high, the material is brittle, and some organic solvents are harmful to the human body, while the hydrothermal method has simple process, convenient operation, The product has the advantages of regular shape and uniform particle size, but there are few relevant literature reports on the MoS2 nano-core-shell nanostructure, and the cost is high and the process is complicated. Chinese patent 201210044621.0 discloses a new type of core-shell- The preparation method of solvent-free nanofluid with corona structure, adopts the direct reduction method to prepare nano-molybdenum disulfide particles with hydroxyl groups on the surface, adds a surface modifier with sulfonic acid groups for sulfonation treatment, and adjusts pH and reaction temperature, and finally passes strong acid Interact with the positive and negative charges of the weak base to firmly bind the trisubstituted amine, and remove the solvent to obtain a uniform and stable nanofluid; however, due to the easy aggregation of nanoparticles during the preparation process, the MoS2The shape of the nano-core-shell nanostructure is not easy to control, and the existing technology is complicated, which affects its large-scale application in the fields of tribology, photochemistry, catalysis, etc.

Method used

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Examples

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Embodiment 1

[0020] 0.88g Na 2 MoO 4 2H 2 O, 0.94g Na 2 S, and 0.41 g of ascorbic acid were added to 60 ml of ethanol-water (2:1) mixed solvent, dissolved to obtain a clear solution, and then 0.30 g of C 27 h 50 After ClN is completely dissolved, use 2mol·L -1 The pH value was adjusted to 12 with NaOH, and after stirring for 30 min, the mixture was transferred to a 100 ml stainless steel reactor, placed in a vacuum oven at 180°C for 36 h, cooled to room temperature, and the reaction product was centrifuged. Repeated washing with deionized water and absolute ethanol, respectively, and finally drying at 80 °C for 10 h under vacuum to obtain a gray-black product powder, that is, molybdenum disulfide nano-core-shell nanostructure.

[0021] figure 1 The XRD pattern shows that the XRD peak position is consistent with the standard diffraction pattern (PDF No.37-1492), and the product is pure MoS 2 Nano-structure, figure 2 It is a low-magnification SEM photo of the product, a large number...

Embodiment 2

[0023] 1.21g Na 2 MoO 4 2H 2 O, 1.36g Na 2 S, and 1.76g of ascorbic acid were added to 60 ml of ethylene glycol-water (2:1) mixed solvent, dissolved to obtain a clear solution, and then 0.27 g of C 27 h 50 After ClN is completely dissolved, use 2mol·L -1 The pH value was adjusted to 14 with NaOH, and after stirring for 30 min, the mixture was transferred to a 100 ml stainless steel reaction kettle, placed in a vacuum oven at 160 °C for 48 h, cooled to room temperature, and the reaction products were separated by centrifugation. Repeated washing with deionized water and absolute ethanol, and finally drying at 80°C for 10 h under vacuum conditions to obtain a gray-black product powder, that is, molybdenum disulfide nano-core-shell nanostructure, the XRD pattern and SEM photo of Example 2 are similar to Examples 1.

Embodiment 3

[0025] 0.73g Na 2 MoO 4 2H 2 O, 0.59g Na 2 S, and 1.06 g of ascorbic acid were added to 60 ml of ethylene glycol-water (2:1) mixed solvent, dissolved to obtain a clear solution, and then 0.32 g of C 27 h 50 After ClN is completely dissolved, use 2mol·L -1 The pH value was adjusted to 13 with NaOH, and after stirring for 30 min, the mixture was transferred to a 100 ml stainless steel reactor, placed in a vacuum oven at 200 °C for 24 h, cooled to room temperature, and the reaction products were separated by centrifugation. Repeated washing with deionized water and absolute ethanol, and finally drying at 80°C for 10 h under vacuum conditions to obtain a gray-black product powder, that is, molybdenum disulfide nano-core-shell nanostructure, the XRD pattern and SEM photo of Example 3 are similar to Examples 1.

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Abstract

The invention discloses a preparation method for a molybdenum disulfide nanometer nuclear shell nano-structure. By adopting a solvent thermal synthesis method, the preparation method specially comprises the following steps: (1) dissolving Na2MoO4.2H2O, Na2S and ascorbic acid into a mixed solvent, adding surface active agent, conducting centrifugal agitating to be evenly dispersed into the solution, and finally adjusting the pH value of the solution as 12-14 with acid; (2) agitating the solution obtained from step (1), transferring into a stainless steel reaction kettle, sealing, conducting constant-temperature reaction, cooling to room temperature to obtain reaction product; and (3) separating the reaction product, washing and drying to obtain the molybdenum disulfide nanometer nuclear shell nano-structure. The method is simple in process, and low in cost, the product prepared is high in purity and yield, has an important application in the fields of friction, photochemistry, lithium electricity and the like, and is hopefully used for large-scale industrial production.

Description

technical field [0001] The invention relates to the field of nanomaterials, in particular to a method for preparing a molybdenum disulfide nano-core-shell nanostructure. Background technique [0002] The core-shell structure (Core-Shell) composite material is a class of particles with a double-layer or multi-layer structure, generally composed of a central core and an outer shell, due to changing the material type of the core and adjusting the thickness of the shell Ideal composite materials with excellent performance can be obtained. The transition metal sulfide core-shell structure and hollow structure have excellent physical and chemical properties, and in tribology, drug delivery carriers, photonic crystals, catalysts and energy storage, and high-performance composite materials There are important applications in many technical fields, among which, MoS 2 It has the characteristics of a special hexagonal layered structure. Its layers are combined by strong chemical bonds...

Claims

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Application Information

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IPC IPC(8): C01G39/06B82Y30/00B82Y40/00
Inventor 唐华唐国钢李长生杨小飞
Owner JIANGSU UNIV
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