Flaky nanometer molybdenum disulfide material, nanometer composite metal anticorrosive coating material and preparation method of flaky nanometer molybdenum disulfide material and nanometer composite metal anticorrosive coating material

A technology of nano-molybdenum disulfide and molybdenum disulfide, which is applied in the direction of anti-corrosion coatings, nanotechnology for materials and surface science, molybdenum sulfide, etc., and can solve the problems of small preparation scale, increased interlayer spacing of molybdenum disulfide, and poor repeatability and other problems, to achieve the effect of simple preparation method, good dispersibility and high yield

Inactive Publication Date: 2014-12-03
EAST CHINA NORMAL UNIV
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AI Technical Summary

Problems solved by technology

At present, micro-mechanical force peeling method, lithium ion intercalation method, liquid phase ultrasonic method, etc. can be used for peeling. Micro-mechanical force peeling method is the most mature method because of its relatively simple operation and high peeling degree. It can obtain monolayer Molybdenum disulfide and the stripped product have high carrier mobility, and are generally used to make field effect transistors. The disadvantage is that the preparation scale is small and the reproducibility is poor (ACS Nano2010, 4, 2695; Nat.Nanotechnol.2011, 6 , 147.); Lithium ion intercalation method is the method with relatively high stripping efficiency at present. Lithium ion intercalation method was first started in 1986. Morrison et al. firstly prepared monolayer molybdenum disulfide by this method. The basic principle is to use lithium Ionic intercalants (such as butyllithium, n-C4H9Li) are intercalated into the molybdenum disulfide powder to form Li x MoS 2 (x ≥ 1) intercalation compound, and then increase the layer of molybdenum disulfide by a large amount of hydrogen generated by the violent reaction between the intercalation compound and the protic solvent (usually water, dilute acid or low-boiling point alcohols can also be used) spacing, and then obtain multi-layer or even single-layer molybdenum disulfide. The basic steps for lithium ion intercalation method to strip molybdenum disulfide are: first place molybdenum disulfide powder and n-butyllithium n-hexane solution in an inert gas at 100 °C React in the environment for 3 days to get the exfoliated intercalation, then add water and other protic solvents, then sonicate for 60 minutes, filter, centrifuge the suspension and wash it with deionized water for several times until neutral, and finally vacuum dry to obtain graphene Molybdenum disulfide, the disadvantage is time-consuming, strict preparation conditions, and the removal of lithium ions can easily lead to the accumulation of graphene-like molybdenum disulfide (Mater.Res.Bull.1986,21,457; Adv.Mater.2002,14,265 .); liquid phase ultrasonic method recently newly developed method, in 2011, Coleman et al. added N-methyl-2-pyrrolidone (NMP) to molybdenum disulfide powder, N-ethyl-2-pyrrolidone (NVP) , isopropanol (IPA), dimethylsulfoxide (DMSO), dimethylformamide (DMF), etc., followed by ultrasonication, centrifugation, and vacuum drying to obtain graphene-like molybdenum disulfide, but its peeling degree and The stripping efficiency is lower than the first two methods, and the yield of flake nanomolybdenum disulfide is very low, and the yield only reaches more than ten percent (Science2011, 331, 568; Adv.Mater.2011, 23, 417)

Method used

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  • Flaky nanometer molybdenum disulfide material, nanometer composite metal anticorrosive coating material and preparation method of flaky nanometer molybdenum disulfide material and nanometer composite metal anticorrosive coating material
  • Flaky nanometer molybdenum disulfide material, nanometer composite metal anticorrosive coating material and preparation method of flaky nanometer molybdenum disulfide material and nanometer composite metal anticorrosive coating material
  • Flaky nanometer molybdenum disulfide material, nanometer composite metal anticorrosive coating material and preparation method of flaky nanometer molybdenum disulfide material and nanometer composite metal anticorrosive coating material

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Add 2 grams of nitric acid into a 100mL round-bottomed flask containing 6 grams of hydrochloric acid, add 0.2 gram of molybdenum disulfide powder, install a straight condenser tube in the round-bottomed flask, and put on a tail gas absorption device, and drain the tail gas with water Absorption, to avoid exhausting the tail gas directly into the air, use an oil bath to heat, raise the oil bath to 110°C, and keep it for 30 minutes. After the reaction is completed, add 30mL deionized water to dilute the reaction solution, and then use centrifugation to separate the product Separated and washed three times with deionized water and once with isopropanol, finally the resulting product was dispersed in 2 g of isopropanol. The SEM figure, TEM figure, HTEM figure, lattice electron diffraction figure of the flaky nano-molybdenum disulfide prepared by the present embodiment and the following examples are respectively as follows Figure 2-5 shown. Compare the SEM images of the mo...

Embodiment 2

[0042] Add 2 grams of nitric acid into a 100mL round-bottomed flask containing 6 grams of hydrochloric acid, add 0.2 gram of molybdenum disulfide powder, install a straight condenser tube in the round-bottomed flask, and put on a tail gas absorption device, and drain the tail gas with water Absorption, to avoid exhausting the tail gas directly into the air, place the reaction bottle in an ultrasonic generator, and perform ultrasonication. The temperature of the water bath is set to 50°C, and ultrasonication is performed for 20 minutes. The product was then separated by centrifugation, washed three times with deionized water and once with isopropanol, and finally the obtained product was dispersed in 2 g of isopropanol.

Embodiment 3

[0044] Add 3 grams of nitric acid into a 100mL round-bottomed flask containing 6 grams of hydrochloric acid, add 0.2 gram of molybdenum disulfide powder, install a straight condenser tube in the round-bottomed flask, and put a tail gas absorption device on it. Absorption, to avoid exhausting the tail gas directly into the air, use an oil bath to heat, raise the oil bath to 110°C, and keep it for 30 minutes. After the reaction is completed, add 30mL deionized water to dilute the reaction solution, and then use centrifugation to separate the product Separated and washed three times with deionized water and once with isopropanol, finally the resulting product was dispersed in 2 g of isopropanol.

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Abstract

The invention discloses a preparation method of a flaky nanometer molybdenum disulfide material. The preparation method comprises the steps of dispersing a raw material, namely molybdenum disulfide with a lamellar crystal structure, into a mixed solution of nitric acid and hydrochloric acid; carrying out liquid phase separation by using a heating or ultrasound method; and reacting to obtain the flaky nanometer molybdenum disulfide material. The invention also discloses a nanometer composite metal anticorrosive coating material and a preparation method thereof. The nanometer composite metal anticorrosive coating material is prepared by compounding flaky nanometer molybdenum disulfide and nanometer silicon dioxide sol. The preparation method disclosed by the invention is simple; the raw material is easily available; the flaky nanometer molybdenum disulfide material and the nanometer composite metal anticorrosive coating material are widely applied to the antirust treatment and performance improvement of metal materials; the service life of metal is prolonged; and the energy consumption is reduced.

Description

technical field [0001] The invention relates to the field of preparation of flaky nanometer materials, in particular to a preparation method of a flaky nanometer molybdenum disulfide material, a nanocomposite metal anti-corrosion coating material and a preparation method thereof. Background technique [0002] Sheet-shaped nano-molybdenum disulfide materials have different thermal, electrical, optical, and mechanical properties from bulk materials, and have broad potential application prospects in the field of optoelectronic devices, composite materials, and friction materials. At present, micro-mechanical force peeling method, lithium ion intercalation method, liquid phase ultrasonic method, etc. can be used for peeling. Micro-mechanical force peeling method is the most mature method because of its relatively simple operation and high peeling degree. It can obtain monolayer Molybdenum disulfide and the stripped product have high carrier mobility, and are generally used to ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06B82Y30/00B82Y40/00C09D1/00C09D5/08
Inventor 林和春罗倩倩彭晖
Owner EAST CHINA NORMAL UNIV
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