CN107512735A - A kind of molybdenum disulfide nano sheet and preparation method thereof - Google Patents

A kind of molybdenum disulfide nano sheet and preparation method thereof Download PDF

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Publication number
CN107512735A
CN107512735A CN201710789452.6A CN201710789452A CN107512735A CN 107512735 A CN107512735 A CN 107512735A CN 201710789452 A CN201710789452 A CN 201710789452A CN 107512735 A CN107512735 A CN 107512735A
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molybdenum disulfide
sputtering
disulfide nano
nano sheet
preparation
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CN201710789452.6A
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Inventor
武卫明
张长松
王书红
周丽敏
郑勇
张楠
侯绍刚
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Anyang Institute of Technology
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Anyang Institute of Technology
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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
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C23C14/0057—Reactive sputtering using reactive gases other than O2, H2O, N2, NH3 or CH4
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0623—Sulfides, selenides or tellurides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties

Abstract

The invention discloses a kind of molybdenum disulfide nano sheet and preparation method thereof, the molybdenum disulfide nano sheet is prepared using the method for reactive magnetron sputtering, and using metal molybdenum as target, using argon gas, hydrogen sulfide is reacting gas for sputter gas, using sheet metal as substrate.As the negative material of lithium ion battery, the molybdenum disulfide nano sheet has higher storage lithium performance, excellent charge-discharge performance and high rate performance；As electrocatalytic hydrogen evolution electrode material and fuel cell anode material, the molybdenum disulfide nano sheet effectively reduces electrode overpotential, reduces electrode polarization resistance.

Description

A kind of molybdenum disulfide nano sheet and preparation method thereof
Technical field
The present invention relates to two-dimension nano materials field, specifically a kind of molybdenum disulfide (MoS2 ) nanometer sheet and its preparation side Method..
Background technology
From the Geim seminar of Univ Manchester UK in the method synthesizing graphite alkene peeled off by micromechanics in 2004 Since, trigger people to graphene and its research boom of composite, meanwhile, class graphene two-dimension nano materials, such as MoS2Nano flake, WS2Nano flake, black phosphorus nano flake, there is good catalytic hydrogen evolution activity and storage lithium performance, be catalyzed And there is potential application value in energy storage field.
Molybdenum disulfide nano sheet (hereinafter referred to as MoS2Nanometer sheet) it can be prepared by a variety of methods, physics can be broadly divided into Method and chemical method, wherein Physical can be divided into the methods of micromechanics is peeled off, liquid/vapor is directly peeled off, and chemical method can divide For chemical vapor deposition (CVD), lithiumation method the methods of.CVD method is to be deposited on solid film by gas phase reaction under high temperature Method in substrate, this method can prepare the MoS of high quality, large area2, but higher cost, complicated technique and tight Its development of severe process regulation conditionality.MoS2Can be prepared with lithiumation method, its general principle be by containing The organic chemical reagent and MoS of lithium2Reaction, MoS is inserted into by lithium ion2The interlayer of crystal, then by the reaction with water and super Sound effect can obtain MoS2Nanometer sheet, but the method needs to carry out under atmosphere of inert gases in process of production, to avoid sky O in gas2And vapor reacts with the organic chemical reagent containing lithium, and it is time-consuming longer, limit it and further apply.Liquid phase machine The method that tool is peeled off can prepare the graphene and class graphene two-dimension nano materials of high quality, but its efficiency is low and cost It is high.
Reactive magnetron sputtering is one kind in physical gas phase deposition technology, can be prepared and provided by the method for magnetron sputtering There are the solid films such as the metal of diverse microcosmic structure, metal oxide, metal nitride, metal sulfide, it is therefore possible to use The technology prepares MoS2Solid film, by controlling sputtering parameter, ultra-thin MoS can be prepared2Nanometer sheet.
The content of the invention
It is an object of the invention to provide a kind of ultra-thin MoS2Nanometer sheet and preparation method thereof.
To reach above-mentioned purpose, the technical scheme is that：
The present invention prepares two-dimentional MoS using the method for reactive magnetron sputtering2Nanometer sheet, using metal molybdenum as target, with Ar and H2S's Mixed gas is sputter gas, using metallic copper, zinc, tin, nickel or aluminium flake as substrate, by changing sputtering parameter, can be prepared Go out the MoS with different-thickness of deposition on the metallic substrate2Nanometer sheet, metal substrate is dissolved i.e. through persalt or nitric acid MoS can be obtained2Nanometer sheet.
Gases used is argon gas and hydrogen sulfide gas, and purity is all on 99.99%.Metallic copper used, zinc, tin, nickel or Aluminium flake is handled by mechanical polishing.
The excellent results of the present invention are：
Ultra-thin MoS2Nanometer sheet can be prepared by the method for reactive magnetron sputtering, and this method technique is simple, short preparation period.Make For the negative material of lithium ion battery, the MoS2Nanometer sheet shows excellent charge-discharge performance and high rate performance and tool There is higher specific capacity；As in elctro-catalyst applied catalysis evolving hydrogen reaction or hydrogen catalytic oxidation reaction, the MoS2Nanometer Piece shows excellent electro catalytic activity, effectively reduces polarization of electrode resistance.
1. the MoS prepared using the present invention2Negative material of the nanometer sheet as lithium ion battery, effectively increase lithium from The specific capacity of the charge-discharge performance of sub- battery, high rate performance and negative pole.
2. the MoS prepared using the present invention2Nanometer sheet is used for the catalytic oxidation of hydrogen as elctro-catalyst, effectively Reduce polarization of electrode resistance.
3. the MoS prepared using the present invention2Nanometer sheet is reacted as elctro-catalyst for catalytic hydrogen evolution, effectively reduces electricity The polarization resistance of pole.
4. the present invention is applied to the fields such as lithium ion battery, fuel cell, electrolytic industry.
Embodiment
Embodiment 1
Using the aluminium flake after polishing as substrate, it is cleaned by ultrasonic aluminium flake with acetone, ethanol, distilled water successively
And after drying, put within the vacuum chamber of magnetic control sputtering device, regulation target-substrate distance is about 6cm, with metal molybdenum materials Expect to be evacuated to 8*10 on 99.99% for target, target purity-4Pa, then carries out chip bench heating, and heating is stable extremely 100 DEG C, it is 10.0 ml min to be passed through argon flow amount-1, hydrogen sulfide flow is 1.0 ml min-1, sputtering power is 9 W cm-2, Sputtering pressure is 0.5Pa, and the speed setting of chip bench is 5 circles/minute, and sputtering time is about 2 minutes, and thickness is about 3 nm, Complete MoS2After the sputtering of film, sputtering sedimentation there is into MoS2It is molten for 10% hydrochloric acid that the aluminium flake substrate of film is immersed in mass fraction To get rid of aluminium substrate in liquid, by centrifuging, washing, being freeze-dried to obtain MoS2Nanometer sheet；With MoS2Nanometer sheet is made For the negative material of lithium ion battery, by being coated on after being mixed with acetylene black and Kynoar on copper sheet（Mass ratio is 80:10:10）, electrode is used as after vacuum drying, using metal lithium sheet as to electrode, with L containing 1mol-1 LiPF6Carbonic acid Vinyl acetate (EC), dimethyl carbonate（DMC）Mixed solution is electrolyte（EC/DMC volume ratio is 1:1）, in 0.01-3V survey Try under voltage, the reversible specific capacity of the electrode is 1200 mAh g after 450 circulations of discharge and recharge-1, in 1000mA g-1 Current density under, the reversible specific capacity of electrode is up to 480 mAh g-1。
Embodiment 2
Using the copper sheet after polishing as substrate, it is cleaned by ultrasonic aluminium flake with acetone, ethanol, distilled water successively
And after drying, put within the vacuum chamber of magnetic control sputtering device, regulation target-substrate distance is about 7cm, with metal molybdenum materials Expect to be evacuated to 8*10 on 99.99% for target, target purity-4Pa, it is 40.0 ml min to be passed through argon flow amount-1, sulphur Change hydrogen flowrate is 3.0 ml min-1, sputtering power is 8 W cm-2, sputtering pressure 0.8Pa, the speed setting of chip bench is 10 Circle/minute, sputtering time are about 3 minutes, and thickness is about 5 nm, complete MoS2After the sputtering of film, sputtering sedimentation is had MoS2The aluminium flake substrate of film is immersed in the salpeter solution that mass fraction is 30% to get rid of aluminium substrate, by centrifuging, Wash, be freeze-dried to obtain MoS2Nanometer sheet；With MoS2Negative material of the nanometer sheet as lithium ion battery, by with second Coated on copper sheet after acetylene black and Kynoar mixing（Mass ratio is 80:10:10）, as electricity after vacuum drying Pole, using metal lithium sheet as to electrode, with L containing 1mol-1 LiPF6Ethylene carbonate (EC), dimethyl carbonate（DMC）Mixing Solution is electrolyte（EC/DMC volume ratio is 1:1）, under 0.01-3V test voltage, it is circulated 200 times by discharge and recharge The reversible specific capacity of the electrode is 910 mAh g afterwards-1, in 1000mA g-1Current density under, the reversible specific capacity of electrode can Up to 460 mAh g-1。
Example 3
Using the nickel sheet after polishing as substrate, it is cleaned by ultrasonic aluminium flake with acetone, ethanol, distilled water successively
And after drying, put within the vacuum chamber of magnetic control sputtering device, regulation target-substrate distance is about 7cm, with metal molybdenum materials Expect to be evacuated to 8*10 on 99.99% for target, target purity-4Pa, it is 30.0 ml min to be passed through argon flow amount-1, sulphur Change hydrogen flowrate is 1.5 ml min-1, sputtering power is 5 W cm-2, sputtering pressure is 0.5 Pa, and the speed setting of chip bench is 10 circles/minute, sputtering time are about 3 minutes, and thickness is about 3 nm, complete MoS2The sputtering of film.There is MoS with sputtering2Nanometer sheet Metal nickel sheet as catalytic hydrogen evolution electrode, in 1mol L-1Sulfuric acid medium in water electrolysis hydrogen production, electrode polarization voltage is obvious Reduce, compared to metal nickel electrode, under conditions of polarizing voltage is -0.2 V, liberation of hydrogen current density is about 28 mA cm-2, tower Fei Er slopes significantly reduce, and are about 45 millivolts/octave, effectively increase the efficiency of liberation of hydrogen, reduce energy consumption.
Example 4
Using the zinc metal sheet after polishing as substrate, it is cleaned by ultrasonic aluminium flake with acetone, ethanol, distilled water successively
And after drying, put within the vacuum chamber of magnetic control sputtering device, regulation target-substrate distance is about 6cm, with metal molybdenum materials Expect to be evacuated to 8*10 on 99.99% for target, target purity-4Pa, it is 20.0 ml min to be passed through argon flow amount-1, sulphur Change hydrogen flowrate is 1.2 ml min-1, sputtering power is 4 W cm-2, sputtering pressure is 0.5 Pa, and the speed setting of chip bench is 10 circles/minute, sputtering time are about 5 minutes, and thickness is about 3 nm, complete MoS2After the sputtering of film, by sputtering sedimentation There is MoS2The zinc metal sheet substrate of film is immersed in the hydrochloric acid solution that mass fraction is 30% to get rid of aluminium substrate, by centrifugation point From, wash, be freeze-dried to obtain MoS2Nanometer sheet, thickness are about 3 nm.

Claims (4)

  1. A kind of 1. molybdenum disulfide nano sheet and preparation method thereof, it is characterised in that：Molybdenum disulfide nano sheet is splashed by magnetic control reaction It is prepared by the method penetrated.
  2. 2. molybdenum disulfide nano sheet according to claim 1 and preparation method thereof, it is characterised in that：Described molybdenum disulfide Nanometer sheet thickness is between 1 nanometer -10 nanometers.
  3. 3. molybdenum disulfide nano sheet according to claim 1 and preparation method thereof, it is characterised in that：Reactive magnetron sputtering side Method is used as sputtering target material using metal molybdenum；Sputter gas used is Ar and H2S gaseous mixtures, H2S volume contents are 0.1-20%；It is used to splash It is metallic copper, zinc, tin, nickel or aluminium flake to penetrate deposition substrate；Its sputtering parameter is：Target-substrate distance is 5-9cm, and the rotating speed of chip bench exists 1-20 circles/minute, sputtering pressure are 0.1 Pa-10 Pa, Sputtering power density P=2-12W/cm2, H2S flows and Ar flows it Than being deposited on gold by controlling the change of sputtering parameter to prepare at 20-600 DEG C for 1/4-1/999, sputtering base reservoir temperature Belong to the MoS with different-thickness on substrate2Nanometer sheet；Metal substrate is dissolved finally by hydrochloric acid or salpeter solution Obtain MoS2Nanometer sheet.
  4. A kind of 4. molybdenum disulfide nano sheet according to claim 1 and preparation method thereof, it is characterised in that：Two described sulphur Change molybdenum nanometer sheet as the negative material of lithium ion battery, can also be applied to the electro-catalysis of hydrogen as electrode catalyst In oxidation reaction or electrocatalytic hydrogen evolution reaction.
CN201710789452.6A 2017-09-05 2017-09-05 A kind of molybdenum disulfide nano sheet and preparation method thereof Pending CN107512735A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109167061A (en) * 2018-08-30 2019-01-08 中南大学 A kind of solid-State Thin Film Li-Ion Batteries 3D film cathode and preparation method thereof
CN109763099A (en) * 2019-01-18 2019-05-17 华南理工大学 A kind of preparation method of molybdenum disulfide film
CN109796044A (en) * 2019-03-22 2019-05-24 南京晓庄学院 Molybdenum disulfide, the molybdenum disulfide of cobalt modification, the nanometer sheet of load Pd and its synthetic method and application
CN111987291A (en) * 2020-08-07 2020-11-24 河北大学 Preparation method of metal sulfide composite electrode for electrochemical lithium storage
CN112359318A (en) * 2020-10-19 2021-02-12 西安交通大学 MoS containing 1T phase2Film and preparation process thereof
CN113346013A (en) * 2021-05-07 2021-09-03 电子科技大学 Preparation method of electronic device, electronic device and information system

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CN103771517A (en) * 2014-01-17 2014-05-07 哈尔滨工业大学 Method for preparing liquid phase dispersion-based two-dimensional MoS2 nanosheets

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109167061A (en) * 2018-08-30 2019-01-08 中南大学 A kind of solid-State Thin Film Li-Ion Batteries 3D film cathode and preparation method thereof
CN109763099A (en) * 2019-01-18 2019-05-17 华南理工大学 A kind of preparation method of molybdenum disulfide film
CN109796044A (en) * 2019-03-22 2019-05-24 南京晓庄学院 Molybdenum disulfide, the molybdenum disulfide of cobalt modification, the nanometer sheet of load Pd and its synthetic method and application
CN111987291A (en) * 2020-08-07 2020-11-24 河北大学 Preparation method of metal sulfide composite electrode for electrochemical lithium storage
CN111987291B (en) * 2020-08-07 2022-12-13 河北大学 Preparation method of metal sulfide composite electrode for electrochemical lithium storage
CN112359318A (en) * 2020-10-19 2021-02-12 西安交通大学 MoS containing 1T phase2Film and preparation process thereof
CN113346013A (en) * 2021-05-07 2021-09-03 电子科技大学 Preparation method of electronic device, electronic device and information system

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Application publication date: 20171226