CN107963667B - A kind of acquisition methods without support MoS2 nanobelt - Google Patents

A kind of acquisition methods without support MoS2 nanobelt Download PDF

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CN107963667B
CN107963667B CN201711191657.0A CN201711191657A CN107963667B CN 107963667 B CN107963667 B CN 107963667B CN 201711191657 A CN201711191657 A CN 201711191657A CN 107963667 B CN107963667 B CN 107963667B
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pmma
mos
core
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moo
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CN107963667A (en
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施姣
黄寒
吴迪
郑晓明
韩欣彤
谢叮咚
蒋杰
高永立
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Central South University
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • 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
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/17—Nanostrips, nanoribbons or nanobelts, i.e. solid nanofibres with two significantly differing dimensions between 1-100 nanometer

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  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The present invention provides a kind of without support MoS2The acquisition methods of nanobelt, comprising the following steps: toasted after spin coating PMMA solution, then sample be placed in KOH corrosive liquid impregnate removing PMMA layers, by floating, be stained with MoO2For core, MoS2It fishes for out and is cleaned with deionized water for the PMMA layer of the core-shell structure of shell, by PMMA/MoO2@MoS2Nanometer rods/SiO2/ Si substrate obtains in acetone soln after colloidal sol without support MoS2.For the present invention independent of substrate template material and structure, process safety is effective and will not destroy MoS2Crystal structure directly acquires unsupported MoS2Nanobelt.

Description

It is a kind of without support MoS2The acquisition methods of nanobelt
Technical field
The present invention relates to MoS2Acquiring technology field is separated, particularly, is related to a kind of without support MoS2The acquisition side of nanobelt Method.
Background technique
As one of the member of Transition-metal dichalcogenide (TMDs), MoS2Due to its unique physics and chemically Matter is widely used in the fields such as catalysis, sensor, solar battery and photoelectric device preparation.Studies have shown that without support MoS2And have support MoS2It compares, the former has better crystallinity and optical quality.So how to obtain high quality without branch Support MoS2It is worth research.
Currently, preparation is without support MoS2There are mainly two types of methods: PMMA secondary transfer method and wet contact printing method.
1. PMMA secondary transfer method specifically comprises the processes of: prepare the controllable MoS of the number of plies on a silicon substrate first2Sample, generally Using CVD method.Then in one layer of PMMA solution of sample surfaces spin coating, heating reinforces and forms PMMA film layer, uses diluted acid (HF) solution or alkali (NaOH, KOH) solution corrosion fall the SiO of silicon base2Layer separates PMMA layers with substrate.MoS2Sample with PMMA layers are transferred to clean special pattern substrate together and (form the Si of hole configurations through over etching3N4Or silicon base) on.Most Afterwards, remaining PMMA ingredient is removed, is can be obtained after dry without support MoS2.In this process, it first passes around etching and forms hole The Si of hole structure3N4Or silicon base is essential, because the two-dimensional material shifted is stratiform, if transfer Substrate does not have hole, then the two-dimensional material will be contacted all with substrate after transfer, not hanging part is difficult to separate.Its Except having during glue except peptizing agent remains in hole after secondary transfer, this is inevitable.
2. wet contact printing method specifically comprises the processes of: with MoS2/SiO2It, will be with MoS for/Si2SiO2/ Si substrate with Patterned Polydimethylsiloxane (PDMS) substrate stacks face-to-face, and silicon wafer is upper, and PDMS is under.With diluted HF Acid solution (16%) from top to bottom drips 1min, corrodes SiO2After layer, Si layers are removed, MoS2It is transferred in PDMS substrate, tilts base Bottom is to remove remaining HF acid solution and drying.Although wet contact printing method is avoided that except glue process, but still extremely rely on In underlying structure, and the original substrate requirements for shifting sample must be able to be corroded by acid-base solution.
Due to without support MoS2Acquisition have the above limitation, use and inconvenient.
Summary of the invention
It is an object of that present invention to provide a kind of without support MoS2The acquisition methods of nanobelt, to solve MoS2Sample shifted The technical issues of underlying structure that hole must be relied in journey, the substrate material corroded by acid-base solution.
To achieve the above object, the present invention provides a kind of without support MoS2The acquisition methods of nanobelt, including following step It is rapid:
A, one layer of PMMA will spin coating PMMA solution: be formed on the sample surfaces spin coating PMMA solution that need to be shifted, sample surface Film；The sample structure are as follows: MoO is formed in sapphire substrates2For core, MoS2For the core-shell structure of shell；
B, sample toasts: the sample of the good PMMA of spin coating being placed on 180 DEG C of warm tables, 5min is toasted, reinforces PMMA film；
C, PMMA layers are removed: sample being placed in KOH corrosive liquid and is impregnated, steep parameters: 90 DEG C, 50min；After 50min, To its cooled to room temperature, it is stained with MoO2For core, MoS2PMMA layer for the core-shell structure of shell has disengaged from process for sapphire-based bottom surface Swim in corrosive liquid upper layer；
D, PMMA layers transfer: with silicon wafer by floating, be stained with MoO2For core, MoS2For the PMMA layer fishing of the core-shell structure of shell It takes out and is cleaned with deionized water, repeated 2~3 times, silicon wafer slant setting is waited into natural air drying；
E, it removes PMMA: the PMMA layer after air-drying being placed in 90 DEG C of acetone solns and dissolves 2h, at this time MoO2For core, MoS2 It is separated for the core-shell structure of shell, MoO2Kernel is detached from silicon chip surface into solution, up to without support MoS in silicon base2。
Preferably, in step A spin coating PMMA solution parameter are as follows: first use low speed 500r/min spin coating 10s, then with high speed 3500r/min spin coating 60s.
Preferably, in step D, when with deionized water cleaning sample, MoO is had on PMMA layer2For core, MoS2For the core of shell The one of shell structure is down.
Preferably, in step C, with stroke one on the PMMA film at the sample substrate edge of tweezers or pocket knife after baking Circle, then sample is placed in KOH corrosive liquid and is impregnated.
Preferably, the silicon wafer in step D is common not Templated silicon wafer.
The invention has the following advantages:
For the present invention independent of substrate template material and structure, process safety is effective and will not destroy MoS2Crystal structure, Directly acquire the MoS of no support (freestanding)2Nanobelt.It can apply: without support two-dimensional atomic crystal and heterogeneous The fields such as preparation, photoelectric device preparation, the pressure sensor of knot.
MoO of the application to be formed in sapphire substrates2For core, MoS2Based on the core-shell structure of shell, in core-shell structure Upper spin coating PMMA layers, core-shell structure is then allowed to fall off from substrate in company with PMMA layers, then take the plane base of any non-template Bottom (not reacting with lye and acetone soln) pulls PMMA layers and core-shell structure out from lye, in acetone dissolution point From, i.e., obtained in the substrate of non-template without support MoS2Structure；Existing transfer method is avoided to be required to be etched into hole The operational deficiencies of the templating substrate of structure.
Other than objects, features and advantages described above, there are also other objects, features and advantages by the present invention. Below with reference to figure, the present invention is described in further detail.
Detailed description of the invention
The attached drawing constituted part of this application is used to provide further understanding of the present invention, schematic reality of the invention It applies example and its explanation is used to explain the present invention, do not constitute improper limitations of the present invention.In the accompanying drawings:
Fig. 1 is the sample structure figure of the step A of the preferred embodiment of the present invention；
Fig. 2 is the sample structure figure of the step C of the preferred embodiment of the present invention；
Fig. 3 is the sample structure figure of the step E of the preferred embodiment of the present invention；
Wherein, 1, sapphire substrates, 2, MoO2, 3, MoS2, 4, PMMA layers, 5, free radical bottom；6, lye；
Fig. 4 (a) is the OM figure of sample before shifting, and Fig. 4 (b) is after shifting without support MoS2OM figure；
Fig. 4 (c) is the 2D-GIXRD figure of sample before shifting；Fig. 4 (d) is the Raman spectrum of transfer front and back sample；
Fig. 5 (a) is that the OM of PMMA secondary transfer result schemes；Fig. 5 (b) is that the OM of mechanical stripping result schemes；
Fig. 5 (c) is the SEM figure that solwution method shifts result.
Specific embodiment
The embodiment of the present invention is described in detail below in conjunction with attached drawing, but the present invention can be limited according to claim Fixed and covering multitude of different ways is implemented.
Referring to Fig. 1, Fig. 2, Fig. 3, the specific embodiment of the application is as described below.
Example one:
1.MoO2@MoS2core-shell(MoO2For core, MoS2For the core-shell structure of shell) Nanorods Samples preparation
Sample used in the present invention is prepared in CVD (Hefei Ke Jing Materials Technology Ltd.) system, S block and MoO3Powder selects c-sapphire substrate as pre-reaction material, substrate, leads to nitrogen as protection and current-carrying gas.It controls first The concentration of reactant processed, in low S/MoO3-xWhen concentration ratio, MoO is grown first in c-sapphire substrate2Nanometer rods increase After the concentration of reactant S steam, MoO2Outermost layer is sulfided into MoS2, that is, MoO required for us is prepared2For core, MoS2For the nuclear shell structure nano rod of shell.
2.PMMA secondary transfer
A. the mechanical pump for opening the configuration of spin coating instrument, sample is placed at spin coating instrument suction piece, on specimen face side.With rubber head dropper PMMA solution is drawn, and is dripped in the sample surface that need to be shifted until PMMA solution covers sample, starting spin coating instrument, spin coating completes it Afterwards, one layer of PMMA film is formed on sample surface, plays the role of supporting layer when transfer.Spin coating parameters: low speed 500r/min, 10s, High speed 3500r/min, 60s；
B. it is the curling for preventing transfer film layer, the sapphire substrates of the good PMMA of spin coating is placed on warm table and are toasted, reinforces PMMA film.Flue curing parameter: 180 DEG C, 5min, baking time is unsuitable too long, otherwise will be difficult to fall off for PMMA layers；
C. KOH corrosive liquid is placed on warm table be preheated to 90 DEG C it is spare.With the sample of tweezers or pocket knife after baking Basal edge exert oneself stroke one circle so that PMMA layers are easier to be detached from；It is deep perpendicular to one circle of substrate surface edge rotation when stroke Degree is scratches PMMA, it is therefore intended that weakens the active force of basal edge and PMMA, and makes corrosive liquid faster from scratching Place starts to corrode.
It is placed in KOH corrosive liquid and impregnates after processing, steep parameters: 90 DEG C, 50min；After 50min, to its natural cooling To room temperature, PMMA layers due under the action of the surface tension of liquid at this time, MoO2Kernel film will be disengaged from substrate surface floating On corrosive liquid upper layer.
D. the PMMA layer of floating is fished for out with clean silicon wafer and is cleaned with deionized water, repeated 2~3 times, it should be noted that PMMA layers of front and back sides guarantee to have every time the one of sample face-down, can guarantee that fishing for rear sample with free radical bottom is strictly in this way Substrate is directly contacted, otherwise transfer failure.Then PMMA layers are fished for clean silicon base, for the planarization for keeping film, Ying Jiang Silicon base slant setting waits natural air drying；It is placed in the place for arbitrarily having supporter with 30 °~90 ° of angle tilt.
Clean silicon wafer can be used any free radical bottom to replace, which is not reacted i.e. with the solution that can be touched in experiment It can.
E. the characteristics of being soluble in organic solvent using PMMA, except glue uses acetone.Sample is placed in acetone soln and is handled, PMMA is soluble in organic solvent, and PMMA can be dissolved during impregnating acetone；MoO at this time2@MoS2Core-shell nanometers Molybdenum oxide in stick can be detached from substrate surface since the active force between substrate is weaker and go in solution, and molybdenum sulfide is then protected It stays.Dehydrated alcohol and deionized water cleaning sample 2~3 times are finally used, transfer work is completed after naturally dry.Dissolution ginseng Number: 90 DEG C, 2h.
Referring to fig. 4, Fig. 4 (a) is the OM figure of sample before shifting, and is the CVD method seen under optical microscopy in c surface sapphire The MoO of upper growth2For core, MoS2For the nanometer rods of the core-shell structure of shell.Fig. 4 (b) is after shifting without support MoS2OM figure；For PMMA auxiliary law will scheme to be left the optical picture without support molybdenum sulfide after a sample is transferred to silicon base.
Fig. 4 (c) is the 2D-GIXRD figure of sample before shifting, and the ear of maize that the point diffraction of Cong Tuzhong can analyze to obtain us is true It is in fact MoO2@MoS2Core-shell nanometer rods；Fig. 4 (d) is the Raman spectrum of transfer front and back sample, and comparison is it can be found that transfer The Raman spectrum of sample afterwards only leaves MoS2Peak.
Comparison example two:
1.MoO2@MoS2The preparation of core-shell Nanorods Samples
Sample used in this example is prepared in CVD (Hefei Ke Jing Materials Technology Ltd.) system, S block and MoO3Powder selects c-sapphire as pre-reaction material, substrate, leads to nitrogen as protection and current-carrying gas.
2. mechanical stripping transfer method
A. MoO will first be grown2@MoS2Core-shell nanometer rods/sapphire substrates are placed on 95 DEG C of hot plate, enhancing Interaction force between adhesive tape and nanometer rods.
B. before the raising of sapphire substrates temperature, Scotch adhesive tape is attached to nanorod surfaces rapidly, quickly uses beaker Bottom of a cup firmly squeezes adhesive tape upper surface, then removes external force, rapidly takes off material.It tears the glue being sticked in sapphire substrates Band is stained with MoO below Scotch adhesive tape at this time2@MoS2Core-shell nanometer rods.
C., adhesive tape is attached to silicon substrate surface cleaned in advance, is then squeezed with bottom of a cup, fills nanometer rods with substrate knot Tap touching, takes adhesive tape off, the silicon base for being stained with nanometer rods is placed in 50 DEG C of hot acetone of heating water bath, dissolves residue glue, follows Ring 2~3 times.
D. alcohol washes silicon base is first used, is then rinsed with deionized water, finally with being dried with nitrogen.By the silicon substrate of drying Moisture removal and remaining organic matter are removed in the hot plate heating that bottom is placed on 120 DEG C.
Comparison example three:
1.MoO2@MoS2The preparation of core-shell Nanorods Samples
Sample used in this example is prepared in CVD (Hefei Ke Jing Materials Technology Ltd.) system, S block and MoO3Powder selects c-sapphire as pre-reaction material, substrate, leads to nitrogen as protection and current-carrying gas.
2. solwution method shifts
A. the dehydrated alcohol of 5ml is added in reagent bottle with liquid-transfering gun, and then places a sample into reagent bottle with tweezers, protected Card solution floods sample.
B. the reagent bottle containing sample is put into ultrasonator, vibrates 30min at room temperature to guarantee that sample can be from substrate Under strip down, duration of oscillation is unsuitable too long in order to avoid sample is by excessive damage.
C. it after shaking, takes out reagent bottle and shakes up, be evenly distributed in sample in solution, drawn with rubber head dropper A small amount of reagent simultaneously drips in clean silicon base.After silicon base natural air drying, transfer work is completed.
Mechanical stripping method shifts result referring to Fig. 5 (b), is only capable of a small amount of MoO2@MoS2Core-shell nanometer rods are precious from indigo plant Ground mass completely strips on bottom, but can not separate MoO2And MoS2.Solwution method shifts result referring to Fig. 5 (c), so that nanometer rods It resolves and splits under sonic oscillation effect, size significantly reduces.Comparison mechanical stripping method and solwution method are known that only PMMA secondary transfer method (referring to Fig. 5 (a)) can obtain completely without support MoS2。
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.

Claims (3)

1. a kind of without support MoS2The acquisition methods of nanobelt, which comprises the following steps:
A, one layer of PMMA film will spin coating PMMA solution: be formed on the sample surfaces spin coating PMMA solution that need to be shifted, sample surface； The sample structure are as follows: MoO is formed in sapphire substrates2For core, MoS2For the core-shell structure of shell；
B, sample toasts: the sample of the good PMMA of spin coating being placed on 180 DEG C of warm tables, 5min is toasted, reinforces PMMA film；
C, PMMA layers are removed: sample being placed in KOH corrosive liquid and is impregnated, steep parameters: 90 DEG C, 50min；After 50min, certainly to it It is so cooled to room temperature, is stained with MoO2For core, MoS2It has disengaged from sapphire substrates surface flotation for the PMMA layer of the core-shell structure of shell and exists Corrosive liquid upper layer；It is enclosed with stroke one on the PMMA film at the sample substrate edge of tweezers or pocket knife after baking, then by sample It is placed in KOH corrosive liquid and impregnates；
D, PMMA layers transfer: with silicon wafer by floating, be stained with MoO2For core, MoS2PMMA layer for the core-shell structure of shell is fished for out It is cleaned, is repeated 2~3 times with deionized water, silicon wafer slant setting is waited into natural air drying；When with deionized water cleaning sample, MoO is had on PMMA layer2For core, MoS2One for the core-shell structure of shell is face-down；
E, it removes PMMA: the PMMA layer after air-drying being placed in 90 DEG C of acetone solns and dissolves 2h, at this time MoO2For core, MoS2For shell Core-shell structure separation, MoO2Kernel is detached from silicon chip surface into solution, up to without support MoS in silicon base2。
2. acquisition methods according to claim 1, which is characterized in that in step A, the parameter of spin coating PMMA solution are as follows: first With low speed 500r/min spin coating 10s, high speed 3500r/min spin coating 60s is then used.
3. acquisition methods according to claim 1, which is characterized in that the silicon wafer in step D is commonly not Templated Silicon wafer.
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CN110767533B (en) * 2019-10-24 2022-05-24 华南理工大学 Wafer-level MoS2Method for preparing single-layer film

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