CN108286042A - A kind of number of plies is uniformly and the preparation method of high quality molybdenum disulfide film - Google Patents
A kind of number of plies is uniformly and the preparation method of high quality molybdenum disulfide film Download PDFInfo
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- CN108286042A CN108286042A CN201810225492.2A CN201810225492A CN108286042A CN 108286042 A CN108286042 A CN 108286042A CN 201810225492 A CN201810225492 A CN 201810225492A CN 108286042 A CN108286042 A CN 108286042A
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- molybdenum disulfide
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- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/305—Sulfides, selenides, or tellurides
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- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
Abstract
Uniform and high quality molybdenum disulfide film the preparation method the invention discloses a kind of number of plies, large area single-layer molybdenum disulfide film is prepared on the silicon substrate for being covered with 300nm thickness silicon dioxide layers using potassium chloride auxiliary chemical vapor deposition method, the amount by controlling different potassium chloride obtains various sizes of single-layer molybdenum disulfide film.The advantage of the invention is effectively prepare the preferable high quality molybdenum disulfide film of uniformity using potassium chloride, and the experimental method is simple for process, it is of low cost, it is suitble to large-scale production, prepared molybdenum disulfide film can be used as two-dimentional transparent semiconductor film and be employed for the fields such as photoelectric device, flexible and transparent device, optical detector, and the invention, which prepares the electronic material and produces, has higher application value and meaning.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of number of plies is uniformly and high quality molybdenum disulfide film
Preparation method.
Background technology
Molybdenum disulfide is the two-dimension nano materials being made of one layer of molybdenum atom and two layers of sulphur atom, has and is similar to graphene
Two-dimensional layered structure, each layer is stacked with to form bulk.Each two dimensional crystal layer thickness is about 0.65nm, these layers be by
Hereby power is combined together weak Robert Van de Walle.Single layer molybdenum disulfide is by the molybdenum atom and two layers of Hexagonal array of one layer of Hexagonal array
Sulphur atom constitute, molybdenum atom layer is clipped between two layers of sulphur atom, and the S-Mo-S atoms that covalent bond is formed are arranged in the form of triangular prism
Row, constitute hexagonal crystallographic texture.Molybdenum disulfide has very high mechanical strength, and has higher Young compared with steel
Modulus, the molybdenum disulfide consubstantiality phase molybdenum disulfide of single layer is compared to firmer.Crystal of molybdenum disulfide layer can deform up to 11% not
Fracture bends to the curvature that radius is 0.75mm, without losing its characteristic electron.These advantages make molybdenum disulfide be expected into
For flexible electronics.Molybdenum disulfide is a kind of unique stratified material for belonging to Transition-metal dichalcogenide, and band gap is with layer
Several change and become direct band-gap semicondictor from indirect band-gap semiconductor.The preparation of molybdenum disulfide film be divided into physical method and
Chemical method, such as：Mechanical stripping, epitaxial growth, chemical vapor deposition, chemical stripping, chemical synthesis etc..Wherein chemical vapor deposition
Area method is of great significance to application of the molybdenum disulfide in terms of microelectronics, is generally acknowledged at present most promising molybdenum disulfide system
Preparation Method.There is researcher to be engaged in the preparation of molybdenum disulfide film at present and achieved certain achievement, such as China is special
Sharp CN201710519326.9 is disclosed a kind of using chemical gas using the method that molybdenum trioxide prepares single-layer molybdenum disulfide film
Phase sedimentation synthesis of carbon/molybdenum disulfide film, molybdenum disulfide size prepared by this method are uneven.
Invention content
For the defect and deficiency of existing technology of preparing, uniform two sulphur of high quality of the number of plies is prepared the present invention provides a kind of
Change the new method of molybdenum film.Preparation method mainly prepares molybdenum disulfide monocrystalline size from increase, improves the knot of molybdenum disulfide
Crystalloid amount.This experimental process profile is simple, and raw material, which obtains, to be easy, and the size for the monocrystalline molybdenum disulfide prepared is larger, is suitble to make
Molybdenum disulfide film is prepared with chemical vapour deposition technique.
To solve the above problems, the technical solution that the present invention takes is：
A kind of number of plies uniformly and the preparation method of high quality molybdenum disulfide film, includes the following steps：
Step 1) is cleaned by ultrasonic silica/silicon substrate using acetone/carbon tetrachloride, ethyl alcohol；
Step 2) configures 20ml " Piranha " solution and hydrophilic solution；
By 1：3 ratio measures the concentrated sulfuric acid of the hydrogen peroxide and 15ml a concentration of 98% of 5ml a concentration of 30% respectively, configuration
Hydrogen peroxide is poured slowly into the concentrated sulfuric acid and is kept stirring in the process, prevents the high temperature in configuration process from causing flying for mixed liquor
It splashes, is cooled to after room temperature and the silica/silicon substrate in step 1) is put into " Piranha " solution, cleaned；
By treated, substrate taking-up is cleaned out with deionized water, and drying is for use；
Step 3) weighs the bright sulfur powder, the potassium chloride of 3mg and the molybdenum trioxide of 0.5mg of 120mg respectively, and bright sulfur powder is placed
In the upstream position of tube-type atmosphere furnace quartz ampoule, molybdenum trioxide powder is positioned on the silica/silicon substrate in step 2)
It is put in tube-type atmosphere furnace heated center position, potassium chloride is put between silica/silicon substrate and bright sulfur powder, in 60sccm argons
Under gas velocity, 780 DEG C of reaction 15min are warming up to, the preparation of molybdenum disulfide film is carried out, is then cooled to room temperature, substrate is taken
Go out to obtain the molybdenum disulfide film prepared using potassium chloride auxiliary.
Preferably, when the silica/silicon substrate is soaked in " Piranha " solution, it is 80 DEG C to keep temperature setting.
Preferably, when the silica/silicon substrate is soaked in " Piranha " solution, soaking time 1h.
Preferably, the use of the quality of bright sulfur powder is used during chemical vapour deposition technique is 120mg.
Preferably, electricity is 0.5mg using the quality of molybdenum trioxide is used during chemical vapour deposition technique.
Preferably, the use of the quality of potassium chloride is used during chemical vapour deposition technique is 3-5mg.
Preferably, the use of distance between potassium chloride and substrate is used during chemical vapour deposition technique is 6cm.
Preferably, the use of the flow of argon gas during chemical vapour deposition technique is 60sccm.
Preferably, the use of the temperature of molybdenum disulfide film is grown during chemical vapour deposition technique it is 780 DEG C.
Preferably, the use of the time of molybdenum disulfide film is grown during chemical vapour deposition technique is 15min.
The present invention has the advantages that：
1) the single layer molybdenum disulfide monocrystalline that size is more uniform, area is larger is being prepared in success；
2) chemical reagent for having used potassium chloride to prepare single layer molybdenum disulfide monocrystalline as auxiliary, and adding method letter are selected
Just, be conducive to repeat to test；
3) emphasis of the invention is tried still in terms of preparing molybdenum disulfide film by preparing molybdenum disulfide chemistry to auxiliary
The addition of agent so that the uniformity of the number of plies of the molybdenum disulfide film prepared on silica/silicon substrate enhances and improves two
Molybdenum sulfide film quality prepares the good large-area high-quality molybdenum disulfide film of uniformity using chemical vapour deposition technique.
4) this technique compares existing technique, provides new thinking and selection, preparation process is simple, and passes through control
Adding the amount of potassium chloride effectively control can prepare the size and the number of plies of molybdenum disulfide monocrystalline, and technological parameter accurately controls, and makes
High for the molybdenum disulfide film quality gone out, the number of plies is uniform, is suitble to repeat to prepare and study.
5) source material safety and environmental protection of the present invention not will produce toxic or environmentally harmful substance.
Description of the drawings
Fig. 1 is that the experiment of embodiment 1, embodiment 2 and comparative example 1 in the present invention prepares schematic diagram；
Fig. 2 is the Raman spectrum of embodiment 1 in the present invention；
Fig. 3 is the metallographic microscope image of embodiment 1 in the present invention；
Fig. 4 is the Raman spectrum of embodiment 2 in the present invention；
Fig. 5 is the metallographic microscope image of embodiment 2 in the present invention；
Fig. 6 is the Raman spectrum of comparative example 1 in the present invention；
Fig. 7 is the metallographic microscope image of comparative example 1 in the present invention.
Specific implementation mode
Below in conjunction with attached drawing and specific embodiment, the present invention will be described in detail, herein illustrative examples of the invention
And explanation is used for explaining the present invention, but it is not as a limitation of the invention.
The present invention purport be by using potassium chloride auxiliary reagent, to play improve molybdenum disulfide film uniformity and
The effect of quality prepares the molybdenum disulfide film for the large-area high-quality having good uniformity with this.Nowadays, chemistry is being utilized
The research field that vapor deposition law technology prepares molybdenum disulfide film has been achieved for certain progress, meanwhile, preparing graphite
Most common auxiliary reagent is -3,4,9,10- tetracarboxylic dianhydrides etc. when alkene film, so using new auxiliary reagent chlorine herein
Change potassium, chemical vapour deposition technique is recycled to prepare graphene film on silica/silicon substrate.
Chemical vapor deposition (CVD) refers to the gas phase reaction under high temperature, for example, metal halide, organic metal, hydrocarbon
The thermal decomposition of compound etc., hydrogen reduction or make its mixed gas occur at high temperature chemical reaction with precipitating metal, oxide,
The method of the inorganic material such as carbide.This technology is initially to be developed as the means of coating, but be not only applied to heat-resisting
The coating of substance, and applied to the refined of high purity metal, powder synthesis, semiconductive thin film etc., be one and have much feature
Technical field.It is technically characterized in that：High-melting-point substances can synthesize at low temperature；Be precipitated substance form monocrystalline, polycrystalline,
Whisker, powder, film etc. are a variety of；Can not only carry out coating on substrate, and can in powder surface coating, etc..Especially
Be that can synthesize high-melting-point substances at low temperature, contribution be made that at energy saving aspect, be as a kind of new technology it is coming,
Equally, molybdenum disulfide film field is being prepared, CVD technology is also acknowledged as preparing large-area high-quality graphene film most suitable
Method.
Embodiment one：
The present embodiment, which is provided, to be assisted preparing the preferable large-area high-quality molybdenum disulfide film of uniformity using potassium chloride
Method, shown in experiment schematic diagram such as Fig. 1 (a), experimentation includes the following steps：
Step 1)：It is used first with acetone/carbon tetrachloride mixed solution, absolute ethyl alcohol according to this sequence respectively to dioxy
SiClx/silicon substrate is cleaned by ultrasonic, and each process continues 30 minutes, the effect of acetone/carbon tetrachloride mixed solution be for
The grease on copper sheet surface is removed, ethyl alcohol is a kind of effective dispersant, and can clean dispersed silicon dioxide/surface of silicon can
Solubility impurity and remaining acetone use deionized water again later, obtain clean silica/silicon substrate.
Step 2)：20ml " Piranha " solution is configured, in order to thoroughly remove the organic impurities of substrate surface, and increases lining
The hydrophily of bottom surface.1 is pressed first：3 ratio measures the hydrogen peroxide and 15ml a concentration of 98% of 5ml a concentration of 30% respectively
Hydrogen peroxide is poured slowly into the concentrated sulfuric acid and is kept stirring in configuration process, prevents the high temperature in configuration process from causing by the concentrated sulfuric acid
The splashing of mixed liquor is cooled to after room temperature silica/silicon substrate being put into " Piranha " solution, is warming up to 80 DEG C, keeps
1h.By treated, substrate taking-up is cleaned out with deionized water, and drying is for use.
Step 3)：The bright sulfur powder, the potassium chloride of 3mg and the molybdenum trioxide of 0.5mg for weighing 120mg respectively, bright sulfur powder is put
It is placed in the upstream position of tube-type atmosphere furnace quartz ampoule, molybdenum trioxide powder is positioned over to the silica/silicon substrate cleaned up
On be put in tube-type atmosphere furnace heated center position, potassium chloride is put between silica/silicon substrate and bright sulfur powder, potassium chloride with
The distance between silica/silicon substrate is 6cm.
Step 4)：It after argon purge quartz ampoule, vacuumizes, and argon gas flow velocity is adjusted to 60sccm.Then press 10
DEG C/temperature rises to 780 DEG C by the heating rate of min, keeps the temperature cooled to room temperature after 15min, sample is taken out etc. to be tested.
Fig. 1 (a) is the experimental provision schematic diagram that molybdenum disulfide film is prepared using potassium chloride auxiliary, and potassium chloride is placed on
Between sulphur powder and molybdenum trioxide.Fig. 2 is the Raman collection of illustrative plates for preparing sample, the molybdenum disulfide sample as can be seen from the figure prepared
Product are single layer, and crystalline quality is higher.
Fig. 3 is the metallographic microscope image of the molybdenum disulfide film prepared using potassium chloride, is as can be seen from the figure prepared
The molybdenum disulfide film gone out is big compared to the film dimensions of unused potassium chloride, and shape is uniform.
Embodiment two：
This comparative example provides a kind of method that the auxiliary reducing potassium chloride usage amount prepares molybdenum disulfide film, including following
Step,
Step 1)：It is identical to the cleaning method of substrate with embodiment one.
Step 2) is identical as embodiment one.
Step 3)：The bright sulfur powder, the potassium chloride of 5mg and the molybdenum trioxide of 0.5mg for weighing 120mg respectively, bright sulfur powder is put
It is placed in the upstream position of tube-type atmosphere furnace quartz ampoule, molybdenum trioxide powder is positioned over to the silica/silicon substrate cleaned up
On be put in tube-type atmosphere furnace heated center position, potassium chloride is put between silica/silicon substrate and bright sulfur powder, potassium chloride with
The distance between silica/silicon substrate is 6cm.
Step 4)：It is identical as embodiment two.
Fig. 4 is the Raman collection of illustrative plates for preparing sample, and the molybdenum disulfide sample as can be seen from the figure prepared is single layer, knot
Crystalloid amount is higher.Fig. 5 is the metallographic microscope image that molybdenum disulfide film is prepared using 5mg potassium chloride auxiliary, can be with from figure
Find out that the molybdenum disulfide film prepared is big compared to the film dimensions of unused potassium chloride, and shape is uniform, but compared to
Then want small using the 3mg molybdenum disulfide monocrystalline sizes prepared.
Comparative example one：
This comparative example provides and does not add the method that potassium chloride prepares molybdenum disulfide film on silica/silicon substrate, real
It tests shown in schematic diagram such as Fig. 1 (b), experimentation includes the following steps：
Step 1)：It is identical as embodiment two.
Step 2)：It is identical as embodiment two.
Step 3)：The bright sulfur powder of 120mg and the molybdenum trioxide of 0.5mg are weighed respectively, and bright sulfur powder is positioned over tubular type atmosphere
Molybdenum trioxide powder is positioned on for use silica/silicon substrate and is put in tube-type atmosphere furnace by the upstream position of stove quartz ampoule
Heated center position.It after argon purge quartz ampoule, vacuumizes, and argon gas flow velocity is adjusted to 60sccm.Then by 10 DEG C/
Temperature is risen to 780 DEG C by the heating rate of min, keeps the temperature cooled to room temperature after 15min, and sample taking-up etc. is to be tested.
Fig. 6 is the Raman collection of illustrative plates for the molybdenum disulfide film prepared, and the method is prepared two are can be seen that from collection of illustrative plates
The molybdenum sulfide number of plies is more.Fig. 7 is the metallographic microscope image for the molybdenum disulfide prepared, it can be seen that auxiliary without using potassium chloride
It helps under conditions of preparation, the monocrystalline size for the molybdenum disulfide prepared is smaller, and shape is uneven.Show auxiliary in no potassium chloride
The number of plies that molybdenum disulfide is prepared in the case of helping is more, second-rate.
By comparative example one it can be seen that the invention method can be to a certain extent compared with embodiment one and embodiment two
It improves and prepares the quality of molybdenum disulfide film and the uniformity of the number of plies on silica/silicon substrate, and participated in by changing in reality
The amount of the potassium chloride of reaction can effectively control the size of the molybdenum disulfide monocrystalline of preparation, it is thin to be conducive to controllable preparation molybdenum disulfide
Film.
The technical solution disclosed in the embodiment of the present invention is described in detail above, specific implementation used herein
Example is expounded the principle and embodiment of the embodiment of the present invention, and the explanation of above example is only applicable to help to understand
The principle of the embodiment of the present invention；Meanwhile for those of ordinary skill in the art, embodiment, is being embodied according to the present invention
There will be changes in mode and application range, in conclusion the content of the present specification should not be construed as the limit to the present invention
System.
Claims (10)
1. a kind of number of plies uniformly and high quality molybdenum disulfide film preparation method, include the following steps：
Step 1) is cleaned by ultrasonic silica/silicon substrate using acetone/carbon tetrachloride, ethyl alcohol；
Step 2) configures 20ml " Piranha " solution and hydrophilic solution；
By 1：3 ratio measures the concentrated sulfuric acid of the hydrogen peroxide and 15ml a concentration of 98% of 5ml a concentration of 30%, configuration process respectively
It is middle that hydrogen peroxide is poured slowly into the concentrated sulfuric acid and is kept stirring, it prevents the high temperature in configuration process from causing the splashing of mixed liquor, waits for
The silica/silicon substrate in step 1) is put into " Piranha " solution after being cooled to room temperature, is cleaned；
By treated, substrate taking-up is cleaned out with deionized water, and drying is for use；
Step 3) weighs the bright sulfur powder, the potassium chloride of 3mg and the molybdenum trioxide of 0.5mg of 120mg respectively, and bright sulfur powder is positioned over pipe
The upstream position of formula atmosphere furnace quartz ampoule will be put on silica/silicon substrate that molybdenum trioxide powder is positioned in step 2)
Potassium chloride is put between silica/silicon substrate and bright sulfur powder by tube-type atmosphere furnace heated center position, in 60sccm argon gas streams
Under speed, 780 DEG C of reaction 15min are warming up to, the preparation of molybdenum disulfide film is carried out, is then cooled to room temperature, substrate is taken out
To the molybdenum disulfide film for using potassium chloride auxiliary to prepare.
2. preparation method as described in claim 1, which is characterized in that it is molten that the silica/silicon substrate is soaked in " Piranha "
When liquid, it is 80 DEG C to keep temperature setting.
3. preparation method as described in claim 1, which is characterized in that it is molten that the silica/silicon substrate is soaked in " Piranha "
When liquid, soaking time 1h.
4. preparation method as described in claim 1, which is characterized in that using chemical vapour deposition technique in the process using bright sulfur powder
Quality is 120mg.
5. preparation method as described in claim 1, which is characterized in that electricity is aoxidized using during chemical vapour deposition technique using three
The quality of molybdenum is 0.5mg.
6. preparation method as described in claim 1, which is characterized in that using chemical vapour deposition technique in the process using potassium chloride
Quality is 3-5mg.
7. preparation method as described in claim 1, which is characterized in that using during chemical vapour deposition technique using potassium chloride with
Distance is 6cm between substrate.
8. preparation method as described in claim 1, which is characterized in that the flow using argon gas during chemical vapour deposition technique is
60sccm。
9. preparation method as described in claim 1, which is characterized in that grow molybdenum disulfide in the process using chemical vapour deposition technique
The temperature of film is 780 DEG C.
10. preparation method as described in claim 1, which is characterized in that grow curing in the process using chemical vapour deposition technique
The time of molybdenum film is 15min.
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| CN108987408A (en) * | 2018-07-25 | 2018-12-11 | 长江存储科技有限责任公司 | A kind of 3D nand memory and its manufacturing method |
| CN109336181A (en) * | 2018-09-20 | 2019-02-15 | 天津大学 | A kind of preparation method of two dimension Transition-metal dichalcogenide |
| CN110416065A (en) * | 2019-07-29 | 2019-11-05 | 湖南大学 | Molybdenum disulfide/bis- tungsten selenide vertical heterojunctions preparation method |
| CN111501012A (en) * | 2020-03-24 | 2020-08-07 | 西北大学 | Double-layer WS2/MoS2Transverse heterojunction material, preparation method and application |
| CN112909275A (en) * | 2021-03-29 | 2021-06-04 | 华中科技大学 | Sp-rich food3Metal-free carbon-based catalyst of hybrid carbon and preparation method thereof |
| CN114231945A (en) * | 2021-12-15 | 2022-03-25 | 江苏籽硕科技有限公司 | Method for preparing molybdenum disulfide film by chemical vapor deposition method |
| CN115490265A (en) * | 2022-09-06 | 2022-12-20 | 西北工业大学宁波研究院 | Preparation method and application of molybdenum disulfide film and flexible health sensor |
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