CN108642541A - The preparation method of titanium doped molybdenum disulfide film with ultraviolet absorption peak - Google Patents
The preparation method of titanium doped molybdenum disulfide film with ultraviolet absorption peak Download PDFInfo
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- CN108642541A CN108642541A CN201810507715.4A CN201810507715A CN108642541A CN 108642541 A CN108642541 A CN 108642541A CN 201810507715 A CN201810507715 A CN 201810507715A CN 108642541 A CN108642541 A CN 108642541A
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- molybdenum disulfide
- absorption peak
- ultraviolet absorption
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- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
- C25D9/08—Electrolytic coating other than with metals with inorganic materials by cathodic processes
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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Abstract
The present invention is to provide a kind of preparation methods of the titanium doped molybdenum disulfide film with ultraviolet absorption peak.Using platinum electrode as anode, monocrystalline silicon piece as cathode, pole span be 2.5~3.5cm, working method as constant current state, cathode surface current density is 0.1~2.5mA/cm2, electro-deposition is carried out in electrodeposit liquid, and MoS is controlled by sedimentation time2Within the scope of 50~1000nm, the electrodeposit liquid is formulated film thickness by vulcanized sodium, sodium molybdate, titanyl sulfate.Method provided by the invention can be used in preparing the titanium doped molybdenum disulfide film with special ultraviolet absorption peak, and raw material sources provided by the invention are extensive, and stable components, disclosure satisfy that the demand of raw material in production, and cost is relatively low, application prospect is extensive.
Description
Technical field
The present invention relates to a kind of electrochemical deposition method, specifically a kind of system of titanium doped molybdenum disulfide film
Preparation Method.
Background technology
In recent years, two-dimensional layer nano material is potentially answered because it possesses in electricity, optics, lubrication and catalysis etc.
With property, so receiving the close attention of researcher.Transition metal stratiform binary compound is one of important materials,
Research wherein in terms of single layer transition metal binary compound is more.
Molybdenum disulfide is more typical transition metal dichalcogenide, possesses the atomic layer knot of the two-dimensional ultrathin of class graphene
Structure, when it is thinned to molybdenum disulfide film by body material, the band gap of system will rise to 1.80eV from 1.29eV, from indirect belt
Gap semiconductor variation is direct band-gap semicondictor, so making it have unique photoelectric characteristic.
The thermal stability and chemical stability of molybdenum disulfide film are preferable, and feature is that have big specific surface area, high table
Face activity and unique chemically and physically characteristic.Molybdenum disulfide due to its structure and characteristic, photoelectric device, kollag,
Field-effect transistor, electrochemical lithium storage and electrochemical hydrogen storage etc. are owned by important researching value and application value.
Due to the quantum size effect of molybdenum disulfide, the electronic structure of molybdenum disulfide is limited, leads to its potential photoelectricity
Performance is difficult to realize.In recent years, scientific research personnel had found to be doped semi-conducting material to change and regulate and control its electronic structure
And correlated performance, this becomes a new hot spot in investigation of materials field, and is potentially researched and developed for molybdenum disulfide film
Provide new method and approach.
Invention content
The purpose of the present invention is to provide a kind of simple for process, it is suitable for photoelectric device, field-effect transistor has purple
The preparation method of the titanium doped molybdenum disulfide film of outer absorption peak.
The object of the present invention is achieved like this：
Using platinum electrode as anode, monocrystalline silicon piece as cathode, pole span be 2.5~3.5cm, working method is constant current shape
State, cathode surface current density are 0.1~2.5mA/cm2, electro-deposition is carried out in electrodeposit liquid, is controlled by sedimentation time
MoS2Within the scope of 50~1000nm, the electrodeposit liquid is formulated film thickness by vulcanized sodium, sodium molybdate, titanyl sulfate.
The present invention can also include：
1, vulcanized sodium in the electrodeposit liquid, sodium molybdate, titanyl sulfate concentration be respectively 20g/L, 10g/L and 0.15~
The configuration method of 0.3g/L, electrodeposit liquid is：Sodium molybdate is mixed and added into distilled water with vulcanized sodium to stir evenly, by sulfuric acid oxygen
It is added in the mixed solution of sodium molybdate and vulcanized sodium after titanium concentrated sulfuric acid stirring and dissolving, acid solution is added dropwise in whipping process makes pH exist
In 9~12 ranges.
2, first monocrystalline silicon piece is pre-processed, the pretreatment is：Use volume ratio for H2O：H2O2：HCl=8：2：1
Cleaning agent cleaning silicon chip substrate, and 80 DEG C of heating water bath 20min, it is HF to be put into volume ratio after distilled water flushing：H2O=1：1
Solution in impregnate 1min, take out, distilled water flushing and being put into distilled water impregnates.
The present invention provides a kind of preparation methods of the titanium doped molybdenum disulfide film with special ultraviolet absorption peak, special
Point is at low cost, surface topography is good, is suitable for photoelectric device, field-effect transistor etc., and simple for process.
The titanium doped MoS of the present invention2Film is used as photoelectric device.The characterization result of product is shown in that Fig. 1-3, Fig. 1 a- Fig. 1 b are
Scanning electron microscope (SEM) figure of 1 sample of embodiment, by Fig. 1 a- Fig. 1 b it is found that titanium doped molybdenum disulfide film surface is uniform, thickness
For 300-400nm.Fig. 2 a- Fig. 2 b are embodiment 1 sample X-ray electron spectrum (XPS) figures, and the sample characteristic peak of S atom passes through
Peak-fit processing is made of two Photoelectron peaks, in conjunction with that can be respectively 161.75eV, 163.32eV, S2p be both corresponded to, with standard card
Piece is found mainly after corresponding to by MoS2In sulphion and titanium disulfide in sulphion composition；The Photoelectron peak of Ti, by scheming
Known to the Photoelectron peak be made of two peaks, in conjunction with can respectively 459.07eV and 462.05eV.It compares and finds with standard card,
In conjunction with can be made of trisulfides two titanium for the peak of 459.07eV；And positioned at the peak of 462.05eV mainly by titanium disulfide group
At.Fig. 3 is uv-vis spectra (UV-Vis) figure of 1 sample of embodiment, as seen from Figure 3, titanium doped MoS2Film has
There is ultraviolet absorption peak.
The simple synthetic method, cost is relatively low, reproducible；Any surfactant and organic solvent are not used,
Environmentally friendly, the film surface appearance obtained is preferable；Different density journey can be prepared by controlling electric current and time
The titanium doped molybdenum disulfide film of degree and different-thickness.The titanium doped molybdenum disulfide film will be imitated in photoelectric device, electro-catalysis, field
The fields such as transistor are answered to have broad application prospects.
Description of the drawings
Fig. 1 a- Fig. 1 b are surface sweeping Electronic Speculum (SEM) figure of 1 sample of embodiment, and wherein Fig. 1 a are section；Fig. 1 b are surface.
Fig. 2 a- Fig. 2 b are embodiment 1 sample X-ray electron spectrum (XPS) figure.
Fig. 3 is uv-vis spectra (UV-Vis) figure of 1 sample of embodiment.
Specific implementation mode
The present invention is further illustrated with reference to embodiments, but the present invention is not limited only to these embodiments, not
Be detached from present inventive concept under the premise of, made by it is any improvement all fall in protection scope of the present invention.
Embodiment 1：
A：Single-sided polishing silicon chip is taken, uses proportioning for H2O：H2O2：(volume ratio=8 HCl：2：1) common 2 in industry
Number cleaning agent cleaning silicon chip substrate, and 80 DEG C of heating water bath 20min, a large amount of distilled water flushings are put into rapidly HF：H2O=1：1
1min is impregnated in solution, is taken out, and distilled water flushing and being put into distilled water impregnates.B：5g sodium molybdates are mixed with 10g vulcanized sodium
And the distilled water of 500ml is added, it is stirred on magnetic stirring apparatus.The 0.1g titanyl sulfates weighed up are stirred in suitable concentrated sulfuric acid
It is added to after dissolving in the mixed solution of sodium molybdate and vulcanized sodium, oxalic acid is added dropwise in whipping process makes PH in 9~12 ranges, i.e.,
Solution becomes dark red from water white transparency.C：Electric deposition device is built, electro-deposition power supply uses DJS-232 type potentiostats, platinum
Electrode is as anode, and monocrystalline silicon piece is as cathode, and for cathode and anode at a distance of (pole span) about 3cm, working method is 0.02A constant current states,
Cathode surface current density is 0.1~2.5mA/cm2.Make MoS by controlling sedimentation time for 15min2Film thickness 50~
Within the scope of 500nm.Sample topography is observed by SEM electron microscopes (Fig. 1), thickness is 300~400nm.
Embodiment 2：
A：Single-sided polishing silicon chip is taken, uses proportioning for H2O：H2O2：(volume ratio=8 HCl：2：1) common 2 in industry
Number cleaning agent cleaning silicon chip substrate, and 80 DEG C of heating water bath 20min, a large amount of distilled water flushings are put into rapidly HF：H2O=1：1
1min is impregnated in solution, is taken out, and distilled water flushing and being put into distilled water impregnates.B：5g sodium molybdates are mixed with 10g vulcanized sodium
And the distilled water of 500ml is added, it is stirred on magnetic stirring apparatus.The 0.1g titanyl sulfates weighed up are stirred in suitable concentrated sulfuric acid
It is added to after dissolving in the mixed solution of sodium molybdate and vulcanized sodium, oxalic acid is added dropwise in whipping process makes PH in 9~12 ranges, i.e.,
Solution becomes dark red from water white transparency.C：Electric deposition device is built, electro-deposition power supply uses DJS-232 type potentiostats, platinum
Electrode is as anode, and monocrystalline silicon piece is as cathode, and for cathode and anode at a distance of (pole span) about 3cm, working method is 0.01A constant current states,
Cathode surface current density is 0.1~2.5mA/cm2.Make MoS by controlling sedimentation time for 15min2Film thickness 50~
Within the scope of 500nm.Sample topography is observed by SEM electron microscopes, thickness is 90~200nm.
From above-described embodiment as can be seen that method provided by the invention can be used in preparing with special ultraviolet absorption peak
Titanium doped molybdenum disulfide film, and raw material sources provided by the invention are extensive, and stable components, it disclosure satisfy that raw material in production
Demand, and cost is relatively low, and application prospect is extensive.
Claims (5)
1. a kind of preparation method of the titanium doped molybdenum disulfide film with ultraviolet absorption peak, it is characterized in that：Using platinum electrode as
Anode, monocrystalline silicon piece as cathode, pole span are 2.5~3.5cm, working method is constant current state, cathode surface current density is
0.1~2.5mA/cm2, electro-deposition is carried out in electrodeposit liquid, and MoS is controlled by sedimentation time2Film thickness is in 50~1000nm
In range, the electrodeposit liquid is formulated by vulcanized sodium, sodium molybdate, titanyl sulfate.
2. the preparation method of the titanium doped molybdenum disulfide film according to claim 1 with ultraviolet absorption peak, feature
It is：Vulcanized sodium in the electrodeposit liquid, sodium molybdate, titanyl sulfate concentration be respectively 20g/L, 10g/L and 0.15~0.3g/L,
The configuration method of electrodeposit liquid is：Sodium molybdate is mixed and added into distilled water with vulcanized sodium to stir evenly, by titanyl sulfate with dense
It is added to after sulfuric acid stirring and dissolving in the mixed solution of sodium molybdate and vulcanized sodium, acid solution is added dropwise in whipping process makes pH 9~12
In range.
3. the preparation method of the titanium doped molybdenum disulfide film according to claim 1 or 2 with ultraviolet absorption peak, special
Sign is：First monocrystalline silicon piece is pre-processed, the pretreatment is：Use volume ratio for H2O：H2O2：HCl=8：2：1 cleaning
Agent cleaning silicon chip substrate, and 80 DEG C of heating water bath 20min, it is HF that volume ratio is put into after distilled water flushing：H2O=1：1 solution
Middle immersion 1min, takes out, and distilled water flushing and being put into distilled water impregnates.
4. the preparation method of the titanium doped molybdenum disulfide film according to claim 1 or 2 with ultraviolet absorption peak, special
Sign is：Constant current 0.02A, sedimentation time 15min.
5. the preparation method of the titanium doped molybdenum disulfide film according to claim 3 with ultraviolet absorption peak, feature
It is：Constant current 0.02A, sedimentation time 15min.
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| CN201810318571 | 2018-04-11 | ||
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109989064A (en) * | 2019-04-11 | 2019-07-09 | 新余学院 | A kind of compound MoS of high-silicon aluminum alloy cylinder sleeve surface etch chemistry2The preparation method of coating |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104495937A (en) * | 2014-12-31 | 2015-04-08 | 中国地质大学（武汉） | Preparation method of carbon-doped molybdenum disulfide nanometer material |
| CN105624756A (en) * | 2015-12-29 | 2016-06-01 | 中国石油大学(华东) | High-activity molybdenum sulfide film electrocatalyst and preparation method thereof |
| CN106086990A (en) * | 2016-08-04 | 2016-11-09 | 北京工业大学 | A kind of method of the immobilized molybdenum bisuphide of porous titania thin films |
| CN106179415A (en) * | 2016-04-20 | 2016-12-07 | 中国计量大学 | A kind of preparation method of nano titanium oxide/molybdenum bisuphide composite material film |
| CN106400045A (en) * | 2016-08-30 | 2017-02-15 | 苏州大学 | Titanium-phosphorus-codoped ferric oxide photoelectrode and preparation method thereof |
-
2018
- 2018-05-24 CN CN201810507715.4A patent/CN108642541A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104495937A (en) * | 2014-12-31 | 2015-04-08 | 中国地质大学（武汉） | Preparation method of carbon-doped molybdenum disulfide nanometer material |
| CN105624756A (en) * | 2015-12-29 | 2016-06-01 | 中国石油大学(华东) | High-activity molybdenum sulfide film electrocatalyst and preparation method thereof |
| CN106179415A (en) * | 2016-04-20 | 2016-12-07 | 中国计量大学 | A kind of preparation method of nano titanium oxide/molybdenum bisuphide composite material film |
| CN106086990A (en) * | 2016-08-04 | 2016-11-09 | 北京工业大学 | A kind of method of the immobilized molybdenum bisuphide of porous titania thin films |
| CN106400045A (en) * | 2016-08-30 | 2017-02-15 | 苏州大学 | Titanium-phosphorus-codoped ferric oxide photoelectrode and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109989064A (en) * | 2019-04-11 | 2019-07-09 | 新余学院 | A kind of compound MoS of high-silicon aluminum alloy cylinder sleeve surface etch chemistry2The preparation method of coating |
| CN109989064B (en) * | 2019-04-11 | 2021-06-11 | 新余学院 | Compound MoS of high silicon aluminum alloy cylinder liner surface chemical etching2Method for producing a coating |
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Application publication date: 20181012 |