CN105624643A - Preparation method for large-area selenium doped molybdenum disulfide thin film material - Google Patents
Preparation method for large-area selenium doped molybdenum disulfide thin film material Download PDFInfo
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- CN105624643A CN105624643A CN201610011797.4A CN201610011797A CN105624643A CN 105624643 A CN105624643 A CN 105624643A CN 201610011797 A CN201610011797 A CN 201610011797A CN 105624643 A CN105624643 A CN 105624643A
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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
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
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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
- C23C16/44—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 method of coating
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Abstract
The invention relates to a preparation method for a large-area selenium doped molybdenum disulfide thin film material. By adopting a chemical vapor deposition method and a double-temperature zone tube furnace, a single-layer selenium doped molybdenum disulfide thin film material of which the area is 1000 to 1200 square microns is obtained by taking Si/SiO2 as a substrate, MoO3 as a molybdenum source, powdered sulfur as a sulfur source and a selenium granule as a selenium source. The chemical vapor deposition method comprises the steps of putting the substrate on a porcelain boat holding the molybdenum source, and putting the porcelain boat in a lower temperature zone of the double-temperature zone tube furnace; putting the porcelain boat holding the sulfur source and the selenium source in an upper temperature zone of the double-temperature zone tube furnace, wherein the mass ratio (S:Se) of the sulfur source to the selenium source is (0.25 to 4) :1, and packaging the double-temperature zone tube furnace. The preparation method disclosed by the invention is simple and easy to operate, short in time and high in repeatability, and has a low requirement on instruments and equipment; the prepared selenium doped molybdenum disulfide thin film material is increased in area by one order of magnitude, has an obvious advantage, and is expected to be applied to fields of optical switches, phototransistors, optical detectors and the like.
Description
Technical field
The preparation method that the present invention relates to a kind of large area selenium doping molybdenum disulfide film material, belongs to semiconductor film material preparation field.
Background technology
Along with the rise of the two-dimensional layer nano materials research upsurge such as Graphene in recent years, novel two-dimensional layer compounds Graphene transient metal chalcogenide compound (TDMCs) of a class causes the extensive concern of the various fields research worker such as physics, chemistry. The general formula of molecular structure of this class material is expressed as MX2, wherein M is transition metal, such as IV race's element (Ti etc.), group �� element (V etc.) and VI race's element (Mo, W etc.); X is chalcogenide, such as S, Se and Te etc.; Typical compound has molybdenum bisuphide (MoS2), two selenizing molybdenum (MoSe2) etc. The two dimensional crystal material with " sandwich " layer structure that this compounds is all made up of the single or multiple lift of hexagonal crystal system, wherein layer of metal molecular composition hexaplanar, be sandwiched in two-layer keep apart in the middle of chalcogen molecule, combine the crystal forming bulk between adjacent atomic layer by faint model ylid bloom action power; Owing to way of stacking is different with interatomic coordination mode between layers, the crystal of transient metal chalcogenide compound can be divided into hexaplanar and orthorhombic system by its symmetry.
Different from the Graphene with two-dimensional layered structure, class Graphene transient metal chalcogenide compound has special band structure, and compared to zero band gap of Graphene, this compounds generally has the natural band-gap energy of 1-1.9eV. The band gap of monolayer molybdenum bisuphide, due to quantum confined effect, reaches 1.9eV; And the band gap of monolayer two selenizing molybdenum reaches 1.5eV. Due to its big band gap and of a relatively high carrier mobility, it has in field of photovoltaic materials and to be widely applied.
In order to improve the class Graphene transient metal chalcogenide compound performance at photoelectric device, regulating the band gap of this material be an important solution is also a bottleneck, because nature seldom exists the nature band gap natural crystal compound at 1-1.9eV, and can be obtained by simple intercalation method of peeling off. A lot of modes can realize the adjustment to two-dimensional layer material band gap, such as chemical doping, ion implanting and introduce functional group etc. at material surface. Recently, Theoretical Calculation and experimentation all demonstrate the preparation that can realize the adjustable two-dimensional layer semi-conducting material of band gap. Chemical gaseous phase depositing process and physical gas-phase deposite method effectively can must prepare the adjustable monolayer selenium doping molybdenum bisuphide of band gap by the concentration of change element sulphur.
Only monolayer or few layer just have the performance of the excellent photoelectricity aspect of said structure, and therefore primary and important task is to prepare monolayer or few this kind of material of layer. The area of the selenium doping molybdenum disulfide film reported in recent document, substantially all in micron level, is 300 square microns as University of Science and Technology of China Xiang Bin teaches the area of the standby selenium doping molybdenum disulfide film of project team system. But large-area selenium doping molybdenum disulfide film does not obtain again, it is therefore desirable to study greater area of selenium doping molybdenum disulfide film, have that high-quality, uniformity be good, the selenium doping molybdenum disulfide film material of the monolayer of different levels of doping simultaneously; Realize a large amount of preparation, it is possible to reach the requirement of industrial mass production.
Adopt chemical vapour deposition technique and double; two temperature-area tubular furnace herein, with Si/SiO2For substrate, employing MoO3As molybdenum source, sulfur powder is as sulfur source, and selenium grain is as selenium source, it is possible to obtain having high-quality, uniformity selenium good, monolayer adulterates molybdenum disulfide film material. Film size prepared by this method can reach 1000-1200 square micron, and so large-area thin film first time at home is synthesized, and really belongs to exception. The method is simple to operate, can complete in the short time, reproducible, it is possible to achieve to prepare in a large number, it is possible to reach the requirement of industrial mass production.
Summary of the invention
The preparation method that it is an object of the invention to provide a kind of large area selenium doping molybdenum disulfide film material, selenium doping molybdenum disulfide film material is prepared by chemical vapour deposition technique, area reaches 1000-1200 square micron, there is the advantages such as high-quality, monolayer, good, the good crystallinity of uniformity simultaneously, the method is simple to operate, less energy consumption, has reached the requirement of large-scale production.
The present invention is realized by the following technical scheme, by selecting molybdenum source, sulfur source and selenium source, in the double; two temperature-area tubular furnace of chemical vapour deposition (CVD), high-temperature low-pressure condition issues biochemical reaction, is then deposited into substrate surface, ultimately generates selenium doping molybdenum disulfide film material.
The preparation method of a kind of large area selenium doping molybdenum disulfide film material, adopts chemical vapour deposition technique and double; two temperature-area tubular furnace, with Si/SiO2For substrate, employing MoO3As molybdenum source, sulfur powder is as sulfur source, and selenium grain, as selenium source, obtains the monolayer selenium doping molybdenum disulfide film material that area is 1000-1200 square micron.
Described substrate is SiO2/ Si, mode ultrasonic in acetone and aqueous isopropanol respectively cleans the organic substance impurity removing substrate surface, rear by deionized water rinse substrate so as to clean, and dry up by nitrogen gun.
Chemical vapour deposition technique is: by SiO2/ Si substrate is placed on the porcelain boat filling molybdenum source, and this porcelain boat is placed in the lower warm area of double; two temperature-area tubular furnace; The porcelain boat filling sulfur source and selenium source is placed in warm area on double; two temperature-area tubular furnace, and wherein the quality S:Se of sulfur source and selenium source is 0.25-4:1, and is encapsulated by double; two temperature-area tubular furnaces.
Noble gas argon is passed into double; two temperature-area tubular furnace, since air in the double; two temperature-area tubular furnace of emptying, it is prevented that the generation of the air impact selenium doping molybdenum disulfide film in double; two temperature-area tubular furnaces and deposition when pyroreaction.
Arrange the rate of heat addition of upper warm area in double; two temperature-area tubular furnace be 3.6-5.5 DEG C/min, 65-85min after rise to reaction temperature 260-306 DEG C, and maintain this reaction temperature 10-20min.
Arranging the rate of heat addition of lower warm area in double; two temperature-area tubular furnace is 10-15 DEG C/min, rises to reaction temperature 650-850 DEG C, and maintain this reaction temperature 10-20min after 65-85min.
When double; two temperature-area tubular furnaces reach reaction temperature, the flow regulating argon is 40sccm, opens hydrogen and to arrange its flow be 5-10sccm; Reaction is down to room temperature after terminating naturally.
Preparation method of the present invention is simple and easy to operate, the time is short, reproducible, to instrument and equipment require low. The high-quality that obtained by chemical vapour deposition technique, the monolayer selenium doping molybdenum disulfide film material that uniformity is good, area can reach 1000-1200 square micron, compared to other method preparing selenium doping molybdenum bisuphide, the area of thin-film material increases an order of magnitude, there is obvious advantage, prepare obtained thin-film material and be expected to be applied to the fields such as photoswitch, phototransistor, photo-detector.
Accompanying drawing illustrates:
Fig. 1 is the experiment easy device figure of the selenium doping molybdenum disulfide film material of embodiment 2 preparation. Sulfur source and selenium source are placed in warm area, and reaction temperature is set as 300 DEG C; Molybdenum source molybdenum trioxide is placed in lower warm area, and reaction temperature is set as 650 DEG C; Carrier gas argon/hydrogen (4:1) is from the entrance thermal treatment zone, left side of double; two temperature-area tubular furnaces.
Fig. 2 is the light microscopic figure of the selenium doping molybdenum disulfide film material of embodiment 2 preparation. The upper left corner is substrate material SiO2/ Si sheet, other regions are selenium doping molybdenum disulfide film material, and good film-forming property, integrity degree is high, and the area of its thin-film material can reach 1100 square microns.
Fig. 3 is the TEM figure of the selenium doping molybdenum disulfide film material of embodiment 2 preparation. Photo shows that the selenium prepared doping molybdenum disulfide film material is monolayer.
The XPS figure of Fig. 4 (A), (B) and (C) molybdenum disulfide film material prepared by embodiment 1,2 and 3, has done peak-fit processing to S element respectively. By picture it can be seen that prepared different selenium doping molybdenum disulfide film material, S:Se corresponding in thin film prepared by embodiment 1,2 and 3 respectively 4.04,0.92 and 0.59.
Detailed description of the invention
Concrete scheme step is as follows:
(1) substrate used in this experiment is SiO2/ Si sheet, cleans the impurity such as organic substance removing substrate surface by mode ultrasonic in acetone and aqueous isopropanol respectively, rear by deionized water rinse substrate so as to clean, and it is standby to dry up substrate by nitrogen gun. Being placed on the porcelain boat filling molybdenum source by substrate after processing, and this porcelain boat is placed in the lower warm area of double; two temperature-area tubular furnace, it is for carrier gas, is positioned at the outlet side of tube furnace; The porcelain boat filling sulfur source and selenium source is placed in the upper warm area of double; two temperature-area tubular furnace, it is for carrier gas, being positioned at the inlet end of tube furnace, wherein original quality ratio (S:Se) of sulfur source and selenium source is between 0.25-4, and is encapsulated by double; two temperature-area tubular furnaces.
(2) when reaction starts, by the noble gas argon access tube formula stove of 500-1000sccm, since air in emptying tube furnace, it is prevented that the generation of the doping of the air impact selenium in tube furnace molybdenum disulfide film and deposition in pyroreaction. Arrange the rate of heat addition of warm area on double; two temperature-area tubular furnace be 3.6-5.5 DEG C/min, 65-85min after rise to reaction temperature 260-306 DEG C; Arrange the rate of heat addition of warm area under double; two temperature-area tubular furnace be 10-15 DEG C/min, 65-85min after rise to reaction temperature 650-850 DEG C; When the temperature of double; two temperature-area tubular furnaces reaches reaction temperature, the flow regulating argon is 40sccm, opens hydrogen and to arrange its flow be 5-10sccm. The constant temperature time of warm area up and down of double; two temperature-area tubular furnaces is set as 10-20min. Reaction is down to room temperature after terminating naturally.
(3) after temperature is down to room temperature, substrate is taken out from double; two temperature-area tubular furnaces, just obtain the selenium doping molybdenum disulfide film material of overlarge area.
3 embodiments of the present invention are given below, are further illustrating the present invention, rather than restriction the scope of the present invention.
Embodiment 1
Weigh 5mg molybdenum trioxide powder, 400mg sulfur powder and 100mg selenium powder (mass ratio of sulfur source and selenium source is 4) and be respectively placed in 30 �� 60mm ceramic boat, the substrate (SiO that will handle well2/ Si) it is respectively placed in acetone, each ultrasonic 20min of isopropanol, to remove the impurity such as the organic substance of substrate surface. Substrate after processing is placed on the porcelain boat filling molybdenum source, and this porcelain boat is placed in the lower warm area of double; two temperature-area tubular furnace (for carrier gas, it is positioned at the outlet side of tube furnace), the porcelain boat filling sulfur source and selenium source is placed in the upper warm area of double; two temperature-area tubular furnace (for carrier gas, it is positioned at the inlet end of tube furnace), finally encapsulate tube furnace. By the noble gas argon access tube formula stove of 1000sccm, since air in emptying tube furnace, it is prevented that the generation of the air impact selenium doping molybdenum disulfide film in double; two temperature-area tubular furnaces and deposition in pyroreaction. Arrange the rate of heat addition of warm area on double; two temperature-area tubular furnace be 4 DEG C/min, 65min after rise to reaction temperature 260 DEG C; Arrange the rate of heat addition of warm area under double; two temperature-area tubular furnace be 10 DEG C/min, 65min after rise to reaction temperature 650 DEG C; When the temperature of double; two temperature-area tubular furnaces reaches reaction temperature, the flow regulating argon is 40sccm, opens hydrogen and to arrange its flow be 5sccm. The constant temperature time of warm area up and down of double; two temperature-area tubular furnaces is set as 10min. Reaction is down to room temperature after terminating naturally. Reaction is down to room temperature after terminating naturally. After temperature is down to room temperature, substrate is taken out from tube furnace, just obtain the selenium doping molybdenum disulfide film material of the good overlarge area of uniformity. Can drawing from Fig. 4 (A), the S:Se in this thin-film material is 4.04. The area of the molybdenum disulfide film material of this selenium doping simultaneously can reach 1000 square microns.
Embodiment 2
Weigh 5mg molybdenum trioxide powder, 250mg sulfur powder and 250mg selenium powder (mass ratio of sulfur source and selenium source is 1) and be respectively placed in the ceramic boat of 30 �� 60mm, the substrate (SiO that will handle well2/ Si) it is respectively placed in acetone, each ultrasonic 20min of isopropanol, to remove the impurity such as the organic substance of substrate surface. Substrate after processing is placed on the porcelain boat filling molybdenum source, and this porcelain boat is placed in the lower warm area of double; two temperature-area tubular furnace (for carrier gas, it is positioned at the outlet side of tube furnace), the porcelain boat filling sulfur source and selenium source is placed in the upper warm area of double; two temperature-area tubular furnace (for carrier gas, it is positioned at the inlet end of tube furnace), finally encapsulate tube furnace. By the noble gas argon access tube formula stove of 750sccm, since air in emptying tube furnace, it is prevented that the generation of the doping of the air impact selenium in tube furnace molybdenum disulfide film and deposition in pyroreaction. Arrange the rate of heat addition of warm area on double; two temperature-area tubular furnace be 5.5 DEG C/min, 50min after rise to reaction temperature 275 DEG C; Arrange the rate of heat addition of warm area under double; two temperature-area tubular furnace be 15 DEG C/min, 50min after rise to reaction temperature 750 DEG C; When the temperature of double; two temperature-area tubular furnaces reaches reaction temperature, the flow regulating argon is 40sccm, opens hydrogen and to arrange its flow be 7sccm. The constant temperature time of warm area up and down of double; two temperature-area tubular furnaces is set as 15min. Reaction is down to room temperature after terminating naturally. As can be drawn from Figure 2, the area of this selenium doping molybdenum disulfide film material can reach 1100 square microns. As can be drawn from Figure 3, this thin-film material is single thin film; Can should drawing from Fig. 4 (B), in this thin-film material, S:Se is 0.92.
Embodiment 3
Weigh 5mg molybdenum trioxide powder, 100mg sulfur powder and 400mg selenium powder (mass ratio of sulfur source and selenium source is 0.25) and be respectively placed in the ceramic boat of 30 �� 60mm, the substrate (SiO that will handle well2/ Si) it is respectively placed in acetone, each ultrasonic 20min of isopropanol, to remove impurity and the organic substance of substrate surface. Substrate after processing is placed on the porcelain boat filling molybdenum source, and this porcelain boat is placed in the lower warm area of double; two temperature-area tubular furnace (for carrier gas, it is positioned at the outlet side of tube furnace), the porcelain boat filling sulfur source and selenium source is placed in the upper warm area of double; two temperature-area tubular furnace (for carrier gas, it is positioned at the inlet end of tube furnace), finally encapsulate tube furnace. By the noble gas argon access tube formula stove of 500sccm, since air in emptying tube furnace, it is prevented that the generation of the doping of the air impact selenium in tube furnace molybdenum disulfide film and deposition in pyroreaction. Arrange the rate of heat addition of warm area on double; two temperature-area tubular furnace be 3.6 DEG C/min, 85min after rise to reaction temperature 306 DEG C; Arrange the rate of heat addition of warm area under double; two temperature-area tubular furnace be 10 DEG C/min, 85min after rise to reaction temperature 850 DEG C; When the temperature of double; two temperature-area tubular furnaces reaches reaction temperature, the flow regulating argon is 40sccm, opens hydrogen and to arrange its flow be 10sccm. The constant temperature time of warm area up and down of double; two temperature-area tubular furnaces is set as 20min. Reaction is down to room temperature after terminating naturally. Can drawing from Fig. 4 (C), in this thin-film material, S:Se is 0.59. The area of the molybdenum disulfide film material of this selenium doping simultaneously can reach 1200 square microns.
Claims (7)
1. a preparation method for large area selenium doping molybdenum disulfide film material, is characterized in that adopting chemical vapour deposition technique and double; two temperature-area tubular furnace, with Si/SiO2For substrate, employing MoO3As molybdenum source, sulfur powder is as sulfur source, and selenium grain, as selenium source, obtains the monolayer selenium doping molybdenum disulfide film material that area is 1000-1200 square micron.
2. the method for claim 1, is characterized in that substrate is SiO2/ Si, mode ultrasonic in acetone and aqueous isopropanol respectively cleans the organic substance impurity removing substrate surface, rear by deionized water rinse substrate so as to clean, and dry up by nitrogen gun.
3. the method for claim 1, is characterized in that chemical vapour deposition technique is: by SiO2/ Si substrate is placed on the porcelain boat filling molybdenum source, and this porcelain boat is placed in the lower warm area of double; two temperature-area tubular furnace; The porcelain boat filling sulfur source and selenium source is placed in warm area on double; two temperature-area tubular furnace, and wherein the quality S:Se of sulfur source and selenium source is 0.25-4:1, and is encapsulated by double; two temperature-area tubular furnaces.
4. method as claimed in claim 3, it is characterized in that noble gas argon passes into double; two temperature-area tubular furnace, since air in the double; two temperature-area tubular furnace of emptying, it is prevented that the generation of the air impact selenium doping molybdenum disulfide film in double; two temperature-area tubular furnaces and deposition when pyroreaction.
5. method as claimed in claim 3, it is characterized in that arranging the rate of heat addition of upper warm area in double; two temperature-area tubular furnace be 3.6-5.5 DEG C/min, 65-85min after rise to reaction temperature 260-306 DEG C, and maintain this reaction temperature 10-20min.
6. method as claimed in claim 3, it is characterized in that arranging the rate of heat addition of lower warm area in double; two temperature-area tubular furnace is 10-15 DEG C/min, rises to reaction temperature 650-850 DEG C, and maintain this reaction temperature 10-20min after 65-85min.
7. method as claimed in claim 3, is characterized in that when double; two temperature-area tubular furnaces reach reaction temperature, and the flow regulating argon is 40sccm, opens hydrogen and to arrange its flow be 5-10sccm; Reaction is down to room temperature after terminating naturally.
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