CN114318297B - Method for preparing tantalum disulfide by normal pressure chemical vapor deposition - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000005229 chemical vapour deposition Methods 0.000 title claims abstract description 11
- JAAVTMIIEARTKI-UHFFFAOYSA-N [S--].[S--].[Ta+4] Chemical compound [S--].[S--].[Ta+4] JAAVTMIIEARTKI-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 27
- 239000000758 substrate Substances 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 238000004140 cleaning Methods 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000012159 carrier gas Substances 0.000 claims abstract description 9
- 239000010453 quartz Substances 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000010445 mica Substances 0.000 claims abstract description 6
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 6
- 238000002309 gasification Methods 0.000 claims abstract description 3
- 238000005303 weighing Methods 0.000 claims abstract description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 22
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims 1
- 239000010410 layer Substances 0.000 abstract description 46
- 239000013078 crystal Substances 0.000 abstract description 38
- 230000008569 process Effects 0.000 abstract description 5
- 239000002356 single layer Substances 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 3
- 239000002360 explosive Substances 0.000 abstract description 3
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract 1
- 229910052731 fluorine Inorganic materials 0.000 abstract 1
- 239000011737 fluorine Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 12
- 230000008859 change Effects 0.000 description 10
- 238000012512 characterization method Methods 0.000 description 6
- 238000001505 atmospheric-pressure chemical vapour deposition Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 241000252506 Characiformes Species 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000003517 fume Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910004537 TaCl5 Inorganic materials 0.000 description 2
- 229910004211 TaS2 Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- OEIMLTQPLAGXMX-UHFFFAOYSA-I tantalum(v) chloride Chemical compound Cl[Ta](Cl)(Cl)(Cl)Cl OEIMLTQPLAGXMX-UHFFFAOYSA-I 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical group [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal chalcogenides Chemical class 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Landscapes
- Chemical Vapour Deposition (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a method for preparing tantalum disulfide by normal pressure chemical vapor deposition, which comprises the steps of cleaning a fluorine crystal mica substrate, and respectively weighing S powder and TaCl 5 A powder; two heating belts are additionally arranged outside the tube furnace, and quartz boats respectively loaded with precursor raw materials are pushed into the corresponding heating belts for gasification; pushing the fluoromica substrate into the central position of the tubular hearth; under the condition of introducing the reducing carrier gas, the continuous supply of the S source is kept, the intermittent supply time of the Ta source is controlled, and the substrate is heated to the reaction temperature to perform the layer-by-layer growth. The heating belt is additionally arranged at the outer end of the reactor, so that the reaction is uniformly participated in, the defect of explosive growth in the growth process is effectively overcome, and the crystallization quality and performance are improved. Intermittent feeding layer-by-layer growth mode realizes the growth of controllable layers. The number of crystal layers prepared is precisely adjustable from a single layer to hundreds of layers.
Description
Technical Field
The invention belongs to the field of two-dimensional material preparation, and in particular relates to a method for preparing 1T-phase tantalum disulfide (1T-TaS) by using an Atmospheric Pressure Chemical Vapor Deposition (APCVD) 2 ) Is a method of (2).
Background
Since graphene was successfully exfoliated in 2004, the field of two-dimensional materials has attracted considerable attention. Among them, transition metal chalcogenides (TMDCs) are excellent candidates for research into photodetectors, capacitors, and field effect transistors, which have high electron mobility, specific surface area, and transmittance. Tantalum disulfide is used as a metallic TMDCs material, has typical Charge Density Wave (CDW) besides the excellent performance of the TMDCs material in the related aspect of a low-dimensional strongly-correlated electron system, shows the characteristics of a low-temperature insulating phase and a high-temperature metal phase, and can induce CDW phase change in a mode of light excitation, electric driving, thermal driving and the like. Based on the phase change mechanism, tantalum disulfide provides good material support for researching a resistance switch and a programmable logic device.
In the reported studies, 1T-T was prepared by Atmospheric Pressure Chemical Vapor Deposition (APCVD)aS 2 CVD method for preparing 1T-TaS 2 The two-dimensional atomic crystal is fed by placing a precursor in a reactor, and the precursor is added into the reactor at one time, so that explosive growth is easy to occur, and the defects of uncontrollable layer number of reactants and irregular crystal form are caused.
The key to study the Charge Density Wave (CDW) related to layer thickness is to prepare materials with different thicknesses, and 1T-TaS cannot be really realized at present 2 Large-scale preparation and controllable layer number. The invention aims to provide a method for controllably preparing 1T-TaS 2 The novel conception of (2) is that the high-quality 1T-TaS with controllable layer number is successfully synthesized by using a CVD method 2 Two-dimensional crystals.
Disclosure of Invention
The invention aims to provide a method for preparing tantalum disulfide by normal pressure chemical vapor deposition, thereby realizing 1T-TaS 2 The number of layers of the two-dimensional crystal is controllable.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for preparing tantalum disulfide by normal pressure chemical vapor deposition, comprising the following steps:
step one, cleaning a substrate: cleaning the fluoromica substrate to thoroughly remove impurities on the substrate;
step two, preparing precursor raw materials: respectively weighing S powder and TaCl 5 A powder; selecting low-melting-point chloride precursor TaCl 5 And oxide precursor Ta 2 O 5 Compared with the prior art, the method greatly reduces the reaction temperature and saves the cost.
Step three, adopting a single-temperature zone tube furnace to carry out chemical vapor deposition reaction: two heating belts are additionally arranged outside the tube furnace, and quartz boats respectively loaded with precursor raw materials are pushed into the corresponding heating belts for gasification; pushing the fluoromica substrate into the central position of the tubular hearth; under the condition of introducing the reducing carrier gas, the continuous supply of the S source is kept, the intermittent supply time of the Ta source is controlled, and the substrate is heated to the reaction temperature to perform the layer-by-layer growth. The heating belt is additionally arranged at the outer end of the reactor, so that the reaction is uniformly participated in, the defect of explosive growth in the growth process is effectively overcome, and the crystallization quality and performance are improved. Intermittent feeding layer-by-layer growth mode realizes the growth of controllable layers.
In the first step, concentrated sulfuric acid and hydrogen peroxide are mixed according to a volume ratio of 7:3 to prepare a cleaning solution for cleaning the fluorogenic mica substrate.
Further, in the second step, S powder and TaCl 5 The powder is prepared according to the proportion of 10:1-5:1 and is respectively placed in two quartz boats.
Further, in the third step, the S powder is positioned at a position 10-12 cm away from the edge of the hearth, and TaCl is positioned at the position 5 The powder is 7-9 cm away from the edge of the hearth.
Further, in the third step, the temperatures of the two heating belts are set to 150-200 ℃.
In the third step, after the fluoromica substrate is pushed into the central position of the hearth, the heating rate is 20 ℃/min, the heating temperature of the reactor is 800-850 ℃, and the heat preservation time is 10-15 min.
Further, the reducing gas used was 5%H 2 ~10% H 2 The flow rate of the carrier gas is 100-120 sccm.
The invention utilizes an improved APCVD growth method to provide a new idea of two-dimensional TMDCs layer number controllable growth, and mainly solves the problem of synthesizing 1T-TaS by the CVD method 2 The number of layers of the two-dimensional crystal is uncontrollable, and the number of layers of the prepared crystal is accurately adjustable from a single layer to hundreds of layers.
According to the method, the feeding mode is changed, two heating belts are respectively placed outside the reactor to gasify two precursors, and the precursors are ensured to participate in the reaction in uniform concentration through a method of feeding at intervals; meanwhile, the carrier gas and the interval time are controlled to realize intermittent supply of raw materials, and the raw materials are grown layer by layer; select low-melting point precursor TaCl 5 A sufficient reaction during CVD deposition is achieved. Finally, 1T-TaS with the thickness of 0.7-nm to 100 nm is prepared 2 Two-dimensional atomic crystals. The 1T-TaS prepared by the system is proved by various high-resolution test means 2 The high quality and crystallinity of two-dimensional atomic crystals successfully characterize the typical low temperature CDW phase change characteristics of the product.
Drawings
FIG. 1 is a 1T-TaS prepared in example 1 of the present invention 2 A schematic of a CVD reaction for two-dimensional atomic crystals;
FIG. 2 is a 1T-TaS prepared in example 1 of the present invention 2 Optical microscope photograph of two-dimensional atomic crystal;
FIG. 3 is a 1T-TaS prepared in example 1 of the present invention 2 AFM characterization of two-dimensional atomic crystals and corresponding height profiles;
FIG. 4 is a 1T-TaS prepared in example 1 of the present invention 2 A Raman characterization diagram of the two-dimensional atomic crystal at room temperature;
FIG. 5 is a 1T-TaS prepared in example 1 of the present invention 2 XRD characterization of the two-dimensional atomic crystal;
FIG. 6 is a 1T-TaS prepared in example 1 of the present invention 2 High Resolution Transmission Electron Microscope (HRTEM) photographs of two-dimensional atomic crystals;
FIG. 7 is a 1T-TaS prepared in example 1 of the present invention 2 Two-dimensional atomic crystal is a graph of resistivity change with temperature.
Detailed Description
The following examples are provided to further illustrate the claimed invention. However, examples are provided to illustrate embodiments of the invention without departing from the scope of the inventive subject matter, and the scope of the invention is not limited by the examples. Unless specifically indicated otherwise, materials and reagents used in the present invention are available from commercial products in the art.
Example 1
(1) Preparing a cleaning solution: the cleaning solution is a piranha solution (mixed by concentrated sulfuric acid and hydrogen peroxide in a ratio of 7:3). The measuring cylinder is used for measuring 70mL of concentrated sulfuric acid and 30mL of hydrogen peroxide respectively, and the hydrogen peroxide is slowly poured into the concentrated sulfuric acid.
Impurity removal: and putting the peeled fluorous crystal mica sheet into a solution, heating to 1 h, and controlling the temperature to 90 ℃. And (3) placing the substrate in a fume hood to volatilize the concentrated sulfuric acid to dilute sulfuric acid, and finally washing and drying the substrate with deionized water for later use.
(2) The mass of S powder is 500mg by an electronic balance, and TaCl is weighed by the electronic balance in a glove box 5 Powder mass50mg, formulated in a 10:1 ratio, were placed in two quartz boats, respectively, for use.
(3) S powder and TaCl weighed in the step (2) are mixed 5 The powder was placed at a distance of 12 cm and 9 cm from the hearth edge, respectively.
Both heating zones were set to 180 ℃. 10% H is selected 2 The flow rate of the carrier gas of the argon-hydrogen mixed gas is 120 sccm. Continuously feeding the S source, controlling the feeding time interval of the Ta source to be 3 min, reacting for 3 min at 820 ℃, and stopping the supply of TaCl5 after the 1T-TaS2 two-dimensional crystal grows the first layer; after 6 min, taCl5 supply was started to perform the second layer 1T-TaS 2 Is a growth of (a). And so on, layer 3, layer 4, layer … …, etc., are grown layer by layer. The heat preservation time is set to be 10 min, and the tube furnace is closed to stop growing after 10 min.
Through the experimental steps, 1T-TaS with different thicknesses is successfully prepared 2 Two-dimensional crystals.
1T-TaS prepared in this example 2 A schematic diagram of a two-dimensional atomic crystal is shown in fig. 1.
1T-TaS prepared in this example 2 The light-sensitive picture of the two-dimensional atomic crystal is shown in fig. 2, wherein the triangle shown in fig. 2-a is a single-layer crystal, the thin-layer crystal is shown in fig. 2-b, and the thick-layer crystal is shown in fig. 2-c. Different thicknesses can be resolved by the transparency observed under an optical microscope, with thinner samples having higher transparency.
1T-TaS prepared in this example 2 The AFM thickness characterization of two-dimensional atomic crystals is shown in fig. 3, where fig. 3a-c are single layer to three layer ultra thin layer AFM data, fig. 3d-f are thin layer sample AFM data less than 10 nm, and fig. 3g-i are thick layer samples, respectively. The thickness distribution of the samples varies from a single layer to hundreds of layers, which fully proves that the samples prepared by the method realize the controllable layer number.
1T-TaS prepared in this example 2 The Raman characterization of the two-dimensional atomic crystal at room temperature is shown in FIG. 4, and the wavenumber is shown in the graph<150 cm -1 The peak of (2) is related to tantalum atom movement, and is shown in 220 cm −1 ~320 cm −1 The phonon modes in the matrix are more related to sulfur atoms, 396 cm −1 The peak at this point is 1T-TaS 2 Is a characteristic peak of (2). The characteristic peak is located at the same position as the TaS of the 1T phase 2 The materials are anastomosed. The Raman characteristic peak is obvious, and the quality of the synthesized sample is good.
1T-TaS prepared in this example 2 The XRD characterization of the two-dimensional atomic crystal is shown in FIG. 5, in which solid line 5-a is hexagonal 1T-TaS 2 Standard XRD data (PDF 01-073-2200), solid line 5-b is TaS 2 XRD measurement results of two-dimensional atomic crystals. It can be seen that the measurement result and the standard data are very consistent, and the TaS synthesized by the experiment can be confirmed 2 Is 1T phase structure.
1T-TaS prepared in this example 2 A high-resolution transmission electron microscope (HRTEM) photograph of the two-dimensional atomic crystal is shown in FIG. 6, FIG. 6-a is a HRTEM overall morphology diagram at lower resolution, and the prepared sample is obviously observed to be in a regular hexagon structure, and the circles in the diagram are carbon films for transfer. TaS can be clearly seen in FIG. 6-b 2 Atomic arrangement of different positions of the sample. The boundary area of the sample and the substrate can be obviously seen, and the diffraction contrast of different areas is obviously different. Structural analysis is performed on the measured high resolution image in combination with fourier transform. FIG. 6-c clearly shows TaS 2 The atomic arrangement of the crystal. FIG. 6-d is a lattice image after Fourier transform (FFT), it can be seen that TaS 2 The two sets of lattice points of the material show that the material has good crystallinity. The interplanar spacing of the (001) planes was measured to be 0.597 nm. In addition, the (100) crystal face, the measured interplanar spacing was 0.291 nm, which matches the theoretical value, and it was confirmed that 1T-TaS was synthesized 2 。
1T-TaS prepared in this example 2 The change of the resistivity of the two-dimensional atomic crystal with temperature is shown in fig. 7, and the resistivity of both ends is measured by preparing electrodes on the surface of the sample through micro-processing technologies such as photoetching, electron beam evaporation electrodes and the like. Figures 7a-b show images of a device having a thickness of 20 a nm and resistance measurements as a function of temperature. As a result, it was observed that during the temperature rise, when heated to 150K, the resistance underwent a sudden step drop, indicating the presence of a CDW phase change, the material underwent a transition from the insulating state to the metallic state. In the cooling process, when the temperature is reduced to 250 to K, the resistor is connected with the resistorA sudden step rise is experienced, the material undergoing a transition from the metallic state to the insulating state; likewise, fig. 7c-d show images of a device having a thickness of 50 a nm a and resistance measurements as a function of temperature. During heating, when the temperature exceeds 150 deg.f K, the resistance drops sharply. During the cooling down, the resistance suddenly increases when the temperature drops to 230 f K f. 1T-TaS of different thickness 2 The resistance of the two-dimensional atomic crystal along with the temperature change effectively illustrates the CDW phase change process, and the larger the thickness is, the lower the phase change temperature in the cooling process is, and the CDW phase change mechanism with the thickness is a brand new thought for designing electronic devices.
Example 2
(1) Preparing a cleaning solution: the cleaning solution is a piranha solution (mixed by concentrated sulfuric acid and hydrogen peroxide in a ratio of 7:3). The measuring cylinder is used for measuring 70mL of concentrated sulfuric acid and 30mL of hydrogen peroxide respectively, and the hydrogen peroxide is slowly poured into the concentrated sulfuric acid.
Impurity removal: and putting the peeled fluorous crystal mica sheet into a solution, heating to 1 h, and controlling the temperature to 90 ℃. And (3) placing the substrate in a fume hood to volatilize the concentrated sulfuric acid to dilute sulfuric acid, and finally washing and drying the substrate with deionized water for later use.
(2) The mass of S powder is 500mg by an electronic balance, and TaCl is weighed by the electronic balance in a glove box 5 The powder is 50mg in mass and is prepared according to the proportion of 10:1 and is respectively placed in two quartz boats for standby.
(3) S powder and TaCl weighed in the step (2) are mixed 5 The powder is respectively arranged at a position 10cm and a position 7cm away from the edge of the hearth. The heating belt temperature was set to 150 ℃. 5% H is selected 2 The flow rate of the carrier gas of the argon-hydrogen mixed gas is 100 sccm. Continuously feeding the S source, controlling the feeding time interval of the Ta source to be 3 min, reacting for 3 min at 800 ℃, and stopping the supply of TaCl5 after the 1T-TaS2 two-dimensional crystal grows the first layer; after 6 min, taCl5 supply was started to perform the second layer 1T-TaS 2 Is a growth of (a). And by analogy, growing the 3 rd layer, the 4 th layer … … and the like layer by layer, setting the heat preservation time to be 10 min, and closing the tube furnace to stop growing after 10 min.
Example 3
(1) Preparing a cleaning solution: the cleaning solution is a piranha solution (mixed by concentrated sulfuric acid and hydrogen peroxide in a ratio of 7:3). The measuring cylinder is used for measuring 70mL of concentrated sulfuric acid and 30mL of hydrogen peroxide respectively, and the hydrogen peroxide is slowly poured into the concentrated sulfuric acid.
Impurity removal: and putting the peeled fluorous crystal mica sheet into a solution, heating to 1 h, and controlling the temperature to 90 ℃. And (3) placing the substrate in a fume hood to volatilize the concentrated sulfuric acid to dilute sulfuric acid, and finally washing and drying the substrate with deionized water for later use.
(2) The mass of S powder is 500mg by an electronic balance, and TaCl is weighed by the electronic balance in a glove box 5 The powder is 100mg in mass and prepared according to the proportion of 5:1, and the powder is respectively placed in two quartz boats for standby.
The difference from example 1 is that in step (3), the S powder and TaCl weighed in step (2) are mixed 5 The powder is respectively placed at the position 11cm and the position 8cm away from the edge of the hearth. Both heating zones were set to 200 ℃. 5% H is selected 2 The flow rate of the carrier gas of the argon-hydrogen mixed gas is 100 sccm. Continuously feeding S source, controlling the feeding time interval of Ta source to be 3 min, reacting for 3 min at 850 ℃, and reacting for 1T-TaS 2 After the two-dimensional crystal grows the first layer, taCl is stopped 5 Supplying; after 6 min, taCl supply was started 5 Performing a second layer 1T-TaS 2 Is a growth of (a). And by analogy, growing the 3 rd layer, the 4 th layer … … and the like layer by layer, setting the heat preservation time to be 15 min, and closing the tube furnace to stop growing after 15 min.
The scope of the present invention is not limited to the above embodiments, but various modifications and alterations of the present invention will become apparent to those skilled in the art, and any modifications, improvements and equivalents within the spirit and principle of the present invention are intended to be included in the scope of the present invention.
Claims (4)
1. A method for preparing tantalum disulfide by normal pressure chemical vapor deposition, which is characterized by comprising the following steps:
step one, cleaning a substrate: cleaning the fluoromica substrate to thoroughly remove impurities on the substrate;
step two, preparing precursor raw materials: respectively weighing S powder and TaCl 5 A powder; s powder and TaCl 5 Powder is prepared according to the proportion of 10:1-5:1 and is respectively placed in two quartz boats;
step three, adopting a single-temperature zone tube furnace to carry out chemical vapor deposition reaction: two heating belts are additionally arranged outside the tube furnace, quartz boats respectively carrying precursor raw materials are pushed into the corresponding heating belts for gasification, the S powder is positioned at a position 10cm to 12 cm away from the edge of the hearth, and TaCl is arranged at the position 5 The temperature of the powder is set to be 150-200 ℃ at the position 7-9 cm away from the edge of the hearth; pushing the fluoromica substrate into the central position of the tubular hearth; under the condition of introducing the reducing carrier gas, the continuous supply of the S source is kept, the intermittent supply time of the Ta source is controlled, and the substrate is heated to the reaction temperature to perform the layer-by-layer growth.
2. The method according to claim 1, characterized in that: in the first step, concentrated sulfuric acid and hydrogen peroxide are mixed according to the volume ratio of 7:3 to prepare the cleaning liquid for cleaning the fluorogenic mica substrate.
3. The method according to claim 2, characterized in that: and thirdly, after the fluoromica substrate is pushed into the central position of the hearth, the heating rate is 20 ℃/min, the heating temperature of the reactor is 800-850 ℃, and the heat preservation time is 10-15 min.
4. A method according to claim 3, characterized in that: the reducing gas is 5%H 2 ~10% H 2 The flow rate of the carrier gas is 100-120 sccm.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02260420A (en) * | 1989-03-30 | 1990-10-23 | Nippon Telegr & Teleph Corp <Ntt> | Selective cvd |
| CN108179399A (en) * | 2018-01-23 | 2018-06-19 | 北京大学 | A kind of method that chemical vapour deposition technique prepares tantalum disulfide |
| CN110438473A (en) * | 2019-09-06 | 2019-11-12 | 左然 | A kind of chemical vapor deposition unit and method |
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| WO2018195004A1 (en) * | 2017-04-17 | 2018-10-25 | Massachusetts Institute Of Technology | Chemical vapor transport growth of two-dimensional transition-metal dichalcogenides |
| US11060186B2 (en) * | 2018-04-13 | 2021-07-13 | Massachusetts Institute Of Technology | In situ generation of gaseous precursors for chemical vapor deposition of a chalcogenide |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02260420A (en) * | 1989-03-30 | 1990-10-23 | Nippon Telegr & Teleph Corp <Ntt> | Selective cvd |
| CN108179399A (en) * | 2018-01-23 | 2018-06-19 | 北京大学 | A kind of method that chemical vapour deposition technique prepares tantalum disulfide |
| CN110438473A (en) * | 2019-09-06 | 2019-11-12 | 左然 | A kind of chemical vapor deposition unit and method |
Non-Patent Citations (1)
| Title |
|---|
| Controlled Synthesis of Atomically Thin 1T-TaS2 for Tunable Charge Density Wave Phase Transitions;Wei Fu等;chemistry of materials;第7613-7618页 * |
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