CN115404460B - One-dimensional MoS 2 Nanotube material and method for preparing same - Google Patents
One-dimensional MoS 2 Nanotube material and method for preparing same Download PDFInfo
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- 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
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Abstract
The invention discloses a one-dimensional MoS 2 Nanotube material and method of making same comprising forming a nanotube material with MoO 3 S powder is used as a primary material, and Te-assisted chemical vapor deposition method is adopted to grow MoS 2 Nanotube material, the single MoS 2 The diameter of the nano tube is 80-200 nm, and the nano tube is deposited on SiO by Te auxiliary chemical vapor deposition method 2 High quality single crystal MoS grown on Si substrate surface 2 The nano tube adopts Te powder as a catalyst in the Te auxiliary chemical vapor deposition process, a template and a specific precursor structure design are not needed, the process is simple, the yield is high, the cost is low, and the method is suitable for batch production; in SiO 2 Direct growth of MoS on Si substrate 2 The nano material prepared by the nano tube has uniform shape and stable structural performance, and can be used as channel materials of field effect transistors, photocatalysis, electrocatalysis, solar cells, flexible sensors, field emission and cathode materials of lithium ion batteries.
Description
Technical Field
The invention belongs to the field of nano materials, and relates to a one-dimensional MoS 2 Nanotube material and method of making the same.
Background
The nanomaterial, due to its unique structure and its unique physical and chemical properties, can be used in biosensors, photocatalysis, electrochemical catalysis, material engineering, environmental engineering, energy conversion and storage, and in biomedical applicationsThe method has wide application in a plurality of fields such as science and the like and shows good performance. Graphene and carbon nanotubes have been fully studied and developed in the last few decades, but because of their zero band gap and non-controllable, their application in logic circuits and other fields has been limited, low-dimensional transition group metal chalcogenides (TMDs) similar in structure to graphene, carbon nanotubes have been recognized as a new trend for nanomaterials, and molybdenum disulfide (MoS 2 ) Exhibits excellent performance when the own dimension changes from zero dimension to three dimension. Zero-dimensional MoS 2 I.e. quantum dots, have special electron and photophysical properties depending on quantum confinement and edge effects, which make their application in bioimaging, luminescence sensing and catalysis possible. The two-dimensional TMDs material has high carrier mobility and adjustable band gap, so that the two-dimensional TMDs material is expected to enlarge the wonderful color in the next-generation semiconductor process. In addition, three-dimensional MoS 2 The block has good application in lubrication due to the small friction coefficient. Although, one-dimensional MoS 2 Materials (nanoribbons, nanowires, nanotubes) are of great importance in exploring a large number of new phenomena, new applications on the nanoscale, but they are of little interest, mainly because of certain challenges in synthesis. In 2001, the MoS was synthesized for a long time under the condition of ultrahigh temperature by adopting a catalytic transport method for the first time 2 Nanotubes, however, have poor morphology and quality, and have been MoS using template methods 2 The nanotube material is generated, but the process is relatively in charge of complexity, and impurity elements are easily introduced in the process of etching the template. As Chinese invention CN202011621439.8 discloses a MoS 2 The preparation method of the nanotube adopts anodic aluminum oxide as a template, adopts atomic layer deposition technology to grow molybdenum disulfide with controllable thickness on the surface of a nano hole of the anodic aluminum oxide template, and then etches the anodic aluminum oxide by using etching liquid to obtain MoS 2 An array of nanotubes. The preparation process is relatively complicated, and H adopted in the preparation process 2 The S gas is not friendly to human body and environment.
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art,the invention provides a method for directly forming SiO 2 One-dimensional MoS grown on surface of Si by adopting chemical vapor deposition method 2 The method of the nano tube has simple process, the reaction source is friendly to the environment, and the MoS prepared by the invention 2 The nano tube material has uniform shape and high single crystal property, and is favorable for the excavation and research of later performance.
In order to solve the problems, the invention adopts the following technical scheme:
one-dimensional MoS 2 A process for preparing the nano-tube material features that SiO is used as raw material 2 Si is a substrate, and a chemical vapor deposition method is adopted to carry out one-dimensional MoS on the silicon dioxide surface of the substrate 2 Growing a nanotube material;
the reaction source of chemical vapor deposition is molybdenum source and sulfur source, and the catalyst is Te powder.
Optionally, the molybdenum source is molybdenum trioxide powder; the Te powder is simple substance Te powder; the sulfur source is simple substance S powder; the dosage of the molybdenum source is 0.1-0.3 mg, the Te powder content is 0.05-0.1 mg, and the sulfur source is sufficient.
Optionally, the chemical vapor deposition growth container is a quartz tube with two open ends, and the carrier gas of the quartz tube is a mixed gas of argon and hydrogen; according to the flow direction of carrier gas, placing Shan Fengkou quartz tube in the described quartz tube, sulfur source is positioned at the sealing end of single-sealing quartz tube, the downstream of sulfur source is equipped with Te powder, the opening end of single-sealing quartz tube is equipped with quartz boat containing molybdenum source, siO 2 SiO of Si substrate 2 The quartz boat is covered face down; the flow rate of the carrier gas argon is 120-150 sccm, and the flow rate of the hydrogen is 15-25 sccm; the reaction temperature of the chemical vapor deposition is 750-850 ℃.
Optionally, the SiO 2 Cutting Si substrate into 1*1-1 x 2cm sheet, and SiO 2 And covering the surface of the quartz boat containing the molybdenum source downwards.
Optionally, the temperature rising rate of the carrier gas is 30 ℃/min.
Optionally, the distance between the Te powder and the sulfur source is 5-7 cm.
Optionally, the chemical vapor deposition has a growth time of 5min.
One-dimensional MoS 2 The preparation method of the nanotube material specifically comprises the following steps:
(1)SiO 2 the Si substrate is cut into regular slices, siO 2 The quartz boat is covered with a molybdenum source face down;
(2) The sulfur source is positioned at the sealing end of the single-sealing quartz tube, 0.05-0.1 mg Te powder is arranged at the position 6cm away from the sulfur source, and a quartz boat containing 0.1-0.15 mg molybdenum source is arranged at the opening end of the single-sealing quartz tube;
(3) The single-seal quartz tube is put into a quartz tube with two open ends, the seal end and the open end of the single-seal quartz tube are arranged along the flow direction of carrier gas, and chemical vapor deposition is carried out at 770-850 ℃.
One-dimensional MoS 2 Nanotube material, the one-dimensional MoS 2 The nanotube material adopts one-dimensional MoS according to any one of the invention 2 The nano tube material is prepared by a preparation method.
Optionally, the one-dimensional MoS 2 The length of the nanotube material is 50-100 mu m, and the diameter is 80-200 nm.
The invention has the advantages that:
(1) MoS prepared by the invention 2 The nanotube material is SiO with thickness of 510 μm and oxide layer thickness of 300nm 2 MoS grown on Si substrate 2 Nanotubes, and MoS 2 Nanotubes parallel to SiO 2 Growing MoS on the surface of the Si oxide layer 2 The length of the nano-tube material is 50-100 mu m, and the diameter is about 100nm; from microstructure MoS 2 The nanotube is in a tubular structure, so that the photoelectric property of the nano material is richer and more interesting due to the curvature effect, and the research on the basic physical property of the material such as quantum confinement effect is created due to the reduction of the dimension. The seed is grown on SiO 2 MoS on Si substrate 2 The nanotube material can be directly processed into a field effect transistor for testing photoelectric performance.
(2) In the preparation of the material, the Te-assisted chemical vapor deposition method is adopted to deposit SiO 2 Growth of one-dimensional tubular structure MoS on Si substrate 2 Nano material and catalyst auxiliary chemical gasThe phase deposition process does not need any template or other complex flow, has simple process, high speed, high yield and low cost, and is suitable for batch production;
(3) The invention prepares one-dimensional tubular structure MoS 2 Compared with H adopted by most of the prior preparation methods, the nano material 2 The S gas adopts S simple substance which is safer and more friendly to the environment and human body.
(4) In SiO 2 Direct growth of one-dimensional tubular structure MoS on Si substrate 2 The nanometer material has homogeneous nanometer tube material and high crystallinity.
Drawings
The accompanying drawings are included to provide a further understanding of the disclosure, and are incorporated in and constitute a part of this specification, illustrate the disclosure and together with the description serve to explain, but do not limit the disclosure. In the drawings:
FIG. 1 is a schematic diagram of experimental preparation of examples and comparative examples in the present invention;
FIG. 2 is an optical micrograph of example 1 of the present invention;
FIG. 3 is a TEM photograph of example 1 of the present invention;
FIG. 4 is a Raman spectrum of example 1 of the present invention;
FIG. 5 is an optical micrograph of example 2 of the present invention;
FIG. 6 is a Raman spectrum of example 2 of the present invention;
FIG. 7 is an optical micrograph of example 3 of the present invention;
FIG. 8 is a Raman spectrum of example 3 of the present invention;
FIG. 9 is an optical photograph of comparative example 1 in the present invention.
Detailed Description
In order that the objects and advantages of the invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings and which are appended to illustrate by way of a comparative example. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The one-dimensional tubular structure MoS prepared by the invention 2 Nano material is directly deposited on SiO by adopting a simple Te auxiliary chemical vapor deposition method 2 Growth of MoS on Si substrate 2 Nanotube material. The one-dimensional tubular structure MoS is obtained by controlling the flow of argon and hydrogen in a reaction system, the reaction temperature, the existence of a catalyst and other factors 2 The nano material does not need any template in the Te auxiliary chemical vapor deposition process, has simple process, high yield and low cost, and is suitable for batch production; moO (MoO) 3 And sulfur simple substance as reaction source to grow MoS with the assistance of Te 2 Nanotube material, moS prepared 2 The nanotube material has uniform morphology and good crystallinity.
The invention comprises the steps of using MoO 3 S powder is used as a primary material, and Te-assisted chemical vapor deposition method is adopted to grow MoS 2 Nanotube material, the single MoS 2 The diameter of the nano tube is 80-200 nm, and the nano tube is deposited on SiO by Te auxiliary chemical vapor deposition method 2 High quality single crystal MoS grown on Si substrate surface 2 The nano tube adopts Te powder as a catalyst in the Te auxiliary chemical vapor deposition process, a template and a specific precursor structure design are not needed, the process is simple, the yield is high, the cost is low, and the method is suitable for batch production; in SiO 2 Direct growth of MoS on Si substrate 2 The nano material prepared by the nano tube has uniform shape and stable structural performance, and can be used as channel materials of field effect transistors, photocatalysis, electrocatalysis, solar cells, flexible sensors, field emission and cathode materials of lithium ion batteries.
In particular, the one-dimensional MoS of the invention 2 Preparation method of nanotube material by SiO 2 Si is taken as a substrate, and a one-dimensional hollowed-out atomic layer MoS is carried out on the silicon dioxide surface of the substrate by adopting a chemical vapor deposition method 2 Growing the nano material; the growth container is a quartz tube, and the carrier gas of the quartz tube is a mixed gas of argon and hydrogen; according to the flow direction of carrier gas, placing Shan Fengkou quartz tube in the quartz tube, placing sulfur source at the bottom of single-seal quartz tube, arranging quartz boat containing Te powder at the downstream of sulfur source, and placing quartz boat containing molybdenum oxide at the port of single-seal quartz tube; the flow rate of the carrier gas argon is 50-150 sccm,the flow rate of the hydrogen is 5-30 sccm; the reaction temperature of the chemical vapor deposition is 700-850 ℃. Experiments show that the one-dimensional hollowed-out atomic layer MoS can be obtained only under the catalysis of Te powder by utilizing the raw materials and the process conditions provided by the invention 2 A nanomaterial. Whereas only two-dimensional MoS can be obtained on a substrate without Te powder as catalyst 2 Nanometer material without obtaining one-dimensional hollowed atomic layer MoS 2 A nanomaterial.
In embodiments of the present disclosure, siO 2 Cutting Si substrate into 1*1-1 x 2cm sheet, and SiO 2 And covering the surface of the quartz boat containing the molybdenum source downwards.
In an embodiment of the present disclosure, the molybdenum source is a molybdenum trioxide powder or a molybdenum chloride powder, preferably a molybdenum trioxide powder; the Te powder is simple substance Te powder; the sulfur source is S powder.
In the examples of the present disclosure, the molybdenum source is used in an amount of 0.1 to 0.3mg, the Te powder is contained in an amount of 0.05 to 0.1mg, and the sulfur source is sufficient.
In embodiments of the present disclosure, the temperature rise rate of the carrier gas is 30 ℃/min.
In embodiments of the present disclosure, the Te powder and the sulfur source are 5 to 7cm apart, preferably 6cm apart.
In embodiments of the present disclosure, the growth time of chemical vapor deposition is 5min.
In embodiments of the present disclosure, moS 2 The length of the nano tube is 30-100 mu m, and the diameter is 80-200 nm.
The method specifically comprises the following steps:
(1)SiO 2 the Si substrate is cut into regular slices, siO 2 The quartz boat is covered with a molybdenum source face down;
(2) The sulfur source is positioned at the sealing end of the single-sealing quartz tube, 0.05-0.1 mg Te powder is arranged at the position 6cm away from the sulfur source, and a quartz boat containing 0.1-0.3 mg molybdenum source is arranged at the opening end of the single-sealing quartz tube;
(3) The single-seal quartz tube is put into a quartz tube with two open ends, the seal end and the open end of the single-seal quartz tube are arranged along the flow direction of carrier gas, and chemical vapor deposition is carried out at 770-850 ℃.
One-dimensional tubular structure MoS 2 Nanometer material, one-dimensional MoS of any one of the invention 2 The nano tube material is prepared by a preparation method. One-dimensional MoS prepared by the method 2 The length of the nanotube material is 30-100 μm, and the diameter is 80-200 nm.
In the following experiments, all raw materials are commercially available and all methods are conventional in the art unless otherwise specified.
Embodiment one:
the embodiment shows a method of forming a silicon oxide film on SiO 2 Preparation of one-dimensional tubular Structure MoS on Si substrate 2 A method of nanomaterial comprising the steps of:
step one: a sufficient amount of sulfur powder was placed at the bottom of a single-seal quartz tube having an inner diameter of 14mm and a length of 36cm, and a quartz boat having 0.05mg of Te powder was placed 6cm from the sulfur source.
Step two: siO is made of 2 Cutting Si substrate into 1cm pieces, blowing clean with air gun, and cleaning SiO 2 Face down on a container containing 0.1mg MoO 3 The powder quartz boat is arranged at the port of the single-seal quartz tube
Step three: placing single-seal quartz tube into quartz tube with inner diameter of 44mm and length of 140cm, adding MoO 3 A section of the powder is directed towards the exhaust end. Heating in the central heating position of a tubular atmosphere furnace to perform one-dimensional tubular structure MoS 2 Chemical vapor deposition of nanomaterials is shown in figure 1 a.
Step four: 200sccm of argon was introduced for 30 minutes to thoroughly purge the tube of residual oxygen. Then continuously introducing a mixed gas of 100sccm of argon and 20sccm of hydrogen, heating the tubular atmosphere furnace to 770 ℃ at a heating rate of 30 ℃/min, preserving heat for 5min, then closing the heater, and naturally cooling to room temperature.
One-dimensional tubular structure MoS obtained at this time 2 The nanomaterial photo is shown in figure 2. As can be seen from the optical photograph of fig. 2, the prepared material is a uniform one-dimensional nanomaterial, and as can be seen from the TEM photograph of fig. 3, the prepared material is a standard tubular structure. The Raman spectrum is shown in FIG. 4, and the measured position has MoS 2 Raman characteristic peaks of (c) (table)The material prepared is MoS 2 The length is 30-100 μm, and the diameter is 80-100 μm.
Embodiment two:
the embodiment shows a method of forming a silicon oxide film on SiO 2 Preparation of one-dimensional tubular Structure MoS on Si substrate 2 A method of nanomaterial comprising the steps of:
step one: a sufficient amount of sulfur powder was placed at the bottom of a single-seal quartz tube having an inner diameter of 14mm and a length of 36cm, and a quartz boat having 0.05mg of Te powder was placed 6cm from the sulfur source.
Step two: siO is made of 2 Cutting Si substrate into 1cm pieces, blowing clean with air gun, and cleaning SiO 2 Face down on the container containing 0.3mgMoO 3 The powder quartz boat is arranged at the port of the single-seal quartz tube
Step three: the single-seal quartz tube was placed in a quartz tube having an inner diameter of 44mm and a length of 140cm, with a section of MoO3 powder added toward the exhaust end. Heating in the central heating position of a tubular atmosphere furnace to perform one-dimensional tubular structure MoS 2 Chemical vapor deposition of nanomaterials is shown in figure 1 a.
Step four: 200sccm of argon was introduced for 30 minutes to thoroughly purge the tube of residual oxygen. Then continuously introducing a mixed gas of 120sccm argon and 25sccm hydrogen, heating the tubular atmosphere furnace to 770 ℃ at a heating rate of 30 ℃/min, preserving heat for 5min, then closing the heater, and naturally cooling to room temperature.
One-dimensional tubular structure MoS obtained at this time 2 The nanomaterial photo is shown in figure 5. As can be seen from a comparison of the optical photographs of fig. 5 and fig. 2, the prepared material is a uniform one-dimensional tubular nanomaterial. The Raman spectrum is shown in FIG. 6, the measured position has MoS 2 Is shown to be MoS 2 The length is 30-100 μm, and the diameter is 80-100 μm.
Embodiment III:
the embodiment shows a method of forming a silicon oxide film on SiO 2 Preparation of one-dimensional tubular Structure MoS on Si substrate 2 A method of nanomaterial comprising the steps of:
step one: a sufficient amount of sulfur powder was placed at the bottom of a single-seal quartz tube having an inner diameter of 14mm and a length of 36cm, and a quartz boat having 0.1mg of Te powder was placed at a distance of 6cm from the sulfur source.
Step two: siO is made of 2 Cutting Si substrate into 1cm pieces, blowing clean with air gun, and cleaning SiO 2 Face down on the container containing 0.1mgMoO 3 The powder quartz boat is arranged at the port of the single-seal quartz tube
Step three: placing single-seal quartz tube into quartz tube with inner diameter of 44mm and length of 140cm, adding MoO 3 A section of the powder is directed towards the exhaust end. Heating in the central heating position of a tubular atmosphere furnace to perform one-dimensional tubular structure MoS 2 Chemical vapor deposition of nanomaterials is shown in figure 1 a.
Step four: 200sccm of argon was introduced for 30 minutes to thoroughly purge the tube of residual oxygen. Then continuously introducing a mixed gas of 120sccm argon and 25sccm hydrogen, heating the tubular atmosphere furnace to 850 ℃ at a heating rate of 30 ℃/min, preserving heat for 5min, then closing the heater, and naturally cooling to room temperature.
One-dimensional tubular structure MoS obtained at this time 2 The nanomaterial photo is shown in figure 7. As can be seen from a comparison of the optical photographs of fig. 7 and fig. 2, the prepared material is a uniform one-dimensional tubular nanomaterial. The Raman spectrum is shown in FIG. 8, the measured position has MoS 2 Is shown to be MoS 2 The length is 30-100 μm, and the diameter is 80-100 μm.
Comparative example one:
this comparative example shows a method for preparing a material without using Te powder as a catalyst, comprising the steps of:
step one: a sufficient amount of sulfur powder was placed at the bottom of a single-seal quartz tube having an inner diameter of 14mm and a length of 36 cm.
Step two: siO is made of 2 Cutting Si substrate into 1cm pieces, blowing clean with air gun, and cleaning SiO 2 Face down on the container containing 0.1mgMoO 3 And the powder quartz boat is arranged at the port of the single-seal quartz tube.
Step three: the single-seal quartz tube is placed at an inner diameter of 44mm and a length ofAdding MoO into a quartz tube with 140cm 3 A section of the powder is directed towards the exhaust end. Heating in the central heating position of a tubular atmosphere furnace to perform one-dimensional tubular structure MoS 2 Chemical vapor deposition of nanomaterials is shown in figure 1 b.
Step four: 200sccm of argon was introduced for 30 minutes to thoroughly purge the tube of residual oxygen. Then continuously introducing a mixed gas of 120sccm argon and 25sccm hydrogen, heating the tubular atmosphere furnace to 770 ℃ at a heating rate of 30 ℃/min, preserving heat for 5min, then closing the heater, and naturally cooling to room temperature. MoS obtained at this time 2 The nanomaterial photo is shown in figure 9. As can be seen from a comparison of the optical photographs of fig. 9 and 2, the material prepared is not a one-dimensional material.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (6)
1. One-dimensional MoS 2 A process for preparing the nano-tube material features that SiO is used as raw material 2 Si is a substrate, and a chemical vapor deposition method is adopted to carry out one-dimensional MoS on the silicon dioxide surface of the substrate 2 Growing a nanotube material;
the reaction source of chemical vapor deposition is a molybdenum source and a sulfur source, and the catalyst is Te powder;
the molybdenum source is molybdenum trioxide powder; the Te powder is simple substance Te powder; the sulfur source is simple substance S powder; the dosage of the molybdenum source is 0.1-0.3 mg, the Te powder content is 0.05-0.1 mg, and the sulfur source is sufficient;
the chemical vapor deposition growth container is a quartz tube with two open ends, and the carrier gas of the quartz tube is a mixed gas of argon and hydrogen; according to the flow direction of carrier gas, placing Shan Fengkou quartz tube in the described quartz tube, sulfur source is positioned at the sealing end of single-sealing quartz tube, the downstream of sulfur source is equipped with Te powder, the opening end of single-sealing quartz tube is equipped with quartz boat containing molybdenum source, siO 2 SiO of Si substrate 2 Face downCoating on a quartz boat; the flow rate of the carrier gas argon is 120-150 sccm, and the flow rate of the hydrogen is 15-25 sccm; the reaction temperature of chemical vapor deposition is 750-850 ℃;
the distance between the Te powder and the sulfur source is 5-7 cm.
2. A one-dimensional MoS as in claim 1 2 The preparation method of the nanotube material is characterized in that the SiO is prepared by 2 The Si substrate is cut into a sheet shape of 1X 1-1X 2cm, siO 2 And covering the surface of the quartz boat containing the molybdenum source downwards.
3. A one-dimensional MoS as in claim 1 2 The preparation method of the nanotube material is characterized in that the temperature rising rate of the carrier gas is 30 ℃/min.
4. A one-dimensional MoS as in claim 1 2 The preparation method of the nanotube material is characterized in that the growth time of the chemical vapor deposition is 5min.
5. One-dimensional MoS 2 Nanotube material, characterized in that the one-dimensional MoS 2 The nano tube material adopts the one-dimensional MoS as set forth in any one of claims 1-4 2 The nano tube material is prepared by a preparation method.
6. A one-dimensional MoS of claim 5 2 The nanotube material is characterized in that the one-dimensional MoS 2 The length of the nanotube material is 50-100 mu m, and the diameter is 80-200 nm.
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