CN216864302U - Two-dimensional material vapor deposition device with uniform temperature field - Google Patents
Two-dimensional material vapor deposition device with uniform temperature field Download PDFInfo
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- CN216864302U CN216864302U CN202220215681.3U CN202220215681U CN216864302U CN 216864302 U CN216864302 U CN 216864302U CN 202220215681 U CN202220215681 U CN 202220215681U CN 216864302 U CN216864302 U CN 216864302U
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Abstract
The utility model belongs to the field of vapor deposition equipment, and particularly relates to a two-dimensional material vapor deposition device with a uniform temperature field, which comprises a reaction tube and a hearth, wherein the hearth wraps the reaction tube and controls the temperature of a reaction tube cavity; the corresponding reaction tube cavity for controlling the temperature of the hearth is a temperature control area which is divided into a volatilization area at the upstream of the airflow and a deposition area at the downstream of the airflow, wherein spiral heating wires with gradually changed screw pitches and a plurality of temperature probes are arranged in the corresponding hearth for controlling the temperature of the deposition area. According to the utility model, the heating wire B and the temperature probe with the structure are jointly innovated, so that the temperature uniformity can be improved, and the deposition effect of a two-dimensional material can be improved.
Description
Technical Field
The utility model belongs to the technical field of two-dimensional material vapor deposition, and particularly relates to a two-dimensional material vapor deposition device with a uniform temperature field.
Background
The two-dimensional material has excellent electrical and optical properties, and can be widely applied to the fields of catalysis, nano tribology, microelectronics, lithium batteries, hydrogen storage, medical treatment and photoelectricity. However, the controllable growth of large-size, uniform, highly oriented single-layer two-dimensional material thin films is a great obstacle in the practical application thereof. A Guangyu team in the physical institute of Chinese academy of sciences independently sets up two-inch multi-source chemical vapor deposition equipment, and successfully prepares 2-inch MoS2 wafers. In 2020, the group further modified the chemical vapor deposition equipment to extend the equipment size to four inches and increase the source path from 3 to 7 paths while the sapphire substrate was placed vertically, with successful epitaxy to a 4 inch continuous single layer MoS2 film. The Wang Xinran team, university of Nanjing, prepared two inch wafers of co-oriented single crystal MoS2 using similar equipment and using C/A face sapphire instead as the substrate. Recently, the liu kailing team of the university of beijing successfully realized the preparation of a 2-inch single-crystal WS2 single-layer film by the CVD method using the interaction of a-plane sapphire surface and steps with a two-dimensional semiconductor, and showed that the substrate is also suitable for epitaxial growth of single crystals MoS2, WSe2 and MoSe 2. However, the obtained single crystals of MoS2, WSe2, and MoSe2 were all hundreds of microns in size. Further efforts are still needed for the universal preparation of wafer-level TMD.
In the prior art, the difficulties that the appearance and the quality of samples deposited at different positions, namely different temperature areas are greatly different due to wide temperature span range and large fluctuation of temperature in a temperature changing area are difficult to overcome, so that the size and the quality of a film are seriously influenced.
SUMMERY OF THE UTILITY MODEL
In order to solve the problems in the prior art, the utility model aims to provide a two-dimensional material vapor deposition device with a uniform temperature field, which aims to realize the uniformity of the temperature field of a substrate and is beneficial to realizing the growth behavior consistency of two-dimensional materials in a wafer-level range, thereby improving the performance of the prepared wafer-level two-dimensional materials.
A two-dimensional material vapor deposition device with a uniform temperature field comprises a reaction tube, a sealing device A and a sealing device B which seal two ends of the reaction tube, and a hearth which wraps the reaction tube and controls the temperature of a reaction tube cavity; the sealing device A is provided with an air inlet pipe for supplying air to the reaction pipe; the sealing device B is provided with an exhaust pipe for outputting gas in the reaction pipe; the corresponding reaction tube cavity for controlling the temperature of the hearth is a temperature control area, the temperature control area is divided into a volatilization area positioned on the side of the sealing device A and a deposition area positioned on the side of the sealing device B, a heating wire A and a temperature probe A for detecting the temperature of the heating wire A are arranged in the corresponding hearth for controlling the temperature of the volatilization area, a heating wire B and a temperature probe B for detecting the temperature of the heating wire B are arranged in the corresponding hearth for controlling the temperature of the deposition area, and the number of the temperature probes B is more than or equal to 2; the heating wire B is a spiral heating wire, and the screw pitch of the heating wire B gradually increases along the airflow direction.
According to the utility model, the spiral heating wire with the gradually-changed screw pitch is innovatively arranged in the hearth of the heating deposition area, the winding density of the spiral heating wire is gradually reduced, and the combination of the multiple temperature probes B is further matched, so that the temperature of the deposition area can be regulated and controlled to be slowly and stably reduced, the interference caused by temperature disturbance is avoided, and the real-time temperature monitoring is facilitated. The utility model can effectively improve the uniformity of the temperature of the deposition area, is beneficial to the consistency of the growth behaviors of the two-dimensional material in the wafer level range and is beneficial to improving the performance of the prepared wafer level two-dimensional material.
In the present invention, the sealing means a and B may be any means known in the industry that can be used for sealing a deposition reaction tube, and may be, for example, a flange.
In the utility model, the reaction tube is a quartz tube or a corundum tube.
The reaction tube is preferably a straight tube, and more preferably a cylindrical straight tube.
The length, the inner diameter and the wall thickness of the reaction tube can be adjusted according to the use requirement.
For example, the outer diameter of the reaction tube is, for example, 50mm to 800 mm; the wall thickness is 1-15% of the outer diameter.
In the utility model, the device also comprises a hearth, and the hearth is coated on the periphery of part of the reaction tubes. And the inner wall of the hearth and the outer wall of the reaction tube are allowed to contain a gap. That is, the reaction tube passes through the heating cavity of the furnace chamber, and both ends of the reaction tube are exposed outside the heating cavity.
In the utility model, a chamber of the reaction tube (a corresponding reaction tube chamber located in a heating cavity of the hearth) controlled by the temperature of the hearth is defined as a temperature control area. Preferably, the length of the temperature control zone accounts for 1/8-7/8 of the total length of the reaction tube.
In the utility model, the temperature control area controls the temperature through the hearth. Further preferably, the temperature is controlled by heating wires (resistance wires) arranged on the hearth. For example, the temperature of the volatilization zone is controlled by heating wire A, and the temperature of the deposition zone is controlled by heating wire B.
Preferably, the heating wire a is a spiral heating wire (spring-like structure).
Preferably, the heating wire A is a constant pitch spiral heating wire. The equal pitch means that the density of the helical winding is the same in the different regions.
In the utility model, heating wires A are arranged at the top and the bottom of the heating and volatilizing zone corresponding to the hearth.
In the utility model, the number of the heating wires A can be further regulated and controlled according to the number of the reaction raw materials. For example, two groups of heating wires A are arranged along the airflow direction. For example, two sets of heating wires A are arranged at the bottom and the top along the airflow direction.
In the present invention, the temperature probe A is disposed in the vicinity of the heating wire A, for example, at a distance of 3cm or less. Preferably, the temperature probes a are arranged in addition to the heating wires a at the bottom, and one temperature probe is arranged per group of heating wires a.
In the utility model, a heating wire B is arranged in a hearth of a heating deposition area; the heating wire B is of a spiral spring-shaped structure, and the thread pitch of the heating wire B is gradually increased along the airflow direction. That is, the spiral density of the heating wire along the airflow direction is gradually reduced.
Preferably, the heating wires B are arranged at the top and the bottom of the hearth of the heating deposition area.
In the utility model, the heating wires A and B can be placed in the inner wall of the hearth and can also be fixed on the hearth by means of the fixing bracket.
Preferably, the temperature probe B is arranged in the vicinity of the heating wire B, for example, at a distance of less than or equal to 3 cm. Preferably, the temperature probe B is disposed in the vicinity of the heating wire B located at the bottom. Further preferably, the number of the temperature probes B is 3-6, and the temperature probes B are uniformly arranged along the length direction of the heating wire B.
In the present invention, the temperature probes a and B may be devices known in the industry capable of detecting temperature, and may be thermocouple probes, for example.
In the utility model, the volatilization area is provided with raw material trays (such as porcelain boats) for holding raw materials, and the number of the raw material trays can be adjusted according to the quantity of the raw materials. For example, when the physical vapor deposition is performed, the number of the raw material trays thereof may be one. When performing chemical vapor deposition, the raw material tray may be one or more.
In the present invention, the deposition area is provided with a deposition substrate, and preferably, the deposition substrate is vertically arranged (arranged perpendicular to the axial direction of the pipeline) in the deposition area. That is, the plane of the deposition substrate is perpendicular to the length direction of the reaction tube.
The research of the utility model finds that the deposition substrate is arranged in the length direction of the reaction pipeline, and is further matched with the gradual change spiral heating wire and the temperature probe, so that the utility model can cooperate with each other, the range of the transverse temperature field of the substrate is greatly reduced, the uniformity of the two-dimensional material deposition temperature field is further improved, the growth temperature of the deposition substrate can be accurately regulated and controlled by adjusting the position of the vertically arranged substrate (namely the distance between the substrate and the source), the growth behavior, quality and uniformity of the two-dimensional material in the wafer level range can be realized, and the preparation of the two-dimensional material wafer is realized. The structure of the utility model has better application effect in the aspect of vapor deposition of wafer-level two-dimensional materials.
The deposition substrate can be vertically arranged in the reaction tube by means of self gravity, and can also be fixed by means of a fixing device. The deposition substrate and the inner wall of the deposition area are allowed to have a gap. Preferably, the planar area of the deposition substrate can be 10-60% of the cross-sectional area of the deposition area.
The utility model discloses a preferable two-dimensional material vapor deposition device with a uniform temperature field, which comprises a reaction tube, a sealing device A and a sealing device B, wherein the sealing device A and the sealing device B are used for sealing two ends of the reaction tube; wherein the sealing device A is provided with an air inlet pipe for supplying air to the reaction pipe; the sealing device B is provided with an exhaust pipe for outputting gas in the reaction pipe;
the middle part of the reaction tube is a temperature control area, wherein the temperature control area close to the sealing device A side is a volatilization area, and the temperature control area close to the sealing device B side is a deposition area; the volatilization area is provided with a porcelain boat for containing raw materials, and the deposition area is provided with a vertically arranged deposition substrate;
a hearth for controlling the temperature of the temperature control area is arranged at the periphery of the temperature control area; two groups of equidistant spiral heating wires A are arranged at the top and the bottom of the inner wall of the hearth for heating the volatilization zone along the airflow direction, and a temperature probe A is arranged near each heating wire A at the bottom; the top and the bottom of the inner wall of the hearth for heating the deposition area are both provided with gradual change spiral heating wires B, and the thread pitch of the gradual change spiral heating wires is gradually increased along the airflow direction; and 3-6 temperature probes B are arranged near the gradual change spiral heating wire B at the bottom and are uniformly arranged along the length direction of the heating wire B.
The method of the present invention is carried out, for example, when physical and chemical vapor deposition is carried out, the reaction raw materials are arranged in the volatilization zone, and the deposition substrate is arranged in the deposition zone in a manner perpendicular to the length of the reaction tube; and continuously introducing carrier gas into the reaction tube, and carrying out temperature control treatment on the temperature control area by means of heating wires A and B, so that the raw materials are volatilized in the volatilization area and are deposited on the deposition substrate by means of the action of the carrier gas. The temperature monitoring device can slowly and stably reduce the temperature, avoid the interference caused by temperature disturbance, and monitor the temperature in real time through the thermocouple. In addition, the substrate is arranged perpendicular to the pipeline, so that the range of the transverse temperature field where the substrate is located is greatly reduced, and the uniformity of the two-dimensional material deposition temperature field is further improved. Thereby realizing the preparation of the high-quality two-dimensional material wafer.
Preferably, the reaction raw material is a gaseous raw material or a solid raw material.
The solid raw material is, for example, powder, particles, metal wires and the like.
For example, the raw materials are Se powder, S powder, Te powder, transition metals and compounds such as molybdenum oxide and other applicable base materials.
The device can be used for preparing various two-dimensional materials, such as nano films, nano sheets, nano belts and superlattice.
The device can be used for preparing high-quality wafer-level two-dimensional materials; for example, two-dimensional materials with a thickness of 0.7-100nm can be prepared.
The specific implementation mode of the equipment of the utility model is as follows:
PVD scheme: when PVD is carried out using a feedstock, the feedstock is subjected to PVD, such as WSe2The raw materials are arranged in a volatilization area, the deposition substrate is arranged in a deposition area in a direction vertical to the length direction of the reaction tube, carrier gas is adopted to carry out gas scrubbing in the reaction tube, and then a temperature control device is adopted to control the temperature of the volatilization area and the reaction deposition area, so that the two-dimensional material is obtained on the substrate.
CVD protocol: when two or more raw materials are used for chemical vapor deposition, different raw materials such as MoO3And S raw materials are respectively arranged in different areas of the volatilization zone (adjusted according to volatilization temperature), the deposition substrate is arranged in the deposition zone in a way of being vertical to the length direction of the reaction tube, carrier gas is adopted to carry out gas scrubbing in the reaction tube, and then a temperature control device is adopted to control the temperature of the volatilization zone and the reaction deposition zone, so that the wafer-level two-dimensional material is obtained on the substrate.
Advantageous effects
1. In the utility model, the gradual change heating wire B with the gradually increased pitch along the airflow direction is innovatively arranged in the deposition area, and the combined control of a plurality of temperature probes is further matched, so that the temperature uniformity in the cavity can be effectively improved, the deposition uniformity of a two-dimensional material can be improved, and the performance of the prepared material can be improved.
2. Under the innovation of the gradient spiral heating wire and the temperature probe, the combined control of the arrangement mode of the substrate vertical pipeline is further matched, so that the range of a transverse temperature field where the substrate is located can be further reduced, and the uniformity of a two-dimensional material deposition temperature field is further improved; thereby realizing the preparation of the high-quality two-dimensional material wafer.
The device effectively overcomes the defects that the deposition temperature difference of samples in different areas of the whole substrate is large when the wafer-level two-dimensional material is produced, and the obtained samples have large shape and size difference, and is beneficial to growing large-size and uniform high-quality two-dimensional materials.
In a word, the utility model can achieve the effects of high efficiency and labor cost saving, simultaneously improves the experimental efficiency, ensures the size and the quality of the growing film material, and is completely suitable for controlling the growth of the two-dimensional material film in the tube furnace. Therefore, the two-dimensional material film grown by the two-dimensional material reaction chamber equipment with the highly uniform temperature field can generate larger market space, and has strong practicability.
Drawings
FIG. 1 is a reaction apparatus according to the present invention;
FIG. 2 is a conventional reaction apparatus;
Detailed Description
Example 1
The vapor deposition reaction chamber and the vapor deposition device of the utility model have the structure shown in figure 1: the device comprises a reaction tube 1 and flanges ( flanges 2 and 3 respectively) for sealing two ends of the reaction tube 1, wherein the flange 2 is provided with an air inlet pipe, and the flange 3 is provided with an exhaust pipe. The middle part of the reaction tube 1 is arranged in a heating chamber of the hearth 4; and the reaction tube chamber controlled by the temperature of the hearth 4 is defined as a temperature control area which is divided into a volatilization area (positioned on the side of the flange 2) positioned at the upstream of the gas flow and a deposition area (positioned on the side of the flange 3) positioned at the downstream of the gas flow. The volatilization zone is provided with porcelain boats 8 for holding raw materials (corresponding porcelain boats can be arranged according to the quantity of the raw materials), the deposition zone is provided with a vertical deposition substrate 7, and the plane of the deposition substrate is vertical to the length direction of the reaction tube.
In the hearth, two groups of spiral heating wires A (heating wires 6) are arranged at the top and the bottom of the hearth of the heating and volatilizing region along the airflow direction, and a temperature probe (also called a thermocouple probe, omitted in the figure and arranged close to the middle of the heating wire A) is arranged in the middle of each spiral heating wire A at the bottom; the top and the bottom of the corresponding hearth of the heating deposition area are both provided with gradually-changed spiral heating wires B (heating wires 5) with gradually-changed and increased screw pitches along the airflow direction; and 3-6 temperature probes (omitted in the drawing) are arranged near the heating wire B at the bottom and are close to the heating wire B and are uniformly arranged along the length direction of the heating wire B.
In the implementation process, raw materials are added into the porcelain boat in the volatilization area, carrier gas is introduced into the system for gas washing, the required carrier gas amount is controlled, temperature control processing is carried out on the temperature control area, the raw materials are volatilized in the volatilization area, the raw materials reach the deposition substrate under the carrier gas, and the raw materials are deposited on the surface of the deposition substrate, so that the corresponding two-dimensional material is prepared.
FIG. 2 is a diagram of a conventional reaction apparatus, which is different from the present invention mainly in that a heating wire and a temperature probe are not provided in a deposition zone in a pitch-graded manner, and moreover, a substrate is provided in a conventional horizontal arrangement. The temperature fields of the two materials show that the device has a more uniform temperature field, and is more beneficial to depositing and obtaining a high-performance two-dimensional material.
The working principle of the utility model is as follows: the heating resistance wire 5 (heating wire B) with the winding density gradually reduced along the airflow direction is introduced, and a plurality of thermocouple probes are arranged, so that the temperature is slowly and stably reduced, the interference caused by temperature disturbance is avoided, and the temperature is monitored in real time through the thermocouples. In addition, the substrate is placed perpendicular to the pipeline, so that the range of a transverse temperature field where the substrate is located is greatly reduced, the uniformity of a two-dimensional material deposition temperature field is further improved, and a high-quality two-dimensional material film with large size, high orientation and uniform thickness distribution can be grown.
Claims (16)
1. A two-dimensional material vapor deposition device with a uniform temperature field comprises a reaction tube, a sealing device A and a sealing device B which seal two ends of the reaction tube, and a hearth which wraps the reaction tube and controls the temperature of a reaction tube cavity; the sealing device A is provided with an air inlet pipe for supplying air to the reaction pipe; the sealing device B is provided with an exhaust pipe for outputting gas in the reaction pipe; the corresponding reaction tube cavity for controlling the temperature of the hearth is a temperature control area, and the temperature control area is divided into a volatilization area positioned on the side of the sealing device A and a deposition area positioned on the side of the sealing device B, and is characterized in that a heating wire A and a temperature probe A for detecting the temperature of the heating wire A are arranged in the corresponding hearth for controlling the temperature of the volatilization area, a heating wire B and a temperature probe B for detecting the temperature of the heating wire B are arranged in the corresponding hearth for controlling the temperature of the deposition area, and the number of the temperature probes B is more than or equal to 2; the heating wire B is a spiral heating wire, and the screw pitch of the heating wire is gradually increased along the airflow direction.
2. A two-dimensional material vapor deposition apparatus having a uniform temperature field as defined in claim 1 wherein the sealing means a and B are both flanges.
3. A two-dimensional material vapor deposition apparatus having a uniform temperature field according to claim 1, wherein the reaction tube is a quartz tube or a corundum tube.
4. A two-dimensional material vapor deposition apparatus having a uniform temperature field as set forth in claim 1, wherein said heating wire a is a spiral heating wire.
5. A two-dimensional material vapor deposition apparatus having a uniform temperature field according to claim 4, wherein the heating wire A is a constant pitch spiral heating wire.
6. A two-dimensional material vapor deposition apparatus having a uniform temperature field as set forth in claim 1, wherein the heating volatilization zone is provided with heating wires a corresponding to both the top and bottom of the furnace.
7. A two-dimensional material vapor deposition apparatus having a uniform temperature field according to claim 6, wherein the heating wires A of the top and bottom are provided in two sets in the gas flow direction.
8. A two-dimensional material vapor deposition apparatus having a uniform temperature field according to claim 6, wherein the temperature probe A is disposed in the vicinity of the bottom heating wire A.
9. A two-dimensional material vapor deposition apparatus having a uniform temperature field as set forth in claim 8, wherein each set of heating wires a is provided with one temperature probe a.
10. A two-dimensional material vapor deposition apparatus having a uniform temperature field as set forth in claim 1, wherein said heating wires B are disposed at the bottom and the top of the respective furnaces.
11. A two-dimensional material vapor deposition apparatus having a uniform temperature field as set forth in claim 10, wherein said temperature probe B is disposed near a heating wire B at the bottom.
12. A two-dimensional material vapor deposition apparatus having a uniform temperature field according to claim 10, wherein 3 to 6 temperature probes B are provided.
13. A two-dimensional material vapor deposition apparatus having a uniform temperature field as set forth in claim 10, wherein said temperature probes are uniformly arranged along the length of the heating wire B.
14. A two-dimensional material vapor deposition apparatus having a uniform temperature field as defined in claim 1 wherein the deposition zone is provided with a deposition substrate.
15. A two-dimensional material vapor deposition apparatus having a uniform temperature field according to claim 14, wherein the deposition substrate is disposed upright in the deposition zone.
16. A two-dimensional material vapor deposition apparatus having a uniform temperature field as defined in claim 1 wherein said volatilization zone is provided with means for containing the feedstock.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220215681.3U CN216864302U (en) | 2022-01-26 | 2022-01-26 | Two-dimensional material vapor deposition device with uniform temperature field |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220215681.3U CN216864302U (en) | 2022-01-26 | 2022-01-26 | Two-dimensional material vapor deposition device with uniform temperature field |
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| CN216864302U true CN216864302U (en) | 2022-07-01 |
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| CN202220215681.3U Active CN216864302U (en) | 2022-01-26 | 2022-01-26 | Two-dimensional material vapor deposition device with uniform temperature field |
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