TWI518198B - System for preparing films - Google Patents

Description

Film preparation system

The present invention relates to a system for preparing a thin film, and more particularly to a cold wall chemical vapor deposition (CVD) reaction system capable of synthesizing a wafer-scale large-area atomic-scale 2D layer material.

It is currently believed that graphite and other low-dimensional layered materials such as boron nitride and transition metal dichalcognides are expected to be applicable to low power, transparent and flexible electronic products. However, the technique of synthesizing large-area 2D-layer materials (2DLM) by chemical vapor deposition (CVD) is not mature enough to be mass-produced. The main obstacle is whether the partial pressure of the reaction gas in the reaction chamber can be precisely controlled.

In other words, solid or liquid precursors are necessary in the growth of atomic 2D layers. For example, the prior art (Lee et al ( Adv Mater. 24 (17), 2320-2325 (2012) DOl: adma.201104798; Adv Mater : (2013) DOT: adma. 201304376)) has confirmed the generation of MoS ₂ and WSe ₂ The monolayer hot-wall CVD method uses a solid (powder or crystal) material as its precursor.

Chemical vapor deposition (CVD) typically requires the precursors to be heated to a higher temperature (near the melting temperature) for vaporization. Thereafter, the vaporized vaporized precursor is introduced into a gas mixing unit (referred to as a shower head) in the main reaction chamber via a line, and then deposited onto the substrate.

Referring to the first figure, there is shown a schematic diagram of a conventional hot wall CVD apparatus 1 comprising: a multi-zone tubular furance 11, a preheating furnace 12, and a Gas control list Element 13, a vacuum pump 14 and the like, wherein the multi-zone tubular furance 11 has a quartz tube or a ceramic tube to form a receiving cavity 111 for the substrate S, the multi-zone tubular furnace 11 One end side is provided with an end cover 112 having a gas circuit 113 communicating with the preheating furnace 12, and the end cover 112 is connected to a pressure sensor 114 and controlled by the pressure sensor 114. Opening and closing, the other side of the multi-zone tubular furnace 11 is in communication with the vacuum pump 14; the preheating furnace 12 is configured to heat and evaporate a solid precursor to be reacted therein; the gas control unit 13 is coupled to The preheating furnace 12 is connected to a gas source 131 equipped with carrier gases, and a gas valve 132 is further disposed between the gas control unit 13 and the preheating furnace 12 to control the inflow and outflow of the carrier gas. The vacuum pump 14 is connected to the multi-zone tubular furnace 11 and is vented outward (ie, in the direction of the black bold arrow A1), thereby forming a vacuum environment in the multi-zone tubular furnace 11.

When the solid precursors B and C are heated in a preheating furnace 12 to form a vapor, the generated steam is transported through the gas circuit 113 and the end cap 112 by the carrier gas sent from the gas source 131 to the gas control unit 12. After reaching the accommodating cavity 111, since the gas circuit 113 is too long, the generated steam is lost due to condensation in the gas circuit 113. Therefore, in this case, the vapor pressures of the solid precursors A and B cannot be precisely controlled, and such design compatibility is poor, and it cannot be widely used in the semiconductor industry, and it is difficult to expand the scale to achieve high productivity, and it is difficult to carry out. Wafer size film growth.

The second figure shows the design of another conventional cold wall CVD apparatus 2 comprising: a reaction chamber 21, a gas control unit 22, a power supply unit 23, a vacuum pump 24, and a pressure The sensor unit 25 further includes a showerhead 211 and a substrate heating unit 212, and the substrate heating unit 212 is disposed opposite to the showerhead 211 with a specific spacing therebetween. The material heating unit 212 has a platform 213 for a substrate S2 disposed thereon; the gas control unit 22 is in communication with the shower head 211 and has a gas source 221 and a gas valve 222, wherein the gas source 221 includes a carrier Gas, and gas valve 222 is located at The gas control unit 22 and the gas source 221 are arranged to control the inflow and out of the carrier gas; the power supply device 23 is electrically connected to the substrate heating unit 212, and has a thermocouple 231 for sensing the temperature of the substrate S2; the vacuum pump The Pu-24 is in communication with the reaction chamber 21 and is vented outward (i.e., in the direction of the black bold arrow A2) to form a vacuum environment in the reaction chamber 21.

Thereby, the cold-wall type CVD apparatus 2 can introduce the gas flow F1 formed by the gaseous precursor output from the gas source 221 through the gas control unit 22 or the vaporized vaporized liquid precursor into the reaction chamber 21 through the shower head 211, and The substrate S2 heated on the substrate heating unit 212 is uniformly sprayed.

Such devices are often used for thin film deposition in the semiconductor industry (see U.S. Patent No. 5,551,985), in which only gaseous (e.g., organometallic compounds) or vaporized liquid precursors can be used (see U.S. Patent). Nos. 6,931,203 and 7,192,866, to avoid the occurrence of a blockage of the precursor at the precursor input or gas circuit due to the excessive length of the gas circuit of the aforementioned hot wall CVD apparatus. However, the use of gaseous organometallic compounds often has unavoidable consequences, namely the formation of carbon residues or defects in the obtained film, which would cause serious contamination problems for atomic 2D layer materials.

On the other hand, since the temperature of the line between the nozzle 211 and the gas control unit 22 cannot be maintained at a high temperature, or the temperature of the line is always much lower than the condensation temperature of the precursor, these vaporized vaporized precursors are in the process of being transported. It will still condense in the pipeline. Since atomic 2DLM is only a few atoms thick, pressure control during growth is extremely important. Obviously, this equipment also causes difficulties in the precise control of precursor pressure. In some instances, although the heating line (not shown) is often used to maintain the line at a particular temperature, the melting point of many solid precursors is much higher than the maximum temperature of the commercial heating jacket, resulting in heating. The sleeve cannot be used at high temperatures.

Therefore, systems for preparing wafer-scale films are still in need of continuous research and development.

In view of the deficiencies of the prior art, it is an object of the present invention to provide a system for preparing a film, particularly for forming a wafer-scale film. The system further adds a heating chamber outside the original reaction tank, that is, directly sets the tubular furnace in the reaction tank, thereby shortening the distance between the precursor and the nozzle, and also reducing the condensation of the precursor due to the temperature difference when transporting between the pipelines. The possibility. The system can also be equipped with multiple sets of heating chambers at the same time for optimum efficiency.

Another object of the present invention is to provide a system for preparing a film, wherein a gas mixing unit (for example, a shower head) is provided with a heater, and the gas mixing unit is designed to be temperature-controlled to improve the inner surface of the gas mixing unit. Large area and low temperature, which is easy to cause the precursor to condense in it.

It is still another object of the present invention to provide a system for preparing a film, the gas mixing unit (e.g., the head) having a detachable filter plate as its output port, thereby being easily and quickly adapted to specific process conditions. Adjust the hole size of the filter plate and the hole design for better fluid uniformity and more flexibility in all types of wafer-scale film process design. Moreover, the detachable filter plate requires more than two devices to visually adjust fluid uniformity.

A further object of the present invention is to provide a system for preparing a film, wherein an auxiliary gas control valve is disposed between the reaction chamber and the heating chamber to effectively finely adjust the amount of precursor entering the reaction chamber to achieve precise control of wafer-scale film synthesis. .

Therefore, the present invention provides a system for preparing a film by using a carrier gas to carry a precursor onto a substrate to form a film, comprising: a reaction chamber comprising a gas mixing unit, a heating platform, and a precursor a gas pipeline, wherein the gas mixing unit is disposed opposite to the heating platform, and the gas mixing unit has a plurality of output ports, wherein the heating platform is provided with the substrate, and the precursor pipeline is mixed with the gas The unit is further connected to the heating chamber, and the heating chamber comprises: a heating unit and a heating pipeline, wherein the heating unit is disposed around the heating pipeline, and the heating pipeline has a relative a first opening and a second An opening, wherein the first opening is connected to the precursor pipeline, and an accommodation space is formed between the first opening and the second opening; a gas control unit is coupled to the second of the heating pipeline The opening is in communication and controls the flow of the carrier gas; a vacuum forming unit is in communication with the reaction chamber and the heating chamber to form a vacuum environment in the reaction chamber and the heating chamber, respectively; and a pressure sensing a unit connected to the reaction chamber to sense a pressure state of the reaction chamber; thereby, the precursor is gasified in the heating chamber, and the carrier gas is transported through the heating line and the precursor line The output port sent to the gas mixing unit is output to the substrate.

In an embodiment, the gas mixing unit may further include a heater. For example, in one embodiment, the heater can be a halogen lamp heater to provide a high temperature above 1000 °C. In another embodiment, the heater can be further electrically connected to a power supply.

In another embodiment, the gas mixing unit may be a nozzle, and the nozzle may include a detachable filter plate having a plurality of filter holes as an output port.

In yet another embodiment, the gas mixing unit can use both the heater and the detachable filter plate for optimal component efficiency. For example, the gas mixing unit may be a temperature-controlled shower head, wherein the temperature-controlled spray head includes a receiving area, a precursor input area, and a filter plate, wherein the heater is disposed in the receiving area, the precursor The input zone is in communication with the precursor line, and the filter plate has a plurality of filter holes as output ports.

In an embodiment, the system further includes an auxiliary gas control valve, which is formed of a high temperature resistant material and disposed in the accommodating space of the heating pipe. Similarly, in other embodiments, the auxiliary gas control valve can be used in conjunction with the aforementioned heater, detachable filter plate, or a combination thereof to achieve optimum system efficiency.

In one embodiment, the high temperature resistant material is a material resistant to 900-1000 degrees or more, such as quartz, but is not limited thereto.

In one embodiment, the auxiliary gas control valve may be a vacuum linear introduction unit including a shaft and a body. The seat system is disposed in the second opening and has a shaft hole penetrating into the receiving space. The shaft is disposed for linear sliding therein, and the shaft further has an abutting end corresponding to the first opening for abutting and closing the first opening.

In an embodiment, the heating pipe may be made of a high temperature resistant material. An exemplary high temperature resistant material is a material that can withstand 900-1000 degrees or more, such as quartz, but is not limited thereto.

In an embodiment, the heating unit is an embedded heating unit embedded in the outside of the heating pipeline.

In one embodiment, the gas control unit may further include a gas control valve and a carrier gas inlet, and the gas control valve is disposed between the carrier gas inlet and the second opening.

In an embodiment, the vacuum forming unit may include a first vacuum pump and a second vacuum pump, wherein the first vacuum pumping system is in communication with the heating pipeline, and the second vacuum pumping system and the reaction chamber and the heating chamber Connected.

In an embodiment, the heating platform can be further electrically connected to a power supply.

In one embodiment, the foregoing system is used to prepare a wafer-scale film.

In one embodiment, the aforementioned system is a chemical vapor deposition reaction system.

The invention also provides a gas mixing list for a system for preparing a film The gas mixing unit includes: an accommodating area, a precursor input area, a filter plate, and a heater, wherein the heater is disposed in the accommodating area, the precursor input area and the precursor pipeline The cells are connected to each other, and the filter plate has a plurality of filter holes as an output port. In one embodiment, the filter plate is detachable.

1‧‧‧hot wall CVD equipment

11‧‧‧Multi-zone tubular furnace

111‧‧‧ accommodating cavity

112‧‧‧End cover

113‧‧‧ gas circuit

114‧‧‧pressure sensor

12‧‧‧Preheating furnace

13‧‧‧ gas control unit

131‧‧‧ gas source

132‧‧‧ gas valve

14‧‧‧vacuum pump

2‧‧‧ Cold wall CVD equipment

21‧‧‧Reaction room

211‧‧‧ sprinkler

212‧‧‧Substrate heating unit

213‧‧‧ platform

22‧‧‧ gas control unit

221‧‧‧ gas source

222‧‧‧ gas valve

23‧‧‧Power supply unit

231‧‧‧ thermocouple

24‧‧‧vacuum pump

25‧‧‧ Pressure Sensor

3‧‧‧Reaction room

31‧‧‧ gas mixing unit

311‧‧‧Receiving area

312‧‧‧Precursor input area

313‧‧‧Removable filter plate

314‧‧‧Halogen heater

315‧‧‧Power supply

316‧‧‧ thermocouple

317‧‧‧filter holes

32‧‧‧heating platform

321‧‧‧Power supply

33‧‧‧Precursor pipeline

34‧‧‧heating room

35‧‧‧heating unit

36‧‧‧heating line

361‧‧‧ first opening

362‧‧‧ second opening

363‧‧‧ accommodating space

4‧‧‧ gas control unit

41‧‧‧ gas source

411‧‧‧ gas valve

42‧‧‧ gas control valve

43‧‧‧ Carrying gas inlet

5‧‧‧vacuum forming unit

51‧‧‧First vacuum pump

52‧‧‧Second vacuum pump

6‧‧‧ Pressure sensing unit

7‧‧‧Auxiliary gas control valve

71‧‧‧ body

711‧‧‧Axis hole

72‧‧‧ shaft

73‧‧ ‧ close loop

A1, A2, A3, A4‧‧‧ black bold arrow

B, C‧‧‧ solid precursors

F1, F2‧‧‧ airflow

P‧‧‧Precursors

G‧‧‧ Carrying gas

S, S2, S3‧‧‧ substrates

The first figure is a schematic diagram of a conventional hot wall CVD apparatus.

The second figure is a schematic diagram of a conventional cold wall CVD apparatus.

The third figure is a schematic diagram of a system for preparing a wafer scale film according to an embodiment of the present invention.

The fourth figure is a cross-sectional view showing the structure of the auxiliary gas control valve in the system for preparing a wafer-scale film according to an embodiment of the present invention.

Fig. 5 is a cross-sectional view showing the structure of an auxiliary gas control valve in a system for preparing a wafer-scale film according to an embodiment of the present invention.

The sixth figure is a comparative diagram of the atomic-grade MoS ₂ film produced on the wafer-scale sapphire substrate by using the system, wherein: Figure A is a photograph of a 2-inch sapphire substrate without a film; Figure B is a film coated with a MoS ₂ film. Photograph of the 2 吋 sapphire substrate; Figure C is the result of Raman spectroscopy of Figure B.

Next, the embodiment of the present invention is described in detail by the following examples, but is not limited thereto. The above and other objects, features and advantages of the present invention will become more apparent from

Please refer to the third figure, which is a system for preparing a wafer-scale film according to an embodiment of the present invention. The system is a cold-wall CVD reaction system, which can be applied to a solid precursor (for example, metal, metal oxide, Metal Sulfide) Synthesize large area atomic 2D layer materials. The system may include elements such as the reaction chamber 3, the gas control unit 4, the vacuum forming unit 5, the pressure sensing unit 6, the auxiliary gas control valve 7, and the like.

The reaction chamber 3 of the present embodiment includes components such as a gas mixing unit 31, a heating platform 32, and a precursor conduit 33. The gas mixing unit 31 is disposed opposite to the heating platform 32 at a specific interval, and the heating platform 32 is provided. A substrate S3 to be reacted is disposed thereon and electrically connected to a power supply 321 . In the present embodiment, the gas mixing unit 31 is a temperature-controlled spray head having a receiving area 311, a precursor input area 312, and a detachable filter plate 313. A halogen lamp heater 314 is heated to a temperature higher than 1000 ° C. The halogen lamp heater 314 is electrically connected to a power supply 315; and the power supply 321 has a thermocouple 316 for sensing the temperature of the substrate S3. . The precursor input area 312 is in communication with the precursor line 33, both of which are air flow conveying lines for conveying the precursor vapor and the gas flow F2 formed by the carrier gas, and the detachable filter plate 313 A plurality of filter holes 317 are provided as gas output ports.

In most of the cold wall CVD processes currently known, it is more difficult to create materials on a wafer sized substrate than on a small sized substrate. One of the key reasons is that the airflow is actually difficult to evenly distribute over a large area substrate. A conventional solution is to use a showerhead to output airflow. However, since the inner surface of the nozzle is large in area and the temperature is low, it is unavoidable that the precursor vapor is vaporized in the nozzle after the vaporized precursor vapor is transported through the pipeline.

In order to solve this problem, in the embodiment, the gas mixing unit 31 is designed as a temperature-controlled nozzle, and a halogen lamp heater 314 is installed in the accommodating area 311, thereby providing a controllable high temperature environment to avoid precursors. The vapor is condensed in the gas mixing unit 31. Moreover, the halogen lamp heater 314 is capable of heating up to greater than 1000 ° C, whereas most of the prior art nozzles are capable of maintaining temperatures above 500 ° C (see US patent no. US 2005/005 6223 A1, US patent no. US 8,551,890 B2, US Patent No. US 8,298,370 B2, US patent no. US 7,192,866 B2), in contrast, the halogen lamp heater 314 employed in the present embodiment can maintain the gas mixing unit 31 at a higher temperature, which is effective Improving the inner surface of the gas mixing unit is likely to cause condensation of the precursor vapor point.

Another feature of the gas mixing unit 31 of the present embodiment is that a detachable filter plate 313 is provided. From the standpoint of fluid mechanics and diffusion kinetics, the vapor, temperature, pressure, gas flow rate and geometry of the filter plates of different precursors will affect the uniformity of the gas stream formed by the precursor vapor or carrier gas, generally In other words, the uniformity adjustment depends on the hole size of the filter plate used and the hole design. The detachable filter plate 313 can be easily and quickly replaced according to specific process conditions, and precisely adjusts and controls the airflow, and provides flexibility for producing various wafer-scale films (for example, atomic 2D layers). For example, at the same time, more than one detachable filter plate 313 is used to achieve better fluid uniformity.

On the other hand, in the growth of the atomic-scale 2D layer, since the atomic-scale 2D layer is only a few atoms thick, pressure control during growth is extremely important. It is often necessary to heat a solid or liquid precursor (e.g., solid sulfur and molybdenum trioxide) to a higher temperature (near the melting temperature) for vaporization. However, since the temperature of the pipeline cannot be maintained at a high temperature or the temperature of the pipeline is always much lower than the condensation temperature of the precursor vapor, these precursors condense in the pipeline during transportation, causing difficulty in precisely controlling the vapor pressure of the precursor. In the prior art, a heating jacket can be installed outside the pipeline to maintain a specific temperature. However, the melting point of many solid precursors is much higher than the maximum withstand temperature of commercial heating jackets, so that the heating jacket cannot be used at high temperatures.

In order to solve this problem, in the system of the present embodiment, a design in which the tubular furnace is disposed in the reaction chamber 3 is adopted, and a heating chamber 34 is further extended in the reaction chamber 3, and includes a heating unit 35 and a heating pipeline. 36 and the like, wherein the heating unit 35 is an embedded tubular heater embedded around the heating pipe 36. The heating pipe 36 is composed of a high temperature resistant material. In the embodiment, the heating pipe 36 is made of quartz, and has a first opening 361 and a second opening 362, wherein the first opening 361 is connected to the precursor line 33, and an accommodating space 363 is formed between the first opening 361 and the second opening 362, and the precursor P to be reacted therein is accommodated by The heating unit 35 heats the precursor P to form precursor vapor, thereby shortening the distance between the precursor vapor and the gas mixing unit 31. In this design, the precursor vapor is maintained in a high temperature state in the heating line 36 by the heating unit 35, and is immediately supplied to the gas mixing unit 31 of the reaction chamber 3 at a high temperature to reduce the possibility of condensation of the precursor. . In order to maintain the reaction chamber 3 and the heating chamber 34 in a vacuum environment, the vacuum forming unit 5 described below (described later) will be used.

The gas control unit 4 is externally connected to a gas source 41 containing a carrier gas (for example, inert gas or nitrogen gas, but not limited thereto). The gas source 41 is provided with a gas valve 411 for controlling the opening and closing of the carrier gas. . The gas control unit 4 further has a gas control valve 42 and a carrier gas inlet 43 which is provided at the carrier gas inlet 43 for controlling the flow of the carrier gas (for example, flow rate and Flow rate). Since the carrier gas can be carried by mixing the precursor vapors to the gas mixing unit 31, the flow rate of the carrier gas can be controlled by the gas control unit 4, and the flow rate of the precursor vapor in the heating line 36 can be controlled together.

The vacuum forming unit 5 includes a first vacuum pump 51 and a second vacuum pump 52, wherein the first vacuum pump 51 is in communication with the heating line 36, and the second vacuum pump 52 is connected to the reaction chamber 3. And the heating chamber 34 is in communication, and is externally exhausted by using the first vacuum pump 51 and the second vacuum pump 52 in combination (for example, the direction indicated by the black bold arrows A3 and A4), and in the reaction chamber 3 and The vacuum chamber is maintained in the heating chamber 4, and the vacuum environment of the reaction chamber 3 is communicated with the heating line 36 to precisely control the pressure of the vaporized precursor.

The pressure sensing unit 6 is connected to the reaction chamber 3 to sense the pressure state of the reaction chamber 3.

The auxiliary gas control valve 7 is composed of a high temperature resistant material. In the present embodiment, the high temperature resistant material means quartz, but is not limited thereto. The auxiliary gas control valve 7 is disposed in an accommodation space 363 formed between the first opening 361 and the second opening 362. Please refer to the fourth and fifth figures. The auxiliary gas control valve 7 is a vacuum linear introduction unit, including: An element 71, a shaft 72, and a plurality of closed-loops 73, wherein the base 71 is disposed in the second opening 362, and the base 71 has a shaft hole 711 extending through the receiving space 363 for the shaft. The rod 72 is threaded therein for linear sliding and is in communication with the carrier gas inflow port 43. The shaft 72 further has a spherical abutting end 721 corresponding to the first opening 361 for resisting and completely closing the first opening when the shaft 72 linearly slides toward the first opening 361. 361. The plurality of closed loops 73 are respectively disposed between the shaft 72 and the shaft hole 711, the gap between the chamber wall of the heating chamber 34 and the heating pipe 36, and the gap between the seat body 71 and the wall of the second opening 362, so that The auxiliary gas control valve 7 is maintained in a gas-closed state.

As can be seen from the foregoing, the flow rate of the precursor vapor can be controlled by the flow rate of the carrier gas. However, even if the gas control unit 4 closes the gas control valve 42 so that the carrier gas cannot enter the heating line 36 through the second opening 362, the flow rate of the precursor vapor cannot be closed to zero, one of which is obvious because of the precursor vapor. It can be delivered to the gas mixing unit 31 by diffusion without the need of an air flow. In order to avoid such a situation, the present embodiment provides the aforementioned auxiliary gas control valve 7 between the heating line 36 and the precursor line 33 connected to the gas mixing unit 31, which is made of quartz, which is incomparable to conventional knowledge. The high temperature resistant commercial control valve, the auxiliary gas control valve 7 of the present embodiment can be applied to a high temperature state. Moreover, as shown in the fourth figure, when the shaft 72 of the auxiliary gas control valve 7 linearly slides in the direction of the second opening 362, the first opening 361 of the heating line 36 is maintained in an open state, so that the precursor vapor can be by. On the other hand, when the shaft 72 of the auxiliary gas control valve 7 linearly slides in the direction of the first opening 361, the abutting end 721 of the shaft 72 will abut and completely close the first opening 361, preventing the precursor vapor by. Thereby, the auxiliary gas control valve 7 can further effectively finely adjust the amount of the precursor and precisely control the final synthesis result of the wafer-scale film.

Further, the auxiliary gas control valve 7 may be used in a state where the heating chamber 34 is not present, and the auxiliary gas control valve 7 may be provided between the precursor line 33 and the gas mixing unit 31.

Please refer to the third to fifth figures when liquid or solid precursors When the heating element 34 is heated and evaporated by the heating unit 35 to form the precursor vapor, the gas control unit 4 turns on the gas control valve 42 to output the carrier gas G, and the carrier gas passes through the carrier gas inlet 43 and the second opening. 362 enters the heating line 36, at which time the auxiliary gas control valve 7 is maintained in the open state, and the precursor vapor is transported through the first opening 361 maintained in the open state by the flow of the carrier gas to enter the precursor line 33. Precursor input area 312. At this time, the halogen lamp heater 314 is turned on, so that the precursor input region 312 of the gas mixing unit 31 is also maintained at a high temperature state, and the gas flow F2 formed by the carrier gas and the precursor vapor is mixed in the precursor input region 312, A plurality of filter holes 317 on the detachable filter plate 313 are uniformly sprayed and coated on the substrate S3 on the heating platform 32 that has been heated to be reacted to form a wafer-scale film.

Please refer to the sixth figure for a comparative diagram of the atomic-grade MoS ₂ film fabricated on a wafer-scale sapphire substrate using the system. Figure A is a photograph of a 2-inch sapphire substrate on which no film is formed; Figure B is a photograph of a 2-inch sapphire substrate coated with a MoS ₂ film; and Figure C is a result of Raman spectroscopy analysis in Figure B. As can be seen from Fig. B, the MoS ₂ film has a high degree of uniformity in the 2-inch region. The reaction conditions for film preparation by using the system are as follows: the solid precursor P in the heating chamber 34 is Mo(CO) ₆ and the temperature is 40 degrees; the carrier gas used in the gas control unit 4 is Ar, and the flow rate is 20 sccm; The intake line (not shown) is passed through H ₂ S, the flow rate is 20 sccm; the temperature of the halogen lamp heater 314 is 300 degrees, the temperature of the substrate heating unit 212 is 700 degrees; the process pressure is 10 Torr; and the process time is 15 minutes. . Further reference to Figure C is a Raman spectral analysis of the circular region locations of Figure B. The E2g and A1g peaks clearly show the presence of a MoS ₂ film on the sapphire substrate. The distance between the peaks of E2g and A1g is about 4 wave numbers, indicating that the MoS ₂ film is about 3 to 4 atomic layers thick.

In summary, the present invention provides a system for preparing a film, particularly for preparing a wafer-scale film, which can be widely applied to various precursors (especially, for example, metals, metal oxides, metal sulfides, etc. are clean. Solid-state precursors) to synthesize high-quality 2D atomic layers of wafer-sized films without the problem of precursor blockage.

It will be apparent to those skilled in the art that various changes can be made in accordance with the embodiments of the present invention without departing from the spirit of the invention. Therefore, it is to be understood that the invention is not limited by the scope of the invention, and is intended to cover the modifications of the spirit and scope of the invention.

3‧‧‧Reaction room

31‧‧‧ gas mixing unit

311‧‧‧Receiving area

312‧‧‧Precursor input area

313‧‧‧Removable filter plate

314‧‧‧Halogen heater

315‧‧‧Power supply

316‧‧‧ thermocouple

317‧‧‧filter holes

32‧‧‧heating platform

321‧‧‧Power supply

33‧‧‧Precursor pipeline

34‧‧‧heating room

35‧‧‧heating unit

36‧‧‧heating line

361‧‧‧ first opening

362‧‧‧ second opening

363‧‧‧ accommodating space

4‧‧‧ gas control unit

41‧‧‧ gas source

411‧‧‧ gas valve

42‧‧‧ gas control valve

43‧‧‧ Carrying gas inlet

5‧‧‧vacuum forming unit

51‧‧‧First vacuum pump

52‧‧‧Second vacuum pump

6‧‧‧ Pressure sensing unit

7‧‧‧Auxiliary gas control valve

A3, A4‧‧‧Black bold arrow

B, C‧‧‧ solid precursors

F2‧‧‧ airflow

P‧‧‧Precursors

G‧‧‧ Carrying gas

S3‧‧‧ substrate

Claims (30)

A system for preparing a film by using a carrier gas to carry a precursor onto a substrate to form a film. The system comprises: a reaction chamber comprising a gas mixing unit, a heating platform, and a precursor conduit. Wherein the gas mixing unit is disposed opposite to the heating platform, and the gas mixing unit has a plurality of output ports, wherein the heating platform is configured to be disposed on the substrate, and the precursor conduit is in communication with the gas mixing unit. The reaction chamber further extends out of a heating chamber, the heating chamber includes: a heating unit and a heating pipe, wherein the heating unit is disposed around the heating pipe, and the heating pipe has a first opening And a second opening, wherein the first opening is connected to the precursor pipeline, and an accommodation space is formed between the first opening and the second opening; a gas control unit is coupled to the heating pipeline The second opening is in communication and controls the flow of the carrier gas; a vacuum forming unit is in communication with the reaction chamber and the heating chamber to respectively respectively in the reaction chamber Forming a vacuum environment in the heating chamber; and a pressure sensing unit connected to the reaction chamber to sense a pressure state of the reaction chamber; thereby, the precursor is vaporized in the heating chamber, and the carrier is transported Gas is transported through the heating line, the precursor line, and the output port sent to the gas mixing unit is output to the substrate. The system of claim 1, wherein the gas mixing unit further comprises a heater. The system of claim 1, wherein the gas mixing unit is a nozzle, and the nozzle comprises a detachable filter plate having a plurality of filter holes as an output port. The system of claim 1, further comprising an auxiliary gas control valve, which is formed of a high temperature resistant material and disposed in the accommodating space of the heating pipe. The system of claim 4, wherein the high temperature resistant material is It is made of quartz. The system of claim 4, wherein the auxiliary gas control valve is a vacuum linear introduction unit, comprising a shaft and a body, the seat system is disposed in the second opening and has a through to the receiving One of the holes of the space for the shaft to be linearly slid therein, and the shaft has abutting end corresponding to the first opening for abutting and closing the first opening. The system of claim 2, wherein the gas mixing unit is a temperature-controlled nozzle, wherein the temperature-controlled nozzle comprises an accommodating area, a precursor input area, and a filter plate, wherein the heater The device is disposed in the accommodating area, and the precursor input area is in communication with the precursor pipeline, and the filter plate has a plurality of filter holes as an output port. The system of claim 7, wherein the filter plate is detachable. The system of claim 2, further comprising an auxiliary gas control valve, which is formed of a high temperature resistant material and disposed in the accommodating space of the heating pipe. The system of claim 9, wherein the high temperature resistant material is quartz. The system of claim 9, wherein the auxiliary gas control valve is a vacuum linear introduction unit, comprising a shaft and a body, the seat system is disposed in the second opening and has a through hole to the receiving One of the holes of the space for the shaft to be linearly slid therein, and the shaft has abutting end corresponding to the first opening for abutting and closing the first opening. The system of claim 3, further comprising an auxiliary gas control valve, which is composed of a high temperature resistant material and disposed in the accommodating space of the heating pipe. The system of claim 12, wherein the high temperature resistant material is quartz. The system of claim 12, wherein the auxiliary gas control valve is a vacuum linear introduction unit, comprising a shaft and a body, the seat system is disposed in the second opening and has a through to the receiving One of the holes of the space for the shaft to be linearly slid therein, and the shaft has abutting end corresponding to the first opening for abutting and closing the first opening. The system of claim 1, wherein the gas mixing unit is a temperature-controlled showerhead, comprising a receiving area, a precursor input area, a detachable filter plate, and a heater, wherein the heating The system is disposed in the accommodating area, the precursor input area is in communication with the precursor pipeline, and the detachable filter plate has a plurality of filter holes as an output port; and the system further comprises: an auxiliary gas The control valve is composed of a high temperature resistant material and is disposed in the accommodating space of the heating pipe. The system of claim 15, wherein the high temperature resistant material is quartz. The system of claim 15 wherein the auxiliary gas control valve is a vacuum linear introduction unit comprising a shaft and a body, the seat system being disposed in the second opening and having a through hole to the receiving One of the holes of the space for the shaft to be linearly slid therein, and the shaft has abutting end corresponding to the first opening for abutting and closing the first opening. The system of claim 2, wherein the heater is a halogen lamp heater. The system of claim 2, wherein the heater is further electrically connected to a power supply. The system of claim 1, wherein the heating pipe is formed of a high temperature resistant material. The system of claim 20, wherein the high temperature resistant material is quartz. The system of claim 1, wherein the heating unit is an embedded heating unit embedded outside the heating pipe. The system of claim 1, wherein the gas control unit further comprises a gas control valve and a carrier gas flow inlet, the gas control valve being disposed between the carrier gas inlet and the second opening . The system of claim 1, wherein the gas control unit is further connected to a gas source. The system of claim 1, wherein the vacuum forming unit comprises a first vacuum pump and a second vacuum pump, wherein the first vacuum pumping system is in communication with the heating line, and the second vacuum pump The pump system is in communication with the reaction chamber and the heating chamber. The system of claim 1, wherein the heating platform is further electrically connected to a power supply. The system of any one of claims 1 to 26, which is used to prepare a wafer-scale film. The system of any one of claims 1 to 26, which is a chemical vapor deposition reaction system. A gas mixing unit for preparing a thin film system, the gas mixing unit comprising: an accommodating area, a precursor input area, a filter plate, and a heater, wherein the heater is disposed in the accommodating area, the precursor The input zone is in communication with the precursor line, and the filter plate has a plurality of filter holes as output ports. The unit of claim 29, wherein the filter plate is detachable.