CN117265507A - Heater module, thin film deposition apparatus and thin film deposition method - Google Patents

Abstract

The application relates to a heater module, a thin film deposition apparatus and a thin film deposition method. The invention relates to a heater module, a thin film deposition device and a thin film deposition method using the heater module. The heater module is applied to a thin film deposition apparatus. The heater module includes a gas mixing chamber, a reaction chamber, and a heater. The gas mixing chamber comprises at least one gas dispersing plate and a baffle plate, and the baffle plate is arranged above the gas dispersing plate. The reaction chamber is disposed downstream of the gas mixing chamber and is in communication with the gas mixing chamber. The heater is adjacently arranged in the gas mixing chamber. The heater module, the thin film deposition device and the thin film deposition method using the heater module can achieve the effect of preparing high-quality thin films.

Description

Heater module, thin film deposition apparatus and method

This application is a divisional application. The filing date of the original application is November 11, 2016, the application number is 201610995091.6, and the invention name is "heater module, thin film deposition device and method".

Technical field

The present invention relates to a heater module, and in particular to a thin film deposition device and method for preparing high-quality thin films using a heater module.

Background technique

Chemical vapor deposition (Chemical Vapor Deposition, CVD) equipment can be divided into hot-wall deposition equipment and cold-wall deposition equipment. Since the cold wall deposition device can control the number of layers of thin film growth by changing the deposition time, and has the advantages of good film thickness uniformity, it is more suitable for preparing nanometer-sized two-dimensional layers than the hot wall deposition device. shape material. However, traditional cold wall deposition devices only heat the substrate, so the reactive gases in different pipelines need to reach the surface of the substrate to have enough heat source for chemical reactions. Since the chemical reaction before film growth is an important factor affecting the quality of the film, before the film grows, the reaction gases in different pipelines need to be maintained at high temperatures in order to carry out sufficient chemical reactions and thereby improve the quality of the deposited film.

Therefore, how to provide a heater module to improve the quality of deposited films is actually one of the current important issues.

Contents of the invention

In view of this, an object of the present invention is to provide a heater module, a thin film deposition device and a method to improve the quality of deposited thin films.

To achieve the above object, the present invention provides a heater module for use in a thin film deposition device. The heater module includes a gas mixing chamber, a reaction chamber and a heater. The gas mixing chamber includes at least one gas dispersion plate and a baffle, and the baffle is disposed above the gas dispersion plate. The reaction chamber is arranged downstream of the gas mixing chamber and communicates with the gas mixing chamber. The heater is located adjacent to the gas mixing chamber.

In one embodiment, the gas mixing chamber further includes a plurality of air inlet channels.

In one embodiment, the gas dispersion plate has a plurality of through holes.

In one embodiment, the heater is selected from one of a light bulb, a lamp tube, a heating coil, or a combination thereof.

In one embodiment, the baffle is a quartz plate.

To achieve the above object, the present invention provides a thin film deposition device including a process chamber and at least one gas supply pipeline. The process chamber includes a base and the aforementioned heater module. At least one gas supply line is connected to the heater module.

In one embodiment, the thin film deposition device is a cold wall chemical vapor deposition device.

In order to achieve the above object, the present invention provides a thin film deposition method, which includes the following steps: heating the substrate to the reaction temperature; providing the first reaction gas and the second reaction gas; isolating the first reaction gas and the second reaction gas; making the first reaction gas The gas and the second reaction gas are maintained at a preheating temperature; at the preheating temperature, the first reaction gas and the second reaction gas are mixed to perform a film forming reaction; and a thin film is deposited on the substrate.

In one embodiment, the step of providing the first reactive gas and the second reactive gas further includes: heating the first precursor to a first temperature to generate the first reactive gas; and heating the second precursor to a second temperature to generate the first reactive gas. A second reaction gas is produced.

In one embodiment, the preheating temperature is 500˜800°C.

In one embodiment, the first precursor is selected from transition metal compounds.

In one embodiment, the second precursor is selected from one of chalcogen elements such as sulfur, selenium, and tellurium.

Based on the above, the present invention adds a heater module to the thin film deposition device, so that the first reaction gas and the second reaction gas can be preheated before mixing, and ensures that the first reaction gas and the second reaction gas can be mixed. The mixing reaction is carried out at high temperature to make the chemical reaction before the film growth more complete, which improves the shortcomings of only heating the substrate in the conventional well-known technology. Therefore, the heater module, film deposition device and method of the present invention can achieve high-quality preparation The efficacy of the film.

Description of the drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings in the following description are: For some embodiments of the present invention, those of ordinary skill in the art can also obtain other drawings based on these drawings without exerting any creative effort.

Figure 1 is a schematic diagram of a thin film deposition device in one embodiment of the present invention;

Figure 2A is a side view of a heater module in one embodiment of the present invention;

Figures 2B to 2F are top views of each component in Figure 2A;

Figure 3 is a graph showing the relationship between temperature and time for growing a MoS ₂ film in one embodiment of the present invention;

Figure 4 is a Raman spectrum of a MoS ₂ film in one embodiment of the present invention;

Figure 5A is a schematic diagram of different measurement positions on the MoS ₂ film in one embodiment of the present invention;

Figure 5B is a photofluorescence (PL) spectrum chart at each measurement position in Figure 5A;

Figure 6 is a schematic flow chart of a thin film deposition method in one embodiment of the present invention.

Detailed ways

The heater module, thin film deposition device and method according to specific embodiments of the present invention will be described below with reference to the relevant drawings. The same components will be described with the same component symbols. The attached drawings are for illustrative purposes only and are not intended to be used. limitations of the invention.

The word "connection" used in this article not only includes direct connections between components, but also includes indirect connections between components. For example, there may be a medium or other component between the two components. Some known components may be omitted to avoid obscuring the concept of the present invention.

Figure 1 is a schematic diagram of a thin film deposition device in one embodiment of the present invention. Referring to Figure 1, the present invention provides a thin film deposition device 100, which includes a process chamber 3, a first gas supply pipeline 10b and a second gas supply pipeline 10a. The process chamber 3 includes a base 4 and a heater module 11 . The base 4 can be raised and lowered according to process requirements to adjust the distance between the substrate 5 and the heater module 11. The first gas supply pipeline 10b and the second gas supply pipeline 10a are respectively connected to the heater module 11, in which the thin film deposition device 100 can It is a cold wall chemical vapor deposition device. In addition, a first heating source 7 is provided around the first gas supply pipe 10b and the second gas supply pipe 10a to heat the first precursor 1 and the second precursor 2. The base 4 can carry the substrate 5 and is provided with a second heating source 6 to heat the substrate 5 .

Figure 2A is a side view of a heater module in one embodiment of the present invention. Referring to FIG. 2A , the present invention provides a heater module 11 that can be installed in the thin film deposition device 100 of FIG. 1 . The heater module 11 includes a gas mixing chamber 113, a reaction chamber 111 and a heater 115. The gas mixing chamber 113 includes at least one gas dispersion plate 112 and a baffle 114 . Figures 2B to 2F are top views of the components in Figure 2A. Please refer to Figures 2A to 2F. The gas mixing chamber 113 may include multiple air inlet channels (1131, 1132, 1133, 1134) for gas inlet from different pipelines, and the gas dispersion plate 112 has multiple through holes. 1121, which can evenly disperse the gas entering the reaction chamber. The four air inlet channels (1131, 1132, 1133, 1134) shown in Figure 2D are only schematic diagrams, and the present invention does not limit the number of air inlet channels.

Based on the above, the reaction chamber 111 in this embodiment is composed of a quartz tube and is disposed downstream of the gas mixing chamber 113 . The upper end of the reaction chamber 111 is connected to the gas mixing chamber 113, and the lower end of the reaction chamber 111 can be directly installed on the process chamber 3 in the thin film deposition apparatus 100, so the substrate 5 can be isolated from the reaction chamber 111. In addition, the heater 115 is provided adjacent to the gas mixing chamber 113 to maintain the gas mixing chamber 113 in a high temperature state. In this embodiment, the heater 115 is disposed above the gas mixing chamber 113 for example only. The heater 115 can also be disposed on both sides of the gas mixing chamber 113 or anywhere around the gas mixing chamber 113 . The baffle 114 is disposed above the gas dispersion plate 112 to isolate the reaction gas in the heater 115 and the gas mixing chamber 113 to prevent the reaction gas from being adsorbed on the surface of the heater 115 . In this embodiment, a quartz plate is used as the baffle 114, so it will not affect the heat transfer of the heater 115, and can prevent the reaction gas from contaminating the heater 115.

In the above embodiment, six light bulbs are used as the heat source of the heater 115. The heater 115 can also be selected from a lamp tube or a heating coil, or any combination of a light bulb, a lamp tube and a heating coil. In addition, the operating temperature of the heater 115 ranges from 50 to 800°C, preferably from 500 to 800°C. The selection of the operating temperature depends on the type of thin film expected to grow.

Figure 3 is a graph showing the relationship between temperature and time for growing a MoS ₂ film in one embodiment of the present invention. Figure 6 is a schematic flow chart of a thin film deposition method in one embodiment of the present invention. Please refer to FIG. 1 , FIG. 2A , FIG. 3 and FIG. 6 at the same time. The following will take growing a molybdenum disulfide (MoS ₂ ) film as an example to illustrate the thin film deposition method provided by the present invention. First, in step S10 , the substrate 5 in the thin film deposition apparatus 100 is heated to a reaction temperature of about 850-950°C, and the process chamber 3 is maintained at a pressure of about 10-30 Torr. In step S11, the first precursor 1 is heated to a temperature of about 65-75°C, the first precursor 1 is evaporated to form the first reaction gas 1a, and the second precursor 2 is heated to a temperature of about 190°C. , the second precursor 2 is evaporated to form the second reaction gas 2a. In this embodiment, the first precursor 1 is molybdenum hexacarbonyl (Mo(CO) ₆ ), and the second precursor 2 is sulfur powder (Sulfur). .

In step S12, the first reaction gas 1a and the second reaction gas 2a are brought into the heater module 11 through the first carrier gas 8 and the second carrier gas 9 respectively. At this time, the first reaction gas 1a can be brought into the heater module 11 through the control of the valve. The reactive gas 1a and the second reactive gas 2a are isolated from each other. In this embodiment, the first carrier gas 8 and the second carrier gas 9 are both argon (Ar). In step S13, the heater 115 is used as a heat source to maintain the first reactive gas 1a and the second reactive gas 2a at a preheating temperature of about 500-800°C. This process lasts for about 10 minutes. In this embodiment, preferably The preheating temperature can be 650℃, 700℃ or 750℃. In step S14, the first reaction gas 1a is brought to the location of the second reaction gas 2a by argon gas, and the first reaction gas 1a and the second reaction gas 2a are mixed at a temperature of about 500-800°C for subsequent steps. film-forming reaction. In step S15, a MoS ₂ thin film is deposited on the substrate 5.

Based on the above, the thin film deposition device and method provided by the present invention can also be used to prepare other types of two-dimensional layered chalcogen compounds. For example: molybdenum sulfide (MoS ₂ ), molybdenum selenide (MoSe ₂ ), molybdenum telluride (MoTe ₂ ), hafnium sulfide (HfS ₂ ), hafnium selenide (HfSe ₂ ), hafnium telluride (HfTe ₂ ), tungsten sulfide (WS ₂ ), tungsten selenide (WSe ₂ ), tungsten telluride (WTe ₂ ), niobium sulfide (NbS ₂ ), niobium selenide (NbSe ₂ ), niobium telluride (NbTe ₂ ), rhenium sulfide (ReS ₂ ) , rhenium selenide (ReSe ₂ ), rhenium telluride (ReTe ₂ ), etc. Wherein, the first precursor can be selected from transition metal compounds, such as molybdenum oxide (MoO ₃ ), tungsten oxide (WO ₃ ), niobium oxide (Nb ₂ O ₅ ), rhenium oxide (ReO ₃ ), hafnium oxide (HfO ₂ ) transition metal oxides, and the second precursor can be selected from one of the chalcogen elements or their compounds. The chalcogen elements are, for example, sulfur, selenium, tellurium, etc.

Figure 4 is a Raman spectrum of a MoS ₂ film in one embodiment of the present invention. Please refer to Figure 4. The Raman spectrum shows two characteristic peaks at 383.5 cm-1 and 405.6 cm-1. Therefore, it can be judged that the prepared film is a multi-layer structure MoS ₂ film.

Figure 5A is a schematic diagram of different measurement positions on the MoS ₂ film in one embodiment of the present invention. Figure 5B is a photofluorescence (PL) spectrum chart at each measurement position in Figure 5A. Please also refer to FIGS. 5A-5B. In this embodiment, a MoS ₂ film is grown on a sapphire substrate, and 9 points on the MoS ₂ film are randomly selected for photoluminescence (PL) analysis. As shown in Figure 5B, the PL intensity of the MoS ₂ film is much greater than the PL intensity of the substrate at each measurement position. Therefore, adding the heater module of the present invention to the film deposition device is helpful in preparing high-quality MoS ₂ films. .

To sum up, the present invention adds a heater module to the thin film deposition device, so that the first reaction gas and the second reaction gas can be preheated before mixing, and ensures that the first reaction gas and the second reaction gas can be mixed. The mixing reaction is carried out at high temperature to make the chemical reaction before the film growth more complete, which improves the shortcomings of only heating the substrate in the conventional well-known technology. Therefore, the heater module, film deposition device and method of the present invention can achieve high-quality preparation The efficacy of the film.

The above embodiments are not intended to limit the present invention. Any equivalent modifications or changes made by those familiar with the art without departing from the spirit and scope of the present invention should be included in the claims.

Claims (13)

1. A heater module, applied to a thin film deposition device, the heater module includes: A gas mixing chamber includes at least one gas dispersion plate, a baffle and a plurality of air inlet channels, the baffle is arranged above the gas dispersion plate, and the gas dispersion plate has a plurality of through holes; A reaction chamber is provided downstream of the gas mixing chamber and communicates with the gas mixing chamber; and A heater is provided adjacent to the gas mixing chamber, and the heater has a first heating source and a second heating source; Wherein, the baffle isolates the heater from the reactive gas in the gas mixing chamber to prevent the reactive gas in the gas mixing chamber from being adsorbed on the heater. 2. The heater module according to claim 1, wherein the heater includes at least one of the following or any combination thereof: a light bulb, a lamp tube, and a heating coil. 3. The heater module of claim 1, wherein the baffle is a quartz plate. 4. A thin film deposition device, comprising: Process chamber, including: The heater module according to any one of claims 1 to 3; and The base carries the substrate and can be raised and lowered according to process needs to adjust the distance between the substrate and the heater module; and The first gas supply pipeline and the second gas supply pipeline are connected to the air inlet channel of the heater module; Wherein, the first reaction gas and the second reaction gas enter the gas mixing chamber through the first gas supply pipe and the second gas supply pipe respectively, and the first gas supply pipe and the second gas mixing chamber The first heating source is arranged around the gas supply pipeline, and the second heating source heats the substrate. 5. The thin film deposition apparatus according to claim 4, wherein the thin film deposition apparatus is a cold-wall chemical vapor deposition apparatus. 6. A thin film deposition method, suitable for thin film deposition devices, the method comprising the following steps: Heating the substrate to reaction temperature; Provide a first reaction gas and a second reaction gas, which include: Before entering the heater module of the thin film deposition device, the first precursor is heated to a first temperature by the heater module of the thin film deposition device to generate the first reaction gas, the heater module includes a gas mixture room and heater; and Before entering the heater module of the thin film deposition device, heating the second precursor to a second temperature through the heater module of the thin film deposition device to generate the second reaction gas; The first reaction gas and the second reaction gas are allowed to enter the gas mixing chamber of the heater module, and the heater of the heater module is isolated from the first reaction gas through the baffle of the gas mixing chamber. The second reaction gas prevents the first reaction gas and the second reaction gas in the gas mixing chamber from being adsorbed on the heater; The heater of the heater module keeps the first reaction gas and the second reaction gas in the gas mixing chamber at a preheating temperature for a period of time, and the preheating temperature is higher than the third A temperature and the second temperature, and less than the reaction temperature; At the preheating temperature, the first reaction gas and the second reaction gas are mixed and reacted; The mixed reacted gas is uniformly dispersed through at least one gas dispersion plate; and A thin film is deposited on the substrate at the reaction temperature. 7. The thin film deposition method according to claim 6, wherein the step of heating the substrate to a reaction temperature is to heat the substrate to a reaction temperature of 850-950°C and maintain it at a pressure of 10-30 Torr. 8. The thin film deposition method according to claim 6, wherein the first temperature is 65˜75°C, the second temperature is 190°C, and the preheating temperature is 500˜800°C. 9. The thin film deposition method according to claim 6, wherein the step of causing the first reaction gas and the second reaction gas to enter the gas mixing chamber of the heater module is to pass the first carrier gas and the second carrier gas respectively. The carrier gas brings the first reaction gas and the second reaction gas into the gas mixing chamber of the heater module. 10. The thin film deposition method according to claim 9, wherein the first carrier gas and the second carrier gas are argon gas. 11. The thin film deposition method according to claim 6, wherein the first precursor is a transition metal compound, and the transition metal compound is molybdenum oxide, tungsten oxide, niobium oxide, rhenium oxide, or hafnium oxide; The second precursor includes one of the following: sulfur, selenium, tellurium and other chalcogen elements or their compounds. 12. The thin film deposition method according to claim 11, wherein the first precursor is molybdenum hexacarbonyl, and the second precursor is sulfur powder. 13. The thin film deposition method according to claim 6, wherein the step of depositing a thin film is to deposit a molybdenum sulfide film, a molybdenum selenide film, a molybdenum telluride film, a hafnium sulfide film, a hafnium selenide film, a hafnium telluride film, sulfide Tungsten film, tungsten selenide film, tungsten telluride film, niobium sulfide film, niobium selenide film, niobium telluride film, rhenium sulfide film, rhenium selenide film, or rhenium telluride film.