LU500345B1 - Preparation method of uniform material layer based on chemical vapor deposition - Google Patents

Preparation method of uniform material layer based on chemical vapor deposition Download PDF

Info

Publication number
LU500345B1
LU500345B1 LU500345A LU500345A LU500345B1 LU 500345 B1 LU500345 B1 LU 500345B1 LU 500345 A LU500345 A LU 500345A LU 500345 A LU500345 A LU 500345A LU 500345 B1 LU500345 B1 LU 500345B1
Authority
LU
Luxembourg
Prior art keywords
precursor
reaction chamber
material layer
substrate
phase source
Prior art date
Application number
LU500345A
Other languages
French (fr)
Inventor
Zeping Wang
Luqi Tao
Feng Zhang
Kai Zheng
Jiabing Yu
Xianping Chen
Original Assignee
Univ Chongqing
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Univ Chongqing filed Critical Univ Chongqing
Application granted granted Critical
Publication of LU500345B1 publication Critical patent/LU500345B1/en

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/458—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for supporting substrates in the reaction chamber
    • C23C16/4581—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for supporting substrates in the reaction chamber characterised by material of construction or surface finish of the means for supporting the substrate
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/305—Sulfides, selenides, or tellurides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
    • C23C16/4481—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation using carrier gas in contact with the source material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45502—Flow conditions in reaction chamber
    • C23C16/45504—Laminar flow
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/46—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for heating the substrate
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/52—Controlling or regulating the coating process

Landscapes

  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Fluid Mechanics (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

A preparation method of a uniform material layer based on chemical vapor deposition, comprising: placing a substrate and an object stage in a reaction chamber, wherein the substrate is arranged on the object stage, and the growth surface of the substrate deviates from the object stage; providing a first gas phase source substance and a second gas phase source substance into the reaction chamber to form a material layer on the growth surface. According to the preparation method of the uniform material layer based on chemical vapor deposition, a substrate and an object stage are placed in a reaction chamber, the growth surface of the substrate deviates from the object stage, and then a first gas phase source substance and a second gas phase source substance are provided in the reaction chamber for chemical vapor deposition reaction to form a material layer on the growth surface of the substrate.

Description

DESCRIPTION Preparation method of uniform material layer based on chemical vapor deposition
TECHNICAL FIELD The invention relates to the field of material preparation, in particular to a preparation method of a uniform material layer based on chemical vapor deposition.
BACKGROUND The existing Chemical Vapor Deposition (CVD) growth method inverts the substrate on the quartz boat, and the growth surface of the substrate is set toward the quartz boat for material growth, and the grown material layer shows uneven crystal distribution on the substrate from the center of the substrate to the sides, and the quality of the obtained material layer is low.
SUMMARY The present invention aims at solving at least one of the technical problems existing in the prior art.
In view of this, the invention provides a preparation method of a uniform material layer based on chemical vapor deposition, comprising the following steps: placing a substrate and an object stage in a reaction chamber, wherein the substrate is arranged on the object stage, and the growth surface of the substrate deviates from the object stage; a first gas phase source substance and a second gas phase source substance are provided into the reaction chamber, and a material layer is formed on the growth surface.
According to the preparation method of the uniform material layer based on chemical vapor deposition, a substrate and an object stage are placed in a reaction chamber, the growth surface of the substrate deviates from the object stage, and then a first gas phase source substance and a second gas phase source substance are provided in the reaction chamber for chemical vapor deposition reaction to form a material layer on the growth surface of the substrate. Compared with the traditional technical scheme that the growth surface of the substrate faces the quartz boat, the airflow velocity distribution on the growth surface of the substrate is more uniform, so that the uniformity and quality of the material layer can be greatly improved.
In addition, according to the preparation method of uniform material layer based on chemical vapor deposition in the above technical scheme provided by the present invention, it can also have the following additional technical characteristics: In the above technical scheme, further, placing the substrate and the stage in the reaction chamber, wherein the substrate is arranged on the stage, and the growth surface of the substrate deviates from the stage comprises the following steps: placing the first quartz boat in the reaction chamber; Covering the heat-resistant sheet on the first quartz boat; Placing the substrate on the heat-resistant sheet with the growth surface of the substrate facing away from the heat-resistant sheet.
In the technical scheme, the specific steps of placing the object stage and the substrate in the reaction chamber are further disclosed. Specifically, a first quartz boat is placed in a reaction chamber, then a heat-resistant sheet is covered on the first quartz boat, the first quartz boat and the heat-resistant sheet are used as an object stage, and finally a substrate is placed on the heat-resistant sheet, wherein the growth surface of the substrate deviates from the heat-resistant sheet.
Specifically, the first quartz boat and the heat-resistant sheet are used as the stage, which can bear the higher temperature in the reaction chamber, has stable chemical properties, and can prevent the stage from influencing the chemical vapor deposition reaction between the first gas phase source material and the second gas phase source material; On the other hand, 1t is convenient to take materials, assemble and place the stage. The heat-resistant sheet is covered on the first quartz boat to prevent the exposed groove of the first quartz boat from affecting the airflow distribution around the substrate, ensure the uniform airflow distribution on the growth surface of the substrate, and further improve the quality and uniformity of the material layer.
In any of the above technical schemes, further, the heat-resistant sheet is a quartz plate.
In this technical scheme, the material selection of the heat-resistant sheet is further provided. The quartz plate has the chemical characteristics of high temperature resistance and low thermal expansion coefficient. When the substrate is placed on the quartz plate, the quartz plate can stably lift the substrate, ensuring that a uniform and high-quality material layer can be formed on the growth surface of the substrate.
In any of the above technical schemes, further, providing the first gas phase source material and the second gas phase source material into the reaction chamber comprises placing the first precursor and the second precursor in the reaction chamber; Heating a first precursor to a first preset temperature through a reaction chamber to generate a first gas phase source substance; Heating the second precursor to a second preset temperature through a reaction chamber to generate a second gas phase source substance; Introducing carrier gas into the reaction chamber.
In this technical solution, specific steps are further provided for providing a first gas phase source substance and a second gas phase source substance into the reaction chamber. Specifically, the first precursor and the second precursor are placed in the reaction chamber, and the first precursor 1s heated to a first predetermined temperature to produce the first vapor phase source material, and the second precursor is heated to a second predetermined temperature to produce the second vapor phase source material; the incoming carrier gas is capable of guiding the first vapor phase source material and the second vapor phase source material above the substrate growth layer. Further, the vapor deposition reaction between the first vapor phase source material and the second vapor phase source material can form a uniform, high-quality material layer on the growth layer of the substrate.
Specifically, the first precursor and the second precursor are placed in a reaction chamber and heated to generate a first gas phase source substance and a second gas phase source substance. On the one hand, the first gas phase source substance and the second gas phase source substance are directly produced in the reaction chamber, which facilitates the vapor deposition reaction between the first gas phase source substance and the second gas phase source substance; On the other hand, the waste heat temperature of the first gas phase source material and the second gas phase source material can be fully utilized for vapor deposition reaction, so that the heat utilization rate can be improved and the formation efficiency of the material layer can be improved.
Specifically, the carrier gas is introduced to guide the first gas phase source material and the second gas phase source material. On the other hand, it can protect the chemical vapor deposition reaction between the first vapor source material and the second vapor source material, and can improve the quality of the material layer.
Specifically, the first preset temperature 1s a temperature at which the first precursor can be sublimated and gasified; The second preset temperature 1s the temperature at which the second precursor can be sublimated and vaporized.
In any of the above technical schemes, further, placing the first precursor and the second precursor in the reaction chamber comprises: placing a second quartz boat in the reaction chamber; Setting a first precursor in a second quartz boat; Placing a second precursor on an object stage; The second precursor is located between the substrate and the first precursor, and the carrier gas is introduced through one end of the reaction chamber near the second quartz boat.
In this technical scheme, a step of placing the first precursor and the second precursor in the reaction chamber is further provided. Specifically, a first precursor is carried by a second quartz boat and a second precursor is carried by a carrier table, and the second precursor is located between the first precursor and the substrate. The location of the first precursor and the second precursor and the introduction mode of the carrier gas are defined. After the carrier gas is introduced into the reaction chamber, it passes through the first precursor and the second precursor in turn and then reaches the substrate, which is convenient for guiding the first gas phase source material and the second gas phase source material above the substrate growth layer and can improve the quality of the substrate material layer.
In any of the above technical schemes, further, the reaction chamber is a tubular furnace, which comprises a first heating zone and a second heating zone, and supplying the first gas phase source material and the second gas phase source material to the upper part of the reaction chamber comprises:
Setting a second quartz boat bearing a first precursor in a first heating zone, and setting an object stage bearing a second precursor in a second heating zone; Adjusting the heating temperature of the first heating zone to a first preset temperature through a tubular furnace to generate a first gas phase source substance; Adjusting the heating temperature of the second heating zone to a second preset temperature through a tubular furnace to generate a second gas phase source substance; Introducing carrier gas through one end of the tubular furnace close to the first heating zone.
In this technical scheme, the type selection of the reaction chamber 1s further provided, and the tubular furnace 1s provided with a first heating zone and a second heating zone, so that the first precursor and the second precursor can be heated respectively, and the use is more convenient.
In any of the above technical schemes, further, the carrier gas is hydrogen and/or argon.
In the technical scheme, the type of carrier gas is further provided, and by providing hydrogen and/or argon, on the one hand, it plays the role of guiding the first gas phase source material and the second gas phase source material, On the other hand, it can protect the chemical vapor deposition reaction between the first vapor source material and the second vapor source material, and can improve the quality of the material layer.
In any of the above technical schemes, further, forming a material layer on the growth surface comprises adjusting the temperature of the substrate to a third preset temperature through the reaction chamber for a first preset time, so that the first gas phase source substance and the second gas phase source substance undergo a vapor deposition reaction to form a material layer on the growth surface.
In this technical scheme, a concrete step of forming a material layer on the growth surface 1s further provided. By adjusting the temperature to the third preset temperature and continuing for the first preset time, the smooth progress of the vapor deposition reaction between the first vapor source substance and the second vapor source substance 1s ensured, and a uniform and high-quality material layer can be formed on the growth surface.
Specifically, the third preset temperature can be selected based on the types of the first precursor and the second precursor or material layer, and the third preset temperature 1s located at a temperature which is beneficial to or can promote the vapor deposition reaction between the first vapor source material and the second vapor source material.
In any of the above technical schemes, further, the first preset time is 3 min to 20min.
In this technical scheme, by selecting the first preset time, it is ensured that there is enough time for the vapor deposition reaction between the first vapor source material and the second vapor source material to form a material layer on the growth surface of the substrate.
In any of the above technical schemes, further, the second precursor is metal oxide, the first precursor is at least one of sulfur powder, selenium powder and tellurium powder, and the second preset temperature is between 600°C and 850°C.
In the technical scheme, the compositions of the first precursor and the second precursor are further provided, wherein the metal oxide can be one of titanium oxide, zirconium oxide, hafnium oxide, vanadium oxide, niobium oxide, tantalum oxide,
molybdenum oxide, tungsten oxide, iron oxide and platinum oxide; Further, the second precursor can also be a mixture of auxiliary agent and metal oxide, for example, the auxiliary agent can be sodium chloride or potassium iodide; Furthermore, the second precursor can also be a variety of metal oxides or a mixture of metal oxides and metal powders, such as a mixture of molybdenum oxide and niobium oxide, a mixture of molybdenum oxide and rhenium powder, a mixture of molybdenum oxide and tungsten oxide, a mixture of tungsten oxide and niobium oxide, etc.
Additional aspects and advantages of the invention will become apparent in the description which follows, or may be learned by practice of the invention.
BRIEF DESCRIPTION OF THE FIGURES The above and/or additional aspects and advantages of the present invention will become apparent and easily understood from the description of embodiments taken in conjunction with the following drawings, in which: Fig. 1 shows a schematic flow chart of a method for preparing a uniform material layer based on chemical vapor deposition according to Embodiment 1 of the present invention; Fig. 2 shows a schematic flow chart of a method for preparing a uniform material layer based on chemical vapor deposition according to Embodiment 2 of the present invention; Fig. 3 shows a schematic flow chart of a method for preparing a uniform material layer based on chemical vapor deposition according to embodiment 3 of the present invention;
Fig. 4 shows a schematic flow chart of a method for preparing a uniform material layer based on chemical vapor deposition according to Embodiment 4 of the present invention; Fig. 5 shows a schematic flow chart of a method for preparing a uniform material layer based on chemical vapor deposition according to Embodiment 5 of the present invention; Fig. 6 shows a schematic flow chart of a method for preparing a uniform material layer based on chemical vapor deposition according to a specific embodiment of the present invention; Fig. 7 shows a structural schematic diagram of preparing a material layer by a tubular furnace according to an embodiment of the present invention; Fig. 8 shows a schematic diagram of airflow distribution on the growth surface of a substrate according to an embodiment of the present invention; Fig. 9 shows a schematic diagram of airflow distribution on the growth surface of a substrate in the prior art.
Among them, the corresponding relationship between the reference numerals and the component names in figs. 7 and 8 is as follows: 8 substrate, 10 stage, 12 tube furnace, 14 second quartz boat, 16 first precursor, 18 second precursor; 1002 First quartz boat, 1004 Quartz plate, 1202 First Heating Zone, 1204 Second Heating Zone.
Among them, the corresponding relationship between the reference numerals and the part names in Fig. 9 is as follows:
8' substrate.
DESCRIPTION OF THE INVENTION In order to better understand the above objects, features and advantages of the present invention, the present invention will be further described in detail with reference to the drawings and specific embodiments. It should be noted that the embodiments of this application and the features in the embodiments can be combined with each other without conflict.
Many specific details are set forth in the following description in order to fully understand the present invention, but the present invention can also be implemented in other ways different from those described here, so the protection scope of the present invention is not limited by the specific embodiments disclosed below.
The preparation method of uniform material layer based on chemical vapor deposition according to some embodiments of the present invention will be described below with reference to Figs.1- 9.
Embodiment 1 As shown in Fig. 1, one embodiment of the present invention provides a method for preparing a uniform material layer based on chemical vapor deposition, which includes: Step 102: Place a substrate and an object stage in a reaction chamber, wherein the substrate is arranged on the object stage, and the growth surface of the substrate deviates from the object stage; Step 104: Provide a first gas phase source material and a second gas phase source material into the reaction chamber, and form a material layer on the growth surface.
According to the preparation method of the uniform material layer based on chemical vapor deposition, a substrate and an object stage are placed in a reaction chamber, the growth surface of the substrate deviates from the object stage, and then a first gas phase source substance and a second gas phase source substance are provided in the reaction chamber for chemical vapor deposition reaction to form a material layer on the growth surface of the substrate. Compared with the traditional technical scheme that the growth surface of the substrate faces the quartz boat, the airflow velocity distribution on the growth surface of the substrate is more uniform, so that the uniformity and quality of the material layer can be greatly improved.
Embodiment 2 As shown in Fig. 2, one embodiment of the present invention provides a method for preparing a uniform material layer based on chemical vapor deposition, which includes: Step 202: Place the first quartz boat in the reaction chamber; Step 204: Cover the quartz on the first quartz boat; Step 206: Place the substrate on the quartz wafer, with the growth surface of the substrate deviating from the quartz wafer; Step 208: Provide the first gas phase source material and the second gas phase source material into the reaction chamber, and form a material layer on the growth surface.
In this embodiment, the specific steps of placing the stage and the substrate in the reaction chamber are further disclosed. Specifically, the first quartz boat is placed in a reaction chamber, then the first quartz boat is covered with a quartz sheet, the first quartz boat and the quartz sheet are used as a stage, and finally the substrate is placed on a quartz sheet, wherein the growth surface of the substrate deviates from the heat-resistant sheet.
Specifically, the first quartz boat and the quartz slice are used as the stage, which can bear the higher temperature of the reaction chamber. Because the stage has stable chemical properties, it can avoid the chemical vapor deposition reaction between the first gas phase source material and the second gas phase source material affected by the change of the chemical properties of the stage at higher temperature, and facilitate the acquisition, combination and placement of the stage. The quartz plate is covered on the first quartz boat to prevent the exposed tank body of the first quartz boat from influencing the airflow distribution around the substrate, ensure the airflow distribution on the substrate growth surface to be uniform, and further improve the quality and uniformity of the material layer.
In this embodiment, the quartz sheet has the chemical characteristics of high temperature resistance and low thermal expansion coefficient. When the substrate is placed on the quartz sheet, the quartz sheet can stably lift the substrate and ensure that a uniform and high-quality material layer can be formed on the growth surface of the substrate.
Embodiment 3 As shown in Fig. 3, an embodiment of the present invention provides a method for preparing a uniform material layer based on chemical vapor deposition, which includes: Step 302: Place the substrate and the stage in the reaction chamber, the substrate is arranged on the stage, and the growth surface of the substrate deviates from the stage; Step 304: A second quartz boat is arranged in the reaction chamber; Step 306: Set the first precursor in the second quartz boat; Step 308: Place the second precursor on the stage; Step 310: Heat the first precursor to a first preset temperature through a reaction chamber to generate a first gas phase source substance;
Step 312: Heat the second precursor to a second preset temperature through the reaction chamber to generate a second gas phase source substance; Step 314: Introduce carrier gas into the reaction chamber; Step 316: Form a material layer on the growth surface.
Wherein the second precursor is positioned between the substrate and the first precursor; The carrier gas is introduced through one end of the reaction chamber near the second quartz boat; The second precursor is metal oxide, the first precursor is at least one of sulfur powder, selenium powder and tellurium powder, and the second preset temperature is between 600 and 850°C.
In this embodiment, a specific step of providing the first gas phase source material and the second gas phase source material into the reaction chamber is further provided. Specifically, a first precursor and a second precursor are placed in a reaction chamber, the first precursor is heated to a first preset temperature to generate a first gas phase source substance, and the second precursor is heated to a second preset temperature to generate a second gas phase source substance; the first gas phase source substance and the second gas phase source substance can be guided above a substrate growth layer by an introduced carrier gas Specifically, the first precursor and the second precursor are placed in a reaction chamber and heated to generate a first gas phase source substance and a second gas phase source substance. On the one hand, the first gas phase source substance and the second gas phase source substance are directly produced in the reaction chamber, which facilitates the vapor deposition reaction between the first gas phase source substance and the second gas phase source substance; On the other hand, the waste heat temperature of the first gas phase source material and the second gas phase source material can be fully utilized for vapor deposition reaction, so that the heat utilization rate can be improved and the formation efficiency of the material layer can be improved.
Specifically, the carrier gas is introduced to guide the first gas phase source material and the second gas phase source material. On the other hand, it can protect the chemical vapor deposition reaction between the first vapor source material and the second vapor source material, and can improve the quality of the material layer.
Specifically, the first preset temperature is a temperature at which the first precursor can be sublimated and gasified; The second preset temperature is the temperature at which the second precursor can be sublimated and vaporized.
In this embodiment, a step of placing the first precursor and the second precursor in the reaction chamber is further provided. Specifically, a first precursor is carried by a second quartz boat and a second precursor is carried by a carrier table, and the second precursor is located between the first precursor and the substrate. The location of the first precursor and the second precursor and the introduction mode of the carrier gas are defined. After the carrier gas is introduced into the reaction chamber, it passes through the first precursor and the second precursor in turn and then reaches the substrate, which is convenient for guiding the first gas phase source material and the second gas phase source material above the substrate growth layer and can improve the quality of the substrate material layer.
In this embodiment, the composition of the first precursor and the second precursor is further provided, wherein the metal oxide can be one of titanium oxide, zirconium oxide, hafnium oxide, vanadium oxide, niobium oxide, tantalum oxide, molybdenum oxide,
tungsten oxide, iron oxide and platinum oxide; Further, the second precursor can also be a mixture of auxiliary agent and metal oxide, for example, the auxiliary agent can be sodium chloride or potassium iodide; Furthermore, the second precursor can also be a variety of metal oxides or a mixture of metal oxides and metals, such as a mixture of molybdenum oxide and niobium oxide, a mixture of molybdenum oxide and rhenium powder, a mixture of molybdenum oxide and tungsten oxide, a mixture of tungsten oxide and niobium oxide, etc.
Embodiment 4 As shown in Fig. 4, an embodiment of the present invention provides a method for preparing a uniform material layer based on chemical vapor deposition, wherein the reaction chamber is a tubular furnace, and the tubular furnace comprises a first heating zone and a second heating zone.
Step 402: Place the substrate and the stage in the reaction chamber, the substrate is arranged on the stage, and the growth surface of the substrate deviates from the stage; Step 404: Set the second quartz boat bearing the first precursor in the first heating zone, and set the stage bearing the second precursor in the second heating zone; Step 406: Adjust the heating temperature of the first heating zone to a first preset temperature through a tubular furnace to generate a first gas phase source substance; Step 408: Adjust the heating temperature of the second heating zone to a second preset temperature through a tubular furnace to generate a second gas phase source substance; Step 410: Introduce carrier gas through one end of the tubular furnace near the first heating zone; Step 412: Form a material layer on the growth surface.
Wherein the carrier gas 1s hydrogen and/or argon.
In this embodiment, the selection of the type of the reaction chamber is further provided. Through the selection of the tube furnace, the tube furnace 1s provided with a first heating zone and a second heating zone, which can heat the first precursor and the second precursor respectively and is more convenient to use.
In this embodiment, the type of carrier gas is further provided, which serves to guide the first gas phase source material and the second gas phase source material by providing hydrogen and/or argon. On the other hand, it can protect the chemical vapor deposition reaction between the first vapor source material and the second vapor source material, and can improve the quality of the material layer.
Embodiment 5 As shown in Fig. 5, an embodiment of the present invention provides a method for preparing a uniform material layer based on chemical vapor deposition, which includes: Step 502: Place the substrate and the stage in the reaction chamber, the substrate is arranged on the stage, and the growth surface of the substrate deviates from the stage; Step 504: Provide a first gas phase source material and a second gas phase source material into the reaction chamber; Step 506: The temperature of the substrate is adjusted to a third preset temperature through the reaction chamber for a first preset time, so that the first gas phase source substance and the second gas phase source substance undergo a vapor deposition reaction to form a material layer on the growth surface.
The first preset time 1s 3 min to 20min.
In this embodiment, a specific step of forming a material layer on the growth surface is further provided. By adjusting the temperature to a third preset temperature and continuing for a first preset time, it is ensured that the vapor deposition reaction between the first vapor source substance and the second vapor source substance is carried out smoothly, and a uniform and high-quality material layer can be formed on the growth surface.
Specifically, the third preset temperature can be selected based on the types of the first precursor and the second precursor or material layer, and the third preset temperature 1s located at a temperature which is beneficial to or can promote the vapor deposition reaction between the first vapor source material and the second vapor source material.
In this embodiment, by selecting the first preset time, it is ensured that there is enough time for the vapor deposition reaction between the first vapor source material and the second vapor source material to form a material layer on the growth surface of the substrate.
Particular embodiments As shown in Figs.6- 9, an embodiment of the present invention provides a method for preparing a uniform material layer based on chemical vapor deposition. as shown in Fig.6, the method for preparing a uniform material layer based on chemical vapor deposition includes: Step 602: Place the substrate and the stage in the reaction chamber, the substrate is arranged on the stage, and the growth surface of the substrate deviates from the stage; Step 604: Provide a first gas phase source material and a second gas phase source material into the reaction chamber, and form a material layer on the growth surface.
As shown in Fig. 7, the arrows on both sides of the tube furnace 12 in Fig. 7 indicate the inlet and outlet directions of the carrier gas, and the arrow direction above the substrate 8 indicates the setting direction of the growth surface of the substrate 8. This embodiment is suitable for, but not limited to, the growth of transition metal sulfides. In this embodiment, taking molybdenum disulfide as an example, a proper amount of sulfur powder is taken as the first precursor 16 and placed in the second quartz boat 14. On the first quartz boat 1002 introduced downstream of the carrier gas, the first quartz boat 1002 and quartz piece 1004 are placed as the stage 10, and molybdenum trioxide is placed on the quartz piece 1004 as the second precursor 18. The first quartz boat 1002 and the second quartz boat 14 are respectively placed in the first heating zone 1202 and the second heating zone 1204 of the tubular furnace 12, and a proper amount of argon gas is introduced as carrier gas, and the first heating zone 1202 and the second heating zone 1204 are heated to a temperature suitable for the growth of molybdenum disulfide respectively, and then kept for a period of time, and after the reaction is finished, the two-dimensional material with uniform growth and high quality is naturally cooled to room temperature under the protection of the carrier gas.
As shown in Fig.9, in the prior art, the substrate 8' is directly inverted on the quartz boat, and the growth surface of the substrate 8' faces the quartz boat. as shown in Fig.8, in this embodiment, the substrate 8 is placed on the quartz piece 1004, and the growth surface of the substrate 8 deviates from the quartz piece. Comparing Fig. 8 with Fig. 9, it can be seen that the airflow velocity distribution on the growth surface of substrate 8 and substrate 8' is obviously different. in the existing method, the airflow velocity at the part (edge part) where the growth surface is in contact with the quartz boat is obviously different from that in the middle area. uneven airflow distribution leads to uneven distribution of the two- dimensional materials growing on the growth surface, which will also affect the quality of the two-dimensional materials growing. however, in the method of this embodiment, the growth surface is placed on the quartz 1004 with the airflow velocity on the surface.
In the description of the present invention, the term "multiple" means two or more. Unless otherwise clearly defined, the orientation or positional relationship indicated by the terms "upper" and "lower" is based on the orientation or positional relationship shown in the drawings, which is only for the convenience of describing the present invention and simplifying the description, but does not indicate or imply that the referred devices or elements must have a specific orientation, be constructed and operated in a specific orientation, so it cannot be understood as limiting the present invention. The terms "connection", "installation" and "fixed" should be understood in a broad sense. For example, "connection" can be a fixed connection, a detachable connection or an integral connection; They can be connected directly or indirectly through an intermediate medium. For ordinary technicians in the field, the specific meanings of the above terms in the present invention can be understood according to specific situations.
In the description of this specification, descriptions of the terms "one embodiment", "some embodiments", "specific embodiments", etc. mean that specific features, structures, materials or characteristics described in connection with this embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic expressions of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner.
The above 1s only a preferred embodiment of the present invention, and 1s not used to limit the present invention. For those skilled in the art, the present invention can be modified and varied. Any modification, equivalent substitution, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims (10)

CLAIMS:
1. A preparation method of a uniform material layer based on chemical vapor deposition, comprising the following steps: placing a substrate and an object stage in a reaction chamber, wherein the substrate is arranged on the object stage, and the growth surface of the substrate deviates from the object stage; providing a first gas phase source substance and a second gas phase source substance into the reaction chamber, and forming a material layer on the growth surface.
2. The method for preparing a uniform material layer based on chemical vapor deposition according to claim 1, wherein placing a substrate and a stage in a reaction chamber, the substrate is arranged on the stage, and the growth surface of the substrate deviates from the stage comprising the following content: placing a first quartz boat in a reaction chamber; covering a heat-resistant sheet on the first quartz boat; placing a substrate on the heat-resistant sheet, wherein the growth surface of the substrate deviates from the heat-resistant sheet.
3. The method for preparing uniform material layer based on chemical vapor deposition according to claim 2, wherein the heat-resistant sheet is a quartz plate.
4. The method for preparing a uniform material layer based on chemical vapor deposition according to claim 1, wherein providing the first gas phase source substance and the second gas phase source substance into the reaction chamber comprises the following steps: placing a first precursor and a second precursor in a reaction chamber;
heating the first precursor to a first preset temperature through a reaction chamber to generate the first gas phase source substance: heating the second precursor to a second preset temperature through a reaction chamber to generate the second gas phase source substance; introducing carrier gas into the reaction chamber.
5. The method for preparing a uniform material layer based on chemical vapor deposition according to claim 4, wherein placing the first precursor and the second precursor in the reaction chamber comprises the following steps: setting a second quartz boat in the reaction chamber; setting a first precursor in the second quartz boat; placing the second precursor on the object stage; wherein the second precursor is located between the substrate and the first precursor, and the carrier gas is introduced through one end of the reaction chamber close to the second quartz boat.
6. The method for preparing a uniform material layer based on chemical vapor deposition according to claim 5, wherein the reaction chamber is a tubular furnace, and the tubular furnace comprises a first heating zone and a second heating zone, and the supplying the first gas phase source material and the second gas phase source material to the upper part of the reaction chamber comprises the following steps: setting the second quartz boat bearing the first precursor in the first heating zone, and setting the stage bearing the second precursor in the second heating zone; adjusting the heating temperature of the first heating zone to a first preset temperature through the tube furnace to generate the first gas phase source substance;
adjusting the heating temperature of the second heating zone to a second preset temperature through the tube furnace to generate the second gas phase source substance: introducing carrier gas through one end of the tubular furnace close to the first heating zone.
7. The method for preparing uniform material layer based on chemical vapor deposition according to any one of claims 4 to 6, wherein the carrier gas is hydrogen and/or argon.
8. The method for preparing a uniform material layer based on chemical vapor deposition according to any one of claims 1 to 6, wherein forming a material layer on the growth surface comprises the following steps: adjusting the temperature of the substrate to a third preset temperature by the reaction chamber for a first preset time, so that the first gas-phase source substance and the second gas-phase source substance carry out vapor deposition reaction, and forming a material layer on the growth surface.
9. The method for preparing uniform material layer based on chemical vapor deposition according to claim 8, wherein the first preset time is 3 minutes to 20 minutes.
10. The method for preparing uniform material layer based on chemical vapor deposition according to any one of claims 4 to 6, wherein the second precursor is metal oxide, the first precursor is at least one of sulfur powder, selenium powder and tellurium powder, and the second preset temperature 1s between 600 and 850°C.
LU500345A 2019-12-23 2020-12-15 Preparation method of uniform material layer based on chemical vapor deposition LU500345B1 (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911336814.1A CN110983297A (en) 2019-12-23 2019-12-23 Method for preparing uniform material layer based on chemical vapor deposition

Publications (1)

Publication Number Publication Date
LU500345B1 true LU500345B1 (en) 2021-07-07

Family

ID=70074632

Family Applications (1)

Application Number Title Priority Date Filing Date
LU500345A LU500345B1 (en) 2019-12-23 2020-12-15 Preparation method of uniform material layer based on chemical vapor deposition

Country Status (3)

Country Link
CN (1) CN110983297A (en)
LU (1) LU500345B1 (en)
WO (1) WO2021129450A1 (en)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110983297A (en) * 2019-12-23 2020-04-10 重庆大学 Method for preparing uniform material layer based on chemical vapor deposition
CN113278949B (en) * 2021-04-16 2022-05-20 中国计量大学 Preparation method for single-layer molybdenum selenide sulfide alloy with adjustable components
CN114411148B (en) * 2021-12-29 2024-05-07 浙江大学杭州国际科创中心 Two-dimensional material, two-dimensional material alloy and two-dimensional material heterojunction preparation method
CN114737170B (en) * 2022-04-15 2024-01-19 北京格安利斯气体管道工程技术有限公司 Gas pipeline reactor for chemical vapor deposition, material prepared by using same and application of material
CN115108580B (en) * 2022-05-11 2024-03-05 中国科学院长春光学精密机械与物理研究所 Gallium oxide micron line preparation method, solar blind ultraviolet detector and preparation method thereof

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2908311C3 (en) * 1979-03-03 1986-07-31 Schott Glaswerke, 6500 Mainz Method and device for the continuous production of preforms for communication fibers with a gradient profile of the refractive index in the light-guiding core
WO2015031461A1 (en) * 2013-08-28 2015-03-05 Massachusetts Institute Of Technology Seed for metal dichalcogenide growth by chemical vapor deposition
CN104746137B (en) * 2015-03-26 2017-06-06 厦门烯成石墨烯科技有限公司 A kind of preparation method of the molybdenum disulfide film of stratiform
CN109321897B (en) * 2017-07-31 2022-01-07 北京北方华创微电子装备有限公司 Atomic layer deposition system and method
CN108423643A (en) * 2018-04-17 2018-08-21 福州大学 A method of bismuth selenide nanometer sheet being prepared in mica substrate by controlling gas flow
CN109023296B (en) * 2018-08-06 2020-08-25 华东师范大学 Method for growing molybdenum-tungsten-selenium alloy on fluorophlogopite substrate through chemical vapor deposition
CN109999850A (en) * 2019-04-23 2019-07-12 福州大学 A kind of orthorhombic phase group-III chalcogenide catalysis material and preparation method
CN110451564B (en) * 2019-08-01 2022-03-18 复旦大学 Preparation method of monolayer molybdenum disulfide based on substrate vulcanization pretreatment
CN110512194A (en) * 2019-08-21 2019-11-29 武汉工程大学 Star-like microwave plasma CVD device and the method for preparing large-area two-dimensional material
CN110983297A (en) * 2019-12-23 2020-04-10 重庆大学 Method for preparing uniform material layer based on chemical vapor deposition

Also Published As

Publication number Publication date
WO2021129450A1 (en) 2021-07-01
CN110983297A (en) 2020-04-10

Similar Documents

Publication Publication Date Title
LU500345B1 (en) Preparation method of uniform material layer based on chemical vapor deposition
Jackson et al. Optimizing AlF3 atomic layer deposition using trimethylaluminum and TaF5: Application to high voltage Li-ion battery cathodes
JP2002508298A (en) Growth of very uniform silicon carbide epitaxial layers
US20120213933A1 (en) Formation of Selenide, Sulfide or Mixed Selenide-Sulfide Films on Metal or Metal Coated Substrates
Jo et al. Formation of large-area MoS2 thin films by oxygen-catalyzed sulfurization of Mo thin films
Bergunde et al. Heat transfer and mass transport in a multiwafer MOVPE reactor: modelling and experimental studies
CN106835071A (en) A kind of preparation method of CVD silicon carbide material
CN110835747B (en) Method for regulating and controlling morphology and defects of molybdenum disulfide through temperature
CN105463577B (en) The manufacturing method and manufacturing device of group III-nitride crystal
CN110373636B (en) Preparation method of molybdenum silicide transition metal compound film material
CN115156524B (en) Ectopic nucleation double-layer MoS2Nanosheets and preparation method thereof
JP2005209766A (en) Method for manufacturing oxide film containing hafnium
CN102560400A (en) Method for doping silicon-based film by eutectic growth
CN112760613B (en) Preparation method of carbon-doped molybdenum disulfide nano material
KR100249825B1 (en) Method of copper chemical vapor deposition using metalorganic precursor
JP4363383B2 (en) Raw material liquid for metal organic chemical vapor deposition method and method for producing Hf-Si-containing composite oxide film using the raw material liquid
CN113201726B (en) Preparation method of two-dimensional material
JPH03104871A (en) Production of thin film by magnetic field microwave plasma cvd method
CN109023300B (en) Gadolinium zirconate film with columnar crystal-like and preparation method thereof
CN103928291B (en) The ameliorative way of semiconductor surface resistance homogeneity
TWI235422B (en) Manufacturing method for semiconductor device
TWI803056B (en) Horizontal Plasma Assisted Chemical Vapor Deposition System
CN116497436B (en) Silicon carbide preparation method and prepared silicon carbide crystal
WO2024147339A1 (en) Sic-containing film, and method for manufacturing same
JP2018044206A (en) Method of forming solid electrolyte membrane

Legal Events

Date Code Title Description
FG Patent granted

Effective date: 20210707