CN119020757B - Solid-state source plasma enhanced chemical vapor deposition equipment and method - Google Patents
Solid-state source plasma enhanced chemical vapor deposition equipment and method Download PDFInfo
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- CN119020757B CN119020757B CN202411489122.1A CN202411489122A CN119020757B CN 119020757 B CN119020757 B CN 119020757B CN 202411489122 A CN202411489122 A CN 202411489122A CN 119020757 B CN119020757 B CN 119020757B
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- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 title claims abstract description 27
- 239000007787 solid Substances 0.000 claims abstract description 161
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- 239000002243 precursor Substances 0.000 claims abstract description 76
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- 238000011144 upstream manufacturing Methods 0.000 claims abstract description 7
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- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 7
- 229910052733 gallium Inorganic materials 0.000 claims description 7
- 238000004891 communication Methods 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 4
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- 229910001195 gallium oxide Inorganic materials 0.000 description 9
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- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
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- 238000007086 side reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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
- C23C16/50—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 using electric discharges
- C23C16/505—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 using electric discharges using radio frequency discharges
-
- 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
- C23C16/45563—Gas nozzles
- C23C16/45565—Shower nozzles
-
- 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)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
本发明属于化学气相沉积技术领域，公开了一种固态源等离子体增强化学气相沉积设备及方法，设备包括：加热装置设置于真空腔室外壁并与固态源蒸发器位置对应；固态源蒸发器为封闭结构，其输气端口与气体喷淋头的中心线以及载气通气孔位于同一水平线；反应气输送装置与气体喷淋头连通；托台设置于气体喷淋头的一侧，托台的中心点与气体喷淋头的中心线位于同一水平线，且托台的倾斜面上设置有衬底；等离子体激活装置设置于真空腔室的外壁且位于固态源蒸发器上游；衬底用于接收沉积其上的呈等离子体状态的反应气体和气态分子。本发明可避免固态前驱体蒸发或升华所得气态分子与反应气体过早反应，改善了沉积生长过程中薄膜的表面平整度和晶体质量。
The present invention belongs to the technical field of chemical vapor deposition, and discloses a solid source plasma enhanced chemical vapor deposition device and method, the device comprises: a heating device is arranged on the outer wall of a vacuum chamber and corresponds to the position of a solid source evaporator; the solid source evaporator is a closed structure, and its gas delivery port is located at the same horizontal line as the center line of a gas shower head and a carrier gas vent; a reaction gas delivery device is connected to the gas shower head; a support is arranged on one side of the gas shower head, the center point of the support is located at the same horizontal line as the center line of the gas shower head, and a substrate is arranged on the inclined surface of the support; a plasma activation device is arranged on the outer wall of the vacuum chamber and located upstream of the solid source evaporator; the substrate is used to receive the reaction gas and gaseous molecules in a plasma state deposited thereon. The present invention can avoid premature reaction of gaseous molecules obtained by evaporation or sublimation of a solid precursor with the reaction gas, and improve the surface flatness and crystal quality of the film during the deposition growth process.
Description
Technical Field
The invention belongs to the technical field of chemical vapor deposition, and particularly discloses solid source plasma enhanced chemical vapor deposition equipment and a method.
Background
The conventional chemical vapor deposition (Chemical Vapor Deposition, CVD) is a technique for forming a solid thin film by chemical reaction of a gas on a surface, and the basic principle is that a gaseous precursor is converted into a solid deposit by chemical reaction, and the solid thin film is deposited on the surface of a substrate, and the reaction mechanism involves gas phase reaction, thermodynamic equilibrium, mass transfer process, and the like.
The traditional chemical vapor deposition method only can use a gas phase reaction precursor, which greatly limits the range of the depositable materials, and most of the gas phase precursor materials are expensive and have different degrees of dangers, meanwhile, byproducts are generated, the byproducts can generate reverse reaction or other side reactions to influence the quality of the deposited film, and the byproducts also have dangers and environmental pollution.
Disclosure of Invention
The invention aims to provide solid source plasma enhanced chemical vapor deposition equipment and a method thereof, which are used for solving the technical problems of limited range of materials which can be deposited, high price, high risk, poor quality of deposited films caused by produced byproducts and the like existing in the prior chemical vapor deposition by using a vapor reaction precursor.
The first aspect of the invention provides a solid source plasma enhanced chemical vapor deposition device, which comprises a reaction gas conveying device, a heating device, a plasma activating device, a solid source evaporator arranged in a vacuum chamber, a gas spray head and a support table;
the heating device is arranged on the outer wall of the vacuum chamber, corresponds to the position of the solid source evaporator and is used for providing evaporation or sublimation heat for the solid precursor in the solid source evaporator;
The solid source evaporator is a closed structure comprising a carrier gas vent hole and a carrier gas port, wherein the carrier gas port, the central line of the gas spray header and the carrier gas vent hole are positioned on the same horizontal line;
the reaction gas conveying device is communicated with the gas spray header and is used for conveying reaction gas to the gas spray header;
The supporting table is arranged on one side of the gas spraying head, the center point of the supporting table and the center line of the gas spraying head are positioned on the same horizontal line, and a substrate is arranged on the inclined surface of the supporting table;
the plasma activating device is arranged on the outer wall of the vacuum chamber and is positioned at the upstream of the solid source evaporator and is used for activating the gas in the vacuum chamber into plasma;
the substrate is configured to receive the reactive gas and the gaseous molecules in a plasma state deposited thereon.
Preferably, the inclination angle of the saddle is smaller than 45 degrees or is horizontally arranged.
Preferably, the gas delivery port of the solid source evaporator is a flat port.
Preferably, a carrier gas delivery device is also included;
the carrier gas delivery device is communicated with the solid source evaporator and is used for delivering carrier gas to the solid source evaporator.
Preferably, the carrier gas delivery device comprises a first delivery tube and a gas flow control device;
The first conveying pipe is connected with a carrier gas vent hole of the solid source evaporator;
the gas flow control device is communicated with the first conveying pipe and is used for controlling the flow of carrier gas in the first conveying pipe.
Preferably, the reaction gas delivery means comprises a second delivery tube;
the second conveying pipe is communicated with the gas spray header;
The gas flow control device is also communicated with the second conveying pipe and is used for controlling the flow of the reaction gas in the second conveying pipe.
Preferably, the gas spray header is of an annular structure, and a plurality of exhaust holes are formed in the inner annular side of the annular structure.
Preferably, the horizontal distance between the gas delivery port of the solid source evaporator and the center point of the gas spray header is less than 17 cm;
The horizontal distance between the gas delivery port of the solid source evaporator and the center point of the gantry is less than 20 cm.
The second aspect of the present invention provides a solid-state source plasma enhanced chemical vapor deposition method based on the solid-state source plasma enhanced chemical vapor deposition apparatus, comprising:
Step 1, placing a solid precursor in a solid source evaporator positioned in a vacuum chamber, wherein the solid precursor is gallium metal;
Step 2, vacuumizing the vacuum chamber, and then evaporating or sublimating the solid precursor by using a heating device to generate gaseous molecules;
And step 3, starting a plasma activating device, introducing carrier gas with preset flow into the solid source evaporator, and introducing reaction gas with preset flow into the gas spray header, so that the pressure in the vacuum chamber is maintained at a preset value for a certain time, and a film deposited on the substrate is obtained.
Preferably, the step 3 specifically includes:
And starting a plasma activating device, introducing carrier gas with preset flow into the solid source evaporator, introducing reactive gas with preset flow into the gas spray head, and introducing inert mixed gas into the vacuum chamber, so that the pressure in the vacuum chamber is maintained at a preset value for a certain time, and a film deposited on the substrate is obtained.
Compared with the prior art, the solid source plasma enhanced chemical vapor deposition equipment and the method have the following beneficial effects:
The invention uses the solid precursor as the precursor source, and the solid precursor is generally more stable at normal temperature and is easy to store and process, so that the possible problems of leakage and degradation of the gaseous precursor in the transportation and storage processes can be avoided. Meanwhile, the solid precursor has higher purity, so that the introduction of impurities can be reduced, fewer byproducts are generated in the chemical reaction process, and the quality and performance of the film can be improved.
The solid source evaporator is a closed structure comprising the carrier gas vent hole and the gas transmission port, so that the premature reaction of gaseous molecules obtained by evaporation or sublimation of the solid precursor and the reaction gas can be avoided, the utilization efficiency of the solid precursor is improved, and the surface flatness and the crystal quality of the film in the deposition growth process are also obviously improved. After the reaction is finished, the method can also effectively prevent the solid precursor from continuing to evaporate and diffuse, and avoid the problem of uneven surface of the film caused by the continuous evaporation and diffusion.
Drawings
FIG. 1 is a schematic diagram of a solid source plasma enhanced chemical vapor deposition apparatus according to an embodiment of the present invention.
Fig. 2 is a schematic structural diagram of a vacuum chamber according to an embodiment of the invention.
Fig. 3 is a schematic structural diagram of a solid source evaporator according to an embodiment of the invention.
Fig. 4 is a schematic structural view of a pallet with an inclination angle of 15 ° according to an embodiment of the present invention.
Fig. 5 is a schematic structural view of a pallet with an inclination angle of 30 ° according to an embodiment of the present invention.
Fig. 6 is a schematic structural diagram of a gas shower head according to an embodiment of the present invention.
FIG. 7 is a schematic view of a flange structure according to an embodiment of the present invention.
Fig. 8 is an SEM image of a gallium oxide thin film obtained according to an embodiment of the present invention.
Fig. 9 is an XRD pattern of a gallium oxide thin film obtained in the example of the present invention.
Fig. 10 is an SEM image of the gallium oxide thin film obtained in the comparative example.
Fig. 11 is an XRD pattern of the gallium oxide thin film obtained in the comparative example.
In the figure, the vacuum chamber is 1, the gas spray head is 2, the tray is 3, the solid source evaporator is 4, the carrier gas vent hole is 41, the gas transmission port is 42, the heating device is 5, the first conveying pipe is 6, the gas flow control device is 7, the plasma activating device is 8, the second conveying pipe is 9, the flange is 10, the vacuum system is 11, the vent port is 12, the sample delivery port flange is 13, and the sample delivery port blind plate is 14.
Detailed Description
The following describes specific embodiments of the present invention in detail. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
The embodiment of the invention provides solid source plasma enhanced chemical vapor deposition equipment, which is shown in fig. 1 to 7, and comprises a reaction gas conveying device, a heating device 5, a plasma activating device 8, a solid source evaporator 4, a gas shower head 2 and a supporting table 3, wherein the solid source evaporator 4, the gas shower head 2 and the supporting table 3 are arranged in a vacuum chamber 1.
The heating device 5 is disposed on the outer wall of the vacuum chamber 1 and corresponds to the position of the solid source evaporator 4, and is used for providing heat of evaporation or sublimation for the solid precursor in the solid source evaporator 4.
The solid source evaporator 4 is a closed structure comprising a carrier gas vent hole 41 and a gas transmission port 42, the gas transmission port 42 is positioned on the same horizontal line with the central line of the gas spray header 2 and the carrier gas vent hole 41, and the solid source evaporator 4 is used for outputting gaseous molecules generated by the solid precursor through the gas transmission port 42 under the drive of the carrier gas input into the carrier gas vent hole 41.
The reaction gas conveying device is communicated with the gas spray header 2 and is used for conveying the reaction gas to the gas spray header 2.
The saddle 3 is arranged at one side of the gas spray header 2, the center point of the saddle 3 and the center line of the gas spray header 2 are positioned on the same horizontal line, and a substrate is arranged on the inclined surface of the saddle 3.
A plasma activation device 8 is provided on the outer wall of the vacuum chamber 1 immediately upstream of the solid source evaporator 4 for activating the gas in the vacuum chamber 1 into plasma.
The substrate is configured to receive the reactive gas and the gaseous molecules in a plasma state deposited thereon.
In the embodiment of the invention, the solid precursor is used as a precursor source, sublimated or evaporated into a gaseous precursor by heating or other modes, and chemical vapor deposition is carried out by utilizing the solid precursor, so that the types of the precursor and the deposited film can be effectively expanded, and a feasible alternative method is provided for the precursor material which is difficult to exist in a gaseous form or is unstable. The sublimation or evaporation temperature of the solid precursor is 50-1100 ℃, and the constant evaporation of the solid precursor is required to be ensured.
The invention uses the solid precursor as the precursor source, and the solid precursor is generally more stable at normal temperature and is easy to store and process, so that the possible problems of leakage and degradation of the gaseous precursor in the transportation and storage processes can be avoided. Because the solid precursor has higher purity, the introduction of impurities can be reduced, and fewer byproducts are generated in the chemical reaction process, so that the quality and performance of the film can be improved.
The equipment of the invention does not simply place the solid precursor at the upstream of the substrate, and then directly introduces the carrier gas and the reaction gas into the reactor chamber (horizontal tubular heating furnace) in a vacuum state for chemical vapor deposition, and the reason is that gaseous molecules generated by the solid precursor and the reaction gas can react in advance to influence the evaporation and gasification efficiency and speed of the solid precursor, and also can generate byproducts to influence the purity of the film. The reaction of gaseous molecules generated by the solid precursor with the reaction gas also reduces the evaporation amount of the solid precursor, thereby directly affecting the growth rate of the film, leading to instability of the thickness or quality of the film, and further affecting the performance and consistency thereof. In addition, after the reaction is finished, the temperature is difficult to quickly reduce, and the solid precursor still can continuously evaporate, so that the surface of the film is rough and uneven, the film thickness is uneven, and the performance of the film is further influenced.
The solid source evaporator 4 is of a closed structure comprising the carrier gas vent hole 41 and the gas transmission port 42, so that the premature reaction of gaseous molecules obtained by evaporation or sublimation of the solid precursor and the reaction gas can be avoided, the utilization efficiency of the solid precursor is improved, and the surface flatness and the crystal quality of the film in the deposition growth process are also obviously improved. After the reaction is finished, the solid source evaporator 4, the adopted gas conveying mode and the conveying end position can also effectively prevent the solid precursor from continuously evaporating and diffusing, and avoid the problem of uneven surface of the film caused by the continuous evaporation and diffusion.
The temperature on the solid state source evaporator 4 of the present embodiment is provided by the heating device 5 and is collected in real time using thermocouple contacts. The heating device 5 according to the embodiment of the present invention can also provide heat to the pallet 3 at the same time.
The solid source evaporator 4 is disposed in the vacuum chamber 1, and is made of quartz, and has a structure as shown in fig. 3, in which a carrier gas vent 41 is disposed at one end, and a gas delivery port 42 is disposed at the other end. The carrier vent 41 and the gas delivery port 42 are in the same horizontal plane, so that the carrier gas fully carries the gaseous molecules generated by the solid precursor in the transmission process, and the flow rate of the carrier gas in the carrier gas vent 41 can be controlled, so that the reaction quantity of the gaseous molecules participating in the reaction can be controlled. The gas delivery port 42 is a rectangular flat port, and then the heating device 5 is used for heating to evaporate or sublimate the solid precursor into a gaseous state, and the gaseous molecules are delivered out through the carrier gas. When no carrier gas is transferred into the solid source evaporator 4, the solid source evaporator 4 is of a closed structure, so that gaseous molecules in the solid source evaporator 4 are not output to the gas delivery port 42, and therefore do not participate in chemical reactions in advance. The solid precursor is arranged in the solid source evaporator 4 and protected by the internal carrier gas, so that the accidental reaction of generated gaseous molecules and reaction gas is effectively avoided, and the purity and the utilization efficiency of the precursor are ensured.
According to the embodiment of the invention, the gas transmission port 42 of the solid source evaporator 4 is set to be a flat port, so that the circulation efficiency of gaseous molecules can be greatly improved and the waste of the gaseous molecules can be reduced. First, since the port shape is flat, the flow area of the gaseous molecules can be increased, and the resistance of the gaseous molecules at the outlet can be reduced, so that the gaseous molecules can more smoothly flow out of the solid source evaporator 4. The design is beneficial to reducing the residence time of the gaseous molecules at the ports, improving the flow speed of the gaseous molecules and further improving the efficiency of the whole reaction system. Second, the use of flat ports can reduce wastage of gaseous molecules. The flat design can ensure that gaseous molecules are distributed more uniformly when flowing out, so that gaseous molecules are prevented from accumulating or forming vortex at the outlet, and the waste of gas is reduced.
In order to facilitate discharging, the embodiment of the invention is provided with a material port on the upper surface of the solid source evaporator 4, and a material plug is used for sealing the solid precursor so that gaseous molecules obtained by evaporation or sublimation can only be output from the flat port in order to prevent the unoriented escape of the solid precursor.
The embodiment of the invention can also use the heating device 5 to jointly control the temperature of the substrate on the solid source evaporator 4 and the supporting table 3, and no temperature area is arranged between the solid source evaporator 4 and the supporting table 3, thereby avoiding chemical reaction between gaseous molecules and reaction gases outside the substrate and accurately controlling the deposition position.
During chemical vapor deposition, the vapor flow and mass transfer within the vacuum chamber 1 is critical to the uniformity and quality of the deposited film. If the flow is uneven or the mass transfer effect is poor, insufficient deposition of the film locally or a change in the composition thereof may be caused. The substrate placement will affect the deposition effect of the thin film, and in the embodiment of the present invention, the inclination angle of the supporting table 3 is defined to be smaller than 45 ° or placed horizontally. Illustratively, the tilt angle may be 15 °, 35 °, 45 °, and the like. The use of a angled pallet 3 is preferred in the present invention because the angled pallet 3 allows for more uniform deposition of a thin film on a substrate.
The cradle 3 of the embodiment of the invention is preferably a quartz cradle because quartz has the advantages of high temperature resistance, corrosion resistance, thermal stability, and the like.
In order to improve the deposition efficiency, a plurality of substrate grooves are sequentially formed along the inclined surface on the supporting table 3, and each substrate groove can be internally provided with a substrate. Illustratively, as shown in fig. 4 and 5, 3 substrate grooves are provided on the stage 3.
In chemical vapor deposition, the nucleation and growth stages require precise control of reaction conditions to ensure the crystalline quality, crystal plane orientation and defect control of the deposited film, especially on large-sized or complex-shaped substrate surfaces, which can lead to film thickness variations or quality instability, ultimately affecting film performance and uniformity. Therefore, the apparatus of the embodiment of the present invention further comprises a carrier gas delivery device, which is in communication with the carrier gas vent 41 of the solid source vaporizer 4, for delivering the carrier gas to the solid source vaporizer 4.
The carrier gas delivery device comprises a first delivery pipe 6 and a gas flow control device 7, wherein the first delivery pipe 6 is communicated with a carrier gas vent 41 of the solid source evaporator 4, and the gas flow control device 7 is communicated with the first delivery pipe 6 and is used for controlling the flow of carrier gas in the first delivery pipe 6.
The first conveying pipe 6 is a quartz air duct, the quartz air duct is inserted into the carrier gas vent hole 41 of the solid source evaporator 4, and illustratively, the diameter of the inner wall of the carrier gas vent hole 41 of the solid source evaporator 4 is the same as the diameter of the outer wall of the quartz air duct, so that the quartz air duct is inserted into the carrier gas vent hole 41 of the solid source evaporator 4, and the air tightness and the stability of gas transmission are ensured.
The gas flow control device 7 consists of a flowmeter, a singlechip or a programmable controller, can precisely control the flow of carrier gas, and correspondingly, also precisely control the flow of gaseous molecules which subsequently participate in chemical reaction in the solid source evaporator 4, thereby ensuring the crystallization quality, crystal face orientation and the like of the deposited film.
The reaction gas conveying device comprises a second conveying pipe 9, wherein the second conveying pipe 9 is communicated with the gas spray header 2, and the gas flow control device 7 is also communicated with the second conveying pipe 9 and is used for controlling the flow of reaction gas in the second conveying pipe 9.
The invention uses the second conveying pipe 9 to convey the reaction gas to the gas spray header 2, wherein the second conveying pipe 9 is a quartz gas guide pipe, the quartz gas guide pipe is inserted into the gas inlet of the gas spray header 2, and the diameter of the inner wall of the gas inlet of the gas spray header 2 is the same as that of the outer wall of the quartz gas guide pipe, so that the quartz gas guide pipe is inserted into the gas inlet of the gas spray header 2, and the air tightness and the gas transmission stability are ensured.
In order to save cost and reduce the volume of the apparatus of the present invention, the reactant gas delivery apparatus and the carrier gas delivery apparatus of the embodiments of the present invention share the gas flow control device 7. Wherein the gas flow rate control device 7 can precisely control the flow rate of the reaction gas, thereby ensuring the crystallization quality, crystal plane orientation, etc. of the thin film obtained by the deposition of the reaction gas and the gaseous molecules.
The mode of activating the gas in the vacuum chamber 1 into the plasma by the plasma activating device according to the embodiment of the invention can be that radio frequency (13.56 MHz) or very high frequency (40 MHz and 60 MHz) is used, and the 60 MHz very high frequency is higher than the plasma density generated by the conventional 13.56 MHz radio frequency, so that the ion flux can be higher, the vacuum wavelength of the 60 MHz very high frequency is 5m, the standing wave effect is not obvious, and the phenomenon of non-uniformity of the plasma is not caused, therefore, the embodiment of the invention preferably uses the gas in the vacuum chamber 1 activated by the very high frequency.
The invention can realize the accurate control of the gas-solid reaction in the film growth process, can accurately control the reaction rate and the reaction time, and improves the stable supply of the solid precursor and the uniformity of the film growth.
In order to facilitate the supply of the reaction gas from multiple angles and ensure the effective progress of the chemical reaction, the gas shower head 2 of the embodiment of the present invention is designed as an annular structure, as shown in fig. 6, and the inner ring side of the annular structure is provided with a plurality of exhaust holes, and the plurality of exhaust holes are uniformly formed on the inner ring side of the annular structure. At this time, the plurality of exhaust holes formed on the inner ring side of the ring structure are arranged around the gas delivery port 42 of the solid source evaporator 4, so that the reaction gas and the gaseous molecules in the solid source evaporator 4 are uniformly contacted, and further can be deposited on the substrate according to the preset flow to perform full reaction, and the reaction position is located near the plasma activating device, so that a film with better quality can be formed on the substrate. Further, to ensure uniform deposition of the gas, the carrier gas vent 41, the gas delivery port 42, and the center line of the gas shower head 2 and the center of the stage 3 of the solid state source vaporizer of the embodiment of the present invention are positioned on the same horizontal line.
To avoid excessive transfer paths of gaseous molecules generated by evaporation or sublimation of solid precursors in the apparatus of the present invention affecting film formation rates, embodiments of the present invention define a horizontal distance between the gas transfer port 42 of the solid source vaporizer 4 and the center point of the gas showerhead 2 of less than 17 cm, which may be, for example, 0 cm, 3 cm, 5 cm, 10 cm, 12 cm, 15 cm, 17 cm, etc., which may also control the location of the chemical reaction. Further, the present invention also sets the horizontal distance between the gas delivery port 42 of the solid source evaporator 4 and the center point of the gantry 3 to be less than 20 cm, which may be 3 cm, 5 cm, 10 cm, 15 cm, 20 cm, etc., as an example, which is a preferred range for film growth.
The vacuum chamber 1 in the embodiment of the present invention adopts a cylindrical quartz tube, the vacuum condition is realized by the vacuum system 11, and the vacuum system 11 can use the device in the prior art, and the present invention is not described herein. To ensure accuracy and stability of the pressure in the vacuum chamber 1, the embodiment of the present invention provides a vacuum gauge connected to the vacuum chamber 1 to measure the pressure in the vacuum chamber 1. Illustratively, the vacuum gauge may be a Pirani vacuum gauge. The vacuum chamber 1 in the embodiment of the invention needs to ensure that the pressure is below 10 -4 Pa in the initial state, and the pressure is 30 Pa-300 Pa when chemical vapor deposition is performed.
In order to ensure the tightness of the vacuum chamber 1, the first conveying pipe 6 and the second conveying pipe 9 are extended into the vacuum chamber 1 by using the flange 10 arranged at the end part of the vacuum chamber 1, so as to provide conditions for performing a CVD experiment. Illustratively, the flange 10 of the present embodiment is configured as shown in fig. 7, having three vent openings on the front side and one vent opening on the side. The two vent ports on the front surface of the flange 10 are respectively connected with the first conveying pipe 6 and the second conveying pipe 9, specifically, are connected by adopting an O-shaped ring clamping sleeve, and the other vent port 12 on the front surface of the flange 10 is directly communicated with the vacuum chamber 1 and is used for injecting inert mixed gas into the vacuum chamber 1 through the vent ports, regulating the pressure in the vacuum chamber 1 and the partial pressure of gaseous molecules and reaction gas, and ensuring that no interference influence of impurity gas exists in the vacuum chamber 1. An air port on the side of the flange 10 is communicated with the vacuum chamber 1, and is connected with a Pirani vacuum gauge for collecting and controlling the pressure of the vacuum chamber 1.
The solid source plasma enhanced chemical vapor deposition apparatus of the present invention is applicable to various chemical vapor deposition methods including Plasma Enhanced Chemical Vapor Deposition (PECVD), low Pressure Chemical Vapor Deposition (LPCVD), and the like.
The invention provides equipment for controlling the reaction rate of gaseous molecules generated by reaction gas and solid precursor under high vacuum and high temperature environment, which ensures that a film with uniform texture and high quality is deposited on a substrate. The equipment provided by the invention can be used for accurately controlling the inflow amount of gaseous molecules generated by the solid precursor, accurately adjusting the reaction rate and the reaction position, effectively avoiding the uncertainty in the existing film preparation process, and avoiding introducing extra impurities. In addition, the equipment has simple structure and convenient operation, and the process for preparing the film by using the equipment is also very simple.
A second aspect of the embodiment of the present invention provides a solid-state source plasma enhanced chemical vapor deposition method based on the solid-state source plasma enhanced chemical vapor deposition apparatus, including:
Step 1, opening a sample delivery port flange 13 connected with the vacuum chamber 1, placing a solid precursor in a solid source evaporator 4 positioned in the vacuum chamber 1, then placing a gas spray header 2 in the vacuum chamber 1 and at a gas delivery port 42 of the solid source evaporator 4, placing a substrate on a tray table 3 and placing the substrate in the vacuum chamber 1, wherein the gas spray header 2 and the solid source evaporator 4 are arranged at the upstream of the tray table 3. Finally, the sample inlet flange 13 is blocked by using a sample inlet blind plate 14. The solid precursor is gallium metal.
And 2, vacuumizing the vacuum chamber 1, and evaporating or sublimating the solid precursor by using the heating device 5 to generate gaseous molecules.
In the embodiment of the invention, the vacuum chamber 1 is vacuumized, so that the pressure in the vacuum chamber is below 10 -4 Pa.
And 3, starting a plasma activating device 8, introducing carrier gas with preset flow into the solid source evaporator 4, and introducing reaction gas with preset flow into the gas spray header 2, so that the pressure in the vacuum chamber 1 is maintained at a preset value for a certain time, and a film deposited on the substrate is obtained.
Further, in order to adjust the pressure in the vacuum chamber 1 and the partial pressure of gaseous molecules and reaction gas in the vacuum chamber 1, the embodiment of the invention can also introduce inert mixed gas into the vacuum chamber 1 so that the pressure in the vacuum chamber 1 is 30 Pa-300 Pa.
And 4, after the reaction is completed, taking out the support table 3 after the temperature of the vacuum chamber 1 is reduced to the room temperature.
The solid precursor In the embodiment of the invention is a material with the gasification temperature of 50-1100 ℃, and can be one or more of gallium (Ga), indium (In), tin (Sn), lead (Pb), cadmium (Cd), zinc (Zn), sulfur (S), arsenic (As), phosphorus (P), selenium (Se), iodine (I), a compound, an alloy and the like, wherein the reaction gas is one or more of hydrogen, oxygen, methane, nitrogen, ammonia and N 2 O.
The invention puts the solid precursor in the solid source evaporator 4 and utilizes the heating device 5 to evaporate the solid precursor within the temperature range of 50-1100 ℃. In order to prevent the gaseous molecules generated by the solid precursor and the reaction gas from prematurely reacting in the evaporation process and generating byproducts, the device of the invention adopts the gas flow control device 7 to precisely control the flow of the carrier gas and the reaction gas, thereby controlling the reaction quantity and the reaction rate of the gaseous molecules generated by the solid precursor and the reaction gas. The vacuum system 11 ensures that the vacuum chamber 1 reaches the required experimental pressure, and the vacuum chamber 1 adopts a cylindrical quartz tube, so that free molecular flow is formed in a high-vacuum environment. To ensure uniform deposition, the inventive gantry is designed as a gantry 3 with a certain tilt angle. After the experiment is finished, gaseous molecules generated by the solid precursor can be prevented from being continuously diffused and affecting the deposition on the surface of the substrate only by closing the flow of the carrier gas. The solid precursor in the equipment is arranged in the solid source evaporator 4 and protected by the internal carrier gas, so that the accidental reaction of gaseous molecules generated by the solid precursor and reaction gas is effectively avoided, and the purity and the utilization efficiency of the precursor are ensured. The Pirani vacuum gauges are arranged on the flanges 10 at the two ends of the vacuum chamber 1 of the equipment, and the pressure condition of the reaction area can be accurately mastered by monitoring.
The effectiveness of the chemical vapor deposition apparatus and method of the present invention will be verified as follows in the process of preparing gallium oxide (Ga 2O3) thin films.
Examples
Step S1, metallic gallium (Ga) is placed in the solid-state source evaporator 4, and placed in the vacuum chamber 1.
And S2, placing the gas spray header 2 in the vacuum chamber 1 and at the gas transmission port 42 of the solid source evaporator 4.
And S3, placing the sapphire substrate which is washed by absolute ethyl alcohol, acetone, isopropanol and deionized water in sequence on a supporting table 3, and placing the sapphire substrate in a vacuum chamber 1, wherein a gas spray head 2 and a solid source evaporator 4 are arranged at the upstream of the supporting table 3.
Step S4, the internal pressure of the vacuum chamber 1 is pumped to 1X 10 -4 Pa through the vacuum system 11. Next, the solid source evaporator 4 was heated to 820 ℃ using the heating device 5. Subsequently, the plasma activation device 8 was set to a power of 100W, and high purity argon gas of 80 sccm was introduced as a carrier gas into the solid source vaporizer 4 through the gas flow control device 7 to transport gaseous molecules generated from gallium. Meanwhile, high-purity oxygen of 5 sccm is used as a reaction gas to be led into the gas spray header 2 to react with gaseous molecules generated by gallium metal, and the pressure in the vacuum chamber 1 is maintained to be 80 Pa.
And S5, stopping heating after the experimental reaction is performed for 30 min, stopping introducing gas, taking out the support table 3 after the temperature of the vacuum chamber 1 is reduced to the room temperature, and taking out the prepared gallium oxide film.
Fig. 8 is an SEM image of the prepared film, and it can be seen from SEM electron microscope scanning analysis of the above prepared gallium oxide film that the gallium oxide film has a flat surface and a relatively dense film.
Fig. 9 is an XRD pattern of the prepared film, from which it can be seen that the crystal plane orientation is uniform, with only 3 main peaks and no impurity peaks.
Comparative example
The comparative example was carried out by using a conventional PECVD method (plasma excitation power: 100W, temperature: 820 ℃, pressure: 95 Pa, growth time: 30 min, ar/O 2 =80:5), and SEM images of the obtained films are shown in FIG. 10, and XRD images of the obtained films are shown in FIG. 11.
As can be seen from fig. 10, the conventional method and apparatus for preparing gallium oxide thin film prepared the thin film has rugged surface. As can be seen from fig. 11, there are a plurality of hetero peaks in the XRD pattern, indicating that the resulting gallium oxide thin film includes a plurality of crystal plane orientations and does not have uniformity.
The solid source plasma enhanced chemical vapor deposition equipment has the advantages that the reaction conditions can be adjusted in real time in the deposition process, and the growth of the film can be optimized according to actual requirements. The method and the device can effectively reduce the defect density in the film and improve the consistency of the crystallization quality and the crystal face orientation by precisely controlling the inlet amount of gaseous molecules generated by the solid precursor, thereby being beneficial to improving the optical, electrical and mechanical properties of the film and being beneficial to realizing a more stable and predictable production process.
The solid source plasma enhanced chemical vapor deposition equipment of the invention precisely controls the evaporation amount of the solid precursor by adjusting the gas flow of the carrier gas and the temperature of the solid precursor, thereby effectively preventing the premature reaction of gaseous molecules generated by the solid precursor and the reaction gas. Meanwhile, the reaction rate can be stably controlled in the chemical vapor deposition process. The equipment not only improves the utilization efficiency of the solid precursor, but also obviously improves the surface evenness and the crystal quality of the film in the deposition and growth process. After the reaction is finished, other devices have the problem that the temperature cannot be reduced in time and the solid precursor can be continuously evaporated, and the solid source evaporator 4 and the gas conveying mode designed by the invention can also effectively prevent the solid precursor from continuously evaporating and diffusing, so that the problem of uneven surface of the film is avoided. The improvements enable the growth process of the film to be more controllable and stable, and provide important technical support for the preparation of high-quality films.
While the invention has been described in terms of preferred embodiments, it will be understood by those skilled in the art that various changes and modifications can be made without departing from the scope of the invention, and it is intended that the invention is not limited to the specific embodiments disclosed.
Claims (7)
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