MOCVD (Metal Organic Chemical Vapor Deposition) equipment capable of grabbing epitaxial sample at any time as required and use method of MOCVD equipment

Abstract

The invention relates to MOCVD (Metal Organic Chemical Vapor Deposition) equipment capable of grabbing an epitaxial sample at any time as required and a use method of the MOCVD equipment, and belongs to the technical field of metal organic chemical vapor deposition. The MOCVD equipment capable of grabbing the epitaxial sample at any time as required comprises an equipment main body, and further comprises an MOCVD reaction chamber for growth, a sampling chamber and a turnover chamber, and the sampling chamber is embedded into the side wall of the reaction chamber; a sampling control system and a heating system are arranged in the sampling chamber; a cooling system, a heating system and a protection system are arranged in the turnover cavity; the sampling control system comprises a micro mechanical system, an acquisition unit, an analysis unit and a feedback regulation unit. According to the invention, the growth condition of the epitaxial sample is analyzed and recorded through the acquisition unit and the analysis unit; an epitaxial sample meeting the requirement is taken out through a sampling control system and is used for experimental analysis. Therefore, the accuracy of scientific experiments is improved, and the time cost and the economic cost generated in the experiment process are reduced.

Description

Technical Field

[0001] The present invention belongs to the technical field of metal organic chemical vapor deposition, and particularly relates to an MOCVD device capable of grabbing epitaxial samples as needed at any time and a using method thereof. Background Art

[0002] Metal organic chemical vapor deposition (MOCVD) is a growth technology for gas-phase epitaxy on a substrate in a thermal decomposition reaction manner. It is widely used in the fields of semiconductors and optoelectronics due to its advantages such as high growth quality, high stability, and high repeatability.

[0003] Currently, when using an MOCVD device for experimental research, experiments are carried out one furnace batch at a time. This process will introduce some uncertain factors, such as external factors like the heating and cooling process, gas purity, and graphite disks, resulting in the accuracy of the experimental process being restricted, and further increasing the economic cost and time cost of scientific experiments. Summary of the Invention

[0004] The present invention aims to solve the technical problem that the process of using an MOCVD device in the prior art will introduce some uncertain factors, resulting in the accuracy of the experimental process being restricted, and further increasing the economic cost and time cost of scientific experiments, and provides an MOCVD device capable of grabbing epitaxial samples as needed at any time and a using method thereof. The MOCVD device of the present invention can improve the accuracy of experiments, reduce the economic cost and time cost generated during the experiment, and improve the use efficiency of the MOCVD device.

[0005] To solve the above technical problem, the technical solution of the present invention is specifically as follows:

[0006] An MOCVD device capable of grabbing epitaxial samples as needed at any time, including a device main body; further including: a reaction chamber, a sampling chamber, and a turnover chamber; the sampling chamber is located between the reaction chamber and the turnover chamber and is embedded in the side wall of the reaction chamber cavity;

[0007] The reaction chamber is used for growing epitaxial samples;

[0008] The sampling chamber is used for taking out the required samples from the reaction chamber and at the same time placing the samples into the turnover chamber;

[0009] The sampling chamber is internally provided with a heating system and a sampling control system;

[0010] The heating system is used for heating the sampling chamber to ensure the operation of the sampling control system;

[0011] The sampling control system includes a microelectromechanical system, a collection unit, a feedback adjustment unit, and an analysis unit;

[0012] The micro mechanical system includes a micro mechanical sampling device, a mechanical protection device, and a mechanical control system. The micro mechanical sampling device further includes a vacuum pump.

[0013] The acquisition unit is used to acquire the reflectivity, rotation speed, and temperature information of the graphite disk surface.

[0014] The analysis unit determines the working time of the micro mechanical system based on the information provided by the acquisition unit. At the same time, it transmits the growth condition information of the reaction chamber to the feedback regulation unit.

[0015] The feedback regulation unit is used to receive the information from the analysis unit, regulate the temperature, pressure, and atmosphere composition in the sampling chamber to make the atmosphere in the sampling chamber the same as that in the reaction chamber, reducing the changes in the flow field and temperature of the reaction chamber caused by sampling. At the same time, it controls whether the micro mechanical system takes out the epitaxial sample.

[0016] The turnover chamber is used to temporarily store the samples taken out from the reaction chamber. The turnover chamber is equipped with a rapid heating system, a cooling system, and a sample protection system.

[0017] The rapid heating system and the cooling system are respectively used to heat and cool the turnover chamber. The sample protection system is used to introduce a protective gas.

[0018] In the above technical solution, the sampling chamber is provided with gate valves on both sides of the reaction chamber and the turnover chamber. The gate valves are normally closed. The internal width of the sampling chamber ≤ 120 mm, and the internal height ≤ 20 mm.

[0019] In the above technical solution, the heating temperature of the rapid heating system ≤ 1000 °C, and the protective gas introduced by the sample protection system is nitrogen and ammonia.

[0020] In the above technical solution, the micro mechanical sampling device is a micro manipulator.

[0021] In the above technical solution, when the micro mechanical system detects that the gate valve is open, it automatically activates the sampling mode. After receiving the sampling command, the micro mechanical sampling device takes out the required epitaxial sample, and the time used ≤ 0.05 S. After the epitaxial sample is taken out, the acquisition unit feeds back the graphite disk surface information to the MOCVD monitoring system, defaulting that there is no sample at this position, and the epitaxial growth proceeds normally.

[0022] A method for using an MOCVD device that can grab epitaxial samples as needed at any time includes the following steps:

[0023] (1) After the graphite disk is filled with substrates, the graphite disk is transferred into the reaction chamber through the transfer cavity by using the micro mechanical sampling device, and then the MOCVD device starts to run the epitaxial structure program.

[0024] (2) When the epitaxial sample grows to the required stage, the sampling control system located in the sampling chamber starts to prepare for work, and the vacuum pump contained in the micro-mechanical sampling device is turned on;

[0025] (3) The analysis unit of the sampling control system starts to work, analyzing the temperature, atmosphere and pressure information in the reaction chamber; the feedback adjustment unit adjusts the temperature, atmosphere and pressure in the sampling chamber according to the aforementioned information; after the temperature, atmosphere and pressure information in the sampling chamber and the reaction chamber are the same, the valve of the sampling chamber is opened; the acquisition unit acquires the reflectivity information and rotational speed information on the surface of the graphite disk, and at the same time feeds the information back to the analysis unit; the analysis unit determines the sampling time according to the rotational speed information provided by the acquisition unit; distinguishes the epitaxial sample and the graphite disk according to the reflectivity information on the surface of the graphite disk; and then transmits the above information to the feedback adjustment unit, and the feedback adjustment unit decides whether the micro-mechanical sampling device works and the working time;

[0026] (4) After the micro-mechanical sampling device takes out the required epitaxial sample, the valve of the sampling chamber is closed, and the feedback adjustment unit adjusts the atmosphere of the sampling control system to a nitrogen atmosphere or a mixed atmosphere of ammonia and nitrogen; the acquisition unit detects the temperature of the epitaxial sample, and when the temperature ≤ 900 °C and the temperature difference from the turnover room temperature ≤ 50 °C, the sample is transferred to the turnover room;

[0027] (5) When the epitaxial sample is detected in the sampling control system, the rapid heating system of the turnover room starts to heat up, and when the temperature difference from the sample temperature ≤ 50 °C, the sample is transferred to the turnover room; the cooling system of the turnover room starts to work;

[0028] (6) After the sampling control system detects that there is no epitaxial sample in the cavity, nitrogen is filled, and after the temperature ≤ 100 °C and the pressure is maintained at 20 mbar, the air intake device of the sampling control system is closed;

[0029] (7) When the temperature T2 in the turnover room is lower than 30 °C, the epitaxial sample is taken out for test analysis and material characterization.

[0030] The beneficial effects of the present invention are:

[0031] A MOCVD device provided by the present invention that can grab epitaxial samples as needed at any time mainly includes a MOCVD reaction chamber for growth, a sampling chamber and a turnover room, and the sampling chamber is embedded in the side wall of the reaction chamber cavity; a sampling control system and a heating system are arranged inside the sampling chamber, and a cooling system, a heating system and a protection system are arranged inside the turnover room; the sampling control system includes a micro-mechanical system, an acquisition unit, an analysis unit and a feedback adjustment unit. The present invention analyzes and records the growth situation of the epitaxial sample through the acquisition unit and the analysis unit; through the sampling control system, the qualified epitaxial sample is taken out for experimental analysis. Thereby improving the accuracy of scientific experiments and reducing the time cost and economic cost generated during the experiment. Description of the Drawings

[0032] The present invention will be further described in detail below in conjunction with the accompanying drawings and specific embodiments.

[0033] Figure 1 It is a top - view structural schematic diagram of an MOCVD device for an epitaxial sample that can be grabbed as needed at any time according to the present invention;

[0034] Figure 2 It is a top - view structural schematic diagram of the sampling chamber of the present invention;

[0035] Figure 3 It is a front - view structural schematic diagram of the sampling chamber of the present invention;

[0036] Figure 4 It is a top - view structural schematic diagram of the turnover chamber of the present invention;

[0037] The reference numerals in the figures are represented as:

[0038] 1 - growth reaction chamber, 2 - sampling chamber, 3 - turnover chamber, 4 - sampling control system, 5 - TM chamber, 6 - loading and unloading chamber, 7 - valve, 8 - micro - mechanical system, 9 - vacuum pump, 10 - heating system, 11 - gas protection device, 12 - rapid heating system, 13 - cooling system, 14 - sample protection system. Specific embodiments

[0039] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. The described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0040] Embodiment 1

[0041] Refer to Figures 1-4 , and specifically describe an MOCVD device for an epitaxial sample that can be grabbed as needed at any time according to the present invention, including a device main body, and further including a reaction chamber 1, a sampling chamber 2, and a turnover chamber 3; a TM chamber 5 and a loading and unloading chamber 6 are sequentially arranged on one side of the reaction chamber 1; the sampling chamber 2 is located between the reaction chamber 1 and the turnover chamber 3 and is embedded in the side wall of the reaction chamber 1. Valves 7 are provided on both sides of the reaction chamber 1 and the turnover chamber 3, and the valves 7 are in a normally closed state; the internal width of the sampling chamber 2 ≤ 120 mm, and its internal height ≤ 20 mm;

[0042] The reaction chamber 1 is used for growing epitaxial samples;

[0043] The sampling chamber 2 is used to take out the required samples from the reaction chamber 1 and at the same time place the samples into the turnover chamber 3;

[0044] Inside the sampling chamber 2, a heating system 10 and a sampling control system 4 are provided.

[0045] The heating system 10 is used to heat the sampling chamber 2 to ensure the operation of the sampling control system 4. The temperature difference between the sampling chamber 2 and the reaction chamber 1 is ≤ 100 °C. The sampling chamber 2 is cooled by a gas through the installation of a gas protection device 11.

[0046] The sampling control system 4 is mainly used to take out the required samples from the reaction chamber 1 and place the samples into the turnover chamber 3 at the same time. It includes a micro-mechanical system 8, a collection unit, a feedback adjustment unit, and an analysis unit.

[0047] The micro-mechanical system 8 includes a micro-mechanical sampling device, a mechanical protection device, and a mechanical control system. The micro-mechanical sampling device also contains a vacuum pump 9. The micro-mechanical sampling device is a micro-manipulator. When the micro-mechanical system 8 detects that the valve 7 is in the open state, it automatically activates the sampling mode. After receiving the sampling command, the mechanical control system controls the micro-mechanical sampling device to quickly take out the required epitaxial sample, and the time used is ≤ 0.05 s. After the epitaxial sample is taken out, the collection unit feeds back the surface information of the graphite disk to the MOCVD monitoring system, and it is defaulted that there is no sample at this position, and the epitaxial growth proceeds normally.

[0048] The collection unit depends on the real-time monitoring system of the MOCVD equipment and is mainly used to collect the reflectivity of the graphite disk surface, the rotation speed of the graphite disk, and temperature information.

[0049] The analysis unit mainly has two functions. One is to distinguish the graphite disk and the epitaxial sample according to the reflectivity of the information provided by the collection unit and determine the working time of the micro-mechanical system 8. The other is to analyze and determine the growth condition information of the temperature, pressure, and atmosphere composition in the reaction chamber 1, and at the same time transmit the above information to the feedback adjustment unit.

[0050] The feedback adjustment unit is used to receive the information from the analysis unit and adjust the temperature, pressure, and atmosphere composition in the cavity of the sampling control system 4 in the sampling chamber 2 to make the atmosphere in the sampling chamber 2 the same as that in the reaction chamber 1, reducing the changes in the flow field and temperature of the reaction chamber 1 caused by sampling. After the pressure, temperature, and atmosphere are the same as those in the reaction chamber 1, quickly open the valve 7, and the mechanical control system controls the micro-mechanical sampling device of the micro-mechanical system 8 to quickly take out the required sample and return to the home position.

[0051] The turnover chamber 3 is used to temporarily store the samples taken out from the reaction chamber 1. A rapid heating system 12, a cooling system 13 and a sample protection system 14 are provided in the turnover chamber 3; the rapid heating system 12 and the cooling system 13 are respectively used to heat and cool the turnover chamber 3; the sample protection system 14 is used to introduce a protective gas. The heating temperature of the rapid heating system 12 is ≤ 1000 °C, and the gases involved in the sample protection system 14 are nitrogen and ammonia.

[0052] After the epitaxial sample is monitored inside and outside the sampling chamber 1, according to the pressure and temperature information provided by the analysis unit, the rapid heating system 12 and the sample protection system 14 in the turnover chamber 3 start to work, the temperature rises rapidly, nitrogen and ammonia are introduced into the chamber, the valve 7 is opened, and the micro-mechanical system 8 transfers the sample into the turnover chamber 3, and the cooling system 13 in the turnover chamber 3 starts to work. The micro-mechanical system 8 in the sampling chamber 2 returns to the home position, the temperature decreases, nitrogen is filled into the chamber, and the pressure is maintained at 20 mbar. After the temperature of the turnover chamber 3 decreases, the sample is taken for testing and analysis.

[0053] Embodiment 2

[0054] The difference between this embodiment and Embodiment 1 is that the present invention also provides a method for using an MOCVD device that can grab epitaxial samples as needed at any time. The specific operation steps are as follows:

[0055] (1) After the graphite tray is filled with substrates, the graphite tray is transferred into the reaction chamber 1 through the transfer cavity by using the micro-mechanical sampling device, and then the device starts to run the epitaxial structure program;

[0056] (2) After the epitaxial sample grows to the experimental requirement stage, the sampling control system 4 in the sampling chamber 2 starts to prepare for work, and the vacuum pump 9 included in the micro-mechanical sampling device is turned on;

[0057] (3) The analysis unit of the sampling control system 4 starts to work, analyzes information such as the growth temperature, atmosphere (the ratio of ammonia, nitrogen and hydrogen), and growth pressure of the materials in the reaction chamber 1. The feedback adjustment unit quickly adjusts the temperature, atmosphere and pressure in the sampling chamber 2 according to the above growth information; after the growth conditions such as temperature, atmosphere and pressure in the sampling chamber 2 are the same as those in the reaction chamber 1, the valve 7 is quickly opened. The acquisition unit quickly acquires the surface reflectivity and rotation speed of the graphite tray, and at the same time feeds the information back to the analysis unit; the analysis unit distinguishes the difference between the epitaxial sample and the surface of the graphite tray according to the difference in the surface reflectivity of the graphite tray, and confirms the working time (≤ 0.5S) of the micro-mechanical sampling device according to the rotation speed. At the same time, the micro-mechanical sampling device quickly extends out of the sampling chamber 2 to take out the required epitaxial sample.

[0058] (4) After the required epitaxial sample is taken out by the micro-mechanical sampling device, the valve 7 is quickly closed, and the gas protection device 11 starts to work; after the feedback adjustment unit detects that the valve 7 is closed, it monitors the temperature T1 of the sampling chamber 2. When 800 °C ≤ T1 ≤ 1200 °C, the atmosphere in the sampling chamber 2 remains unchanged; when T1 ≤ 800 °C, the atmosphere in the sampling chamber 2 is adjusted to a nitrogen atmosphere or a mixed atmosphere of ammonia and nitrogen.

[0059] (5) When the temperature T1 of the sampling chamber 2 ≤ 900 °C, the rapid heating system 12 of the transfer chamber 3 starts to work; at the same time, nitrogen is introduced into the transfer chamber 3. When the pressure in the transfer chamber 3 is the same as that in the sampling chamber 2 and the temperature difference from the sampling chamber 2 ≤ 50 °C, the valve 7 is opened, and the epitaxial sample is transferred into the transfer chamber 3. The cooling system 13 of the transfer chamber 3 starts to work. At this time, the valve 7 between the transfer chamber 3 and the sampling chamber 2 is not temporarily closed, and the nitrogen introduced into the transfer chamber 3 is used to replace the mixed atmosphere in the sampling chamber 2; when the temperature T2 of the transfer chamber ≤ 500 °C, the valve 7 is closed.

[0060] (6) After the sampling control system 4 detects that there is no epitaxial sample in the sampling chamber 2, nitrogen is filled. After the temperature ≤ 100 °C and the pressure is maintained at 20 mbar; the intake device, the heating system 10 of the sampling control system 4 are closed, and the cooling is stopped.

[0061] (7) When the temperature T2 in the transfer chamber 3 ≤ 30 °C, nitrogen is filled into the transfer chamber 3 to 1 atmosphere, and the outer valve 7 is opened to take out the epitaxial sample for testing analysis and material characterization.

[0062] The preferred embodiments of the present invention disclosed above are only used to help explain the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to only the specific implementation manners. Obviously, many modifications and changes can be made according to the content of this specification. These embodiments are selected and specifically described in this specification to better explain the principle and practical application of the present invention, so that those skilled in the art can well understand and utilize the present invention. The present invention is only limited by the claims and their full scope and equivalents.

Claims

1. A MOCVD device capable of grabbing epitaxial samples at any time as needed, comprising a device body; It is characterized in that Also includes: A reaction chamber (1), a sampling chamber (2) and a turnover chamber (3); the sampling chamber (2) is located between the reaction chamber (1) and the turnover chamber (3), and is embedded in the side wall of the reaction chamber (1); The reaction chamber (1) is used for growing epitaxial samples; The sampling chamber (2) is used to take out the required sample from the reaction chamber (1) and place the sample into the turnover chamber (3); The sampling chamber (2) is provided with a heating system (10) and a sampling control system (4); The heating system (10) is used to heat the sampling chamber (2) to ensure that the sampling control system (4) works; The sampling control system (4) comprises a micro-mechanical system (8), a collection unit, a feedback adjustment unit and an analysis unit; The micromechanical system (8) comprises a micromechanical sampling device, a mechanical protection device and a mechanical control system, and the micromechanical sampling device also comprises a vacuum pump (9); The collection unit is used to collect reflectivity, rotation speed and temperature information of the graphite disk surface; The analysis unit determines the working time of the micro-mechanical system (8) based on the information provided by the acquisition unit; at the same time, the growth condition information of the reaction chamber (1) is transmitted to the feedback adjustment unit; The feedback adjustment unit is used to receive information from the analysis unit, adjust the temperature, pressure and atmosphere composition in the sampling chamber (2), make the atmosphere in the sampling chamber (2) the same as that in the reaction chamber (1), and reduce the flow field and temperature changes in the reaction chamber (1) caused by sampling; at the same time, control whether the micro-mechanical system (8) takes out the epitaxial sample; The turnover chamber (3) is used to temporarily store samples taken out from the reaction chamber (1), and a rapid heating system (12), a cooling system (13) and a sample protection system (14) are provided in the turnover chamber (3); The rapid heating system (12) and cooling system (13) are used to heat and cool the turnover chamber (3) respectively; the sample protection system (14) is used to introduce protective gas.

2. The MOCVD device capable of grabbing epitaxial samples at any time as required according to claim 1, characterized in that: The sampling chamber (2) is provided with gate valves (7) on both sides of the reaction chamber (1) and the turnover chamber (3), and the gate valves (7) are in a normally closed state; the internal width of the sampling chamber (2) is ≤120 mm, and the internal height is ≤20 mm.

3. The MOCVD device capable of grabbing epitaxial samples at any time as required according to claim 1, characterized in that: The heating temperature of the rapid heating system (12) is ≤1000°C, and the protective gas introduced into the sample protection system (14) is nitrogen and ammonia.

4. The MOCVD device capable of grabbing epitaxial samples at any time as required according to claim 1, characterized in that: The micro-mechanical sampling device is a micro-manipulator.

5. The MOCVD device capable of grabbing epitaxial samples at any time as required according to claim 2, characterized in that: The micro-mechanical system (8) automatically turns on the sampling mode when detecting that the gate valve (7) is open. After receiving the sampling command, the micro-mechanical sampling device takes out the required epitaxial sample in a time of ≤0.05S. After the epitaxial sample is taken out, the acquisition unit feeds back the graphite disk surface information to the MOCVD monitoring system, assuming that there is no sample at this position and the epitaxial growth proceeds normally.

6. A method for using the MOCVD device capable of grabbing epitaxial samples at any time as required according to any one of claims 1 to 5, characterized in that: The following steps are involved: (1) After the graphite disk is filled with substrates, the graphite disk is transferred into the reaction chamber (1) through the transmission cavity using a micro-mechanical sampling device, and the MOCVD equipment starts to run the epitaxial structure program; (2) When the epitaxial sample grows to the required stage, the sampling control system (4) located in the sampling chamber (2) begins preparation work, and the vacuum pump (9) contained in the micro-mechanical sampling device is turned on; (3) The analysis unit of the sampling control system (4) starts to work and analyzes the temperature, atmosphere and pressure information in the reaction chamber (1); the feedback adjustment unit adjusts the temperature, atmosphere and pressure in the sampling chamber (2) according to the above information; after the temperature, atmosphere and pressure information of the sampling chamber (2) and the reaction chamber (1) are the same, the gate valve (7) of the sampling chamber (2) is opened; the collection unit collects the surface reflectivity information and the rotation speed information of the graphite disk, and feeds the information back to the analysis unit; the analysis unit determines the sampling time according to the rotation speed information provided by the collection unit; distinguishes the epitaxial sample and the graphite disk according to the surface reflectivity information of the graphite disk; and then transmits the above information to the feedback adjustment unit, which determines whether the micro-mechanical sampling device is working and the working time; (4) After the micro-mechanical sampling device takes out the required epitaxial sample, the gate valve (7) of the sampling chamber (2) is closed, and the feedback adjustment unit adjusts the atmosphere of the sampling control system (4) to a nitrogen atmosphere or a mixed atmosphere of ammonia and nitrogen. The collection unit detects the temperature of the epitaxial sample, which is ≤900°C and has a temperature difference of ≤50°C with the turnover chamber (3), and transfers the sample to the turnover chamber (3); (5) When the epitaxial sample is detected in the sampling control system (4), the rapid heating system (12) of the turnover chamber (3) starts to increase the temperature. When the temperature difference with the sample temperature is ≤50°C, the sample is transferred into the turnover chamber (3); the cooling system (13) of the turnover chamber (3) starts to work; (6) After the sampling control system (4) detects that there is no epitaxial sample in the cavity, nitrogen is filled in, and after the temperature is ≤100°C and the pressure is maintained at 20 mbar, the gas inlet device of the sampling control system (4) is closed; (7) When the temperature T2 in the turnover chamber (3) is lower than 30°C, the epitaxial samples are taken out for testing, analysis and material characterization.

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