CN207405234U - A kind of device for being used to prepare nitride material - Google Patents

Abstract

The utility model discloses a device for preparing nitride materials, which comprises a cavity, a gas ionizer, a metal source generating device, a vacuum system, a sample table, a cavity heating device, a vacuum gauge, a thermometer, a film thickness gauge and Control system, wherein: the cavity is composed of an upper cavity and a lower cavity that are separated from each other and can be integrated into one, the metal source generating device includes a crucible, a coil and a metal protection device, the metal protection device is composed of a crucible base and a blocking cover, and the vacuum The system includes a dry pump, a molecular pump and a cryopump, and the sample stage includes a slide rack, a substrate cooling device and a sample stage rotating device. The method for preparing nitrides in the utility model is an anion and cation layer-by-layer stacking mode, which has better material quality and faster nitride preparation rate. The utility model has the advantages of low energy consumption, high material quality, low carbon pollution, no component segregation, large production capacity and many other advantages.

Description

A kind of device for preparing nitride material

technical field

The utility model relates to the field of semiconductor light-emitting devices, in particular to a device for preparing nitride materials (such as gallium nitride, aluminum nitride, indium gallium nitrogen and aluminum indium gallium nitrogen) based on chemical vapor deposition.

Background technique

Nitride materials are widely used in light-emitting diodes, electronic devices, solar cells and other fields due to their excellent performance, and have a huge market and attractive application prospects.

At present, nitride materials are mainly prepared by metalorganic chemical vapor deposition. The device used in the preparation process - MOCVD has a complex structure, high cost, huge energy consumption, high cost and low production capacity. In addition, there are many technical problems such as carbon pollution and component segregation in the process of preparing nitrides by MOCVD, which have a negative impact on the performance of the prepared devices.

Other devices for preparing nitride materials include molecular beam epitaxy, hydride vapor phase epitaxy, magnetron sputtering, etc., all of which have their own shortcomings. For example, the growth rate of molecular beam epitaxy is slow, and only small-sized nitride materials can be prepared; hydride vapor phase epitaxy is mainly used to prepare bulk materials, and it is difficult to prepare complex quantum well structures; magnetron sputtering is mainly used to prepare aluminum nitride materials, which is difficult It is suitable for the preparation of materials with complex components such as gallium nitride and indium gallium nitride.

Contents of the invention

The purpose of the utility model is to provide a device for preparing nitride materials with low energy consumption, high material quality, low carbon pollution, no component segregation, and large production capacity.

The purpose of this utility model is achieved in that:

A device for preparing nitride materials, including a control system, characterized in that it also includes a cavity, a gas ionizer, a metal source generating device, a vacuum system, a sample stage, a cavity heating device, a vacuum gauge, a thermometer and a membrane Thick meter, of which:

The cavity is composed of an upper cavity and a lower cavity that are separated from each other and can be integrated. The lower cavity that opens upward is fixed, and an "L" shaped transmission device fixing rod is provided on the right side wall of the top of the lower cavity. , the fixed base of the transmission device is set on the vertical rod of the transmission device fixed rod, the outer end of the rotating arm of the transmission device is fixed on the top right side wall of the upper cavity, and the transmission device makes the hemispherical and The upper cavity that opens downward can move up and down in the axial direction or rotate horizontally in the axial direction above the lower cavity, so that the upper cavity and the lower cavity can be closed and separated, and the gas cavity of the cavity can be connected with the outside world When the upper cavity and the lower cavity are closed, the cavity is sealed by the sealing ring;

Several gas ionizers placed vertically are set at the bottom of the lower cavity, the air inlet at the bottom of the gas ionizer is located outside the cavity for accessing external gas, and the middle and upper parts of the gas ionizer are set at the bottom of the cavity In the gas chamber, a high-frequency sensor is set on the outer wall of the middle part of the gas ionizer, which is used to ionize the gas to obtain the source of nitrogen atoms and n-type dopant sources for preparing nitrides. Adjust the height and direction of the gas outlet, which is used to send the ionized plasma into the gas chamber;

Several metal source generating devices are installed at the bottom of the lower chamber and in the gas chamber. The metal source generating device includes a crucible, a coil and a metal protection device. The metal protection device is composed of a crucible base and a blocking cover. The upwardly opening crucible base is fixed in the lower chamber. The bottom surface of the crucible is equipped with a crucible for holding metal sources in the base of the crucible, and a coil is wound around the outer wall of the crucible. The coil can heat the crucible and control the temperature of the crucible within the range of 0--1200 ° C, which is used to obtain and prepare nitrogen. The gaseous metal source of the chemical compound is covered with a barrier cover for isolating the metal source and the gas chamber on the top of the crucible. The upper end of the gas charging tube with gas charging valve is set at the bottom of the crucible base, and the lower end of the gas charging tube passes through the bottom of the lower cavity. The bottom surface is exposed outside the cavity, and inert gas can be introduced into the gas-filled tube to prevent the metal source in the crucible from being oxidized when the metal protection device is connected to the outside world;

The vacuum system includes three sets of pumps: dry pump, molecular pump and cryopump. The input end of the dry pump used for low vacuum pumping is set on the middle side wall of the lower chamber, and the input of the molecular pump used for high vacuum pumping The terminal is connected to the output end of the dry pump; the cryopump is set on the top of the upper cavity for pumping air during the preparation of materials;

In the upper chamber and on the top of the gas chamber, a sample stage is provided. The sample stage includes a carrier, a substrate cooling device and a sample stage rotating device. The hollow groove provided on the carrier is used to hold the The substrate is placed, and the substrate cooling device is covered above the carrier, and the closed channel in the substrate cooling device is filled with cooling liquid. By controlling the flow speed of the cooling liquid, the temperature of the substrate surface can be controlled, including magnetic coupling. The sample table rotating device of the rotor is set on the middle top of the slide rack, and the magnetically coupled rotor drives the slide rack to rotate through gears;

A cavity heating device is provided above the middle of the bottom plate of the lower cavity and in the gas cavity, and the gas cavity is heated by a heat radiation method;

In the middle of the side wall of the lower chamber and in the gas chamber from top to bottom, there are vacuum gauges, thermometers and film thickness gauges in sequence. The vacuum gauge is an ionization vacuum gauge for measuring the internal pressure of the gas chamber; the thermometer is a platinum resistance thermometer. Used to measure the internal temperature of the gas chamber; the film thickness meter is a quartz crystal oscillator used to measure the film thickness during the nitride preparation process;

The transmission device, gas ionizer, vacuum pump system, substrate cooling device, chamber heating device, vacuum gauge, thermometer, and film thickness gauge are respectively connected to the control system through wires.

The number of gas ionizers is 2-4, and the number of metal source generating devices is 4-6.

Several gas ionizers and several metal source generating devices are arranged in a staggered manner.

The shape of the hollow groove in the middle of the slide holder in the sample stage is similar to that of the standard substrate, and the size of the hollow groove in the middle of the slide holder is slightly smaller than that of the standard substrate.

Carriers can be removed for access to substrates.

When the specification of the substrate is different from the standard substrate and smaller than the size of the standard substrate, a spare slide holder is provided on the slide holder, the size of the spare slide holder is the same as that of the standard substrate, and the spare slide holder is hollowed out Smaller grooves are used to accommodate non-standard substrates that are smaller in size than standard substrates.

The blocking cover of the metal protection device is installed on the electric support rod that can move up and down and rotate left and right. Under the command of the control system, the electric support rod can open the blocking cover when it moves upwards, and rotate to make the blocking cover leave the crucible. The gaseous metal source in the crucible enters the gas chamber; the electric support rod rotates so that the blocking cover faces the crucible, and then closes when it moves downward, and the blocking cover isolates the gaseous metal source in the crucible from the gas chamber.

The blocking cover of the metal protection device is automatically closed when the gas chamber is connected to the outside world, and at the same time the gas filling valve is automatically opened and the protective gas is introduced to protect the metal source in the crucible from being oxidized.

The fixed rod of the transmission device is a hydraulic rod or an air pressure rod; the sealing ring is a metal sealing ring or a rubber ring sealing ring.

The cavity heating device is a halogen lamp or an infrared quartz radiation lamp; the material of the crucible is graphite, tungsten or molybdenum.

A flow meter is connected to the air inlet at the bottom of the gas ionizer to adjust the gas flow through the gas ionizer.

The utility model uses metals such as gallium, aluminum, indium, and magnesium as metal sources, and obtains gaseous metal atoms such as gallium, aluminum, indium, and magnesium through evaporation as the source of cations in nitrides, and uses high-frequency induction to ionize ammonia. Gas or nitrogen can obtain nitrogen ions as the source of anions in nitrides, and undergo chemical reactions at lower temperatures (such as 0-200 ° C) and deposit on the surface of the substrate to obtain nitride materials. The utility model prepares complex multi-layer nitride structures, such as light-emitting diodes, Schottky diodes, high-speed electron transfer transistors, solar cells and other devices, by controlling the opening and closing and flow of various metal sources and ionized gases.

The working temperature of the utility model (such as 0-200°C) is much lower than that of the traditional nitride preparation device MOCVD (such as 700-1100°C), and the energy consumption in the working process is greatly reduced; and at low temperature, indium The chemical reaction of the gallium nitrogen material is in a non-equilibrium state, which avoids the segregation of the indium component; the metal source material used in the utility model does not contain carbon elements, so there is no carbon pollution problem; the method of preparing the nitride in the utility model is as follows: The layer-by-layer stacking mode of anion and cation has better material quality and faster nitride preparation rate. Therefore, the utility model has many advantages such as low energy consumption, high material quality, low carbon pollution, no component segregation, and large production capacity.

Description of drawings

Fig. 1 is a schematic diagram of the device structure of the utility model for preparing nitride materials;

Among them: 1─cavity, 11─upper chamber, 12─lower chamber, 13─transmission device, 2─gas ionizer, 21─air inlet, 22─high frequency sensor, 23─gas outlet, 3 ─Metal source generator, 31─crucible, 32─coil, 33─metal protection device, 331─blocking cover, 332─inflatable valve, 41─dry pump, 42─molecular pump, 43─cryopump, 51─carrier , 52─substrate cooling device, 53─sample table rotating device, 6─heating device, 7─vacuum gauge, 8─thermometer, 9─film thickness gauge;

Figure 2 is a schematic top view of the slide rack and the spare slide holder.

Detailed ways

The utility model is described in detail below in conjunction with accompanying drawing and embodiment.

A device for preparing nitride materials, including a cavity 1, a gas ionizer 2, a metal source generating device 3, a vacuum system 4, a sample stage 5, a cavity heating device 6, a vacuum gauge 7, a thermometer 8, a membrane Thickness meter 9 and control system, wherein:

The cavity 1 is composed of an upper cavity 11 and a lower cavity 12 that are separated from each other and can be integrated. The lower cavity 12 that opens upwards is fixed. The fixed rod 14 of the transmission device, the fixed base of the transmission device 13 is sleeved on the vertical bar of the transmission device fixed rod 14, and the outer end of the rotating arm of the transmission device 13 is fixed on the top right side wall of the upper cavity 11, in the transmission device Driven by 13, the semicircular and downwardly open upper cavity 11 can move up and down in the axial direction or rotate horizontally in the axial direction above the lower cavity 12, so that the upper cavity 11 and the lower cavity 12 can Closing and separating realize the communication and isolation between the gas chamber 16 of the chamber 1 and the outside world. When the upper chamber 11 and the lower chamber 12 are closed, the chamber 1 is sealed by the sealing ring 15; the fixed rod 14 of the transmission device is a hydraulic rod ;

Three vertically placed gas ionizers 2 are uniformly arranged at the bottom of the lower chamber 12, and the air inlet 21 at the bottom of the gas ionizer 2 is located outside the chamber 1 for accessing external gas. The air inlet 21 at the bottom end is connected with a flow meter to adjust the gas flow rate through the gas ionizer 2. The middle outer wall is covered with a high-frequency sensor 22, which is used to ionize the gas to obtain the source of nitrogen atoms and n-type dopants for preparing nitrides. The top of the gas ionizer 2 is provided with a gas outlet 23 that can adjust the height and direction , for sending the ionized plasma into the gas chamber 16;

4 metal source generating devices 3 are evenly arranged on the bottom of the lower cavity 12 and in the gas chamber 16. The metal source generating devices 3 include a crucible 31, a coil 32 and a metal protection device 33. The metal protection device 33 consists of a crucible base 333 and a blocking cover 331 The crucible base 333 opening upwards is fixed on the bottom surface of the lower chamber 12, and the crucible base 333 is provided with a crucible 31 for containing metal sources. The material of the crucible 31 is graphite, and a coil 32 is wound around the outer wall of the crucible 31. The coil 32 can heat the crucible 31 and control the temperature of the crucible 31 in the range of 0--1200°C, which is used to obtain the gaseous metal source for preparing nitrides, and the top of the crucible 31 is covered with a barrier cover for isolating the metal source and the gas chamber 16 331, the upper end of the inflation pipe 334 with the inflation valve 332 is located at the bottom of the crucible base 333, the lower end of the inflation pipe 334 passes through the bottom plate 121 of the lower cavity 12 and is exposed outside the cavity 1, and the inflation pipe 334 can pass through Enter an inert gas to prevent the metal source in the crucible 31 from being oxidized when the metal protection device 33 communicates with the outside world;

The vacuum system 4 includes three sets of pumps: a dry pump 41, a molecular pump 42 and a cryopump 43. The input end of the dry pump 41 for pumping air under low vacuum is arranged on the right side wall of the middle part of the lower chamber 12 to communicate with the gas chamber 16. , the input end of the molecular pump 42 used for pumping air under high vacuum is connected to the output end of the dry pump 41; the cryopump 43 is arranged on the top of the upper cavity 11, and is used for pumping air during the preparation of materials;

In the upper chamber, the top of the gas chamber 16 is provided with a sample stage 5, the sample stage 5 includes a slide frame 51, a substrate cooling device 52 and a sample stage rotating device 53, and the hollow part in the middle of the slide frame 51 is used to The bottom holds the substrate, and the top of the carrier 51 is covered with a bottom cooling device 52. The closed channel in the bottom cooling device 52 is filled with cooling liquid, and the temperature of the substrate surface can be controlled by controlling the flow rate of the cooling liquid. , the sample stage rotation device 53 containing the magnetic coupling rotor 531 is arranged at the middle bottom of the carrier 51, and the magnetic coupling rotor drives the carrier 51 to rotate through the gear 532;

Above the middle of the bottom plate of the lower cavity 12, a cavity heating device 6 is provided in the gas cavity 16, and the gas cavity 16 is heated by a heat radiation method, and the cavity heating device 6 is an infrared quartz radiation lamp;

On the upper part of the left side wall of the lower cavity 12, in the gas cavity 16, a vacuum gauge 7, a thermometer 8 and a film thickness gauge 9 are sequentially arranged from top to bottom. The vacuum gauge 7 is an ionization vacuum gauge for measuring the inside of the gas cavity 16. pressure; the thermometer 8 is a platinum resistance thermometer for measuring the internal temperature of the gas chamber 16; the film thickness meter 9 is a quartz crystal oscillator for measuring the film thickness in the nitride preparation process;

The transmission device 13, the gas ionizer 2, the vacuum pump system 4, the substrate cooling device 52, the chamber heating device 6, the vacuum gauge 7, the thermometer 8, and the film thickness gauge 9 are respectively connected to the control system through wires.

The blocking cover 331 of the metal protection device 33 is installed on the electric support rod 34 that can move up and down and rotate left and right. When the electric support rod 34 moves upwards, the blocking cover 331 can be opened and rotated to make the blocking cover 331 leave the sky above the crucible 31, so that The gaseous metal source in the crucible 31 enters the gas cavity 16; the electric support rod 34 rotates so that the blocking cover 331 faces the crucible 31, and then closes when moving downwards, and the blocking cover 331 isolates the gaseous metal source in the crucible 31 from the gas cavity 16.

The blocking cover 331 of the metal protection device 33 is automatically closed when the gas chamber 16 communicates with the outside world, and at the same time the gas filling valve 332 is automatically opened and the protective gas is introduced to protect the metal source in the crucible 31 from being oxidized.

Two gas ionizers 2 and four metal source generating devices 3 are arranged in a staggered manner, and two metal source generating devices 3 are arranged between every two gas ionizers 2 .

The shape of the hollow groove 511 in the middle of the slide holder 51 in the sample stage 5 is similar to that of the standard substrate, and the size of the hollow groove 511 in the middle of the slide holder 51 is slightly smaller than that of the standard substrate.

When the specifications of the substrate are different from the standard substrate and less than the size of the standard substrate, a spare slide support 512 is provided on the slide rack 51, the size of the spare slide support 512 is the same as the standard substrate size, and the spare slide The holder 512 is hollowed out into smaller grooves 513 to accommodate non-standard substrates that are smaller in size than standard substrates.

The carrier 51 is disassembled to take and place the substrate.

Claims (10)

1. A device for preparing nitride materials, including a control system, characterized in that: it also includes a cavity, a gas ionizer, a metal source generating device, a vacuum system, a sample stage, a cavity heating device, a vacuum gauge, Thermometers and film thickness gauges, of which: The cavity is composed of an upper cavity and a lower cavity that are separated from each other and can be integrated. The lower cavity that opens upward is fixed, and an "L" shaped transmission device fixing rod is provided on the right side wall of the top of the lower cavity. , the fixed base of the transmission device is set on the vertical rod of the transmission device fixed rod, and the outer end of the rotating arm of the transmission device is fixed on the top right side wall of the upper cavity, driven by the transmission device, the hemispherical and downward The open upper cavity can move up and down in the axial direction or rotate horizontally in the axial direction above the lower cavity, so that the upper cavity and the lower cavity can be closed and separated, and the gas cavity of the cavity can be connected and separated from the outside world. , when the upper cavity and the lower cavity are closed together, the cavity is sealed by a sealing ring; Several gas ionizers placed vertically are set at the bottom of the lower cavity, the air inlet at the bottom of the gas ionizer is located outside the cavity for accessing external gas, and the middle and upper parts of the gas ionizer are set at the bottom of the cavity In the gas chamber, a high-frequency sensor is set on the outer wall of the middle part of the gas ionizer, which is used to ionize the gas to obtain the source of nitrogen atoms and n-type dopant sources for preparing nitrides. Adjust the height and direction of the gas outlet, which is used to send the ionized plasma into the gas chamber; Several metal source generating devices are installed at the bottom of the lower chamber and in the gas chamber. The metal source generating device includes a crucible, a coil and a metal protection device. The metal protection device is composed of a crucible base and a blocking cover. The upwardly opening crucible base is fixed in the lower chamber. The bottom surface of the crucible is provided with a crucible for containing metal sources in the base of the crucible, and a coil is wound around the outer wall of the crucible. The coil heats the crucible and controls the temperature of the crucible within the range of 0--1200 ° C. It is used to obtain and prepare nitrides The gaseous metal source is covered with a barrier cover for isolating the metal source and the gas chamber on the top of the crucible. The upper end of the gas-filled tube with a gas-filled valve is set at the bottom of the crucible base, and the lower end of the gas-filled tube passes downward through the bottom of the lower cavity. And exposed outside the cavity, the inert gas is passed into the inflatable tube to prevent the metal source in the crucible from being oxidized when the metal protection device communicates with the outside world; The vacuum system includes three sets of pumps: dry pump, molecular pump and cryopump. The input end of the dry pump used for low vacuum pumping is set on the middle side wall of the lower chamber, and the input of the molecular pump used for high vacuum pumping The terminal is connected to the output end of the dry pump; the cryopump is set on the top of the upper cavity for pumping air during the preparation of materials; In the upper chamber and on the top of the gas chamber, a sample stage is provided. The sample stage includes a carrier, a substrate cooling device and a sample stage rotating device. The hollow groove provided on the carrier is used to hold the The substrate is placed, and the substrate cooling device is covered above the carrier, and the closed channel in the substrate cooling device is filled with cooling liquid. By controlling the flow speed of the cooling liquid, the temperature of the substrate surface can be controlled, including magnetic coupling. The sample table rotating device of the rotor is set on the middle top of the slide rack, and the magnetically coupled rotor drives the slide rack to rotate through gears; A cavity heating device is provided above the middle of the bottom plate of the lower cavity and in the gas cavity, and the gas cavity is heated by a heat radiation method; In the middle of the side wall of the lower chamber and in the gas chamber from top to bottom, there are vacuum gauges, thermometers and film thickness gauges in sequence. The vacuum gauge is an ionization vacuum gauge for measuring the internal pressure of the gas chamber; the thermometer is a platinum resistance thermometer. Used to measure the internal temperature of the gas chamber; the film thickness meter is a quartz crystal oscillator used to measure the film thickness during the nitride preparation process; The transmission device, gas ionizer, vacuum pump system, substrate cooling device, chamber heating device, vacuum gauge, thermometer, and film thickness gauge are respectively connected to the control system through wires. 2. The device for preparing nitride materials according to claim 1, characterized in that: the number of gas ionizers is 2-4, and the number of metal source generating devices is 4-6. 3. The device for preparing nitride materials according to claim 2, characterized in that several gas ionizers and several metal source generating devices are arranged in a staggered manner. 4. The device for preparing nitride materials according to claim 1, characterized in that: the shape of the hollow groove in the middle of the carrier in the sample stage is similar to the shape of the standard substrate, and the hollow in the middle of the carrier is The dimensions of the grooves are slightly smaller than those of standard substrates. 5. The device for preparing nitride materials according to claim 1 or 4, characterized in that the carrier can be detached for taking and placing the substrate. 6. The device for preparing nitride materials according to claim 1, characterized in that: when the specification of the substrate is different from the standard substrate and smaller than the size of the standard substrate, a spare carrier is provided on the carrier The size of the spare slide holder is the same as that of the standard substrate, and the spare slide holder is hollowed out into smaller grooves to accommodate non-standard substrates whose size is smaller than the standard substrate. 7. The device for preparing nitride materials according to claim 1, characterized in that: the blocking cover of the metal protection device is mounted on an electric support rod that can move up and down and rotate left and right. 8. The device for preparing nitride materials according to claim 1, characterized in that: the fixed rod of the transmission device is a hydraulic rod or a pneumatic rod; the sealing ring is a metal sealing ring or a rubber ring sealing ring. 9. The device for preparing nitride materials according to claim 1, characterized in that: the cavity heating device is a halogen lamp or an infrared quartz radiation lamp; the material of the crucible is graphite, tungsten or molybdenum. 10 . The device for preparing nitride materials according to claim 1 , wherein a flow meter is connected to the gas inlet at the bottom of the gas ionizer to adjust the gas flow through the gas ionizer. 11 .