CN115627526A - Crucible and silicon carbide crystal growth device - Google Patents
Crucible and silicon carbide crystal growth device Download PDFInfo
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- CN115627526A CN115627526A CN202211360240.3A CN202211360240A CN115627526A CN 115627526 A CN115627526 A CN 115627526A CN 202211360240 A CN202211360240 A CN 202211360240A CN 115627526 A CN115627526 A CN 115627526A
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- crucible
- crystal growth
- silicon carbide
- growth
- pressure sensor
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- 239000013078 crystal Substances 0.000 title claims abstract description 69
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 25
- 229910002804 graphite Inorganic materials 0.000 claims description 25
- 239000010439 graphite Substances 0.000 claims description 25
- 238000005070 sampling Methods 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000009413 insulation Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 230000001133 acceleration Effects 0.000 claims description 7
- 239000004964 aerogel Substances 0.000 claims description 5
- 239000004065 semiconductor Substances 0.000 description 4
- 238000000859 sublimation Methods 0.000 description 3
- 230000008022 sublimation Effects 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/002—Controlling or regulating
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a crucible and a silicon carbide crystal growth device, wherein a growth platform is arranged in the crucible for crystal growth, a support rod is arranged at the bottom of the growth platform for supporting the growth platform, a pressure sensor is arranged in the support rod for measuring a pressure signal for calculating the crystal growth speed, and the crucible can acquire the crystal growth speed in the crucible in real time, so that the temperature control precision in the crystal growth process can be improved.
Description
Technical Field
The invention relates to the technical field of silicon carbide crystal materials, in particular to a crucible and a silicon carbide crystal growth device.
Background
Silicon carbide single crystal materials are representative of third-generation wide band gap semiconductor materials, have properties such as a wide bandgap, high thermal conductivity, high electron saturation mobility, and high breakdown electric field, are significantly superior to first-generation semiconductor materials such as silicon and second-generation semiconductor materials such as GaAs, and are considered to be ideal semiconductor materials for manufacturing optoelectronic devices, high-frequency high-power devices, high-temperature electronic devices, and the like. The LED light source has wide application in the aspects of white light illumination, light storage, screen display, aerospace, high-temperature radiation environment, oil exploration, automation, radar and communication, electric vehicles, power electronics and the like.
The growth of silicon carbide single crystal materials is difficult, and a Physical Vapor Transport (PVT) method is generally adopted at present, in which silicon carbide powder is a common raw material, the silicon carbide powder is heated to a certain temperature and is obviously sublimated, and decomposed silicon carbide gas is transported along a temperature gradient and is condensed at a silicon carbide seed crystal. The PVT method for growing SiC single crystal mainly comprises three processes, namely decomposition and sublimation of raw materials, mass transmission and crystallization on seed crystal.
The three processes are all carried out in a sealed crucible, the growth temperature is controlled to be 2000-2400 ℃, and an operator can only control the temperature outside the crucible; the sublimation speed is a function of the temperature of the material source, the sublimation speed influences the crystal growth speed, and the crystal growth speed influences the quality, so the crystal growth speed can be indirectly controlled by controlling the temperature parameter, but the growth speed of the crystal in the crucible cannot be known, the crystal growth speed can be indirectly calculated only by analyzing the relationship between the temperature and the growth speed or the relationship between the power and the growth speed, and the defect of low control precision exists.
Disclosure of Invention
The invention aims to provide a crucible and a silicon carbide crystal growth device, which can improve the temperature control precision in the crystal growth process by monitoring the crystal growth speed in the crucible.
In order to achieve the purpose, the invention provides the following scheme:
a crucible, comprising: the device comprises a dry pot body, a crucible cover, a porous graphite inner wall, a growth platform, a support rod and a pressure sensor;
the inner wall of the porous graphite is arranged inside the crucible body, and a cavity between the inner wall of the porous graphite and the side wall of the crucible body is used for placing a silicon carbide source;
the crucible cover is arranged at the top of the crucible body;
the growth table is positioned inside the inner wall of the porous graphite and arranged at the top end of the supporting rod, and the growth table is used for placing seed crystals;
the bracing piece runs through the bottom of the crucible body, the bottom of bracing piece is located the outside of the crucible body, pressure sensor sets up the bottom of bracing piece.
Optionally, an axial through hole is formed in the support rod, and an infrared temperature sensor is further arranged at the position outside the crucible body in the through hole.
Optionally, the crucible still includes the graphite felt, the graphite felt sets up the crucible body's below, the bracing piece runs through the graphite felt.
Optionally, the crucible further includes a heat insulation pad, the heat insulation pad is located below the graphite felt, the support rod penetrates through the heat insulation pad, and the pressure sensor is disposed in the through hole at a position surrounded by the heat insulation pad.
Optionally, the heat insulation pad is an aerogel heat insulation pad.
Optionally, the crucible body and the crucible cover are made of graphite.
A silicon carbide crystal growth apparatus comprising: a heating device, a controller and the crucible;
the crucible is arranged in the heating device;
a signal output line of a pressure sensor of the crucible is connected with the controller;
the controller is connected with the control end of the heating device;
the controller is used for calculating the crystal growth speed according to the pressure signal detected by the pressure sensor and controlling the heating device according to the crystal growth speed.
Optionally, the calculating the crystal growth speed according to the pressure signal detected by the pressure sensor specifically includes:
calculating the growth speed of the crystal according to the pressure signal detected by the pressure sensor by using the following formula;
wherein v represents a crystal growth rate, m 2 Represents the mass of the crystal on the growth stage at the current sampling time, m 1 Representing the quality of the crystal on the growth stage at the previous sampling instant, t representing the sampling interval, F 2 A pressure signal representing the current sampling instant, F 1 Pressure signal, g, representing the previous sampling instant 2 Representing the equivalent gravitational acceleration, g, in the crucible at the current sampling moment 1 Representing the equivalent gravitational acceleration in the crucible at the previous sampling instant.
Optionally, the mode of controlling the heating device according to the crystal growth speed is a PID control method.
Optionally, the controller is a PLC.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
the invention discloses a crucible and a silicon carbide crystal growth device, wherein a growth platform is arranged in the crucible for crystal growth, a support rod is arranged at the bottom of the growth platform for supporting the growth platform, a pressure sensor is arranged in the support rod for measuring a pressure signal for calculating the crystal growth speed, and the crucible can acquire the crystal growth speed in the crucible in real time, so that the temperature control precision in the crystal growth process can be improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a schematic structural diagram of a crucible provided in an embodiment of the present invention;
fig. 2 is a control principle of the silicon carbide crystal growth apparatus according to the embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a crucible and a silicon carbide crystal growth device, which can improve the temperature control precision in the crystal growth process by monitoring the crystal growth speed in the crucible.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Example 1
Embodiment 1 of the present invention provides a crucible, as shown in fig. 1, including: a dry pot body 2, a crucible cover 1, a porous graphite inner wall 4, a growth platform 5, a support rod 6 and a pressure sensor (not shown in figure 1); the porous graphite inner wall 4 is arranged inside the crucible body 2, and a cavity between the porous graphite inner wall 4 and the side wall of the crucible body 2 is used for placing a silicon carbide source 3; the crucible cover 1 is arranged at the top of the crucible body 2; the growth table 5 is arranged at the top end of the support rod 6; the growth table 5 is used for placing seed crystals; the support rod 6 penetrates through the bottom of the crucible body 2, and the bottom end of the support rod 6 is positioned outside the crucible body 2; an axial through hole 7 is formed in the supporting rod 6, and the pressure sensor 7 is arranged at the bottom end of the supporting rod 6. An infrared temperature sensor is also arranged in the through hole 7 and is arranged at a position in the through hole 7 outside the crucible body 2, and the temperature of the crystal growing on the growth table 5 is measured by adopting a mode of emitting infrared rays to the growth table 5.
Illustratively, the crucible further comprises a graphite felt 8, the graphite felt 8 being disposed below the crucible body 2. The support rod 6 penetrates through the graphite felt 8.
Illustratively, an aerogel thermal insulation pad 9 is introduced under the graphite felt because the pressure sensor cannot resist the high temperature influence of the thermal field, and the pressure sensor is disposed in the through hole 7 at a position surrounded by the aerogel thermal insulation pad 9. The heat insulation material can well obstruct heat, cannot be inductively heated, and cannot occupy large volume, so that the introduction of the pressure sensor becomes practical.
Illustratively, the material of the crucible body and the material of the crucible cover are both graphite.
Example 2
An embodiment 2 of the present invention provides a silicon carbide crystal growth apparatus, including: a heating device, a controller and the crucible; the crucible is arranged in the heating device; a signal output line of a pressure sensor of the crucible is connected with the controller; the controller is connected with the control end of the heating device; the controller is used for calculating the crystal growth speed according to the pressure signal detected by the pressure sensor and controlling the heating device according to the crystal growth speed.
The principle of calculating the crystal growth speed according to the pressure signal detected by the pressure sensor and controlling the heating device according to the crystal growth speed is shown in fig. 2:
the pressure sensor transmits a real-time pressure signal (weight value) to the PLC, the PLC analyzes and calculates data to obtain a real-time growth speed, then the growth speed is compared with a process requirement to carry out PID calculation, an adjusting instruction is issued to the heating power supply, and the heating power supply adjusts power according to the adjusting instruction, so that the growth speed meets the process requirement.
Illustratively, the PLC analyzes and calculates the data, and the formula of the crystal growth rate is:
wherein v represents a crystal growth rate, m 2 Represents the mass of the crystal on the growth stage at the current sampling time, m 1 Representing the quality of the crystal on the growth stage at the previous sampling instant, t representing the sampling interval, F 2 A pressure signal representing the current sampling instant, F 1 Indicating the pressure signal at the previous sampling instant, g 2 Represents the equivalent gravitational acceleration, g, in the crucible at the current sampling moment 1 Representing the equivalent gravitational acceleration in the crucible at the previous sampling instant. Illustratively, the embodiment of the present invention provides a calibration device, which comprises a mass block and a support body, the calibration device is not shown in fig. 1, and has a structure similar to that of the growth stage 5 and the support rod 6, except that no seed crystal is placed on the mass block, and no through hole may be provided in the support body, specifically: the mass block is arranged at the top end of the support body, and the mass block and the top end of the support body are both positioned in the dry pot body 2; the supporter runs through the bottom of the crucible body 2, and the bottom of supporter is located the outside of the crucible body 2, and the bottom of supporter is provided with the pressure sensor who is used for the calibration, calculates this equivalent acceleration of gravity through the known mass (the quality of quality piece) among the calibrating device and the pressure that the pressure sensor that is used for the calibration detected.
Based on the embodiment, the invention adopts a pull-down growth mode, and adds a high-precision pressure sensor to monitor the crystal growth speed, and the crystal growth speed is fed back to the PLC to adjust the heating power of the heating device, so that the growth speed can be directly monitored and stably controlled in a reasonable range.
In order to avoid the influence of heat on the pressure sensor, the aerogel heat-insulating bottom cushion is introduced, so that the measured crystal growth speed is more accurate.
For the system disclosed by the embodiment, the description is relatively simple because the system corresponds to the method disclosed by the embodiment, and the relevant points can be referred to the method part for description.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (10)
1. A crucible, characterized in that it comprises: the device comprises a dry pot body, a crucible cover, a porous graphite inner wall, a growth platform, a support rod and a pressure sensor;
the inner wall of the porous graphite is arranged inside the crucible body, and a cavity between the inner wall of the porous graphite and the side wall of the crucible body is used for placing a silicon carbide source;
the crucible cover is arranged at the top of the crucible body;
the growth table is positioned inside the inner wall of the porous graphite and arranged at the top end of the supporting rod, and the growth table is used for placing seed crystals;
the bracing piece runs through the bottom of the crucible body, the bottom of bracing piece is located the outside of the crucible body, pressure sensor sets up the bottom of bracing piece.
2. The crucible of claim 1, wherein the support rod has an axial through hole formed therein, and an infrared temperature sensor is further disposed in the through hole at a position outside the crucible body.
3. The crucible of claim 1 further comprising a graphite felt disposed below the body, the support rods extending through the graphite felt.
4. The crucible of claim 3, further comprising a thermal insulation pad located below the graphite felt, the support rod extending through the thermal insulation pad.
5. The crucible of claim 4, wherein the thermal insulation pad is an aerogel thermal insulation pad.
6. The crucible of claim 1 wherein the material of the body and the lid is graphite.
7. A silicon carbide crystal growth device, comprising: heating means, a controller and a crucible as claimed in any one of claims 1 to 6;
the crucible is arranged in the heating device;
a signal output line of a pressure sensor of the crucible is connected with the controller;
the controller is connected with the control end of the heating device;
the controller is used for calculating the crystal growth speed according to the pressure signal detected by the pressure sensor and controlling the heating device according to the crystal growth speed.
8. The silicon carbide crystal growth device according to claim 7, wherein the calculating of the crystal growth rate from the pressure signal detected by the pressure sensor specifically comprises:
calculating the growth speed of the crystal according to the pressure signal detected by the pressure sensor by using the following formula;
wherein v represents a crystal growth rate, m 2 Representing the mass of the crystal on the growth stage at the current sampling instant, m 1 Representing the quality of the crystal on the growth stage at the previous sampling instant, t representing the sampling interval, F 2 A pressure signal representing the current sampling instant, F 1 Pressure signal, g, representing the previous sampling instant 2 Representing the equivalent gravitational acceleration, g, in the crucible at the current sampling moment 1 Representing the equivalent gravitational acceleration in the crucible at the previous sampling instant.
9. The silicon carbide crystal growth apparatus according to claim 7, wherein the means for controlling the heating means according to the crystal growth rate is a PID control method.
10. The silicon carbide crystal growth apparatus according to claim 7, wherein the controller is a PLC.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211360240.3A CN115627526A (en) | 2022-11-02 | 2022-11-02 | Crucible and silicon carbide crystal growth device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211360240.3A CN115627526A (en) | 2022-11-02 | 2022-11-02 | Crucible and silicon carbide crystal growth device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115627526A true CN115627526A (en) | 2023-01-20 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211360240.3A Pending CN115627526A (en) | 2022-11-02 | 2022-11-02 | Crucible and silicon carbide crystal growth device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115627526A (en) |
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2022
- 2022-11-02 CN CN202211360240.3A patent/CN115627526A/en active Pending
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