CN115142133A - Control system and control method for growth speed of silicon carbide crystal and crystal growth furnace - Google Patents
Control system and control method for growth speed of silicon carbide crystal and crystal growth furnace Download PDFInfo
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- CN115142133A CN115142133A CN202210726104.5A CN202210726104A CN115142133A CN 115142133 A CN115142133 A CN 115142133A CN 202210726104 A CN202210726104 A CN 202210726104A CN 115142133 A CN115142133 A CN 115142133A
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- 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
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- C30B29/36—Carbides
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- 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
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Abstract
The invention discloses a control system and a control method for the growth speed of a silicon carbide crystal and a crystal growth furnace, wherein the control system comprises an airflow sensing device, a weight sensing device and an airflow regulating and controlling device, the airflow sensing device consists of a plurality of airflow sensing unit parts, each airflow sensing unit part comprises a shell and a built-in part which freely moves in the shell, and a plurality of air holes are formed in the shell; the weight sensing device is used for sensing the current weight of the airflow sensing device in the moving process of the built-in part; the airflow regulating and controlling device is connected with the weight sensing device and used for regulating the flow parameter value of the airflow according to the current weight of the airflow sensing device so as to control the growth speed of the silicon carbide crystal and reflect the flow parameter value of the airflow from the side surface through the weight of the airflow sensing device. According to the control method, the flow parameter value of the gas flow is adjusted according to the weight of the gas flow induction device, so that the growth speed of the crystal is controlled.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a control system and a control method for the growth speed of a silicon carbide crystal and a crystal growth furnace.
Background
Silicon carbide (SiC) substrates can be classified into a conductive type silicon carbide substrate and a semi-insulating silicon carbide substrate. The conductive silicon carbide substrate slice is mainly used in the fields of high power and high voltage, such as new energy automobiles, high-speed rail transportation, power grid inverters and the like; the existing methods for preparing the silicon carbide substrate mainly comprise physical vapor phase transport (PVD), chemical vapor phase transport (CVD), a high-temperature solution method and the like.
The preparation of conductive silicon carbide crystals by primer-gas phase transport (PVD) is one of the most common methods. In the prior art, silicon carbide powder is heated, when the temperature reaches above 2100 ℃, the silicon carbide powder is heated to sublimate into silicon carbide gas, the silicon carbide gas is mixed with introduced carrier gas to form mixed gas flow, the mixed gas flow moves towards the direction of silicon carbide seed crystals, and the silicon carbide gas is deposited and grows on the silicon carbide seed crystals, so that the silicon carbide crystals are successfully grown. Therefore, the growth speed of the silicon carbide crystal is closely related to the moving speed of the mixed gas flow to the silicon carbide seed crystal, the growth speed of the silicon carbide crystal is high when the flowing speed of the mixed gas flow is high, and the flow speed of the mixed gas flow is related to the sublimation speed of the silicon carbide gas and the flow speed of the carrier gas. In the prior art, the flow velocity of the mixed gas flow is controlled mainly by regulating and controlling the flow velocity of the carrier gas, but the flow velocity of the mixed gas flow is also influenced by the sublimation rate of the silicon carbide powder, however, the silicon carbide crystal grows in an unobservable manner, the sublimation rate of the silicon carbide powder is difficult to accurately measure and calculate, and further, the flow parameters of the mixed gas flow in the crystal growth process cannot be accurately controlled. In addition, under the high-temperature condition, the sublimation temperature of carbon is different from that of silicon, so that the atomic ratio of carbon to silicon in the gas phase is too high, impurities such as carbon coating and the like can be formed in the growing silicon carbide crystal, and the growth quality of the silicon carbide crystal is influenced.
Disclosure of Invention
The present invention is intended to solve at least the existing problems one of the technical problems in the art. Therefore, the invention provides a control system for the growth speed of the silicon carbide crystal, which can enable the growth of the silicon carbide crystal to be visualized by measuring the weight, so as to adjust the flow parameters of the gas flow in the crystal growing process and further realize the control of the growth speed of the silicon carbide crystal.
The invention also provides a control method of the growth speed of the silicon carbide crystal based on the control system.
The invention also provides a silicon carbide crystal growth furnace.
The system for controlling the growth speed of the silicon carbide crystal comprises an airflow sensing device, a weight sensing device and an airflow regulating device;
the gas flow induction device is arranged on the silicon carbide powder, the silicon carbide powder is placed in the crucible, the gas flow induction device is composed of a plurality of gas flow induction unit pieces, each gas flow induction unit piece comprises a containing cavity formed by a shell and a built-in piece arranged in the containing cavity, a plurality of gas holes are formed in the shell, in the crystal growth process, gas flows to the direction of silicon carbide seed crystals through the containing cavity through the gas holes, and the built-in pieces are suitable for moving in the containing cavity under the power action of the gas flow; the weight sensing device is used for sensing the current weight of the air flow sensing device in the moving process of the built-in part; and the airflow regulating and controlling device is connected with the weight sensing device and is used for regulating the flow parameter value of the airflow according to the current weight of the airflow sensing device so as to control the growth speed of the silicon carbide crystal.
In some embodiments, the airflow sensing unit element is adapted to form, under the power of the airflow: the first state that the built-in part is in contact with the inner side surface of the shell close to the silicon carbide powder, the second state that the built-in part is suspended in the shell, or the third state that the built-in part is in contact with the inner side surface of the shell, which is originally the silicon carbide powder.
Furthermore, the airflow sensing unit part is made of graphite, the airflow sensing unit parts are tightly arranged on the silicon carbide powder, and the airflow sensing unit part is made of graphite, so that a carbon source in airflow can be adsorbed, the condition of forming carbon coating and other impurities in the crystal growth process is effectively reduced, and the quality of the silicon carbide crystal is improved.
In some embodiments, the airflow sensing device further comprises a filter carrier box, wherein a receiving cavity is formed on the filter carrier box, the receiving cavity is provided with open openings which are oppositely arranged, and the airflow sensing unit element is arranged in the receiving cavity and can freely move in the receiving cavity. The filtering loading box is connected with the single independent air flow induction unit piece into a whole, so that the filtering loading box is more convenient to move.
Furthermore, a spacing space is formed between the airflow induction device and the silicon carbide powder, so that the uniformity of upward diffusion of airflow is facilitated.
The method for controlling the growth rate of a silicon carbide crystal according to the second aspect of the invention, including the system for controlling the growth rate of a silicon carbide crystal according to the first aspect of the invention, comprises the following steps:
the weight sensing device acquires the current weight of the airflow sensing device;
comparing the current weight of the airflow sensing device with a set first threshold range, wherein the first threshold range is the weight range of the airflow sensing device when the built-in piece of the weight sensing unit piece in a first preset number range is suspended in the shell;
if the current weight of the airflow sensing device is larger than the first threshold range, increasing the current flow parameter value of the airflow through an airflow regulating device to increase the crystal growth speed, and if the current weight of the airflow sensing device is smaller than the first threshold range, reducing the current flow parameter value of the airflow through the airflow regulating device to reduce the crystal growth speed.
According to the control method of the invention, by arranging the control device of the first aspect, the current weight of the airflow sensing device is obtained according to the weight sensing device, the current weight is compared with the set first threshold range, and the current flow parameter value of the airflow, namely the diffusion speed of the mixed airflow of the silicon carbide gas and the carrier gas, is adjusted according to the comparison result, so that the aim of controlling the growth speed of the silicon carbide crystal is achieved, and the quality of the silicon carbide crystal is effectively improved.
In some embodiments, the method further comprises:
comparing the current weight of the airflow sensing device with a set second threshold range, wherein the second threshold range is the weight range of the airflow sensing device when the built-in piece of the weight sensing unit piece in a second preset number range is suspended in the shell, and the second threshold range is larger than the first threshold range; and if the current weight of the airflow sensing device is smaller than the second threshold range, reducing the flow parameter value of the current airflow through an airflow regulating and controlling device so as to reduce the crystal growth speed. The second threshold range is set to be compared with the current weight obtained by the airflow sensing device, and the current flowing parameter value of the airflow is adjusted according to the comparison result, so that the growth speed of the silicon carbide crystal is controlled, and the quality of the silicon carbide crystal is further improved.
In some embodiments, the method of increasing a current flow parameter value of a gas by a gas flow regulating device comprises: controlling the carrier gas flow rate to increase the flow parameter value of the gas flow; the method for reducing the current gas flow parameter value through the gas flow regulating device comprises the following steps: the carrier gas flow rate is controlled to decrease the flow parameter value of the gas flow. The gas flow parameter value is controlled by regulating the flow speed of the carrier gas, so that the diffusion speed of the gas flow is controlled.
In some embodiments, the method of increasing a current flow parameter value of a gas by a gas flow regulating device may further include: controlling the crystal growth temperature to be increased so as to increase the sublimation rate of the silicon carbide powder and further increase the flow parameter value of the airflow; the method for reducing the current gas flow parameter value through the regulating device comprises the following steps: the crystal growth temperature is controlled to be reduced so as to reduce the sublimation rate of the silicon carbide powder and further reduce the flow parameter value of the airflow. The sublimation speed of the silicon carbide powder is controlled by regulating and controlling the crystal growth temperature, so that the flow parameter value of the airflow is controlled, and the control on the growth speed of the silicon carbide crystal is realized.
A silicon carbide crystal growth furnace according to a third aspect of the present invention includes a system for controlling the growth rate of a silicon carbide crystal according to the first aspect of the present invention.
Compared with the prior art, the invention has the following advantages:
1) According to the technical scheme, the power action of mixed gas flow in the crucible is sensed through the gas flow sensing device, the weight sensing device is used for measuring the current weight of the gas flow sensing device, the current weight of the gas flow sensing device reflects the flow parameter value of the gas flow from the side surface, the growth condition of the silicon carbide crystal is obtained, the growth speed of the silicon carbide crystal is visualized, the gas flow regulating and controlling device is used for regulating and controlling the flow parameter of the gas flow according to the growth condition of the silicon carbide crystal, and the control of the crystal growth speed is further realized.
2) The invention measures the current weight of the airflow sensing device in real time through the weight sensing device, compares the current weight with a preset threshold range, judges whether the flow parameter value of the carbon airflow needs to be adjusted, and can more accurately control the growth speed of the silicon carbide crystal, thereby optimizing the process and growing perfect crystal ingots.
3) The invention adjusts the carbon-silicon atomic ratio in the gas phase by controlling the flow parameter values of the gas flow in different stages, reduces or even avoids the phenomenon of forming carbon coating and other impurities in the growing silicon carbide crystal, thereby improving the growth quality of the silicon carbide crystal.
Drawings
FIG. 1 is a schematic view of an airflow sensing device according to an embodiment of the present invention;
FIG. 2 is a state diagram of the airflow sensing unit piece in the first state according to the embodiment of the invention;
FIG. 3 is a state diagram illustrating the state of the air flow sensing unit piece in the second state according to the embodiment of the present invention;
FIG. 4 is a state diagram illustrating the air flow sensing unit piece in a third state according to one embodiment of the present invention;
FIG. 5 is a schematic view of a control system of one embodiment of the present invention in use;
FIG. 6 is a schematic representation of the use of the control system of one embodiment of the present invention;
FIG. 7 is a schematic view showing the positions of the gas flow sensing device and the crucible according to one embodiment of the present invention;
FIG. 8 is a schematic diagram of a filter cartridge according to one embodiment of the present invention;
FIG. 9 is a schematic cross-sectional view of FIG. 8;
FIG. 10 is an enlarged schematic view of portion A of FIG. 9;
FIG. 11 is a flow chart of a control method of one embodiment of the present invention.
Reference numerals:
100-an airflow sensing unit; 101-a housing; 102-air holes; 103-a built-in part; 104 — a first space;
200-crucible; 201-a lid;
300-a filtration cartridge; 301-a housing chamber;
400-silicon carbide powder;
500-seed crystal;
600-weight sensing means; 601-a load cell; 602-a weighing bar; 603-a weighing platform;
700-a growth base;
800-crystal growth furnace.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
The following disclosure provides many different embodiments, or examples, for implementing different features of the invention. To simplify the disclosure of the present invention, the components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit the present invention. Furthermore, the present invention may repeat reference numerals and/or letters in the various examples. This repetition is for the purpose of simplicity and clarity and does not in itself dictate a relationship between the various embodiments and/or configurations discussed. In addition, the present invention provides examples of various specific processes and materials, but one of ordinary skill in the art may recognize the applicability of other processes and/or the use of other materials.
A control system for growing a silicon carbide crystal according to an embodiment of the first aspect of the present invention will now be described with reference to the accompanying drawings, the control system of this embodiment being implemented in accordance with silicon carbide crystal growing apparatus commonly used in the art.
Referring to fig. 1 to 5, a system for controlling the growth rate of a silicon carbide crystal according to an embodiment of the present invention includes an airflow sensing device, a weight sensing device 600, and an airflow regulating device; the air flow induction device is arranged on the silicon carbide powder 400, the silicon carbide powder 400 is placed in the crucible 200, the air flow induction device is composed of a plurality of air flow induction unit pieces 100, each air flow induction unit piece 100 comprises a containing cavity formed by a shell 101 and an embedded piece 103 arranged in the containing cavity, the shell 101 and the embedded piece 103 are one of a sphere, a cylinder or a square, and the shell 101 and the embedded piece 103 are both spheres. Referring to fig. 2, the housing 101 is provided with a plurality of air holes 102, during the crystal growth process, the air flow flows (i.e. diffuses upwards) towards the silicon carbide seed crystal 500 through the air holes 102 of the air flow sensing unit 100, the embedded part 103 is adapted to move in the accommodating cavity under the power of the air flow, in order to ensure that the flow parameter value of the air flow can be adjusted by blocking part of the air holes 102 of the housing 101 when the embedded part 103 moves in the housing 101, the volume ratio of the embedded part 103 to the housing 101 is preferably set to 1: (5-7).
The airflow sensing unit piece 100 is suitable for forming a first state that the built-in part 103 is in contact with the inner side surface of the shell 101 close to the silicon carbide powder 400, a second state that the built-in part 103 is suspended in the shell 101, or a third state that the built-in part 103 is in contact with the inner side surface of the shell 101 far from the silicon carbide powder 400 under the power action of the airflow.
When the airflow sensing unit piece 100 is in the first state, the buoyancy of the airflow to the built-in piece 103 is smaller than the gravity of the built-in piece 103, and the built-in piece 103 is located at the bottom wall of the casing 101 and blocks part of the air holes 102 in the bottom wall of the casing 101. Referring to fig. 2, when the airflow sensing unit 100 is in the second state, the buoyancy of the airflow to the built-in part 103 is equal to the gravity of the built-in part 103, the built-in part 103 is suspended in the casing 101, that is, the built-in part 103 is in a suspended state, and all the air holes 102 of the casing 101 are in an open state. Referring to fig. 3, when the airflow sensing unit 100 is in the third state, the buoyancy of the airflow to the built-in part 103 is greater than the gravity of the built-in part 103, and the built-in part 103 is located at the top wall of the housing 101 and blocks part of the air hole 102 at the top wall of the housing 101, see fig. 4.
The weight sensing device 600 is used to sense the current weight of the air flow sensing device during the movement of the built-in 103. The weight sensing device 600 can weigh the airflow sensing device in two preferred ways:
the first method is as follows: the weight of the gas flow sensing device was calculated by weighing the whole crucible 200 and then calculating the weight of the gas flow sensing device based on the weighed weight, such as: the weight sensing device 600 comprises a weighing sensor 601, a weighing rod 602 and a weighing platform 603, wherein the weighing sensor 601 is fixed on a platform (or ground) below the crystal growth furnace 800, one end of the weighing rod 602 is installed at the central position of the weighing sensor 601, the other end of the weighing rod is installed with the weighing platform 603, the weighing platform 603 is located in the crystal growth furnace 800, the crucible 200 is placed on the weighing platform 603, referring to fig. 5, and the current weight of the airflow sensing device can be calculated by the formula (1):
M＝M1-M2 (1)
wherein, M1 is the current weight of the crucible 200, the cover 201, the seed crystal 500, the silicon carbide powder 400 and the gas flow reaction device, M2 is the total weight of the crucible 200, the cover 201, the seed crystal 500 and the silicon carbide powder 400, in the crystal growth process, after the silicon carbide powder 400 is heated and sublimated into silicon carbide gas, the silicon carbide gas can be adsorbed by the seed crystal 500 and grow into silicon carbide crystal, because the amount of the silicon carbide gas discharged out of the crucible 200 is very small, therefore, the amount can be ignored), therefore, the weight of M1 is not changed, and is a fixed value.
The second method comprises the following steps: weight sensing device 600 directly weighs the airflow sensing device, such as: the middle portion of the bottom of the crucible 200 is recessed toward the top of the crucible 200 to form a first space for accommodating the weight-sensing device 600. The weight sensing device 600 comprises a load cell 601 and a load bar 602, the load bar 602 being mounted in a central position of the load cell 601, see fig. 6. In use, the crucible 200 and the load cell 601 are placed on the growth susceptor 700, the weight sensing device 600 is placed in the first space 104, and the weighing rod 602 is connected to the gas flow sensing device through the top wall of the first space 104. In order to ensure the accuracy of the weighing, the weighing bar 602 and the air flow guide should both have a certain clearance from the top wall of the first space 104. In other words, the weighing rod 602 and the air flow inducing means are not in contact with the top wall of the first space 104, the silicon carbide powder 400 is placed in the crucible 200, and the height of the silicon carbide powder 400 is lower than the top wall of the first space 104.
Of course, the airflow sensing device may be weighed in other ways.
The gas flow regulating device is connected to the weight sensing device 600, and is configured to adjust a flow parameter value of the gas flow, that is, a diffusion rate of a mixed gas flow (gas) of the silicon carbide gas and the carrier gas, according to a current weight of the gas flow sensing device, so as to control a growth rate of the silicon carbide crystal. The gas flow regulating device can be a controller of the silicon carbide growth equipment, and can also be an independent microcontroller, and if the gas flow regulating device is the independent microcontroller, the following two preferable modes can be adopted:
the method I comprises the following steps: the independent micro-controller is respectively connected with the carrier gas control valve and the heater, and the flow rate of the carrier gas is adjusted by controlling the opening degree of the carrier gas control valve so as to adjust the flow parameter value of the airflow, or the power of the heater is controlled to control the crystal growth temperature so as to adjust the sublimation rate of the silicon carbide powder 400 so as to adjust the flow parameter value of the airflow.
The second method comprises the following steps: the independent microcontroller is connected with the silicon carbide growth equipment controller, the independent microcontroller transmits the received weight information transmitted by the weight sensing device 600 to the silicon carbide growth equipment controller, and the silicon carbide growth equipment controller controls the gas-carrying control valve and the heater according to the received weight information so as to adjust the flow parameter value of the air flow.
In some embodiments, referring to fig. 5, a plurality of airflow sensing unit pieces 100 are closely laid on the silicon carbide powder 400, and adjacent airflow sensing unit pieces are closely connected, so that it is effectively ensured that the airflow can pass through each airflow sensing unit piece 100 in the process of diffusion, so as to accurately visualize the flow parameter value of the airflow through the weight of the airflow sensing device; the gas flow induction unit 100 is made of graphite, and may also be made of other materials, such as one or more of molybdenum, tantalum, niobium or tungsten, but this embodiment is preferably made of graphite, because graphite can effectively adsorb a carbon source in a gas flow, and impurities such as carbon coating are reduced or even avoided in a crystal growth process, thereby improving the quality of the silicon carbide crystal.
In some embodiments, referring to fig. 7 to 10, in order to facilitate the taking and placing of the airflow sensing unit piece 100, the airflow sensing device further includes a filter carrier 300, the filter carrier 300 is made of graphite, a receiving cavity 301 is formed on the filter carrier 300, the receiving cavity 301 has an open opening arranged oppositely, the airflow sensing unit piece 100 is placed in the receiving cavity 301 and can freely move in the receiving cavity 301, in other words, the airflow sensing unit piece 100 can only move in the receiving cavity 301 without being separated from the receiving cavity 301. Since the air current sensing unit piece 100 is integrated in the filter loading box 300, when in use, only the filter loading box 300 needs to be put into or taken out of the crucible 200, on one hand, the air current sensing unit piece 100 is convenient to put and take, on the other hand, the air current sensing unit piece does not need to be put into or taken out singly, and the working efficiency is improved.
In some embodiments, a space is formed between the airflow sensing device and the silicon carbide powder 400, and when the airflow sensing device is composed of a plurality of airflow sensing unit pieces 100, two adjacent airflow sensing unit pieces 100 are fixedly connected together, for example, mechanically connected together. The space can be 5mm-10mm, referring to fig. 6, the mixed gas flow can diffuse to a certain extent in the space, so that the gas flow diffuses upwards more uniformly, and the accuracy of the flow parameter value of the gas flow reflected by the weight of the gas flow sensing device is further improved.
The invention also provides an embodiment of a method for controlling the growth rate of a silicon carbide crystal, which comprises the airflow sensing device in the embodiment, and referring to fig. 11, the method comprises the following specific steps:
the weight sensing device 600 acquires the current weight of the air flow sensing device. Comparing the current weight of the airflow sensing device with a set first threshold range, wherein the first threshold range is the weight range of the airflow sensing device when the built-in part 103 of the weight sensing unit elements in a first preset number range is suspended in the shell 101; if the current weight of the airflow sensing device is larger than the first threshold range, the current flow parameter value of the airflow is increased through the airflow regulating device to increase the growth speed of the crystal, and if the weight of the current airflow sensing device is smaller than the first threshold range, the current flow parameter value of the airflow is reduced through the airflow regulating device to reduce the growth speed of the crystal.
In some embodiments, referring to fig. 11, the control method further comprises: comparing the current weight of the airflow sensing device with a set second threshold range, wherein the second threshold range is the weight range of the airflow sensing device when the built-in part 103 of the weight sensing unit elements in a second preset number range is suspended in the shell 101, and the second threshold range is larger than the first threshold range; and if the current weight of the airflow sensing device is smaller than the second threshold range, reducing the flow parameter value of the current airflow through the airflow regulating and controlling device so as to reduce the growth speed of the crystal. The control method is mainly used in the early stage and the later stage of crystal growth, the temperature in the crystal growth furnace 800 is lower in the early stage and the later stage of crystal growth, and the sublimation temperature of carbon is lower than the sublimation temperature of silicon, so that the growth defects of impurities such as carbon packages and the like in the early stage and the later stage of crystal growth of the silicon carbide crystal are reduced or even avoided, the weight of the air flow induction device (namely the state of the air flow induction unit element 100) is controlled by adjusting the flow rate of mixed air flow through the embodiment, the upward diffusion speed of the air flow is adjusted through the air flow induction device, and the growth speed of the silicon carbide crystal is further controlled.
In some embodiments, a method of increasing a current flow parameter value of a gas through a gas flow regulating device comprises: controlling the carrier gas flow rate to increase the flow parameter value of the gas flow; the method for reducing the current gas flow parameter value through the gas flow regulating and controlling device comprises the following steps: the carrier gas flow rate is controlled to decrease the flow parameter value of the gas flow. The flow parameter value of the gas stream is controlled by the flow rate of the carrier gas.
In some embodiments, a method of increasing a current flow parameter value of a gas through a gas flow regulating device comprises: controlling the crystal growth temperature to be increased so as to increase the sublimation rate of the silicon carbide powder 400 and further increase the flow parameter value of the airflow; the method for reducing the current gas flow parameter value through the regulating device comprises the following steps: the temperature of the grown crystal is controlled to be reduced so as to reduce the sublimation rate of the silicon carbide powder 400 and further reduce the flow parameter value of the airflow. Of course, other means such as controlling the pressure may be employed, but for the accuracy of the control, the present embodiment preferably controls the flow parameter value of the gas flow by controlling the flow rate of the carrier gas and the growth temperature.
To further clarify the control method of the present invention, the control method of the present invention is further illustrated by the following two preferred embodiments:
example 1: taking the example of adjusting the flow parameter value of the gas flow by adjusting the flow rate of the carrier gas, the carrier gas is one or more of argon, helium and nitrogen, and in this embodiment, the carrier gas is preferably argon.
The air flow sensing apparatus of the present embodiment includes an air flow sensing unit 100, and a filter cartridge 300 carrying the air flow sensing unit 100, where the housing 101 and the built-in part 103 of the air flow sensing unit 100 are both spheres, and preferably, the volume ratio of the built-in part 103 to the housing 101 is 1:6, the airflow induction device is made of graphite materials.
The first threshold range is: 85% -100% of the weight of the airflow sensing unit piece 100 in the second state, wherein the second threshold range is as follows: 85% -100% of the weight of the airflow sensing unit piece 100 in the first state, and the outer size of the filtering loading box 300 is matched with the inner size of the crucible 200; the weight sensing device 600 weighs the airflow sensing device in the first manner (see fig. 6); the airflow regulating and controlling device is a controller (hereinafter referred to as a controller) of the silicon carbide growth equipment, and the specific method comprises the following steps:
1) Placing the silicon carbide powder 400 into the crucible 200, and installing an airflow sensing device at the top end of a weighing rod of the weight sensing device 600, wherein the airflow sensing device is suspended 10mm above the silicon carbide powder 400, so that a 10mm space is formed between the filtering and loading box 300 and the silicon carbide powder 400, and then a cover adhered with seed crystals 500 is covered, and the airflow sensing device of the embodiment is laid in three layers;
2) The crucible 200 covered with the lid is entirely placed in the growth chamber of the silicon carbide apparatus and seated on the growth base 700, and the weight sensing device 600 on the growth base 700 weighs the airflow sensing device in real time.
3) Controlling a vacuum pump to vacuumize the growth chamber through a controller, controlling the pressure in the growth chamber to be 300pa, controlling the crystal growth temperature to be 2250 ℃, controlling a gas carrying valve to be opened, controlling the flow rate of the carrier gas to be 100sccm, and introducing the carrier gas into the growth chamber from bottom to top;
4) The controller controls a heater in the silicon carbide growth equipment to work to heat the crucible 200, when the temperature in the crucible 200 reaches more than 2100 ℃, the silicon carbide powder 400 is heated and sublimated into silicon carbide gas under the drive of axial temperature gradient, and is mixed with carrier gas permeating into the crucible 200 to form mixed gas flow, when the mixed gas flow passes through the gas flow induction device in the upward diffusion process, on one hand, the gas flow induction device is made of graphite and has a porous spherical structure with a large specific surface area, the gas flow induction device effectively adsorbs a carbon source in the mixed gas, defects in the silicon carbide crystal growth process are reduced, on the other hand, the flow velocity of the mixed gas flow exerts certain buoyancy on the built-in part 103, the weight of the built-in part 103 is changed, and the weight induction device 600 acquires the current weight of the gas flow induction device and transmits the acquired current weight information to the controller;
5) The controller compares the received current weight of the airflow sensing device with a first threshold range and a second threshold range stored in the controller, adjusts the flow parameter value of the airflow according to the comparison result, and further controls the growth speed of the silicon carbide crystal, which specifically comprises the following steps:
silicon carbide crystal growth earlier stage (heating stage):
the crucible 200 is in a silicon-rich gas atmosphere, if the current weight of the gas flow sensing device is less than the second threshold range, which indicates that the flow rate of the mixed gas flow is too large, and part of the gas flow sensing unit pieces 100 are in the second or third state, the controller controls the flow rate of the carrier gas to be reduced, i.e. controls the gas carrying valve to reduce the opening degree, and reduces the flow rate of the carrier gas, so that the flow rate of the mixed gas flow is reduced, 85% -100% of the gas flow sensing unit pieces 100 are in the first state, even if the current weight of the gas flow sensing device is equal to or greater than the second threshold range, so that the upward diffusion speed of the mixed gas flow is reduced through the gas flow sensing device, and the growth speed of the silicon carbide crystal is reduced.
If the current weight of the gas flow sensing device is equal to or greater than the second threshold range, the flow rate of the mixed gas flow is the optimal flow rate of the stage, namely the flow rate is the optimal growth rate of the silicon carbide crystal at the stage, and the flow parameter value of the gas flow does not need to be adjusted.
In this stage, since the mixed gas mass moves to the surface of the seed crystal, starts spiral growth and is stacked one on another, the slow growth of the crystal is controlled in order to prevent the phase change caused by misarrangement of atoms.
In the middle growth stage of the silicon carbide crystal:
if the current weight of the airflow sensing device is larger than the first threshold range, it is indicated that the flow rate of the mixed airflow is too small, so that part of the airflow sensing unit 100 is in the first state, that is, the built-in part 103 blocks part of the air holes 102 in the bottom wall of the housing 101, further reducing the upward diffusion speed of the mixed airflow, and reducing the growth speed of the silicon carbide gas, the controller controls the carrier gas valve to increase the opening degree and increase the carrier gas flow rate, so that the flow rate of the mixed airflow is increased, so that 85% -100% of the airflow sensing unit 100 is in the second state, that is, the built-in part 103 is in a suspended state in the housing 101, when the mixed airflow passes through the airflow sensing device, the upward diffusion speed of the mixed airflow is not affected, and the growth speed of the silicon carbide crystal is increased;
if the current weight of the airflow sensing device is smaller than the first threshold range, which indicates that the flow rate of the mixed airflow is too large, so that most of the airflow sensing units are in the third state, that is, the built-in part 103 blocks part of the air holes 102 on the top wall of the shell 101, when the mixed airflow passes through the airflow sensing adjusting device, the upward diffusion speed of the mixed airflow is reduced, so that the growth speed of the silicon carbide crystal is reduced, the controller controls the air carrying valve to reduce the opening degree, so as to reduce the flow rate of the mixed airflow, so that 85% -100% of the airflow sensing units 100 are in the second state, and therefore the flow rate of the mixed airflow is not affected when passing through the airflow sensing device, so as to accelerate the growth speed of the silicon carbide crystal.
If the current weight of the airflow sensing device is equal to the first threshold range, the flow rate of the mixed airflow is the optimal flow rate of the mixed airflow in the stage, namely the flow rate is the optimal growth rate of the silicon carbide crystal, so that the high-quality silicon carbide crystal can be grown conveniently without adjusting the flow parameter value of the airflow.
The mixed gas concentration in the crucible is high at this stage, the mixed gas mass is easy to stack on a new growth interface, and thick crystal ingots are easy to grow, so that the rapid growth of crystals is controlled at this stage.
In the later growth stage (temperature reduction stage) of the silicon carbide crystal:
if the current weight of the air flow sensing device is smaller than the second threshold range, which indicates that the flow rate of the mixed air flow is too high, so that part of the air flow sensing unit 100 is in the second or third state, the controller controls the flow rate of the carrier air flow to be reduced, namely controls the carrier air valve to reduce the opening degree, so as to reduce the flow rate of the mixed air flow, so that 85% -100% of the air flow sensing unit 100 is in the first state, namely the built-in part 103 blocks part of the air holes 102 in the bottom wall of the shell 101, and therefore the upward diffusion speed of the mixed air flow is reduced through the air flow sensing device, the growth speed of the silicon carbide crystal is further reduced, meanwhile, the carbon wrapping in the later stage of the crystal ingot is reduced, and the overall quality of the silicon carbide crystal is improved.
If the current weight of the airflow sensing device is equal to or greater than the second threshold range, the flow rate of the mixed airflow is the optimal flow rate at the stage, namely the flow rate is the optimal growth rate of the silicon carbide crystal, so that the high-quality silicon carbide crystal can be grown conveniently without adjusting the flow parameter value of the airflow.
The ratio of silicon carbide in the mixed gas in the crucible is reduced and the ratio of carbon particles and other impurities in the mixed gas is increased at this stage, so that the growth speed of the crystal needs to be reduced, the slow growth of the crystal is controlled at this stage, and the quality of the crystal at the tail end of the ingot is maintained.
6) And finishing the growth of the silicon carbide crystal ingot, and taking out the crystal ingot.
Example 2: take the regulation of the flow parameter value of the air flow by regulating the crystal growth temperature as an example
The difference between the present embodiment and embodiment 1 is that the present embodiment controls the flow parameter value of the airflow by adjusting the crystal growth temperature, so as to adjust the position of the embedded component 103 in the housing 101, so that the airflow sensing unit 100 is in different states, and the current weight of the airflow sensing device is used to visualize and determine the flow parameter value of the airflow, and the specific differences are as follows:
silicon carbide crystal growth early stage (heating stage):
the crucible 200 is in a silicon-rich gas atmosphere, if the current weight of the airflow sensing device is smaller than a second threshold range, which indicates that the flow rate of the mixed airflow is too high, and thus part of the airflow sensing unit pieces 100 are in a second or third state, the controller controls the crystal growth temperature to be reduced, namely, the power of the heater is reduced, so that the sublimation rate of the silicon carbide powder 400 is reduced, the flow rate of the mixed airflow is reduced, 85% -100% of the airflow sensing unit pieces 100 are in a first state, and the upward diffusion speed of the mixed airflow is reduced through the airflow sensing device, so that the growth speed of the silicon carbide crystal is reduced.
If the current weight of the airflow sensing device is equal to or larger than the second threshold range, the flow rate of the mixed airflow is the optimal flow rate of the stage, and the flow parameter value of the airflow does not need to be adjusted.
In the middle growth stage of the silicon carbide crystal:
if the current weight of the airflow sensing device is greater than the first threshold range, it is indicated that the flow rate of the mixed airflow is too small, so that part of the airflow sensing unit 100 is in the first state, that is, the built-in component 103 blocks part of the air holes 102 in the bottom wall of the shell 101, further reducing the upward diffusion rate of the mixed airflow, and causing the growth rate of the silicon carbide gas to be slow, the controller controls the crystal growth temperature to be increased, that is, the power of the heater is increased, so as to increase the sublimation rate of the silicon carbide powder 400, thereby increasing the flow rate of the mixed airflow, so that 85% -100% of the airflow sensing unit 100 is in the second state, and since all the air holes 102 are in the open state when the airflow sensing unit 100 is in the second state, the flow rate of the mixed airflow is not affected by the airflow sensing device, thereby accelerating the growth rate of the silicon carbide crystal;
if the current weight of the airflow sensing device is smaller than the first threshold range, it indicates that the flow rate of the mixed airflow is too high, so that part of the airflow sensing units is in the third state, that is, the built-in part 103 blocks part of the air holes 102 on the top wall of the housing 101, and when the mixed airflow passes through the airflow sensing adjustment device, the upward diffusion speed of the mixed airflow is reduced, so that the growth speed of the silicon carbide crystal is reduced, the controller controls the crystal growth temperature to be reduced, so as to reduce the sublimation rate of the silicon carbide powder 400, so that the flow rate of the mixed airflow is reduced, so that 85% -100% of the airflow sensing units 100 are in the second state, that is, the built-in part 103 is in a suspended state in the housing 101, so that the flow rate of the mixed airflow is not affected when passing through the airflow sensing device, and the growth speed of the silicon carbide crystal is further increased.
If the current weight of the airflow sensing device is equal to the first threshold range, the flow rate of the mixed airflow is the optimal flow rate in the stage, so that high-quality silicon carbide crystals can be grown conveniently without adjusting the flow parameter values of the airflow. Multiple experiments prove that the optimal flow rate of the mixed gas flow at the stage is 3-7g/h.
In the later growth stage (temperature reduction stage) of the silicon carbide crystal:
if the current weight of the airflow sensing device is smaller than the second threshold range, which indicates that the sublimation rate of the silicon carbide powder 400 is too high, the flow rate of the mixed airflow is too high, and part of the airflow sensing unit pieces 100 are in the second or third state, the controller controls the crystal growth temperature to be reduced, so that the sublimation rate of the silicon carbide powder 400 is reduced, the flow rate of the mixed airflow is reduced, the growth speed of the silicon carbide crystal is reduced, meanwhile, 85% -100% of the airflow sensing unit pieces 100 are in the first state, namely, the built-in piece 103 blocks part of the air holes 102 in the bottom wall of the shell 101, the upward diffusion speed of the silicon carbide powder 400 is reduced, the growth speed of the silicon carbide crystal is further reduced, meanwhile, the later-stage carbon wrapping of the crystal ingot is reduced, and the overall quality of the silicon carbide crystal is improved.
If the current weight of the airflow sensing device is equal to or greater than the second threshold range, the flow parameter value of the mixed airflow is the optimal speed at the stage, and the flow parameter value of the airflow does not need to be adjusted.
The control method of the embodiment effectively reduces the carbon-silicon atomic ratio in the gas phase, reduces or even avoids the formation of impurities such as carbon coating in the growing silicon carbide crystal, improves the quality of the silicon carbide crystal, effectively reduces the production cost of enterprises, and improves the economic benefit of the enterprises. The invention adjusts the flow parameter value of the air flow according to the weight change of the air flow induction device, and simultaneously reflects the flow parameter value of the mixed air flow through the weight of the air flow induction device, thereby calculating the growth speed of the silicon carbide crystal, enabling the crystal growth speed to be visualized and realizing the control of the crystal growth speed in the growth process of the silicon carbide crystal. The invention optimizes the process, thereby growing a perfect crystal ingot.
According to the crystal growth furnace 800 of the embodiment of the invention, the crystal growth furnace 800 comprises the control system for the growth speed of the silicon carbide crystal of the embodiment.
The control system includes:
the device comprises an airflow sensing device, the airflow sensing device is arranged on silicon carbide powder 400, the silicon carbide powder 400 is contained in a crucible 200, the airflow sensing device is composed of a plurality of airflow sensing unit pieces 100, each airflow sensing unit piece 100 comprises a containing cavity formed by a shell 101 and an embedded piece 103 arranged in the containing cavity, a plurality of air holes 102 are formed in the shell 101, in the crystal growth process, airflow flows to the direction of silicon carbide seed crystals 500 through the containing cavity through the air holes 102, and the embedded pieces 103 are suitable for moving in the containing cavity under the power action of the airflow;
a weight sensing means 600, the weight sensing means 600 being for sensing a current weight of the air flow sensing means in a process of moving the built-in unit 103;
and the airflow regulating device is connected with the weight sensing device 600 and is used for regulating the flow parameter value of the airflow according to the current weight of the airflow sensing device so as to control the growth speed of the silicon carbide crystal.
According to the control system provided by the invention, the current weight of the airflow sensing device is measured in real time through the weight sensing device 600, and the flow parameter value of the airflow is adjusted according to the measured current weight, so that the growth speed of the silicon carbide crystal is controlled, meanwhile, a worker can know the flow parameter value of the current airflow according to the measured current weight and calculate the growth speed of the silicon carbide crystal according to the flow parameter value, and the growth speed of the silicon carbide crystal is visualized.
Other configurations of the 8230, such as 8230and 8230, and the like, and operations according to embodiments of the present invention are known to those of ordinary skill in the art and will not be described in detail herein.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are not to be considered limiting of the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; the connection can be mechanical connection, electrical connection or communication; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood according to specific situations by those of ordinary skill in the art.
In the present invention, unless otherwise expressly stated or limited, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through an intermediate. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Moreover, various embodiments or examples and features of various embodiments or examples described in this specification can be combined and combined by one skilled in the art without being mutually inconsistent.
While embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims (10)
1. A system for controlling the growth rate of a silicon carbide crystal, comprising:
the gas flow induction device is arranged on the silicon carbide powder, the silicon carbide powder is placed in the crucible, the gas flow induction device is composed of a plurality of gas flow induction unit pieces, each gas flow induction unit piece comprises a containing cavity formed by a shell and an embedded piece arranged in the containing cavity, a plurality of gas holes are formed in the shell, in the crystal growth process, gas flows to the direction of silicon carbide seed crystals through the containing cavity through the gas holes, and the embedded pieces are suitable for moving in the containing cavity under the power action of the gas flow;
a weight sensing means for sensing a current weight of the air flow sensing means during movement of the insert;
and the airflow regulating and controlling device is connected with the weight sensing device and is used for regulating the flow parameter value of the airflow according to the current weight of the airflow sensing device so as to control the growth speed of the silicon carbide crystal.
2. The system for controlling the growth rate of a silicon carbide crystal according to claim 1, wherein the gas flow sensing unit is adapted to form, under the power of the gas flow: the first state that the built-in part is contacted with the inner side surface of the shell close to the silicon carbide powder, the second state that the built-in part is suspended in the shell, or the third state that the built-in part is contacted with the inner side surface of the shell far away from the silicon carbide powder.
3. The system for controlling the growth rate of silicon carbide crystals according to claim 1 or 2, wherein the gas flow induction unit is made of graphite, and a plurality of gas flow induction units are closely arranged on the silicon carbide powder.
4. The system for controlling the growth rate of a silicon carbide crystal according to claim 3, wherein the airflow sensing device further comprises a filtering loading box, a containing cavity is formed in the filtering loading box, the containing cavity is provided with open openings which are arranged oppositely, and the airflow sensing unit is arranged in the containing cavity and can freely move in the containing cavity.
5. A system for controlling the growth rate of a silicon carbide crystal according to claim 1 or claim 2 wherein the gas flow inducing means forms a plenum with the silicon carbide powder.
6. A method for controlling the growth rate of a silicon carbide crystal, comprising the apparatus of any one of claims 1-5, and comprising the steps of:
the weight sensing device acquires the current weight of the airflow sensing device;
comparing the current weight of the airflow sensing device with a set first threshold range, wherein the first threshold range is the weight range of the airflow sensing device when the built-in piece of the weight sensing unit piece in a first preset number range is suspended in the shell;
if the current weight of the airflow sensing device is larger than the first threshold range, increasing the current flow parameter value of the airflow through an airflow regulating device to increase the crystal growth speed, and if the current weight of the airflow sensing device is smaller than the first threshold range, reducing the current flow parameter value of the airflow through the airflow regulating device to reduce the crystal growth speed.
7. A method according to claim 6, further comprising:
comparing the current weight of the airflow sensing device with a set second threshold range, wherein the second threshold range is the weight range of the airflow sensing device when the built-in piece of the weight sensing unit piece in a second preset number range is suspended in the shell, and the second threshold range is larger than the first threshold range;
and if the current weight of the airflow sensing device is smaller than the second threshold range, reducing the flow parameter value of the current airflow through an airflow regulating and controlling device so as to reduce the crystal growth speed.
8. A method according to claim 6 or 7, wherein the silicon carbide crystal growth rate is controlled by the control of the growth rate,
the method for increasing the current flow parameter value of the gas through the gas flow regulating and controlling device comprises the following steps: controlling the carrier gas flow rate to increase the flow parameter value of the gas flow;
the method for reducing the current gas flow parameter value through the gas flow regulating device comprises the following steps: the carrier gas flow rate is controlled to decrease the flow parameter value of the gas flow.
9. A method for controlling the growth rate of a silicon carbide crystal according to claim 6 or 7 wherein the method of increasing the current flow parameter value of the gas through the gas flow regulating device comprises: controlling the crystal growth temperature to be increased so as to increase the sublimation rate of the silicon carbide powder and further increase the flow parameter value of the airflow;
the method for reducing the current gas flow parameter value through the regulating device comprises the following steps: the crystal growth temperature is controlled to be reduced so as to reduce the sublimation rate of the silicon carbide powder and further reduce the flow parameter value of the airflow.
10. A silicon carbide crystal growth furnace, characterized in that the crystal growth furnace comprises a control system for the growth rate of a silicon carbide crystal according to any one of claims 1 to 5.
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| CN112481699A (en) * | 2020-11-11 | 2021-03-12 | 山东天岳先进科技股份有限公司 | Preparation method of high-quality silicon carbide single crystal and silicon carbide single crystal |
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| JP2013126931A (en) * | 2011-12-19 | 2013-06-27 | Showa Denko Kk | Apparatus for producing silicon carbide single crystal, and method for producing silicon carbide single crystal |
| CN112481699A (en) * | 2020-11-11 | 2021-03-12 | 山东天岳先进科技股份有限公司 | Preparation method of high-quality silicon carbide single crystal and silicon carbide single crystal |
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