CN115287762A - Crystal crystal interface control device and silicon carbide crystal growth method - Google Patents

Crystal crystal interface control device and silicon carbide crystal growth method Download PDF

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Publication number
CN115287762A
CN115287762A CN202211219373.9A CN202211219373A CN115287762A CN 115287762 A CN115287762 A CN 115287762A CN 202211219373 A CN202211219373 A CN 202211219373A CN 115287762 A CN115287762 A CN 115287762A
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crystal
tray
graphite
conductive coil
graphite rod
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CN202211219373.9A
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CN115287762B (en
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薛卫明
马远
潘尧波
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Clc Semiconductor Co ltd
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Clc Semiconductor Co ltd
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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
    • 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
    • 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
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/10—Heating of the reaction chamber or the substrate
    • 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
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/16—Controlling or regulating

Abstract

The invention provides a crystal crystallization interface control device and a silicon carbide crystal growth method, and particularly relates to the technical field of crystal growth. The crystal crystallization interface control device comprises a tray, a plurality of graphite rods, a plurality of conductive coils and a plurality of lifting mechanisms, wherein the graphite rods are arranged on one side of the tray, which is far away from the seed crystals, and a space is reserved between the graphite rods and the tray; the plurality of conductive coils are respectively sleeved on the plurality of graphite rods correspondingly, and are connected with an alternating current power supply; the plurality of lifting mechanisms are respectively used for controlling the distance between the corresponding plurality of graphite rods and/or the plurality of conductive coils and the tray. And adjusting the distance between the corresponding graphite rod and/or conductive coil and the tray by using the lifting mechanism, so that the temperature distribution on the tray meets the temperature distribution of the required crystal crystallization interface shape. When the control device provided by the invention is used for growing crystals, the consistency of a crystallization interface is better, and the yield of subsequent epitaxy and devices is improved.

Description

Crystal crystal interface control device and silicon carbide crystal growth method
Technical Field
The invention relates to the technical field of crystal growth, in particular to a crystal crystallization interface control device and a silicon carbide crystal growth method.
Background
Silicon carbide crystal as semiconductor substrate material may be used in producing silicon carbide-base power device and microwave RF device via epitaxial growth, device manufacture and other steps. When a silicon carbide single crystal substrate is prepared, a bulk crystal is generally obtained by Physical Vapor Transport (PVT) method or Liquid Phase Epitaxy (LPE) growth, and then a substrate sheet is obtained by machining. Therefore, the quality of the bulk crystal directly determines the quality of the silicon carbide single crystal substrate, and the defects on the bulk crystal determine the order of magnitude of the fundamental defects of the silicon carbide single crystal substrate.
At present, methods for controlling defects of a silicon carbide single crystal substrate include: after the crystal patterning treatment, the defects are repaired by utilizing the lateral growth of the crystal, such as patent CN111958070B and JP2006052097A; in addition, a special atmosphere is added in the PVT growth environment or the structure of a seed crystal tray is adjusted, such as patents CN112160028A, CN106435734A and US7501022B 2; the PVT gas phase transportation process is improved, and the purity of the raw material is improved so as to avoid the defects caused by impurities, such as CN110983434A and US8741413B2; and more so, the defects, such as CN1926266A and CN111051581A, are improved by using a Chemical Vapor Deposition (CVD) process. However, the above solution has many disadvantages, such as patterned seed crystal, or seed crystal holder special structure, in which the shape of crystal growth interface is only fixed and changed in the initial stage during the growth process, and the crystallization interface is not controlled during most of the crystal growth process; improvements in gas phase transport processes may have some improvements in micropipe or carbon encapsulation, but not in Stacking Faults (SF), threading dislocations (TSD) or Basal Plane Dislocations (BPD). The CVD process can improve the number of defects on the substrate wafer to some extent, but the TSD is not repaired or only replaced by SF defects during the epitaxy process.
Therefore, it is desirable to provide a growth method that can control the crystalline interface of a silicon carbide crystal to ameliorate the above problems.
Disclosure of Invention
In view of the above disadvantages of the prior art, the present invention provides a crystal interface control device and a method for growing a silicon carbide crystal to control the crystal interface of the silicon carbide crystal and improve the crystal quality.
In order to achieve the above objects and other related objects, the present invention provides a crystal crystallization interface control device, including a tray, a plurality of graphite rods, a plurality of conductive coils and a plurality of lifting mechanisms, wherein the tray is used for mounting a seed crystal, the plurality of graphite rods are disposed on a side of the tray away from the seed crystal, and a space is left between the graphite rods and the tray; the number of the conductive coils is equal to that of the graphite rods, the conductive coils are respectively sleeved on the graphite rods, and the conductive coils are connected with an alternating current power supply; the number of the lifting mechanisms is equal to that of the graphite rods, and the plurality of lifting mechanisms are respectively used for controlling the distance between the plurality of graphite rods and/or the plurality of conductive coils and the tray; after the conductive coil is connected with the alternating current power supply, the lifting mechanism is utilized to adjust the distance between the corresponding graphite rod and/or the conductive coil and the tray, so that the seed crystal at the corresponding position has the corresponding temperature, and the crystal crystallization interface is adjusted.
In an example of the invention, the tray, the graphite rod and the conductive coil are all made of graphite materials, and the density of the graphite materials is 1.6-1.8 g/cm 3 The thermal conductivity is 80 to 150 Wm -1 K -1 The resistivity is 1 to 50 [ mu ] omega m.
In an example of the invention, the frequency of the alternating current power supply is 0.1 to 10 KHz, the voltage of the alternating current power supply loaded on the conductive coil is 0.1 to 20V, or the current of the alternating current power supply loaded on the conductive coil is 0.1 to 10A.
In an example of the present invention, the lifting mechanism includes a first lifting mechanism for driving the graphite rod and a second lifting mechanism for driving the conductive coil, the first lifting mechanism includes a first driving device, a first lifting platform and a first connecting rod, the first driving device drives the first lifting platform to lift, the first connecting rod is mounted on the first lifting platform, one end of the graphite rod is connected to the first connecting rod, and the other end of the graphite rod extends towards the direction of the tray; the second lifting mechanism comprises a second driving device, a second lifting platform and a second connecting rod, the second driving device is used for driving the second lifting platform to lift, the second connecting rod is installed on the second lifting platform, and the conductive coil is installed at the bottom of the second connecting rod and sleeved on the graphite rod.
In an example of the present invention, the first driving device and the second driving device have the same structure, the first driving device includes a driving motor, a lead screw and a bellows, one end of the lead screw is connected to an output shaft of the driving motor, the other end of the lead screw is rotatably mounted on a flange outside the crystal growth apparatus, the first lifting platform is in threaded connection with the lead screw, the bellows is sleeved on the outside of the first connecting rod, one end of the bellows is fixed on the first lifting platform, and the other end of the bellows is fixed on the flange.
In an example of the present invention, the crystal crystallization interface control device further includes a temperature measuring mechanism for measuring a temperature of the graphite rod, and the temperature measuring mechanism is connected to one end of the graphite rod.
In another aspect, the present invention provides a method for growing silicon carbide crystals, comprising at least the steps of:
providing a crystal crystallization interface control device of the invention;
mounting a silicon carbide seed crystal on a tray of the crystal crystallization interface control device, and placing the crystal crystallization interface control device in crystal growth equipment;
adjusting the temperature and pressure in the crystal growth equipment, adjusting the distance between a graphite rod and/or a conductive coil at a corresponding position and the tray according to the shape of a required crystal crystallization interface, and simultaneously loading alternating current to the conductive coil to keep the growth for 1 to 50 hours so as to determine an initial growth interface of the crystal;
keeping the temperature and the pressure in the crystal growth equipment unchanged, and gradually adjusting the distance between the graphite rod and/or the conductive coil at the corresponding position and the tray in the growth process according to the defect distribution condition of the initial growth interface of the crystal, so that the crystal stably grows for 50 to 150 hours;
adjusting the pressure of the crystal growth equipment to 50-500 mbar, and gradually adjusting the distance between the graphite rod and/or the conductive coil and the tray within 10-20 h to ensure that the temperature difference between the graphite rod at the edge part and the graphite rod at the center part is 5-55 ℃ so as to reduce the temperature difference between the axial direction and the radial direction of the crystal;
and (5) after the growth is finished, cooling and taking out the crystal.
In an example of the present invention, the determining the initial crystal growth interface includes: heating the temperature of the raw materials in the crystal growth equipment to 1600-2400 ℃, and adjusting the pressure in the crystal growth equipment to 200-800 mbar; and when the temperature of the raw materials is raised to 1700-2500 ℃, and the pressure in the crystal growth equipment is reduced to 0.1-100 mbar, adjusting the distance between the graphite rod and/or the conductive coil at the corresponding position and the tray, so that the crystal grows for 1-50 hours according to the required shape.
In an example of the invention, in the process of crystal growth, the distance between the graphite rod and the tray is 0.5-50 mm.
In one example of the invention, in the crystal growth process, the conductive coil and the graphite rod generate relative displacement of 0-100 mm.
In one example of the invention, the control of the pressure in the crystal device is realized by adjusting the content of inert gas in the crystal device, and the inert gas can be argon (Ar) or nitrogen (N) 2 ) Or hydrogen (H) 2 ）。
According to the crystal crystallization interface control device, a plurality of graphite rods and conductive coils are arranged on one side of the tray, and eddy currents are generated in the graphite rods and the tray locally or in the conductive crystals by loading alternating current on the conductive coils; the distances between the graphite rods and/or the conductive coils at different positions and the tray are adjusted through the lifting mechanism, so that the joule heat generated by the eddy currents at different positions is different, the temperatures at different positions of the tray are adjusted, and the control of a crystal crystallization interface is realized. The crystal growth interface can be changed in the growth process by adopting the crystal crystallization interface control device to grow the silicon carbide crystal, so that the microscopic defects in the crystal are reduced, and the uniform doping concentration in the crystal is improved; meanwhile, in the later stage of crystal growth, a smaller temperature gradient can be obtained, and high-quality silicon carbide single crystals can be obtained.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts:
FIG. 1 is a schematic structural diagram of a crystal crystallization interface control device according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a lifting mechanism in an embodiment of a crystal crystallization interface control apparatus according to the present invention;
FIG. 3 is a schematic diagram of the distribution of a graphite rod and a conductive coil over a tray in an embodiment of the crystal crystallization interface control apparatus of the present invention;
FIG. 4 is a flow chart of a method of growing a silicon carbide crystal according to the present invention;
FIG. 5 is a photograph of a silicon carbide substrate prepared in one embodiment of a silicon carbide crystal growth method of the invention;
FIG. 6 is a photograph of a silicon carbide substrate prepared in another embodiment of a silicon carbide crystal growth method of the invention;
fig. 7 is a photograph of a silicon carbide substrate prepared in a comparative example.
Description of the element reference numerals
100. A tray; 110. seed crystal; 120. a graphite rod; 130. a conductive coil; 140. a lifting mechanism; 141. a first lifting mechanism; 1411. a first driving device; 14111. a drive motor; 14112. a screw rod; 14113. a bellows; 1412. a first lifting platform; 1413. a first connecting rod; 142. a second lifting mechanism; 1421. a second driving device; 1422. a second lifting platform; 1423. a second connecting rod; 200. a crucible; 210. raw materials; 220. and (4) a flange.
Detailed Description
The following embodiments of the present invention are provided by specific examples, and other advantages and effects of the present invention will be readily apparent to those skilled in the art from the disclosure of the present invention. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention. It is to be noted that the features in the following embodiments and examples may be combined with each other without conflict. It is also to be understood that the terminology used in the examples is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present invention. Test methods in which specific conditions are not specified in the following examples are generally carried out under conventional conditions or under conditions recommended by the respective manufacturers.
It should be understood that the terms "upper", "lower", "left", "right", "middle" and "one" used herein are for clarity of description only, and are not intended to limit the scope of the invention, and that changes or modifications in the relative relationship may be made without substantial technical changes and modifications.
Referring to fig. 1 to 7, the present invention provides a crystal growth interface control apparatus and a crystal growth method, which can change a crystal growth interface, reduce crystal micro defects, and improve crystal quality.
Referring to fig. 1 to 3, the crystal crystallization control apparatus of the present invention includes a tray 100, a plurality of graphite rods 120, a plurality of conductive coils 130, and a plurality of lifting mechanisms 140, wherein the tray 100 is used for mounting seed crystals 110, and the number of the lifting mechanisms 140, the graphite rods 120, and the conductive coils 130 is the same; a plurality of graphite rods 120 are arranged on one side of the tray 100, which faces away from the seed crystal 110, and the graphite rods 120 are spaced from the tray 100; the conductive coil 130 is a spiral coil, the conductive coils 130 are respectively sleeved on the graphite rods 120 correspondingly, and the conductive coils 130 are connected with an alternating current power supply; the plurality of lifting mechanisms 140 are respectively used for controlling the distance between the plurality of graphite rods 120 and/or the plurality of conductive coils 130 and the tray 100, wherein after the conductive coils 130 are connected with an alternating current power supply, eddy currents are generated inside the graphite rods 120, the tray 100 and/or the conductive type crystals, and the lifting mechanisms 140 are used for adjusting the distance between the graphite rods 120 and/or the conductive coils 130 at the corresponding positions and the tray 100, so that the seed crystals at the corresponding positions have corresponding temperatures, and the temperature distribution of the tray 100 meets the temperature distribution of the shape of the crystal interface of the required crystal, thereby achieving the purpose of adjusting the crystal interface.
Referring to fig. 1, in an embodiment, the tray 100, the graphite rod 120, and the conductive coil 130 are made of graphite material, and the density of the graphite material is 1.6 to 1.8 g/cm 3 The thermal conductivity is 80 to 150 Wm -1 K -1 The resistivity is 1 to 50 [ mu ] omega m. The density of the graphite material can be 1.6 to 1.8 g/cm 3 Of any value, e.g. 1.6 g/cm 3 、1.7 g/cm 3 Or 1.8 g/cm 3 Etc.; the thermal conductivity of the graphite material can be 80 to 150 Wm -1 K -1 Of any value, e.g. 80 Wm -1 K -1 、100 Wm -1 K -1 、120 Wm -1 K -1 Or 150 Wm -1 K -1 Etc.; the resistivity of the graphite material may be any value within 1 to 50 [ mu ] omega m, for example, 1 [ mu ] omega m, 10 [ mu ] omega m, 30 [ mu ] omega m or 50 [ mu ] omega m. The graphite material has good conductivity, when alternating current is introduced into the conductive coil 130, the conductive coil 130 generates an alternating magnetic field, because the graphite rod 120 (conductor) in the middle of the conductive coil 130 is a closed circuit which can be equivalent to a circle in the circumferential direction, and the magnetic flux in the closed circuit is continuously changed, induced electromotive force and induced current can be generated in the circumferential direction of the graphite rod 120, and the direction of the current is rotated along the circumferential direction of the graphite rod to form an eddy current. The eddy current generates heat in the graphite rod 120, and the temperature of the tray 100 at different positions can be adjusted by changing the distance between the graphite rod 120 at different positions and the tray 100, thereby achieving the purpose of adjusting the crystal crystallization interface. Preferably, one end of the graphite rod 120 is connected to a temperature measuring mechanism (not shown), and the temperature of the graphite rod 120 can be obtained in real time through the temperature measuring mechanism.
As an example, the frequency of the ac power supply connected to the conductive coil 130 is 0.1 KHz to 10 KHz, and may be any value within 0.1 KHz to 10 KHz, such as 0.1 KHz, 3 KHz, 7 KHz, or 10 KHz. The voltage loaded on the conductive coil 130 by the alternating current power supply is 0.1-20V, for example, the voltage can be any value within 0.1-20V such as 0.1V, 5V, 10V, 15V or 20V; or the current loaded on the conductive coil 130 by the alternating current power supply is 0.1 to 10A, for example, the current can be any value within 0.1 to 10A such as 0.1A, 3A, 7A or 10A.
Referring to fig. 1 to 3, a plurality of graphite rods 120 and a plurality of conductive coils 130 are respectively suspended above the tray 100 by a plurality of lifting mechanisms 140, and preferably, the plurality of graphite rods 120 are uniformly distributed above the tray 100. The number of the graphite rod 120, the conductive coil 130 and the lifting mechanism 140 is not limited herein, and the number of the graphite rod, the conductive coil 130 and the lifting mechanism 140 is consistent. In an example, nine graphite rods 120 and nine conductive coils 130 are uniformly distributed above the tray 100, the nine graphite rods 120 are radially distributed above the tray 100, that is, one graphite rod 120 is arranged corresponding to the center of the tray 100, four graphite rods 120 in the outer ring of the central graphite rod 120 are uniformly arranged in the outer ring of the central graphite rod 120, and four graphite rods 120 are uniformly arranged outside the graphite rods 120 in the outer ring of the outer ring. Correspondingly, the bottom of each graphite rod 120 is sleeved with a conductive coil 130. The nine graphite rods 120 and the nine conductive coils 130 are lifted and lowered by nine lifting mechanisms 140, respectively.
Referring to fig. 1 and 2, in an embodiment, the lifting mechanism 140 includes a first lifting mechanism 141 and a second lifting mechanism 142, the first lifting mechanism 141 is used for adjusting the lifting of the graphite rod 120 to adjust the distance between the graphite rod 120 and the tray 100; the second elevating mechanism 142 is used to adjust the elevation of the conductive coil 130 to adjust the distance between the conductive coil 130 and the tray 100. In this embodiment, the first lifting mechanism 141 includes a first driving device 1411, a first lifting platform 1412, and a first connecting rod 1413 for installing the graphite rod 120, the first driving device 1411 is used for driving the first lifting platform 1412 to lift, the first connecting rod 1413 is installed on the first lifting platform 1412, one end of the graphite rod 120 is fixedly connected to the first connecting rod 1413, and the other end extends toward the tray 100. The first driving device 1411 drives the first lifting platform 1412 to move up and down to drive the first connecting rod 1413 to move up and down, and further drives the graphite rod 120 fixedly connected with the first connecting rod 1413 to move up and down, so as to adjust the distance between the graphite rod 120 and the tray 100. The first driving device 1411 comprises a driving motor 14111, a lead screw 14112 and a corrugated pipe 14113, for example, the driving motor 14111 is arranged outside the crystal growth equipment (crystal growth furnace), one end of the lead screw 14112 is rotatably installed on the flange 220 outside the crystal growth equipment, the other end of the lead screw 14112 is connected with the output end of the driving motor 14111, the first lifting platform 1412 is arranged in a direction parallel to the tray 100 and is fixed on the flange 220 through a corrugated pipe 14113, the first lifting platform 1412 is in threaded connection with the lead screw 14112, the corrugated pipe 14113 is sleeved on the outer side of the first connecting rod 1413, one end of the corrugated pipe 14113 is fixed on the first lifting platform 1412, and the other end of the corrugated pipe 8978 is fixed on the flange 220. When the driving motor 14111 is started, the lead screw 14112 rotates synchronously with the output shaft of the driving motor 14111, and at the same time, the first lifting platform 1412 moves along the lead screw 14112, thereby moving the graphite rod 120.
Referring to fig. 1 and 2, the second lifting mechanism 142 includes a second driving device 1421, a second lifting platform 1422, and a second connecting rod 1423, the second driving device 1421 is used for driving the second lifting platform 1422 to lift, the second connecting rod 1423 is installed on the second lifting platform 1422, the second connecting rod 1423 is used for supporting the conductive coil 130, and the conductive coil 130 is fixed at the bottom of the second connecting rod 1423 and is sleeved on the corresponding graphite rod 120. Preferably, the second lifting mechanism 142 includes two L-shaped second connecting rods 1423 disposed in parallel, one of the second connecting rods 1423 is fixedly connected to the head of the conductive coil 130, the other one is fixedly connected to the tail of the conductive coil 130, and the two connecting rods are disposed to fix the conductive coil 130 below the second lifting platform 1422 so that the second lifting platform 1422 moves synchronously with the conductive coil 130. Preferably, the second connecting bar 1423 is a copper bar through which an ac power source may be loaded onto the electrically conductive coil 130, causing eddy currents to be generated on the graphite rod 120. The second driving device 1421 may have the same structure as the first driving device 1411, that is, a driving motor, a lead screw, and a bellows, and the specific installation manner may refer to the description of the first driving device 1411. Of course, in other embodiments, the first driving device 1411 and the second driving device 1421 may be other driving devices, and any device capable of driving the graphite rod 120 and the conductive coil 130 to move up and down may be used.
Referring to fig. 1-4, the present invention further provides a method for growing a silicon carbide crystal, comprising the steps of:
s1, providing a crystal crystallization interface control device;
s2, mounting the silicon carbide seed crystal 110 on a tray 100 of a crystal crystallization interface control device, and placing the crystal crystallization interface control device in crystal growth equipment;
s3, adjusting the temperature and pressure in crystal growth equipment, adjusting the distance between the graphite rod 120 and/or the conductive coil 130 at the corresponding position and the tray 100 according to the shape of the required crystal interface, loading alternating current on the conductive coil 130, and keeping the growth for 1 to 50 hours to determine the initial growth interface of the crystal;
s4, keeping the temperature and the pressure in the crystal growth equipment unchanged, and gradually adjusting the distance between the graphite rod 120 and/or the conductive coil 130 at the corresponding position and the tray 100 in the growth process according to the defect distribution condition of the initial growth interface of the crystal to stably grow for 50-150 h;
s5, adjusting the pressure of crystal growth equipment to 50-500 mbar, and gradually adjusting the distances between the graphite rod 120, the coil 130 and the tray 100 within 10-20 h to ensure that the temperature difference between the graphite rod 120 at the edge part and the graphite rod 120 at the central part is 5-55 ℃ so as to reduce the temperature difference between the axial direction and the radial direction of the crystal;
and S6, after the growth is finished, cooling and taking out the crystal.
Referring to fig. 1, fig. 3 and fig. 4, specifically, the crystal crystallization interface control device in step S1 is the crystal crystallization interface control device of the present invention, and the structure thereof can be referred to the above detailed description, which is not repeated herein. Here, the sizes of the tray 100, the graphite rod 120 and the conductive coil 130 are not limited, and may be set according to specific requirements. In one embodiment, the thickness of the tray 100 is 15 mm, nine sets of graphite rods 120 and conductive coils 130 are radially distributed above the tray 100, the diameter of the graphite rods 120 is 10 mm, the conductive coils 130 are sleeved on the outer sides of the graphite rods 120, and the inner diameter of the conductive coils 130 is 20 mm. The bottom of the conductive coil 130 is spaced from the upper surface 35mm of the tray 100 and the bottom of the graphite rod 120 is flush with the conductive coil 130.
Referring to fig. 1 and 4, in step S2, the silicon carbide seed crystal 110 is fixedly installed on the tray 100, and the tray 100 with the seed crystal 110 installed thereon is placed in a crystal growth apparatus, wherein the crystal growth apparatus is a conventional growth furnace used for growing silicon carbide crystals, a crucible 200 for growing crystals is installed in the furnace, raw materials 210 for growing silicon carbide crystals are contained in the crucible 200, and the tray 100 is installed above the crucible 200. The graphite rod 120 and the conductive coil 130 are suspended above the tray 100 by the elevating mechanism 140.
Referring to fig. 1 and 4, step S3, after step S2 is finished, the method starts to grow crystals according to the shape of the crystal interface of the desired crystal, which specifically includes: adjusting the temperature and pressure in the furnace, and raising the temperature of the raw material in the crucible 200 to 1600 to 2400 ℃, for example, 1600 ℃, 2000 ℃, 2200 ℃, 2400 ℃, or 2400 ℃; the furnace is filled with inert gas, such as Ar, so that the pressure in the furnace reaches 200 to 800 mbar, such as 200 mbar, 400 mbar, 600 mbar or 800 mbar. When the temperature of the raw material 210 is raised to 1700 to 2500 ℃, for example 1700 ℃, 2100 ℃, 2300 ℃ or 2500 ℃ and the like, the pressure in the furnace is reduced to 0.1 to 100 mbar, for example 0.1 mbar, 30 mbar, 70 mbar or 100 mbar and the like, the distance between the graphite rod 120 and/or the conductive coil 130 and the tray 100 at different positions is adjusted according to the shape of the required crystal interface, and meanwhile, an alternating current is loaded on the conductive coil 130, and the growth is maintained for 1 to 50 hours, for example, 10 h, 30 h or 50 h and any value in the above range is kept, so as to determine the initial crystal growth interface. If the shape of the crystal crystallization interface is needed in actual production, for example, the shape of the crystal initial growth interface is thick in the middle and thin at the edge, the graphite rod 120 and the conductive coil 130 at the central position are adjusted upwards by the lifting mechanism 140, or the graphite rod 120 is kept still and only the conductive coil 130 is adjusted to increase the distance between the graphite rod 120 and the conductive coil 130 and the tray 100, and the temperature at the central position of the tray 100 is reduced, so that the central position is preferentially crystallized. In other embodiments, the distance between the graphite rod 120 and the conductive coil 130 of the edge position and the tray 100 may also be adjusted to preferentially crystallize the edge position. The graphite rod 120 and the conductive coil 130 which are adjusted are not limited, and the graphite rod and the conductive coil are set according to specific requirements, so that the crystal is required to grow preferentially, and the temperature of the corresponding position is adjusted correspondingly.
Further, in the crystal growth process, the distance between the graphite rod 120 and the tray 100 is 0.5 to 50 mm, for example, any value in the range of 0.5 to 50 mm, such as 0.5 mm, 10 mm, 30 mm or 50 mm, and the value can be specifically selected according to the crystal shape. The conductive coil 130 and the graphite rod 120 can generate relative displacement of 0 to 100 mm, for example, the relative displacement of the conductive coil 130 and the graphite rod is any value within the range of 0 to 100 mm, such as 15 mm, 50 mm, 75 mm or 100 mm. As an example, in the initial position, the distance between the graphite rod 120 and the tray 100 is 35mm, the graphite rod 120 in the central position can be adjusted from 35mm to 50 mm in the early growth stage, or the graphite rod 120 is kept stationary, and the distance between the conductive coil 130 and the tray 100 is adjusted to 50 mm, so that the conductive coil 130 and the graphite rod 120 generate a relative displacement of 15 mm.
Referring to fig. 1 and 4, in step S4, after the initial growth of the crystal is finished, the pressure and temperature in the furnace are kept unchanged, and according to the defect distribution of the initial growth interface of the crystal, the distance between the graphite rod 120 and/or the conductive coil 130 and the tray 100 at different positions is gradually adjusted in the subsequent growth process, and the crystal is continuously grown for 50 to 150 hours, for example, 50 h, 80 h, 120 h or 150 h, etc. For example, in step S3, the central graphite rod 120 is adjusted from 35mm to 50 mm, and in this step, the graphite rod 120 is gradually adjusted within 80 h of crystal growth, so that the distance between the graphite rod 120 and the tray 100 is slowly reduced from 50 mm to 35 mm; the distance between the graphite rods 120 and the tray 100 at the edge is gradually increased from 35mm to 50 mm. That is, step S4 and step S3 correspond to each other.
Referring to fig. 1 and 4, in step S5, ar is filled into the furnace, and the pressure in the furnace is adjusted to 50 to 500 mbar, such as 50 mbar, 100 mbar, 200 mbar, 300 mbar, 400 mbar, or 500 mbar; the distance between the graphite rod 120 and/or the conductive coil 130 and the tray 100 is adjusted step by step, so that the temperature difference between the graphite rod 120 at the edge part and the graphite rod 120 at the central part is 5-55 ℃, so as to reduce the temperature difference between the axial direction and the radial direction of the crystal, and the process is kept at 10-20 h, such as 10 h, 15 h or 20 h. Namely, the temperature difference between the graphite rod 120 at the edge part and the graphite rod 120 at the central part is adjusted to 5 to 55 ℃ within 10 to 20 hours, for example, 5 ℃, 15 ℃, 25 ℃, 35 ℃, 45 ℃ or 55 ℃. The specific operation can be, for example, gradually adjusting the distance between the graphite rod 120 at the central position and the tray 100 from 35mm to 8mm in 10 h; the distance between the graphite rod 120 at the edge position and the tray 100 is gradually adjusted from 50 mm to 12 mm.
Referring to fig. 4, step S6, after the growth is finished, the temperature is slowly decreased, and the crystal is taken out of the furnace.
The crystal growth method of the present invention is specifically described below by using specific embodiments, the thickness of the tray 100 in the crystal crystallization interface control device adopted in the following embodiments is 15 mm, nine groups of graphite rods 120 and conductive coils 130 are radially distributed above the tray 100, the diameter of the graphite rods 120 is 10 mm, the conductive coils 130 are sleeved on the outer sides of the graphite rods 120, and the inner diameter of the conductive coils 130 is 20 mm. The bottom of the conductive coil 130 is spaced from the upper surface 35mm of the tray 100 and the bottom of the graphite rod 120 is flush with the conductive coil 130.
Example 1
Step one, placing a crystal crystallization interface control device in crystal growth equipment, installing a tray 100 provided with seed crystals 110 in a graphite crucible, and containing raw materials 210 for growing silicon carbide in the crucible 200;
step two, heating the raw materials to 2200 ℃, and filling Ar into the furnace to ensure that the pressure in the furnace reaches 400 mbar; when the temperature of the nine graphite rods 120 reaches 2200 ℃ and the temperature of the raw material 210 reaches 2300 ℃, the graphite rods 120 and the conductive coils 130 in the central part are synchronously adjusted upwards, so that the distance between the five central conductive coils 130 and the graphite rods 120 and the tray 100 reaches 50 mm, and the distance between the four graphite rods 120 and the conductive coils 130 in the edge part keeps 35 mm; loading a 2.7 kHz, 0.5A alternating current to the conductive coil 130 to load the coil with 0.2 kw power; when the temperature of nine graphite rods 120 is basically consistent to 2250 ℃, ar is reduced to reduce the pressure in the furnace to 20 mbar, and N is charged 2 (ii) a Keeping all parameters to stably grow 20 h;
step three, keeping the power of the conductive coils 130 unchanged, adjusting the distance between the five central graphite rods 120 and the conductive coils 130 and the tray 100 from 50 mm to 35mm in the 80 h, and slowly raising the distance between the four outer graphite rods 120 and the conductive coils 130 and the tray 100 from 35mm to 50 mm;
step four, filling Ar, raising the pressure in the furnace to 200 mbar, adjusting the distance between the five graphite rods 120 and the conductive coil 130 at the central part and the tray 100 from 35mm to 8mm by using 10 h, simultaneously reducing the distance between the four graphite rods 120 and the conductive coil 130 at the edge part and the tray 100, adjusting the distance from 50 mm to 12 mm, and keeping the power of the conductive coil 130 unchanged during the period so that the temperature difference between the four graphite rods 120 at the edge part and the five graphite rods at the central part is 15 ℃;
and step five, after the growth is finished, slowly cooling, and taking out the crystal from the furnace.
The crystal prepared in example 1 is mechanically processed to obtain a silicon carbide substrate, and as shown in fig. 5, the silicon carbide substrate prepared in example 1 utilizes an eddy current generated on a graphite rod by a coil, so that a crystal interface has better consistency, a slight uneven doping phenomenon exists only in a facet direction, and the yield of subsequent epitaxy and devices is improved.
Example 2
Step one, placing a crystal crystallization interface control device in crystal growth equipment, installing a tray 100 provided with seed crystals 110 in a graphite crucible, and containing raw materials 210 for growing silicon carbide in the crucible 200;
step two, heating the raw materials to 2200 ℃, and filling Ar into the furnace to ensure that the pressure in the furnace reaches 400 mbar; when the temperature of the nine graphite rods 120 reaches 2200 ℃ and the temperature of the raw material 210 reaches 2300 ℃, only adjusting the conductive coil 130 at the central part to ensure that the distance between the conductive coil 130 at the central part and the tray 100 is increased from 35mm to 50 mm, the conductive coil 130 and the graphite rods 120 generate the relative displacement of 15 mm, and the distance between the four conductive coils 130 at the edge part still keeps 35 mm; the conductive coil 130 is loaded with alternating current of 1 kHz and 1A, so that the coil is loaded with 1 kw power; when the temperature of nine graphite rods 120 is basically consistent to 2250 ℃, ar is reduced to reduce the pressure in the furnace to 20 mbar, and N is charged 2 (ii) a Keeping all parameters to stably grow 20 h;
step three, keeping the power of the coil unchanged, slowly descending the distance between the conductive coil 130 at the central part and the tray 100 from 50 mm to 15 mm by using 80 h, and keeping the graphite rod 120 unchanged so that the conductive coil 130 and the graphite rod 120 generate the relative displacement of 35 mm; the positions of the four outside conductive coils 130 are always kept unchanged;
filling Ar into the furnace to enable the pressure in the furnace to rise to 200 mbar, reducing five graphite rods 120 and conductive coils 130 at the central part by utilizing 10 h to enable the distance between the graphite rods 120 and the conductive coils 130 and the tray 100 to be adjusted to 8mm, simultaneously reducing four graphite rods 120 and conductive coils 130 at the edge part to be adjusted to be 12 mm, and keeping the power of the conductive coils 130 unchanged during the period to enable the temperature difference between the four graphite rods at the edge part and the graphite rods at the central part to be 15 ℃;
and step five, after the growth is finished, slowly cooling, and taking out the crystal from the furnace.
The silicon carbide substrate prepared by machining the crystal prepared in example 2 is, as shown in fig. 6, a crystalline interface of the silicon carbide substrate prepared in example 2 has excellent consistency by using joule heat generated by eddy currents induced in the conductive coil, the tray, and the crystal, and a phenomenon of uneven doping hardly occurs, so that yield of subsequent epitaxy and devices is improved.
Comparative example
Comparative example silicon carbide was prepared using a conventional crystal growth method, as follows:
step one, a tray and seed crystals are arranged in crystal growth equipment;
step two, raising the temperature of the material source to 2200 ℃, and controlling the pressure in the equipment to be 600 mbar;
step three, when the temperature reaches 2200 ℃, reducing Ar in the furnace to reduce the pressure to 20 mbar and simultaneously doping 0.1 percent of N 2 ；
Step four, keeping the temperature and the pressure, and stably growing 100 h;
step five, increasing Ar gas in the furnace body to increase the pressure in the furnace to 200 mbar;
and step six, slowly cooling, and taking out crystals.
The crystal prepared by the comparative example is mechanically processed to obtain a silicon carbide substrate, as shown in fig. 7, a plurality of small patches with uneven impurity concentration exist on the silicon carbide substrate, and certain negative effects are exerted on the stability of subsequent epitaxial growth and the yield of devices.
According to the crystal crystallization interface control device, a plurality of graphite rods and conductive coils are arranged on one side of the tray, and eddy currents are generated in the graphite rods and the tray locally or in the conductive crystals by loading alternating current on the conductive coils; the distances between the graphite rods and the conducting coils at different positions and the tray are adjusted through the lifting mechanism, so that the heat generated by the eddy currents at different positions is different, the temperature of different positions of the tray is adjusted, and the control of a crystal crystallization interface is realized. The crystallization interface of the crystal grown by the crystallization control device has better consistency, and the yield of subsequent epitaxy and devices is improved. Therefore, the invention effectively overcomes some practical problems in the prior art, thereby having high utilization value and use significance.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.

Claims (10)

1. A crystal crystallization interface control device, comprising:
a tray for mounting seed crystals;
the graphite rods are arranged on one side, away from the seed crystal, of the tray, and a space is reserved between the graphite rods and the tray;
the quantity of the conductive coils is equal to that of the graphite rods, the conductive coils are respectively sleeved on the graphite rods correspondingly, and the conductive coils are connected with an alternating current power supply; and
the lifting mechanisms are equal to the graphite rods in number and are respectively used for controlling the distance between the corresponding graphite rods and/or the conductive coils and the tray;
after the conductive coil is connected with the alternating current power supply, the lifting mechanism is utilized to adjust the distance between the corresponding graphite rod and/or the conductive coil and the tray, so that the seed crystal at the corresponding position has the corresponding temperature, and the crystal crystallization interface is adjusted.
2. The crystal crystallization interface control device according to claim 1, wherein the tray, the graphite rod and the conductive coil are all made of graphite material, and the density of the graphite material is 1.6 to 1.8 g/cm 3 The thermal conductivity is 80 to 150 Wm -1 K -1 The resistivity is 1 to 50 [ mu ] omega m.
3. The crystal crystallization interface control device according to claim 1, wherein the frequency of the alternating current power supply is 0.1 to 10 KHz, the voltage of the alternating current power supply loaded on the conductive coil is 0.1 to 20V, or the current of the alternating current power supply loaded on the conductive coil is 0.1 to 10A.
4. The crystal crystallization interface control device according to claim 1, wherein the lifting mechanism comprises a first lifting mechanism for driving the graphite rod and a second lifting mechanism for driving the conductive coil, the first lifting mechanism comprises a first driving device, a first lifting platform and a first connecting rod, the first driving device drives the first lifting platform to lift, the first connecting rod is mounted on the first lifting platform, one end of the graphite rod is connected with the first connecting rod, and the other end of the graphite rod extends towards the tray; the second lifting mechanism comprises a second driving device, a second lifting platform and a second connecting rod, the second driving device is used for driving the second lifting platform to lift, the second connecting rod is installed on the second lifting platform, and the conductive coil is installed at the bottom of the second connecting rod and sleeved on the graphite rod.
5. The crystal growth interface control device of claim 4, wherein the first driving device and the second driving device have the same structure, the first driving device includes a driving motor, a lead screw and a bellows, one end of the lead screw is connected to an output shaft of the driving motor, the other end of the lead screw is rotatably mounted on a flange outside the crystal growth apparatus, the first lifting platform is in threaded connection with the lead screw, the bellows is sleeved outside the first connecting rod, one end of the bellows is fixed on the first lifting platform, and the other end of the bellows is fixed on the flange.
6. The crystal crystallization interface control device according to claim 1, further comprising a temperature measuring mechanism for measuring a temperature of the graphite rod, the temperature measuring mechanism being connected to one end of the graphite rod.
7. A method of growing a silicon carbide crystal, comprising at least the steps of:
providing a crystal crystallization interface control device according to any one of claims 1 to 6;
mounting a silicon carbide seed crystal on a tray of the crystal crystallization interface control device, and placing the crystal crystallization interface control device in crystal growth equipment;
adjusting the temperature and pressure in the crystal growth equipment, adjusting the distance between a graphite rod and/or a conductive coil at a corresponding position and the tray according to the shape of a required crystal crystallization interface, and simultaneously loading alternating current to the conductive coil to keep the growth for 1 to 50 hours so as to determine an initial growth interface of the crystal;
keeping the temperature and the pressure in the crystal growth equipment unchanged, and gradually adjusting the distance between the graphite rod and/or the conductive coil at the corresponding position and the tray in the growth process according to the defect distribution condition of the initial growth interface of the crystal, so that the crystal stably grows for 50 to 150 hours;
adjusting the pressure of the crystal growth equipment to 50-500 mbar, and gradually adjusting the distance between the graphite rod and/or the conductive coil and the tray within 10-20 h to ensure that the temperature difference between the graphite rod at the edge part and the graphite rod at the center part is 5-55 ℃ so as to reduce the temperature difference between the axial direction and the radial direction of the crystal;
and (5) after the growth is finished, cooling and taking out the crystal.
8. The method of growing a silicon carbide crystal according to claim 7 wherein the determining an initial crystal growth interface comprises: heating the temperature of the raw materials in the crystal growth equipment to 1600-2400 ℃, and adjusting the pressure in the crystal growth equipment to 200-800 mbar; and when the temperature of the raw materials is raised to 1700-2500 ℃, and the pressure in the crystal growth equipment is reduced to 0.1-100 mbar, adjusting the distance between the graphite rod and/or the conductive coil at the corresponding position and the tray, so that the crystal grows for 1-50 hours according to the required shape.
9. The method for growing the silicon carbide crystal according to claim 7, wherein the distance between the graphite rod and the tray is 0.5-50 mm in the crystal growing process.
10. The silicon carbide crystal growth method according to claim 7, wherein in the crystal growth process, the conductive coil and the graphite rod produce relative displacement of 0-100 mm.
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