CN117646279A - Double-heater device for growing silicon carbide single crystal by liquid phase method and method thereof - Google Patents
Double-heater device for growing silicon carbide single crystal by liquid phase method and method thereof Download PDFInfo
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- CN117646279A CN117646279A CN202410126416.1A CN202410126416A CN117646279A CN 117646279 A CN117646279 A CN 117646279A CN 202410126416 A CN202410126416 A CN 202410126416A CN 117646279 A CN117646279 A CN 117646279A
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- 239000013078 crystal Substances 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 47
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 36
- 239000007791 liquid phase Substances 0.000 title claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 62
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- 230000009977 dual effect Effects 0.000 claims abstract description 20
- 238000012544 monitoring process Methods 0.000 claims abstract description 4
- 238000004140 cleaning Methods 0.000 claims description 58
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 8
- 230000005540 biological transmission Effects 0.000 claims description 4
- 239000006184 cosolvent Substances 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 3
- 230000000087 stabilizing effect Effects 0.000 claims 1
- 238000009529 body temperature measurement Methods 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 5
- 238000004891 communication Methods 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 230000008878 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 229910003468 tantalcarbide Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 210000001503 joint Anatomy 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000004781 supercooling Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- 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
- C30B9/00—Single-crystal growth from melt solutions using molten solvents
- C30B9/04—Single-crystal growth from melt solutions using molten solvents by cooling of the solution
- C30B9/08—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using other solvents
- C30B9/12—Salt solvents, e.g. flux growth
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to the technical field of crystal growth, in particular to a double-heater device for growing silicon carbide single crystals by a liquid phase method and a method thereof; the present invention provides a dual heater apparatus for growing silicon carbide single crystals by a liquid phase method, comprising: the device comprises a reaction bin, a crucible, a first heating unit, a second heating unit and a temperature measuring piece, wherein the reaction bin is hollow, and the crucible is fixed in the reaction bin; the temperature measuring piece is detachably arranged on the reaction bin and is suitable for monitoring the temperature in the crucible; the first heating unit is fixed at the upper part of the outer wall of the crucible; the second heating unit is fixed at the lower part of the outer wall of the crucible, and the first heating unit is arranged above the second heating unit; during assembly, the second heating unit is fixed outside the crucible, and then the second first heating unit is fixed outside the crucible; the first heating unit and the second heating unit can individually heat the crucible.
Description
Technical Field
The invention relates to the technical field of crystal growth, in particular to a double-heater device for growing silicon carbide single crystals by a liquid phase method and a method thereof.
Background
Third generation semiconductor high-power electronic devices represented by silicon carbide (SiC) are one of the fastest growing power semiconductor devices in the power electronics field at present. Silicon carbide, which is a typical representative of third generation semiconductor materials, is one of the most widely used wide bandgap semiconductor materials at the most mature level of current crystal production technology and device manufacturing, and has been currently forming a global material, device and application industry chain. Is an ideal semiconductor material in high-temperature, high-frequency, radiation-resistant and high-power application occasions.
When the SiC crystal is grown by a resistance liquid phase method, silicon and a cosolvent are filled into a graphite crucible, heating and melting are carried out by a graphite resistance heating unit, carbon in graphite is dissolved by the silicon solution to form a silicon solution containing carbon, then SiC seed crystal is immersed into the solution, so that the vicinity of the seed crystal is supercooled to obtain a carbon supersaturation state, and carbon is precipitated on the seed crystal for epitaxial growth of the SiC single crystal.
In the conventional single crystal growth process by a single heating unit resistance method:
on one hand, the resistance heating unit cannot be lifted up and down to supercool the vicinity of the monocrystalline seed crystal to obtain a carbon supersaturated state, if the aim of supercooling the vicinity of the monocrystalline seed crystal is achieved by lifting the crucible to different positions of the heating unit, meanwhile, unavoidable liquid level fluctuation and instability of a solution temperature field cause solution fluctuation and unstable growth interface, and the solution temperature field is generated in the solution, so that the solution is floated, and the monocrystalline grows to have the conditions of wrapping or polycrystal and impurity crystal;
on the other hand, in the growth process, the upper and lower heat preservation layers are recycled, the heat preservation performance is reduced, the temperature gradient can not meet the use requirement of people, and the repeatability is difficult to guarantee. Therefore, the liquid phase resistance method needs to be found out, the silicon carbide single crystal growth period is simple to operate, the safety is high, the temperature gradient is efficiently found, the growth interface temperature can be kept stable, the solution is stable, and the requirements of high-efficiency, high-stability and high-repeatability long-time growth of the SiC single crystal are met. Therefore, it is necessary to develop a dual heater apparatus for growing silicon carbide single crystals by a liquid phase method and a method thereof.
Disclosure of Invention
The invention aims to provide a double-heater device for growing silicon carbide single crystals by a liquid phase method and a method thereof.
In order to solve the above technical problems, the present invention provides a dual heater apparatus for growing silicon carbide single crystals by a liquid phase method, comprising:
the device comprises a reaction bin, a crucible, a first heating unit, a second heating unit and a temperature measuring piece, wherein the reaction bin is hollow, and the crucible is fixed in the reaction bin;
the temperature measuring piece is detachably arranged on the reaction bin and is suitable for monitoring the temperature in the crucible;
the first heating unit is fixed at the upper part of the outer wall of the crucible;
the second heating unit is fixed at the lower part of the outer wall of the crucible, and the first heating unit is arranged above the second heating unit;
during assembly, the second heating unit is fixed outside the crucible, and then the first heating unit is fixed outside the crucible;
the first heating unit and the second heating unit can individually heat the crucible.
Preferably, the first heating unit includes: the first heater, the first supporting leg, the first electrode column and the first reflecting plate, the first electrode column is vertically arranged, the first supporting leg is fixed at the upper end of the first electrode column,
the first heater is fixed on the first supporting leg, is electrically connected with the first electrode column, and is arranged on the upper part of the outer wall of the crucible;
the first reflecting plate is fixed above the crucible and is suitable for reflecting heat emitted from the crucible back to the surface of the solution in the crucible.
Preferably, the second heating unit includes: the second heater, the second supporting leg, the second electrode column and the second reflecting plate are vertically arranged, and the second electrode column is arranged on the inner side of the first electrode column;
the second supporting leg is fixed on the second electrode column, the second heater is fixed on the second supporting leg, and the second heater is arranged at the lower part of the outer wall of the crucible;
the second reflecting plate is fixed below the crucible and is suitable for reflecting heat emitted by the crucible to the bottom of the crucible.
Preferably, a fixed cylinder is slidably arranged at the upper end of the reaction bin, the inside of the fixed cylinder is hollow, and the fixed cylinder is vertically arranged.
Preferably, the outer wall of the fixed cylinder is provided with a plurality of limiting grooves, a plurality of linkage cleaning pieces are slidably arranged in the limiting grooves, and the linkage cleaning pieces are linked with the temperature measuring pieces;
the temperature measuring piece is suitable for pushing the fixed cylinder to slide vertically downwards.
Preferably, a conical groove is formed in the upper end of the reaction bin, and the conical groove is abutted to the lower end of the linkage cleaning piece.
Preferably, a fixing groove is formed in the temperature measuring piece, and the upper end of the linkage cleaning piece is slidably arranged in the fixing groove.
Preferably, a lifting groove is formed in the temperature measuring piece along the axial direction, and the fixed cylinder is arranged in the lifting groove in a sliding manner.
Preferably, the upper end of the linkage cleaning piece is provided with a cleaning brush, the cleaning brush faces the photosensitive piece of the temperature measuring piece, and the upper end of the linkage cleaning piece is in butt joint with the photosensitive piece.
Preferably, a connecting piece is fixed between two adjacent linkage cleaning pieces, and the connecting piece is a flexible piece.
Preferably, a driving shaft is rotatably arranged in the reaction bin, the driving shaft is fixed at the lower end of the crucible, and the driving shaft is suitable for driving the crucible to circumferentially rotate.
On the other hand, the invention also provides a working method of the double-heater device for growing silicon carbide single crystals by a liquid phase method, which comprises the following steps:
when the temperature measuring piece is disassembled, the temperature measuring piece is pressed, and the temperature measuring piece pushes the linkage cleaning piece and the fixed cylinder to synchronously move downwards;
after the linkage cleaning piece moves downwards to be in abutting connection with the side wall of the lifting groove, the lifting groove is suitable for pushing the linkage cleaning piece to move towards the axis direction of the fixed cylinder;
after each linkage cleaning piece moves to the inner end to be abutted, the temperature measuring piece is circumferentially arranged, the cleaning hairbrush is suitable for cleaning impurities on the bottom wall of the photosensitive film,
the temperature measuring piece is suitable for being separated from the linkage cleaning piece so as to conveniently detect the temperature measuring piece and ensure the measurement accuracy of the temperature measuring piece;
when the crucible is in operation, 5000g of silicon and a cosolvent are sequentially placed into the crucible, and no impurity is required to enter the crucible in the process;
placing the crucible into a reaction bin, adjusting the position of the crucible to enable the first heater to be aligned with the upper part of the crucible and the second heater to be aligned with the lower part of the crucible,
vacuumizing the reaction bin, replacing the reaction bin with argon, controlling the argon flow to be 10L under flowing argon, heating the reaction bin after the pressure is stabilized at 600mbar-800mbar, setting the power of a first heater to be 5-10kw for auxiliary material melting, and setting the power of a second heater to be 10-18kw for main material melting;
after complete melting, the power of the first heater and the power of the second heater are adjusted, the temperature measuring piece starts to work, after the temperature is stable, the transmission shaft drives the crucible to circumferentially rotate, the rotating speed of the crucible is 20-30rpm, so that the solutions are fully and uniformly mixed for 1 hour;
after being fully uniform, the seed crystal is contacted, the power of the first heater and the power of the second heater are adjusted, the temperature of the lower part of the crucible are 2000+/-10 ℃, the temperature of the upper part of the crucible is 1950+/-10 ℃, the rotation speed of the seed crystal support is 50-100rpm, and the seed crystal is raised at the speed of 0.25mm/h, so that the SiC single crystal is epitaxially grown on the seed crystal by combining carbon and silicon.
The double-heater device for growing the silicon carbide single crystal by the liquid phase method has the advantages that the arrangement of the first heating unit and the second heating unit can accurately regulate and control the axial temperature, ensure the radial gradient and be beneficial to increasing the thickness of the single crystal and improving the quality of the single crystal for a long time; the decisive dependence on thermal field insulation is reduced, the use cost of the insulation felt is reduced, and the quality of single crystal growth is improved. And the cooperation of temperature measurement spare and linkage clearance spare, not only convenient to detach temperature measurement spare, simultaneously, in the temperature measurement in-process, can adjust the temperature measurement scope to in the crucible to make temperature measurement spare temperature measurement average more accurate.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
In order to make the above objects, features and advantages of the present invention more comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a perspective view of a preferred embodiment of a dual heater apparatus for growing silicon carbide single crystals by a liquid phase method according to the present invention;
FIG. 2 is a perspective view of a reaction cartridge of the present invention;
FIG. 3 is a perspective view of the thermometric component of the present invention;
FIG. 4 is a perspective view of the stationary barrel of the present invention;
FIG. 5 is a perspective view of the stationary drum and ganged cleaning element of the present invention;
FIG. 6 is a schematic cross-sectional view of a temperature sensing member and a ganged cleaning member of the present invention.
In the figure:
1. a reaction bin; 11. a fixed cylinder; 110. a limit groove; 12. a linkage cleaning piece; 121. a positioning sheet is arranged on the upper part; 122. a lower locating piece; 123. an arc plate; 13. a conical groove; 14. a connecting piece; 15. a drive shaft;
2. a crucible;
3. a first heating unit; 31. a first heater; 32. a first support leg; 33. a first electrode column; 34. a first reflection plate;
4. a second heating unit; 41. a second heater; 42. a second support leg; 43. a second electrode column; 44. a second reflection plate;
5. a temperature measuring member; 51. a lifting groove; 52. a fixing groove.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In accordance with a first embodiment, as shown in fig. 1 to 6, the present invention provides a dual heater apparatus for growing silicon carbide single crystals by a liquid phase method, comprising: the reaction chamber 1 is hollow, the crucible 2 is fixed in the reaction chamber 1; the temperature measuring piece 5 is detachably arranged on the reaction bin 1, and the temperature measuring piece 5 is suitable for monitoring the temperature in the crucible 2; the crucible 2 is detachably arranged in the reaction bin 1; the first heating unit 3 is fixed at the upper part of the outer wall of the crucible 2; the second heating unit 4 is fixed at the lower part of the outer wall of the crucible 2, and the first heating unit 3 is arranged above the second heating unit 4; wherein, in order to avoid the assembly interference, the second heating unit 4 is firstly fixed outside the crucible 2, and then the second heating unit 4 is fixed outside the crucible 2 during the assembly; the first heating unit 3 and the second heating unit 4 can individually heat the crucible 2. The second heating unit 4 and the first heating unit 3 may have different heating temperatures for the lower and upper portions of the crucible 2 according to the crystal growth needs. Through the arrangement of the first heating unit 3 and the second heating unit 4, the axial temperature can be accurately regulated and controlled, the radial gradient is ensured, and the thickness and the quality of single crystals are increased for a long time; the decisive dependence on thermal field insulation is reduced, the use cost of the insulation felt is reduced, and the quality of single crystal growth is improved.
Referring to fig. 1, the first heating unit 3 includes: the first heater 31, the first supporting legs 32, the first electrode columns 33 and the first reflecting plates 34, wherein the first electrode columns 33 are vertically arranged, the first electrode columns 33 are fixed in the reaction bin 1, and the first electrode columns 33 are axially arranged along the reaction bin 1. The first supporting leg 32 is fixed at the upper end of the first electrode column 33, and the first supporting leg 32 is suitable for supporting and fixing the first heater 31; the first heater 31 is fixed on the first supporting leg 32, the first heater 31 is electrically connected with the first electrode column 33, and the first heater 31 is arranged at the upper part of the outer wall of the crucible 2; the first heater 31 is circumferentially arranged around the crucible 2, the first reflecting plate 34 is fixed above the crucible 2, and the first reflecting plate 34 is suitable for reflecting heat emitted from the crucible 2 back to the surface of the solution in the crucible 2. The first heater 31 is suitable for heating the upper portion of the crucible 2, so as to avoid the phenomenon that the heat loss of the surface layer of the solution is too fast, the appearance of a wrapping or polycrystal on the floating crystal or the monocrystal, and the overlarge power loss, the first reflecting plate 34 is a tantalum carbide reflecting plate, and the first reflecting plate 34 can reflect the heat loss of the upper end of the crucible 2 to the surface of the solution in the crucible 2, so that the stability of the temperature of the solution is ensured.
Referring to fig. 1, the second heating unit 4 includes: a second heater 41, a second supporting leg 42, a second electrode post 43, and a second reflecting plate 44, the second electrode post 43 being vertically disposed, and the second electrode post 43 being disposed inside the first electrode post 33; the second supporting leg 42 is fixed on the second electrode column 43, the second heater 41 is fixed on the second supporting leg 42, and the second heater 41 is arranged at the lower part of the outer wall of the crucible 2; the second heater 41 is circumferentially disposed around the crucible 2. The second reflecting plate 44 is fixed below the crucible 2, and the second reflecting plate 44 is adapted to reflect heat emitted from the crucible 2 to the bottom of the crucible 2. In order to avoid the uneven solution temperature and the overlarge power loss caused by the too fast heat dissipation of the bottom of the crucible 2, the second reflecting plate 44 is a tantalum carbide reflecting plate, and the second reflecting plate 44 can reflect the heat dissipated by the crucible 2 back to the bottom of the crucible 2, so that the solution uniformity is ensured, the crystal quality is improved, and the stability of long-time growth is ensured.
Referring to fig. 3 and 4, in order to facilitate fixing the temperature measuring member 5, a fixing cylinder 11 is slidably disposed at the upper end of the reaction chamber 1, the fixing cylinder 11 is hollow, and the fixing cylinder 11 is vertically disposed. The reaction bin 1 is provided with a through hole matched with the fixed cylinder 11, and the fixed cylinder 11 can vertically move up and down relative to the reaction bin 1. By moving the fixed cylinder 11 up and down, the distance between the temperature measuring member 5 and the crucible 2 can be adjusted to adjust the measuring and detecting range of the temperature measuring member 5.
Referring to fig. 4, the outer wall of the fixed cylinder 11 is provided with a plurality of limit grooves 110, a plurality of linkage cleaning members 12 are slidably arranged in the limit grooves 110, and the linkage cleaning members 12 are linked with the temperature measuring member 5; wherein the temperature measuring piece 5 is suitable for pushing the fixed cylinder 11 to slide vertically downwards. The linkage cleaning members 12 are adapted to slide radially relative to the fixed cylinder 11, and in an initial state, the outer ends of the linkage cleaning members 12 are abutted against the inner wall of the conical groove 13, at this time, the space range formed by the inner ends of the linkage cleaning members 12 is the largest, and the range of the crucible 2 which can be detected by the temperature measuring member 5 is the largest. The linkage cleaning member 12 includes: the upper positioning plate 121, the lower positioning plate 122 and the circular arc plate 123, wherein the upper positioning plate 121 and the lower positioning plate 122 are parallel to each other, the upper positioning plate 121 and the lower positioning plate 122 are respectively and vertically fixed at two ends of the circular arc plate 123, the circular arc plate 123 is vertically arranged, and the circular arc plate 123 is suitable for sliding horizontally in the limiting groove 110; the upper positioning piece 121 is disposed above the lower positioning piece 122.
Referring to fig. 6, a conical groove 13 is formed at the upper end of the reaction chamber 1, and the conical groove 13 abuts against the lower end of the linkage cleaning member 12. The lower locating piece 122 is suitable for abutting against the conical groove 13. The temperature measuring part 5 pushes the fixed cylinder 11 and the linkage cleaning part 12 to synchronously move downwards, and the side wall of the conical groove 13 is suitable for pushing the lower locating piece 122 to move towards the axis direction of the fixed cylinder 11 so as to gradually keep the upper locating piece 121 away from the fixed groove 52.
Further, a fixing groove 52 is formed in the temperature measuring member 5, and the upper end of the linkage cleaning member 12 is slidably disposed in the fixing groove 52. The upper positioning piece 121 is adapted to be inserted into the fixing groove 52. When the temperature measuring piece 5 is fixed, the linkage cleaning piece 12 is pushed to move towards the axis direction of the fixed cylinder 11 until the outer wall of each upper locating piece 121 can be abutted against the side wall of the lifting groove 51, the temperature measuring piece 5 is pressed, so that the upper locating piece 121 corresponds to the fixed groove 52, the linkage cleaning piece 12 is pulled outwards, the upper locating piece 121 is inserted into the fixed groove 52, and at the moment, the bottom wall of the light sensitive piece of the temperature measuring piece 5 is close to the upper surface of the upper locating piece 121.
Referring to fig. 6, in order to adapt to the fixed cylinder 11, a lifting groove 51 is formed in the temperature measuring member 5 along the axial direction, and the fixed cylinder 11 is slidably disposed in the lifting groove 51. The fixed cylinder 11 is adapted to be inserted into the elevation groove 51.
In order to be convenient for clear up temperature measurement spare 5, linkage clearance spare 12 upper end is provided with the clearance brush, the clearance brush is towards the sensitive piece of temperature measurement spare 5, just linkage clearance spare 12 upper end and sensitive piece butt. The temperature measuring piece 5 is pressed so that the fixed cylinder 11 contracts inwards towards the reaction bin 1, the side wall of the conical groove 13 is suitable for pushing the lower locating piece 122 to contract inwards, the lower locating piece 122 synchronously drives the upper locating piece 121 to contract inwards, the upper locating piece 121 is separated from the inner part of the fixing groove 52, at the moment, the contact range of the upper locating piece 121 and the light sensitive piece of the bottom wall of the temperature measuring piece 5 is the largest, the temperature measuring piece 5 is rotated circumferentially, and the cleaning brush is suitable for cleaning impurities on the light sensitive piece.
Further, a connecting piece 14 is fixed between two adjacent linkage cleaning pieces 12, and the connecting piece 14 is a flexible piece. The connecting piece 14 has elasticity, and after the linkage cleaning piece 12 is inserted into the fixing groove 52, the connecting piece 14 is suitable for pushing the two linkage cleaning pieces 12 to slide outwards, so that each lower positioning piece 122 can be abutted against the inner wall of the conical groove 13.
In order to drive the crucible 2 to rotate circumferentially, a driving shaft 15 is rotatably arranged in the reaction chamber 1, the driving shaft 15 is fixed at the lower end of the crucible 2, and the driving shaft 15 is suitable for driving the crucible 2 to rotate circumferentially. The driving shaft 15 is detachably connected with the crucible 2, a driving piece is fixed at the bottom of the reaction bin 1, the driving shaft 15 is in transmission connection with the driving piece, and the driving piece is suitable for driving the crucible 2 to circumferentially rotate.
In a second embodiment, on the basis of the first embodiment, a working method of a dual heater device for growing a silicon carbide single crystal by a liquid phase method is further provided, wherein the dual heater device for growing a silicon carbide single crystal by a liquid phase method is as described in the first embodiment, and a specific mechanism is the same as that in the first embodiment, and the working method of the dual heater device for growing a silicon carbide single crystal by a liquid phase method is not repeated here, and is as follows:
when the temperature measuring piece 5 is disassembled, the temperature measuring piece 5 is pressed, and the temperature measuring piece 5 pushes the linkage cleaning piece 12 and the fixed cylinder 11 to synchronously move downwards;
after the linkage cleaning member 12 moves downwards to be in contact with the side wall of the lifting groove 51, the lifting groove 51 is suitable for pushing the linkage cleaning member 12 to move towards the axis direction of the fixed cylinder 11;
after each linkage cleaning piece 12 moves to the inner end to be abutted, the temperature measuring piece 5 is circumferentially arranged, the cleaning brush is suitable for cleaning impurities on the bottom wall of the photosensitive film,
the temperature measuring piece 5 is suitable for being separated from the linkage cleaning piece 12 so as to be convenient for detecting the temperature measuring piece 5 and ensure the accuracy of the measurement of the temperature measuring piece 5;
when in work, 5000g of silicon and cosolvent are sequentially put into a crucible 2, and no impurity enters the crucible 2 in the process;
placing the crucible 2 into the reaction chamber 1, adjusting the position of the crucible 2 such that the first heater 31 is aligned with the upper portion of the crucible 2, the second heater 41 is aligned with the lower portion of the crucible 2,
vacuumizing the reaction chamber 1, replacing the reaction chamber with argon, controlling the argon flow to 10L under flowing argon, heating the reaction chamber 1 after the pressure is stabilized at 600mbar-800mbar, setting the power of the first heater 31 to 5-10kw for auxiliary material melting, and setting the power of the second heater 41 to 10-18kw for main material melting;
after complete melting, the power of the first heater 31 and the second heater 41 is adjusted, the temperature measuring piece 5 starts to work, after the temperature is stable, the transmission shaft drives the crucible 2 to circumferentially rotate, the rotating speed of the crucible 2 is 20-30rpm, so that the solution is fully and uniformly mixed for 1h;
after sufficient uniformity, the seed crystal is contacted, the temperature of the lower part of the crucible 2 is 2000.+ -. 10 ℃ and the temperature of the upper part of the crucible 2 is 1950.+ -. 10 ℃ by adjusting the power of the first heater 31 and the second heater 41, the rotation speed of the seed crystal holder is 50-100rpm, and the seed crystal is raised at a speed of 0.25mm/h, and the SiC single crystal is epitaxially grown on the seed crystal by combining carbon and silicon.
The components (components not illustrating specific structures) selected in the application are all common standard components or components known to those skilled in the art, and the structures and principles of the components are all known to those skilled in the art through technical manuals or through routine experimental methods. Moreover, the software programs referred to in the present application are all prior art, and the present application does not relate to any improvement of the software programs.
In the description of embodiments of the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
In the description of the present invention, it should be noted that the directions or positional relationships indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the several embodiments provided in this application, it should be understood that the disclosed systems, devices, and methods may be implemented in other manners. The above-described apparatus embodiments are merely illustrative, for example, the division of the units is merely a logical function division, and there may be other manners of division in actual implementation, and for example, multiple units or components may be combined or integrated into another system, or some features may be omitted, or not performed. Alternatively, the coupling or direct coupling or communication connection shown or discussed with each other may be through some communication interface, device or unit indirect coupling or communication connection, which may be in electrical, mechanical or other form.
The units described as separate units may or may not be physically separate, and units shown as units may or may not be physical units, may be located in one place, or may be distributed on a plurality of network units. Some or all of the units may be selected according to actual needs to achieve the purpose of the solution of this embodiment.
In addition, each functional unit in the embodiments of the present invention may be integrated in one processing unit, or each unit may exist alone physically, or two or more units may be integrated in one unit.
With the above-described preferred embodiments according to the present invention as an illustration, the above-described descriptions can be used by persons skilled in the relevant art to make various changes and modifications without departing from the scope of the technical idea of the present invention. The technical scope of the present invention is not limited to the description, but must be determined according to the scope of claims.
Claims (11)
1. A dual heater apparatus for growing a silicon carbide single crystal by a liquid phase method, comprising:
the device comprises a reaction bin (1), a crucible (2), a first heating unit (3), a second heating unit (4) and a temperature measuring piece (5), wherein the interior of the reaction bin (1) is hollow, and the crucible (2) is fixed in the reaction bin (1);
the temperature measuring piece (5) is detachably arranged on the reaction bin (1), and the temperature measuring piece (5) is suitable for monitoring the temperature in the crucible (2);
the first heating unit (3) is fixed at the upper part of the outer wall of the crucible (2);
the second heating unit (4) is fixed at the lower part of the outer wall of the crucible (2), and the first heating unit (3) is arranged above the second heating unit (4);
wherein, during assembly, the second heating unit (4) is fixed outside the crucible (2) firstly, and then the second heating unit is fixed outside the crucible (2);
the first heating unit (3) and the second heating unit (4) can independently heat the crucible (2);
the first heating unit (3) comprises: the first heater (31), the first supporting leg (32), the first electrode column (33) and the first reflecting plate (34), the first electrode column (33) is vertically arranged, the first supporting leg (32) is fixed at the upper end of the first electrode column (33),
the first heater (31) is fixed on the first supporting leg (32), the first heater (31) is electrically connected with the first electrode column (33), and the first heater (31) is arranged at the upper part of the outer wall of the crucible (2);
the first reflecting plate (34) is fixed above the crucible (2), and the first reflecting plate (34) is suitable for reflecting heat emitted from the crucible (2) back to the surface of the solution in the crucible (2).
2. A dual heater apparatus for growing a silicon carbide single crystal by a liquid phase process according to claim 1, wherein:
the second heating unit (4) includes: the second heater (41), a second supporting leg (42), a second electrode column (43) and a second reflecting plate (44), wherein the second electrode column (43) is vertically arranged, and the second electrode column (43) is arranged on the inner side of the first electrode column (33);
the second supporting leg (42) is fixed on the second electrode column (43), the second heater (41) is fixed on the second supporting leg (42), and the second heater (41) is arranged at the lower part of the outer wall of the crucible (2);
the second reflecting plate (44) is fixed below the crucible (2), and the second reflecting plate (44) is suitable for reflecting heat emitted by the crucible (2) to the bottom of the crucible (2).
3. A dual heater apparatus for growing a silicon carbide single crystal by a liquid phase method according to claim 2, wherein:
the upper end of the reaction bin (1) is slidably provided with a fixed cylinder (11), the inside of the fixed cylinder (11) is hollow, and the fixed cylinder (11) is vertically arranged.
4. A dual heater apparatus for growing a silicon carbide single crystal by a liquid phase process according to claim 3, wherein:
a plurality of limiting grooves (110) are formed in the outer wall of the fixed cylinder (11), a plurality of linkage cleaning pieces (12) are arranged in the limiting grooves (110) in a sliding mode, and the linkage cleaning pieces (12) are linked with the temperature measuring pieces (5);
wherein the temperature measuring piece (5) is suitable for pushing the fixed cylinder (11) to slide vertically downwards.
5. A dual heater apparatus for growing a silicon carbide single crystal by a liquid phase method according to claim 4, wherein:
the upper end of the reaction bin (1) is provided with a conical groove (13), and the conical groove (13) is abutted to the lower end of the linkage cleaning piece (12).
6. A dual heater apparatus for growing a silicon carbide single crystal by a liquid phase method according to claim 5, wherein:
a fixed groove (52) is formed in the temperature measuring piece (5), and the upper end of the linkage cleaning piece (12) is arranged in the fixed groove (52) in a sliding mode.
7. A dual heater apparatus for growing a silicon carbide single crystal by a liquid phase method according to claim 6, wherein:
a lifting groove (51) is formed in the temperature measuring piece (5) along the axial direction, and the fixed cylinder (11) is arranged in the lifting groove (51) in a sliding mode.
8. A dual heater apparatus for growing a silicon carbide single crystal by a liquid phase process according to claim 7, wherein:
the upper end of the linkage cleaning piece (12) is provided with a cleaning brush, the cleaning brush faces the photosensitive piece of the temperature measuring piece (5), and the upper end of the linkage cleaning piece (12) is abutted to the photosensitive piece.
9. A dual heater apparatus for growing a silicon carbide single crystal by a liquid phase process according to claim 8, wherein:
a connecting piece (14) is fixed between two adjacent linkage cleaning pieces (12), and the connecting piece (14) is a flexible piece.
10. A dual heater apparatus for growing a silicon carbide single crystal by a liquid phase process according to claim 9, wherein:
the reaction bin (1) is rotatably provided with a driving shaft (15), the driving shaft (15) is fixed at the lower end of the crucible (2), and the driving shaft (15) is suitable for driving the crucible (2) to circumferentially rotate.
11. A method of operating a dual heater apparatus for growing a silicon carbide single crystal by a liquid phase method, characterized by using a dual heater apparatus for growing a silicon carbide single crystal by a liquid phase method as set forth in claim 10, comprising the steps of:
when the temperature measuring piece (5) is disassembled, the temperature measuring piece (5) is pressed, and the temperature measuring piece (5) pushes the linkage cleaning piece (12) and the fixed cylinder (11) to synchronously move downwards;
after the linkage cleaning piece (12) moves downwards to be in contact with the side wall of the lifting groove (51), the lifting groove (51) is suitable for pushing the linkage cleaning piece (12) to move towards the axis direction of the fixed cylinder (11);
after each linkage cleaning piece (12) moves to the inner end to be abutted, the temperature measuring piece (5) is circumferentially arranged, the cleaning hairbrush is suitable for cleaning impurities on the bottom wall of the photosensitive film,
the temperature measuring piece (5) is suitable for being separated from the linkage cleaning piece (12) so as to conveniently detect the temperature measuring piece (5) and ensure the measurement accuracy of the temperature measuring piece (5);
when the crucible works, 5000g of silicon and a cosolvent are sequentially placed into the crucible (2), and no impurity enters the crucible (2) in the process;
placing the crucible (2) into a reaction bin (1), adjusting the position of the crucible (2) to enable a first heater (31) to be aligned with the upper part of the crucible (2) and a second heater (41) to be aligned with the lower part of the crucible (2),
vacuumizing the reaction bin (1) and replacing the reaction bin with argon, controlling the argon flow to be 10L under flowing argon, starting heating after the pressure in the reaction bin (1) is 600mbar-800mbar and stabilizing the pressure, setting the power of a first heater (31) to be 5-10kw for auxiliary material melting, and setting the power of a second heater (41) to be 10-18kw for main material melting;
after complete melting, the power of the first heater (31) and the power of the second heater (41) are adjusted, the temperature measuring piece (5) starts to work, after the temperature is stable, the transmission shaft drives the crucible (2) to rotate circumferentially, the rotating speed of the crucible (2) is 20-30rpm, and the solution is fully and uniformly mixed for 1 hour;
after sufficient uniformity, the seed crystal is contacted, the power of the first heater (31) and the power of the second heater (41) are adjusted to ensure that the temperature of the lower part of the crucible (2) is 2000+/-10 ℃, the temperature of the upper part of the crucible (2) is 1950+/-10 ℃, the rotation speed of the seed crystal support is 50-100rpm, and the seed crystal is raised at the speed of 0.25mm/h, and the SiC single crystal is epitaxially grown on the seed crystal by combining carbon and silicon.
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