CN115537926B - Large-size physical vapor phase method silicon carbide growth crucible capable of improving growth efficiency - Google Patents
Large-size physical vapor phase method silicon carbide growth crucible capable of improving growth efficiency Download PDFInfo
- Publication number
- CN115537926B CN115537926B CN202211523878.4A CN202211523878A CN115537926B CN 115537926 B CN115537926 B CN 115537926B CN 202211523878 A CN202211523878 A CN 202211523878A CN 115537926 B CN115537926 B CN 115537926B
- Authority
- CN
- China
- Prior art keywords
- crucible
- silicon carbide
- growth
- powder source
- physical vapor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 157
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 133
- 238000000034 method Methods 0.000 title claims abstract description 49
- 239000012808 vapor phase Substances 0.000 title claims abstract description 33
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 142
- 239000013078 crystal Substances 0.000 claims abstract description 117
- 239000000843 powder Substances 0.000 claims abstract description 75
- 229910052786 argon Inorganic materials 0.000 claims abstract description 71
- 239000007789 gas Substances 0.000 claims abstract description 61
- 238000010438 heat treatment Methods 0.000 claims abstract description 45
- 238000000151 deposition Methods 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 33
- 229910002804 graphite Inorganic materials 0.000 claims description 33
- 239000010439 graphite Substances 0.000 claims description 33
- 238000007664 blowing Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000009826 distribution Methods 0.000 abstract description 45
- 230000009471 action Effects 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000000859 sublimation Methods 0.000 description 41
- 230000008022 sublimation Effects 0.000 description 41
- 230000008569 process Effects 0.000 description 16
- 230000000694 effects Effects 0.000 description 11
- 230000008021 deposition Effects 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 238000004364 calculation method Methods 0.000 description 4
- 238000005240 physical vapour deposition Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/002—Controlling or regulating
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 field of production of silicon carbide by a physical vapor phase method, in particular to a large-size silicon carbide growth crucible for improving growth efficiency by the physical vapor phase method, which comprises a crucible main body and a crucible top cover, wherein the crucible main body sequentially comprises a powder source region and a seed crystal growth region from bottom to top; and a seed crystal for depositing the silicon carbide crystal is placed on one side, facing the cavity, of the crucible top cover, and a second heating device is also arranged above the crucible top cover. According to the invention, the first heating device is additionally arranged at the bottom of the crucible main body, so that the central temperature of the powder source is raised, meanwhile, the argon inlet is additionally arranged on the side wall surface of the crucible main body, and under the action of argon gas flow, high-temperature gas flow close to the wall surface of the crucible is conveyed to the center of the powder source, so that the central temperature of the powder source is further raised, and the uniformity of the internal temperature distribution of the powder source is also improved.
Description
Technical Field
The invention relates to the field of production of silicon carbide by a physical vapor phase method, in particular to a large-size silicon carbide growth crucible by the physical vapor phase method, which can improve the growth efficiency.
Background
Silicon carbide, a representative wide bandgap material for the third generation semiconductor, is a semiconductor material that is expected to dominate the semiconductor industry, following the first generation semiconductor material Si and the second generation semiconductor material GaAs. Compared with the first two generations of semiconductor materials, the silicon carbide has excellent semiconductor performance, the forbidden band width of the silicon carbide is 2-3 times of that of the silicon, the thermal conductivity of the silicon carbide is 3.3 times of that of the silicon, the breakdown field strength of the silicon is 10 times of that of the silicon, and the saturated electron mobility of the silicon carbide is 2.5 times of that of the silicon. Based on the above properties, silicon carbide materials are increasingly widely used in electronic devices with more severe working environment and higher performance requirements (such as high temperature, high frequency, corrosion resistance, radiation resistance and high power). At present, silicon carbide is already in the fields of aerospace, communication, petroleum industry, new energy automobiles, machining and the like.
The growth of large-size silicon carbide crystals is mainly realized by using a physical vapor transport Process (PVT), and the method is also the key point of the future production research of large-size silicon carbide. For example, the invention relates to a graphite crucible for growing large-size silicon carbide single crystals by a physical vapor deposition method and application thereof, and the graphite crucible comprises a crucible barrel for containing silicon carbide raw materials and an upper cover, wherein the upper part of the inner wall of the crucible barrel and the outer wall of the upper cover are provided with threads which are screwed with each other, and the upper cover is connected with the crucible barrel through the threads; a positioning block for placing a porous graphite plate is arranged on the inner wall of the crucible barrel; and a porous graphite plate is placed on the positioning block, and the outer diameter of the porous graphite plate is adapted to the inner diameter of the crucible barrel. The method effectively avoids the influence of the carbonization of the silicon carbide raw material on the crystal growth in the growth process, and improves the stability and the success rate of the crystal growth.
However, the research of the applicant of the present invention finds that in the growth process of the silicon carbide crystal by the PVT method, as the size increases, a plurality of new problems are generated in the growth process of the silicon carbide crystal. The method mainly focuses on two aspects, one is that the central temperature of the silicon carbide powder source is reduced more, the internal temperature distribution of the powder source is uneven, the sublimation efficiency of the powder source close to a crucible is high, the sublimation efficiency of the central part is low, even the powder source is hardened, and the growth speed and efficiency of crystals are reduced; secondly, the radial temperature distribution of the silicon carbide seed crystal is more obvious along with the increase of the size, so that the problems of stress concentration, crystal cracking, dislocation increase and the like of the crystal in the growth process are caused.
Disclosure of Invention
The invention provides a large-size physical vapor phase method silicon carbide growth crucible for improving growth efficiency, aiming at overcoming the defects that the temperature distribution of a silicon carbide powder source is uneven, the temperature difference between the powder source and seed crystals is reduced and the radial temperature gradient distribution of the seed crystals is uneven in the process of producing bulk silicon carbide crystals by a physical vapor phase method (PVT) in the prior art.
In order to realize the purpose of the invention, the invention is realized by the following technical scheme:
a large-size physical vapor phase method silicon carbide growth crucible capable of improving growth efficiency comprises a crucible main body, wherein a cavity is arranged in the crucible main body, the cavity sequentially comprises a powder source area for placing a silicon carbide powder source and a seed crystal growth area for depositing a silicon carbide crystal from bottom to top, a first heating device protruding towards the inside of the powder source area is arranged at the center of the bottom of the crucible main body, an argon inlet for blowing high-temperature gas close to the wall surface of the crucible main body to the center of the powder source area is formed in the side edge of the crucible main body, and an argon outlet for enabling argon to flow out of the seed crystal growth area is further formed in the side edge of the top of the crucible main body;
the silicon carbide crucible is characterized by further comprising a crucible top cover, wherein seed crystals for depositing silicon carbide crystals are placed on one side, facing the cavity, of the crucible top cover, and a second heating device is arranged above the crucible top cover.
In the prior art, in the process of producing the blocky silicon carbide crystal by adopting a physical vapor phase method (PVT), a heat source is usually started outside a crucible, and then heat sequentially enters the crucible along the crucible, so that a silicon carbide powder source is heated, the silicon carbide powder source is heated and then sublimated to form silicon carbide steam, and the silicon carbide steam rises above the crucible and then deposits on the surface of seed crystal above the crucible, so that the silicon carbide crystal is formed.
However, the applicant of the present invention has found that since heat is conducted from the outside of the crucible to the inside of the crucible, the temperature of the portion of the silicon carbide powder source near the wall surface of the crucible is inevitably higher than that of the silicon carbide powder source near the center of the crucible, and thus the problem of uneven temperature distribution of the silicon carbide powder source occurs. At this moment, the sublimation rate of the silicon carbide powder source close to the wall surface of the crucible is far higher than that of the silicon carbide powder source at the center of the crucible, so that the silicon carbide powder source close to the center of the crucible is hardened, and the sublimation rate and the efficiency of the silicon carbide powder source are further reduced.
Aiming at the defect in the prior art, the bottom of the crucible main body is provided with the first heating device protruding towards the interior of the powder source region on the basis of the traditional crucible, and the first heating device can play a role in heating the silicon carbide powder source at the center in the process of depositing silicon carbide crystals, so that the temperature distribution condition of the interior of the powder source can be effectively improved, the temperature of the center of the powder source can be increased, the temperature difference of the inner part and the outer part of the silicon carbide powder source can be reduced, the optimization of a thermal field can be realized, the hardening phenomenon of the silicon carbide powder source close to the center of the crucible can be prevented on the premise of not influencing the sublimation efficiency of part of the silicon carbide powder source close to the wall surface of the crucible, and the sublimation rate and the sublimation efficiency of the center of the powder source can be improved.
Because the silicon carbide gas formed after the silicon carbide powder source is heated and sublimated can flow in the silicon carbide powder source, when the first heating device is arranged, certain blocking effect on the flow of the silicon carbide sublimation gas in the silicon carbide powder source can be certainly realized, so that the flow of the silicon carbide sublimation gas in the silicon carbide powder source is disordered, the silicon carbide sublimation gas is not favorably diffused to a seed crystal growth area above the crucible main body, and the deposition effect of the silicon carbide is finally influenced. Therefore, aiming at the problem, the side edge of the crucible body is specially provided with an argon inlet for blowing the high-temperature gas close to the wall surface of the crucible body to the center of the powder source area, argon can be introduced into the argon inlet in the growth process, the argon is discharged from an argon outlet at the top after passing through the silicon carbide powder source, so that the flow of silicon carbide sublimation gas is guided, the silicon carbide sublimation gas is more stable in the process of diffusing to a seed crystal growth area above the crucible body, and the final silicon carbide deposition effect is ensured. In addition, the introduction of the argon can blow high-temperature gas close to the wall surface to the center of the powder source so as to further improve the uniformity of the temperature distribution in the powder source.
In addition, although the first heating device is additionally arranged at the center of the powder source, so that the average temperature of the whole powder source is relatively raised, the growth temperature of the seed crystal is inevitably influenced due to the introduction of argon gas into the side wall of the crucible main body, and in order to keep the stability of the growth temperature of the seed crystal, the second heating device is additionally arranged at the top of the top cover of the crucible, so that the influence of the argon gas on the temperature of the seed crystal can be reduced, the temperature environment of the growth area of the seed crystal can be always in a stable level, and the deposition effect of the silicon carbide crystal is improved.
In the crucible in the prior art, the sublimation gas of silicon carbide formed after the powder source region is heated diffuses towards the seed crystal growth region above the crucible main body, and the crucible in the prior art does not have a shielding part in the seed crystal growth region, so the sublimation gas of silicon carbide not participating in the deposition of the silicon carbide can flow upwards along the inner wall of the crucible until reaching the uppermost end of the crucible, then flow towards the seed crystal and deposit the silicon carbide crystal on the surface of the seed crystal, and the gas which does not participate in the deposition of the silicon carbide crystal can form a gas circulation loop with the sublimation gas of silicon carbide flowing upwards in the seed crystal growth region, so that the silicon carbide crystal is deposited on the surface of the seed crystal continuously. However, these gas flow conditions have two disadvantages: first, because carborundum sublimation gas is direct along the inner wall of crucible upflow to crucible top, the carborundum sublimation gas that consequently lies in the crucible top this moment is lower with the carborundum sublimation gas's that lies in the bottom difference in temperature, leads to carborundum sublimation gas to be difficult to at seed crystal surface deposit to cause the reduction of seed crystal surface recrystallization rate, slowed down the growth rate of carborundum. Secondly, because it is along the edge of crucible that it flows to the center department of seed crystal gradually behind the crucible upper end that flows, consequently the silicon carbide sublimation gas can lead to the silicon carbide sublimation gas to flow to the center department temperature of seed crystal and can take place to descend from the edge of seed crystal at the in-process that flows, thereby has formed the crystal and has followed the inhomogeneous phenomenon of radial temperature gradient distribution, thereby causes the crystal growth interface roughness too big, or produces M shape interface, thereby is unfavorable for the steady growth of crystal.
According to the invention, through the arrangement of the first heating device and the argon inlet, the silicon carbide sublimation gas is subjected to the flow guide effect of the argon when being formed in the powder source area, so that the silicon carbide sublimation gas can be gathered towards the center of the powder source area, and then the silicon carbide sublimation gas can flow upwards along the center of the powder source area, vertically flows upwards into the seed crystal growth area and then contacts with the seed crystal to deposit the silicon carbide crystal, and then the undeposited silicon carbide sublimation gas flows to the inner wall of the crucible along the radial direction of the seed crystal and flows to the outside of the crucible along the argon outlet, so that the internal airflow is not influenced.
Because the flow distribution condition of silicon carbide sublimation gas is changed, the deposition temperature can be kept consistent in the process of depositing the silicon carbide crystal on the surface of the seed crystal, and the distribution uniformity of the silicon carbide gas on the surface of the seed crystal and the crystal growth efficiency are improved under the action of various factors.
Preferably, the first heating device comprises a graphite column groove protruding towards the inner part of the powder source region;
a first heater is arranged in the graphite column groove.
The first heater in the first heating device is not in direct contact with the silicon carbide powder source in the powder source region, but is arranged in the graphite column groove protruding towards the inside of the powder source region, when the first heater is started, heat generated by the first heater can be transferred to the center of the silicon carbide powder source along the graphite column groove, and therefore the temperature at the center of the silicon carbide powder source can be kept stable and uniform.
Preferably, the first heater is a cylindrical resistance heater.
Preferably, the height of the graphite column groove is lower than that of the silicon carbide powder source in the powder source region.
Preferably, the argon gas inlet is located below the upper surface of the silicon carbide powder source placed inside the powder source region.
The argon is introduced into the argon inlet, so that the uniformity of the temperature distribution in the silicon carbide powder source is improved, the silicon carbide sublimation gas is guided to flow and diffuse horizontally to the seed crystal growth area more stably, and when the argon inlet is arranged above the upper surface of the silicon carbide powder source, the purpose of improving the uniformity of the temperature distribution in the silicon carbide powder source cannot be achieved, and the stable flow of the silicon carbide sublimation gas to the seed crystal growth area can be disturbed. Therefore, the argon inlet is arranged below the upper surface of the silicon carbide powder source, so that the stable flow of silicon carbide sublimation gas to a seed crystal growth area can be maintained on the premise of improving the uniformity of the temperature distribution in the silicon carbide powder source.
Preferably, the argon inlets are layered above and below each other, and the argon inlets in each layer are uniformly arrayed around the powder source region.
According to the invention, the argon inlet with a multilayer structure is arranged, so that the effect of argon on improving the uniformity of the temperature distribution in the silicon carbide powder source can be effectively improved, and the stability of airflow can be maintained.
Preferably, the argon inlet and the argon outlet are internally blocked by a porous graphite sheet.
Preferably, the second heating means comprises a disc-shaped resistance heater disposed above the crucible top cover;
and a gap is formed between the second heating device and the crucible top cover.
Preferably, the radius of the second heating device is larger than or equal to the radius of the seed crystal.
According to the invention, the control effect of the heat source can be effectively ensured by setting the radius of the second heating device to be more than or equal to that of the seed crystal, so that the temperature stability of the growth area of the seed crystal is ensured.
Preferably, a layer of heat preservation graphite felt is further sleeved outside the crucible main body.
Therefore, the invention has the following beneficial effects:
(1) The first heating device is additionally arranged at the bottom of the crucible body, so that the central temperature of the powder source is increased, meanwhile, the argon inlet is additionally arranged on the side wall surface of the crucible body, and under the action of argon gas flow, high-temperature gas flow close to the wall surface of the crucible is conveyed to the center of the powder source, so that the central temperature of the powder source is further increased, and the uniformity of the temperature distribution in the powder source is also improved;
(2) The argon inlet arranged at the lower part of the crucible main body and the outlet arranged at the top of the crucible main body improve the stability of airflow in the crucible, and further improve the uniformity of the temperature gradient distribution on the surface of the seed crystal and the uniformity of the distribution of the silicon carbide solute;
(3) The second heating device arranged above the top of the crucible body can further improve the temperature environment for seed crystal growth and improve the uniformity of temperature gradient distribution on the growth surface of the seed crystal;
(4) The specific structure of the invention can adjust the height of the newly added second heating device and the arrangement position of the argon inlet according to the actual growth condition so as to adjust the distribution condition of the temperature field in the powder source. The positions of the argon outlet and the second heating device at the top of the crucible are adjusted, so that the temperature field distribution of the seed crystal domain can be improved, and the device has strong adaptability;
(5) The structure of the invention controls and adjusts the temperature fields of the powder source and the seed crystal, and is also suitable for growing other types of crystals by a physical vapor transport method. The invention improves the PVT method growth system, has simple structure, easy implementation, lower cost and reusability.
Drawings
FIG. 1 is a schematic perspective view of a large-size physical vapor phase method silicon carbide growth crucible for improving growth efficiency according to the present invention.
FIG. 2 is a schematic cross-sectional view and a schematic size diagram of a large-sized physical vapor phase method silicon carbide growth crucible for improving growth efficiency.
FIG. 3 is a schematic view of the structure of a conventional silicon carbide growth crucible.
FIG. 4 is a cloud view of the internal flow field distribution of two different silicon carbide growth crucibles;
the left side (a) of the figure is a distribution cloud picture of an internal flow field of a traditional silicon carbide growth crucible;
the right side (b) in the figure is a distribution cloud picture of an internal flow field of the large-size physical vapor phase method silicon carbide growth crucible for improving the growth efficiency.
Figure 5 is a cloud of temperature profiles inside two different silicon carbide growth crucibles.
The left side (a) of the figure is a cloud of the internal temperature profile of a conventional silicon carbide growth crucible;
the right side (b) in the figure is a cloud picture of the internal temperature distribution of the large-size physical vapor phase method silicon carbide growth crucible for improving the growth efficiency.
FIG. 6 shows the radial temperature gradient profile of the seed crystal under two different growth crucibles.
Wherein: the device comprises a crucible main body 1, a crucible top cover 2, a cavity 3, a seed crystal growth region 4, a powder source region 5, a seed crystal 6, a first heating device 7, an argon inlet 8, an argon outlet 9, a second heating device 10, a graphite column groove 11, a first heater 12, a porous graphite sheet 13, a heat preservation graphite felt 14 and an electromagnetic coil 15.
Detailed Description
The invention is further described with reference to the drawings and the detailed description. Those skilled in the art will be able to implement the invention based on these teachings. Furthermore, the embodiments of the present invention described in the following description are generally only a part of the embodiments of the present invention, and not all of the embodiments. Therefore, all other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without making creative efforts shall fall within the protection scope of the present invention.
As shown in figures 1 and 2, the invention provides a large-size physical vapor phase method silicon carbide growth crucible capable of improving growth efficiency, which comprises a crucible main body 1 and a crucible top cover 2 arranged above the crucible main body 1, wherein a cavity 3 is arranged in the crucible main body 1, the cavity 3 sequentially comprises a powder source area 5 for placing a silicon carbide powder source and a seed crystal growth area 4 for circulating silicon carbide gas from bottom to top, and a seed crystal 6 for depositing silicon carbide crystals is placed on one side of the crucible top cover 2 facing the cavity 3.
The crucible body 1 is provided with a first heating device 7 protruding towards the inside of the powder source region 5 at the center of the bottom thereof, and the first heating device comprises a graphite column groove 11 protruding towards the inside of the powder source region 5, a first heater 12 is arranged inside the graphite column groove 11, and the first heater 12 can be selected from cylindrical resistance heaters in some embodiments. Therefore, it can play the heating effect to the carborundum powder source that is located powder source zone 5 center department after starting first heater 12 in-process of deposit carborundum crystal, thereby can effectively improve the inside temperature distribution condition in powder source, improve the temperature at powder source center, make the inside and outside partial difference in temperature in carborundum powder source reduce, thereby realize the optimization of thermal field, under the prerequisite that does not influence the sublimation efficiency of the partial carborundum powder source of nearly crucible wall, the phenomenon of hardening of the carborundum powder source of nearly crucible center department has been prevented, the sublimation rate and the efficiency at powder source center have been promoted.
Meanwhile, the side edge of the crucible main body 1 is provided with a plurality of groups of argon inlets 8 and argon outlets 9, the insides of the argon inlets 8 and the argon outlets are blocked by the porous graphite sheets 13, and after argon is introduced into the inlets of the argon inlets 8, the argon can blow high-temperature gas close to the wall surface of the crucible main body 1 to the center of the powder source region 5, so that the central temperature of the powder source and the uniformity of the internal temperature distribution of the powder source are further improved.
In the invention, the argon inlets 8 are arranged in a layered manner from top to bottom (in the embodiment, the number of the argon inlets 8 is 3, and the number of the argon inlets 8 in each layer is 4), and the argon inlets 8 in each layer are uniformly arrayed around the powder source region 5.
Because the argon gas lets in by argon gas entry 8, then is discharged by the argon gas export 9 at top to can guide carborundum sublimation gas to flow, make carborundum sublimation gas more steady to the 4 diffusion in-process of the seed crystal growth region of crucible main part 1 top, ensured final carborundum deposit effect.
To carborundum sublimation gas's flow, because carborundum sublimation gas has received the water conservancy diversion effect of argon when the powder source district 5 is inside to be formed, make carborundum sublimation gas can assemble to the center department of powder source district 5, thereby make carborundum sublimation gas can flow upwards along the center of powder source district 5, then vertical upward flow to the seed crystal growth region 4 in then contact deposit carborundum crystal with seed crystal 6 earlier, then undeposited carborundum sublimation gas is then along the radial flow to the inner wall of crucible main part 1 of seed crystal 6, and flow to crucible main part 1 outside along argon outlet 9, thereby do not exert an influence to the inside air current of crucible main part 1. According to the invention, the flow distribution condition of silicon carbide sublimation gas is changed, so that the deposition temperature can be kept consistent in the process of depositing the silicon carbide crystal on the surface of the seed crystal 6, and the distribution uniformity of the silicon carbide gas on the surface of the seed crystal and the crystal growth efficiency are improved under the action of various factors.
In addition, the invention is also provided with a second heating device 10 above the crucible top cover 2, and in a preferred mode, the second heating device 10 can be selected to be a disc-shaped resistance heater. The reason is that although the first heating device 7 is additionally arranged at the center of the powder source, the average temperature of the whole powder source is relatively increased, the growth temperature of the seed crystal is inevitably influenced due to the fact that argon is introduced into the side wall of the crucible main body 1, and the second heating device 10 is additionally arranged at the top of the crucible top cover 2 for keeping the stability of the growth temperature of the seed crystal, so that the influence of the argon on the temperature of the seed crystal 6 can be reduced, the temperature environment of the seed crystal growth area 4 can be in a stable level all the time, and the deposition effect of the silicon carbide crystal is improved. In a preferred mode, the radius of the disc-shaped resistance heater is larger than or equal to that of the seed crystal 6, so that the temperature stability of the seed crystal growth region is ensured.
The overall device size of the present invention is set as follows:
H1＜H；
δ = 5~15mm；
r = 35~45mm;
di = 10~30mm;
do = 25~45mm;
R＞ Rs；
Rh ＞ Rs
wherein H1 is the height of newly-increased graphite column groove 11, H is carborundum powder source height, delta is newly-increased graphite column groove 11 wall thickness, R is graphite column groove 11 external diameter, di is argon gas inlet 8 diameter, do is argon gas outlet 9 diameter, R is cavity 3 inside radius, rh is disc type resistance heater radius, rs is seed crystal 6 radius.
The graphite column groove 11 with the cylindrical resistance heater of the first heater 12 designed by the invention is arranged in the silicon carbide powder source, the central temperature of the powder source can be effectively improved under the action of the first heater 12, and meanwhile, the multilayer argon inlet 8 additionally arranged on the side wall of the silicon carbide powder source can effectively blow high-temperature gas on the graphite wall surface of the crucible main body 1 to the center of the powder source, so that the distribution uniformity of the internal temperature field of the powder source is improved. Meanwhile, the second heating device 10 (namely, a disc-shaped resistance heater) arranged above the crucible top cover 2 can improve the temperature gradient distribution in the growth process of the seed crystal and create a better temperature environment for the growth of the crystal.
In the actual growth process, the height of the central graphite column groove 11, the arrangement of the argon inlet 8, the power of the newly added first heater 12 (namely, a cylindrical resistance heater) and second heating device 10 (namely, a disc-shaped resistance heater) and the like can be adjusted according to specific growth conditions so as to ensure that the crystal growth environment reaches the optimal condition.
The embodiment of the invention is only an example for the technical scheme of the invention, and the large-size physical vapor phase method silicon carbide growth crucible for improving the growth efficiency is not limited to the silicon carbide growth, but is subject to the scope defined by the claims. Any modification, supplement or equivalent replacement by a person skilled in the art on the basis of this embodiment is within the scope of the invention as claimed in the claims.
[ application example ]
In order to verify the operation effect of the large-size physical vapor phase method silicon carbide growth crucible for improving the growth efficiency, the inventor constructs a multi-physical field model of the large-size physical vapor phase method silicon carbide growth crucible for improving the growth efficiency according to the structure and the size of the crucible, carries out simulation calculation on a multi-physical field flow field and a thermal field, and compares the calculation result (comprising a temperature field, a crucible internal flow field and a seed crystal radial temperature gradient) with the traditional silicon carbide growth crucible (the structure of which is shown in figure 3).
The traditional silicon carbide growth crucible for calculation and comparison has the advantages that the inner diameter of the crucible body 1 is 0.2m, the height of the crucible body 1 is 0.36m, a powder source is placed at the bottom of the crucible body 1, the height of the silicon carbide powder source is 0.2m, the wall thickness of the crucible body 1 is 0.02m, and the seed crystal 6 is arranged at the position of the crucible top cover 2 and has the circular diameter of 0.16m.
The calculation adopted large-size physical vapor phase method silicon carbide growth crucible for improving the growth efficiency has the following specific structure and size: the inner diameter of a crucible body 1 is 0.2m, the height of the crucible body 1 is 0.36m, the height of a silicon carbide powder source is 0.2m, a central graphite column groove is 110.18m, the diameter of an argon inlet 8 is 0.02m, the central distance between the argon inlets 8 of two adjacent layers is 0.06m, the diameter of an argon outlet 9 is 0.04m, the diameter of a seed crystal 6 is 0.16m, the diameter of a disc type resistance heater is 0.24m, the outer diameter of a graphite column groove 11 is 0.04m, and the wall thickness of the graphite column groove 11 is 0.01m.
As an example, the basic structures of the two growing systems are the same, the same electromagnetic coil current is adopted, the number of the coils is 1000A, the number of the coils is 8, and the centers of the coil groups are aligned with the position 1/2 of the height of the powder source.
The invention relates to a large-size physical vapor phase method silicon carbide growth crucible for improving growth efficiency, wherein the silicon carbide growth process comprises the following steps:
(1) And placing the silicon carbide powder source in a powder source area 5 at the bottom of the crucible body 1, and introducing argon from the bottom of the crucible body 1 for 3min at an argon inlet flow rate of 0.01m/s to exhaust other gases in the crucible.
(2) The electromagnetic coil 15 is connected with the first heater 12 in the graphite column groove 11, the coil current and the power of the first heater 12 are adjusted, so that the temperature rising speed of the first heater 12 is similar to that of the crucible wall surface, and the whole temperature rising stage comprises the following 3 stages: the electromagnetic coil 15 and the first heater 12 are controlled in the first stage to enable the temperature to reach 1650-1740 ℃, the duration time of the heating stage is preset to be 15-30min, the electromagnetic coil 15 and the first heater 12 are controlled in the second heating stage to enable the temperature to reach 2185-2285 ℃, the duration time of the heating stage is preset to be 24h-36h, the electromagnetic coil 15 and the first heater 12 are controlled in the third stage to enable the temperature to reach 2300-2400 ℃, and the duration time of the heating stage is preset to be 8-12h.
(3) The power of the second heating means 10 (disk resistance heat source) at the top of the crucible is adjusted to ensure that the seed crystal is maintained at the proper growth temperature.
Compared with the traditional silicon carbide growth crucible, the silicon carbide growth process comprises the following steps:
(1) A silicon carbide powder source is placed in a powder source region 5 at the bottom of the crucible body 1.
(2) The electromagnetic coil 15 is switched on, and the current power of the coil is adjusted, so that the crucible is heated, and the whole heating stage comprises the following 3 stages: the electromagnetic coil 15 is controlled in the first stage to enable the temperature to reach 1650-1740 ℃, the duration of the temperature rise stage is preset to be 15-30min, the electromagnetic coil 15 is controlled in the second temperature rise stage to enable the temperature to reach 2185-2285 ℃, the duration of the temperature rise stage is preset to be 24h-36h, the electromagnetic coil 15 is controlled in the third stage to enable the temperature to reach 2300-2400 ℃, and the duration of the temperature rise stage is preset to be 8-12h.
(3) And (5) growing a seed crystal.
By way of example, fig. 4 is a cloud image of the internal flow field distribution of two different silicon carbide growth crucibles, wherein the left side (a) in the figure is the cloud image of the internal flow field distribution of a conventional silicon carbide growth crucible, and the right side (b) in the figure is the cloud image of the internal flow field distribution of a large-size physical vapor phase silicon carbide growth crucible for improving the growth efficiency. As can be seen from the flow field distribution cloud chart, by adopting the large-size physical vapor phase method silicon carbide growth system for improving the growth efficiency, the flow condition in the crucible main body 1 is obviously changed, the airflow flows in from the argon inlet 8 at the bottom of the crucible main body 1, flows upwards along the center and finally flows out from the argon outlet 9 at the top of the crucible main body 1, and the high-temperature sublimation gas on the wall surface of the crucible main body 1 at the bottom can be brought to the center of the powder source area 5 to improve the central temperature of the silicon carbide powder source, and meanwhile, because the high-temperature airflow flows to the seed crystal along the center of the crucible main body 1, the central temperature of the seed crystal 6 can be improved to a certain extent, so that the surface temperature distribution condition of the seed crystal 6 is improved, and the growth interface of the seed crystal 6 reaches an ideal state.
FIG. 5 is a cloud image of the internal temperature distribution of two different silicon carbide growth crucibles, wherein the left side (a) of the cloud image is the internal temperature distribution of a conventional silicon carbide growth crucible, and the right side (b) of the cloud image is the internal temperature distribution of a large-sized physical vapor phase silicon carbide growth crucible according to the present invention, which is proposed to improve the growth efficiency. As can be seen from the temperature distribution cloud chart, the large-size physical vapor phase method silicon carbide growth crucible for improving the growth efficiency has the advantages that the internal temperature of the powder source is obviously improved, the temperature distribution is more uniform, and the sublimation rate and efficiency of the silicon carbide powder are favorably improved. Meanwhile, the temperature of the seed crystal growth area 4 is still kept at a better level due to the action of a second heating device 10 (a disc type resistance heat source) additionally arranged at the top of the crucible top cover 2.
FIG. 6 is a graph showing radial temperature gradient distribution of seed crystals in two different growth crucibles, in which the basic structure is shown as the radial temperature gradient distribution of seed crystals in a conventional SiC growth crucible, and the optimized structure is shown as the radial temperature gradient distribution of seed crystals in a large-sized PVD SiC growth crucible for improving growth efficiency according to the present invention, and it can be seen from the graph that the radial temperature gradient distribution uniformity of seed crystals 6 is improved accordingly by using the large-sized PVD SiC growth crucible for improving growth efficiency according to the present invention, which is advantageous for improving the interface shape during crystal growth.
Claims (9)
1. The large-size physical vapor phase method silicon carbide growth crucible capable of improving growth efficiency is characterized by comprising a crucible main body (1), wherein a cavity (3) is arranged in the crucible main body, the cavity (3) sequentially comprises a powder source area (5) for placing a silicon carbide powder source and a seed crystal growth area (4) for depositing silicon carbide crystals from bottom to top, a first heating device (7) protruding towards the inside of the powder source area (5) is arranged at the center of the bottom of the crucible main body (1), an argon inlet (8) for blowing high-temperature gas close to the wall surface of the crucible main body (1) to the center of the powder source area (5) is formed in the side edge of the top of the crucible main body (1), an argon outlet (9) for enabling argon to flow out of the seed crystal growth area (4) is further formed in the side edge of the top of the crucible main body (1), and the argon inlet (8) is located below the upper surface of the silicon carbide powder source placed in the powder source area (5);
the silicon carbide crucible is characterized by further comprising a crucible top cover (2), wherein a seed crystal (6) for depositing silicon carbide crystals is placed on one side of the crucible top cover facing the cavity (3), and a second heating device (10) is arranged above the crucible top cover (2).
2. A large-sized physical vapor phase silicon carbide growth crucible for increasing growth efficiency as claimed in claim 1, wherein said first heating means (7) comprises a graphite column groove (11) protruded toward the inside of the powder source region (5);
a first heater (12) is arranged in the graphite column groove (11).
3. A large size physical vapor phase silicon carbide growth crucible for increasing growth efficiency as claimed in claim 2 wherein said first heater (12) is a cylindrical resistance heater.
4. A large size physical vapor phase silicon carbide growth crucible for improving growth efficiency according to claim 2 or 3, wherein the height of the graphite pillar groove (11) is lower than the height of the silicon carbide powder source inside the powder source region (5).
5. The large-size physical vapor phase silicon carbide growth crucible for improving growth efficiency according to claim 1, wherein the argon gas inlets (8) are layered on top of each other, and the argon gas inlets (8) in each layer are uniformly arrayed around the powder source region (5).
6. A large size physical vapor phase silicon carbide growth crucible for increasing growth efficiency as claimed in claim 5, wherein the argon gas inlet (8) and the argon gas outlet (9) are internally sealed by a porous graphite sheet (13).
7. A large size physical vapor phase silicon carbide growth crucible for improving growth efficiency as claimed in claim 1 wherein said second heating means (10) comprises a disc shaped resistance heater disposed above the crucible top cover (2);
a gap is reserved between the second heating device (10) and the crucible top cover (2).
8. The large-size physical vapor phase silicon carbide growth crucible for improving growth efficiency as claimed in claim 7, wherein the radius of the second heating means (10) is equal to or larger than the radius of the seed crystal (6).
9. The large-size physical vapor phase silicon carbide growth crucible for improving the growth efficiency as claimed in claim 1, wherein the crucible main body (1) is further sleeved with a layer of heat preservation graphite felt (14).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211523878.4A CN115537926B (en) | 2022-12-01 | 2022-12-01 | Large-size physical vapor phase method silicon carbide growth crucible capable of improving growth efficiency |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211523878.4A CN115537926B (en) | 2022-12-01 | 2022-12-01 | Large-size physical vapor phase method silicon carbide growth crucible capable of improving growth efficiency |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115537926A CN115537926A (en) | 2022-12-30 |
| CN115537926B true CN115537926B (en) | 2023-03-17 |
Family
ID=84722381
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211523878.4A Active CN115537926B (en) | 2022-12-01 | 2022-12-01 | Large-size physical vapor phase method silicon carbide growth crucible capable of improving growth efficiency |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115537926B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116377567B (en) * | 2023-06-05 | 2023-10-13 | 苏州优晶光电科技有限公司 | A silicon carbide single crystal growth device and growth method |
| CN116815320B (en) * | 2023-06-28 | 2024-01-12 | 通威微电子有限公司 | Silicon carbide crystal growth device and method and silicon carbide crystal |
| CN116988144B (en) * | 2023-08-16 | 2024-07-16 | 浙江晶越半导体有限公司 | Method for reducing dislocation in silicon carbide single crystal and improving growth efficiency |
| EP4575047A1 (en) * | 2023-12-19 | 2025-06-25 | SiCrystal GmbH | Crucible for producing a sic volume mono crystal and a method for growing a sic volume mono crystal |
| CN118547371B (en) * | 2024-07-29 | 2025-02-21 | 浙江晶越半导体有限公司 | Growth furnace for rapidly growing high-quality 8-inch silicon carbide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009051701A (en) * | 2007-08-28 | 2009-03-12 | Denso Corp | Silicon carbide single crystal manufacturing apparatus and manufacturing method thereof |
Family Cites Families (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4503736B2 (en) * | 1999-08-31 | 2010-07-14 | 独立行政法人産業技術総合研究所 | Method and apparatus for producing single crystal |
| JP4499698B2 (en) * | 2006-10-04 | 2010-07-07 | 昭和電工株式会社 | Method for producing silicon carbide single crystal |
| SE537049C2 (en) * | 2008-12-08 | 2014-12-16 | Ii Vi Inc | Process and apparatus for growth via axial gradient transport (AGT) using resistive heating |
| KR101731239B1 (en) * | 2012-04-20 | 2017-04-28 | 투-식스 인코포레이티드 | LARGE DIAMETER, HIGH QUALITY SiC SINGLE CRYSTALS, METHOD AND APPARATUS |
| JP6111873B2 (en) * | 2013-06-04 | 2017-04-12 | 新日鐵住金株式会社 | Method for producing silicon carbide single crystal ingot |
| CN108138359A (en) * | 2015-10-02 | 2018-06-08 | 昭和电工株式会社 | Sic single crystal ingot |
| CN216107323U (en) * | 2021-09-15 | 2022-03-22 | 浙江大学 | Resistance-type and induction-type double-heating silicon carbide single crystal growth device |
| CN216688415U (en) * | 2021-12-29 | 2022-06-07 | 浙江大学杭州国际科创中心 | Crucible structure for improving powder source temperature field |
| CN216786307U (en) * | 2022-02-10 | 2022-06-21 | 福建北电新材料科技有限公司 | Crystal growing device |
| CN115074821A (en) * | 2022-04-29 | 2022-09-20 | 连城凯克斯科技有限公司 | Thermal field structure and method for growing silicon carbide by graphite resistance heating |
| CN115305573B (en) * | 2022-10-11 | 2023-03-24 | 浙江晶越半导体有限公司 | Crucible for growth of silicon carbide crystal by physical vapor phase method for optimizing thermal field |
-
2022
- 2022-12-01 CN CN202211523878.4A patent/CN115537926B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009051701A (en) * | 2007-08-28 | 2009-03-12 | Denso Corp | Silicon carbide single crystal manufacturing apparatus and manufacturing method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115537926A (en) | 2022-12-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN115537926B (en) | Large-size physical vapor phase method silicon carbide growth crucible capable of improving growth efficiency | |
| CN115305573B (en) | Crucible for growth of silicon carbide crystal by physical vapor phase method for optimizing thermal field | |
| KR102331308B1 (en) | Large size, high-purity silicon carbide single crystal, substrate, and manufacturing method and device for the same | |
| CN108060392B (en) | A controllable linear evaporation device and coating method | |
| US20150083046A1 (en) | Carbon fiber ring susceptor | |
| CN113122924B (en) | Crystal growth assembly, crystal growth apparatus and method | |
| KR20240178256A (en) | High-quality silicon carbide crystal growth device and method | |
| US6099650A (en) | Structure and method for reducing slip in semiconductor wafers | |
| US6800136B2 (en) | Axial gradient transport apparatus and process | |
| CN109881186A (en) | A kind of device for being heated at high temperature in CVD equipment to substrate | |
| CN104514034A (en) | High-temperature device and method for silicon carbide growth | |
| JP2003086516A (en) | Susceptor, CVD device, film forming method, and semiconductor device | |
| CN114134571B (en) | Crucible assembly and single crystal growing apparatus having the same | |
| CN115142132A (en) | Silicon carbide crystal growth device and large-size silicon carbide crystal growth method | |
| Arai et al. | Highly uniform growth in a low-pressure MOVPE multiple wafer system | |
| CN118547371B (en) | Growth furnace for rapidly growing high-quality 8-inch silicon carbide | |
| CN207713807U (en) | A kind of controllable linear vaporising device | |
| WO2019114233A1 (en) | Infrared heating lamp tube device | |
| CN222251121U (en) | Growing crucible | |
| CN114150377B (en) | Thick film growth equipment | |
| CN116988144B (en) | Method for reducing dislocation in silicon carbide single crystal and improving growth efficiency | |
| US20220386422A1 (en) | Heating body of epitaxial growth device | |
| CN116555898A (en) | Silicon carbide crucible structure grown by PVT method with high powder source utilization rate and growth method thereof | |
| KR101395222B1 (en) | Apparatus and method for processing substrate | |
| CN117867647A (en) | Growth method and growth system for low-defect high-quality silicon carbide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |