CN116607216A - Method and system for adjusting internal temperature field of resistance silicon carbide growth furnace and growth method - Google Patents
Method and system for adjusting internal temperature field of resistance silicon carbide growth furnace and growth method Download PDFInfo
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- CN116607216A CN116607216A CN202310890304.9A CN202310890304A CN116607216A CN 116607216 A CN116607216 A CN 116607216A CN 202310890304 A CN202310890304 A CN 202310890304A CN 116607216 A CN116607216 A CN 116607216A
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 313
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 309
- 230000012010 growth Effects 0.000 title claims abstract description 95
- 238000000034 method Methods 0.000 title claims abstract description 77
- 239000013078 crystal Substances 0.000 claims abstract description 177
- 239000002994 raw material Substances 0.000 claims abstract description 123
- 238000010438 heat treatment Methods 0.000 claims abstract description 29
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 19
- 239000010439 graphite Substances 0.000 claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000013585 weight reducing agent Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 45
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 42
- 238000006243 chemical reaction Methods 0.000 claims description 38
- 229910052757 nitrogen Inorganic materials 0.000 claims description 22
- 229910052786 argon Inorganic materials 0.000 claims description 21
- 238000001514 detection method Methods 0.000 claims description 15
- 238000000137 annealing Methods 0.000 claims description 7
- 230000000630 rising effect Effects 0.000 claims description 2
- 230000007547 defect Effects 0.000 abstract description 17
- 230000001105 regulatory effect Effects 0.000 abstract description 9
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 238000001212 derivatisation Methods 0.000 abstract description 2
- 230000003750 conditioning effect Effects 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 238000001953 recrystallisation Methods 0.000 description 3
- 230000003698 anagen phase Effects 0.000 description 2
- BULVZWIRKLYCBC-UHFFFAOYSA-N phorate Chemical compound CCOP(=S)(OCC)SCSCC BULVZWIRKLYCBC-UHFFFAOYSA-N 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 101150061215 outM gene Proteins 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/003—Heating or cooling of the melt or the crystallised material
-
- 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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/006—Controlling or regulating
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
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- Crystallography & Structural Chemistry (AREA)
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- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention belongs to the technical field of derivatization of silicon carbide crystal growth, and particularly relates to a real-time regulating method, a regulating system and a growing method for an internal temperature field of a resistance-method silicon carbide growing furnace. The real-time adjusting method comprises the steps of obtaining leakage amount of silicon carbide raw materials in a silicon carbide growing furnace in real time, and obtaining thickness of a silicon carbide crystal block grown by a resistance method according to the leakage amount of the silicon carbide raw materials and a first preset relation, wherein the leakage amount of the silicon carbide raw materials is weight reduction amount of materials in a crucible in the growing furnace; and according to the thickness of the silicon carbide crystal block and a second preset relation, acquiring the height of the crucible in the growth furnace after the crucible is moved upwards, and according to the height of the crucible after the crucible is moved upwards, moving the position of the crucible upwards. The method can effectively control the position of the silicon carbide growth interface relative to the graphite heating element in real time, reduce the formation of crystal defects and improve the crystal quality.
Description
Technical Field
The invention relates to the technical field of derivatization of silicon carbide crystal growth, in particular to a real-time regulating method, a regulating system and a growing method of an internal temperature field of a resistance silicon carbide growing furnace.
Background
Silicon carbide has the advantages of wide band gap, high critical breakdown field strength, high thermal conductivity, high carrier saturation mobility and the like, and is widely concerned with the development of semiconductor industry, and has irreplaceable advantages in the fields of high-temperature, high-voltage, high-frequency and other electronic application.
The Physical Vapor Transport (PVT) method is the main method for industrially producing silicon carbide single crystals at present, and specifically, the gas produced by sublimation and decomposition of the silicon carbide raw material is transported to the surface of a seed crystal for recrystallization to obtain the silicon carbide single crystals with larger area, in the crystal growth stage, along with the continuous growth of the crystal, the thickness of the silicon carbide single crystals can be increased, the position of a silicon carbide growth interface relative to a graphite heating body outside a crucible can be changed, the temperature distribution of the silicon carbide growth interface can be changed, however, the temperature distribution of the silicon carbide growth interface affects the growth process and the quality of the silicon carbide single crystals, the excessive growth temperature easily causes defects such as polytype of the crystal, the excessively low growth temperature easily forms defects such as polycrystal, and the temperature of the silicon carbide growth interface needs to be controlled.
At present, in the process of growing silicon carbide single crystals by a resistance method, the lifting of a crucible is mostly regulated according to a set program, and the silicon carbide single crystals are difficult to grow according to the expected growth speed and the expected growth quality in the process of growing the crystals due to the influence of uncontrollable factors such as equipment deviation, installation deviation, fluctuation of pressure in a growth furnace and crucible temperature, and the like, and the position of a silicon carbide growth interface is easy to deviate from the expected position greatly, so that if the lifting of the crucible is regulated according to the set program, the defects such as polycrystal, polymorphism and the like of the crystals can be caused.
Disclosure of Invention
The invention aims to overcome the defect that the position of a silicon carbide growth interface is easy to deviate from an expected position greatly and possibly cause polycrystal and polytype of crystals when a silicon carbide single crystal is produced by a resistance method in the prior art, and provides a real-time regulating method, a regulating system and a growth method for the internal temperature field of a resistance silicon carbide growth furnace.
In order to achieve the above object, in a first aspect, the present invention provides a method for real-time adjustment of an internal temperature field of a resistive silicon carbide growth furnace, the method comprising:
acquiring leakage amount of a silicon carbide raw material in a silicon carbide growth furnace in real time, and acquiring thickness of a silicon carbide crystal block grown by a resistance method according to the leakage amount of the silicon carbide raw material and a first preset relation, wherein the leakage amount of the silicon carbide raw material is weight reduction amount of materials in a crucible in the growth furnace;
and according to the thickness of the silicon carbide crystal block and a second preset relation, acquiring the height of the crucible in the growth furnace after the crucible is moved upwards, and according to the height of the crucible after the crucible is moved upwards, moving the position of the crucible upwards.
In some preferred embodiments, the first preset relationship is a relationship of the amount of leakage of the silicon carbide feedstock to the weight of the silicon carbide crystal mass;
the obtaining of the thickness of the silicon carbide crystal block sequentially comprises obtaining the weight of the silicon carbide crystal block according to the leakage amount of the silicon carbide raw material and the first preset relation, and obtaining the thickness of the silicon carbide crystal block according to the weight of the silicon carbide crystal block.
More preferably, the silicon carbide raw material has a leakage amount ofM Leakage of The weight of the silicon carbide crystal block isM Crystal block The first preset relation is thatM Crystal block =M Leakage of ×k 1 。
In some preferred embodiments, the first preset relationship includes a third preset relationship that is a relationship of a leakage amount of the silicon carbide raw material to a reaction amount of the silicon carbide raw material and a fourth preset relationship that is a relationship of a reaction amount of the silicon carbide raw material to a weight of the silicon carbide crystal mass;
the obtaining of the thickness of the silicon carbide crystal block sequentially comprises obtaining the reaction quantity of the silicon carbide raw material according to the leakage quantity of the silicon carbide raw material and the third preset relation, obtaining the weight of the silicon carbide crystal block according to the reaction quantity of the silicon carbide raw material and the fourth preset relation, and obtaining the thickness of the silicon carbide crystal block according to the weight of the silicon carbide crystal block.
More preferably, the silicon carbide raw material has a leakage amount ofM Leakage of The reaction amount of the silicon carbide raw material isM Reaction The weight of the silicon carbide crystal block isM Crystal block The third preset relationship is thatM Reaction =M Leakage of ×k 3 The fourth preset relationship is thatM Crystal block =M Reaction ×k 4 。
More preferably, the silicon carbide growth furnace is charged with a weight ofM Total (S) The silicon carbide raw material of the device is reacted completely, and the leakage amount of the silicon carbide raw material is measuredM Total leakage of Measuring the weight of a silicon carbide crystal massM Total crystal block ；
Calculation ofM Total (S) /M Total leakage of Obtainingk 3 Calculation ofM Total crystal block /M Total (S) Obtainingk 4 ；
Or, calculateM Total crystal block /M Total leakage of Obtainingk 1 。
In some preferred embodiments, the silicon carbide crystal mass has a thickness ofT Crystal block The initial height of the crucible is 0, and the height of the crucible after the crucible is moved up isH Crucible pot The second preset relationship is thatH Crucible pot =T Crystal block ×k 2 The saidk 2 0.9 to 1.1.
In a second aspect, the present invention provides a real-time adjustment system employing the real-time adjustment method of the first aspect, the system comprising: the device comprises a leakage detection module, a PLC logic control module and a mechanical driving module;
the leakage detection module is used for detecting and outputting the leakage of the silicon carbide raw material in the silicon carbide growth furnace; the PLC logic control module is used for receiving the leakage amount of the silicon carbide raw material, and calculating and outputting the height of the crucible in the growth furnace after the crucible is moved upwards according to the leakage amount of the silicon carbide raw material, the first preset relation and the second preset relation; the mechanical driving module is used for receiving the height of the crucible after the crucible is moved upwards, and the crucible is moved upwards according to the height of the crucible after the crucible is moved upwards.
In some preferred embodiments, the leak detection module includes a weight sensor and the mechanical drive module includes a lift motor.
In a third aspect, the present invention provides a method for growing silicon carbide using the real-time conditioning method of the first aspect, the method comprising:
and (3) heating: placing the crucible filled with the silicon carbide raw material and the seed crystal into a silicon carbide growth furnace, vacuumizing, introducing nitrogen and argon into a furnace shell cavity, enabling the pressure in the furnace shell cavity to reach 10000 Pa-20000 Pa, enabling the flow of the nitrogen to be 0.45L/h-0.55L/h, enabling the flow of the argon to be 0.75L/h-0.85L/h, heating to the temperature of the crucible to reach 2100-2300 ℃, and controlling the pressure in the furnace shell cavity to be reduced to 200-1000 Pa;
and (3) a growth stage: on the premise of keeping the pressure in the furnace shell cavity and the temperature of the crucible, the flow of the nitrogen is adjusted to be 0.04-0.07L/h, and the flow of the argon is adjusted to be 0.7-0.9L/h;
and (3) an annealing stage: the flow of the nitrogen is adjusted to be 0.25L/h-0.35L/h, the flow of the argon is adjusted to be 0.45L/h-0.55L/h, the pressure in the furnace shell cavity is increased to 50000 Pa-70000 Pa, the temperature of the crucible is reduced to 800-900 ℃, and the temperature is kept for 3-5 h and then gradually reduced until the heating power of the graphite heating body in the growing furnace is 0;
the real-time conditioning method of the first aspect is employed during the warming phase, the growing phase and the annealing phase.
According to the method, the leakage amount of the silicon carbide raw material in the silicon carbide growing furnace is obtained in real time, the real-time thickness of the grown silicon carbide crystal block is obtained according to the leakage amount of the silicon carbide raw material obtained in real time and the first preset relation, the height to which the crucible in the growing furnace should be moved upwards is obtained according to the thickness of the obtained silicon carbide crystal block and the second preset relation, the crucible is moved upwards according to the height to which the crucible should be moved upwards, and the position of the crucible can be adjusted according to the thickness of the grown silicon carbide crystal block in real time, so that the position of a silicon carbide growing interface relative to a graphite heating element can be adjusted in real time, the temperature of the silicon carbide growing interface can be adjusted, the formation of defects such as polycrystal, polytype and the like can be reduced, and the crystal quality can be improved.
The leakage amount of the silicon carbide raw material is reflected as the weight reduction amount of the materials in the crucible in the growth furnace, and the inventor finds that the leakage amount of the silicon carbide raw material has strong correlation with the thickness of the silicon carbide crystal block.
According to the real-time regulation system for the internal temperature field of the resistance method silicon carbide growth furnace, the leakage quantity detection module can output the leakage quantity of the silicon carbide raw material in real time, the PLC logic control system can output the height of the crucible after the crucible is moved upwards in real time according to the leakage quantity of the silicon carbide raw material, and the mechanical driving module can adjust the height of the crucible in real time, so that the silicon carbide growth interface keeps the optimal position relative to the graphite heating body, the silicon carbide growth interface keeps the optimal temperature, and the crystal quality is improved.
According to the growth method of the silicon carbide, disclosed by the invention, the leakage amount of the silicon carbide raw material can better reflect the thickness of the silicon carbide crystal block obtained by growth by controlling the pressure, the argon flow and the nitrogen flow in the furnace shell cavity in the temperature rising stage, the growth stage and the annealing stage, the accuracy of the thickness of the obtained silicon carbide crystal block is improved, the temperature of a silicon carbide growth interface is better controlled, and the crystal quality is improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of the conditioning logic of one embodiment of the conditioning system of the present invention.
Fig. 2 is a schematic structural view of an embodiment of a silicon carbide growth furnace according to the present invention.
Description of the reference numerals
1-silicon carbide raw material; 2-silicon carbide crystal blocks; 3-crucible; 4-a leak detection module; 5-a mechanical drive module; 6-graphite heating element.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The inventors of the present invention have found that, when a silicon carbide single crystal is grown by the resistance method, the growth rate of the single crystal is easily affected by uncontrollable factors such as pressure in a growth furnace and fluctuation in crucible temperature, and that defects such as polycrystal and polymorphism are easily increased by adjusting the elevation of the crucible according to a set program.
In this regard, in a first aspect, referring to fig. 2, the present invention provides a method for real-time adjustment of an internal temperature field of a resistive silicon carbide growth furnace, the method comprising:
acquiring leakage amount of a silicon carbide raw material 1 in a silicon carbide growth furnace in real time, and acquiring thickness of a silicon carbide crystal block 2 grown by a resistance method according to the leakage amount of the silicon carbide raw material 1 and a first preset relation, wherein the leakage amount of the silicon carbide raw material 1 is weight reduction amount of materials in a crucible in the growth furnace;
and according to the thickness of the silicon carbide crystal block 2 and a second preset relation, acquiring the height of the crucible 3 in the growth furnace after the crucible 3 is moved upwards, and according to the height of the crucible 3 after the crucible 3 is moved upwards, moving the position of the crucible 3 upwards.
The thickness of the silicon carbide crystal block grown by the resistance method refers to the calculated thickness of the silicon carbide crystal block grown by the resistance method according to the leakage amount of the silicon carbide raw material and a first preset relation; the height of the crucible after the crucible is moved up means the height to which the crucible should be moved up in order to stabilize the temperature field inside the growth furnace.
When silicon carbide is grown in a growing furnace by adopting a resistance method, silicon carbide raw materials are sublimated and decomposed to generate gas, a part of the gas can be transported to the surface of a seed crystal for crystallization, because each part of a crucible is made of graphite, the crucible is assembled by threads and the like, the crucible is not completely sealed, and the other part of the gas can leak out of the crucible, the inventor finds that the leakage amount of the part of the silicon carbide raw materials has strong correlation with the thickness of a silicon carbide crystal block grown by adopting the resistance method, and the thickness of the silicon carbide crystal block can influence the position of a silicon carbide growth interface relative to a graphite heating body 6 outside the crucible, and the silicon carbide growth interface needs to be in an optimal position relative to the graphite heating body 6 outside the crucible so as to enable the silicon carbide growth interface to have optimal temperature distribution.
According to the invention, the leakage amount of the silicon carbide raw material in the silicon carbide growing furnace is obtained in real time, the thickness of the silicon carbide crystal block grown by a resistance method is obtained in real time based on a first preset relation, the correlation between the leakage amount of the silicon carbide raw material and the thickness of the silicon carbide crystal block grown by the resistance method is utilized, the thickness of the silicon carbide crystal block in real time is obtained only by measuring the weight reduction amount of the material in the crucible in real time, the method is convenient and easy to obtain, the cost is lower, and the more accurate thickness of the silicon carbide crystal block can be obtained. The actual growth interface of the crystal is slightly convex, but the thickness deviation of the slightly convex is generally within 0.2%, the thickness of the silicon carbide crystal block grown by the obtained resistance method, actually the calculated thickness of the silicon carbide crystal block, is an average thickness, and the optimal position of the silicon carbide growth surface relative to the graphite heating body can be maintained by adjusting the position of the crucible according to the calculated thickness of the silicon carbide crystal block due to small thickness deviation of each position of the silicon carbide crystal block.
In some preferred embodiments, the first preset relationship is a relationship of the leakage amount of the silicon carbide raw material 1 and the weight of the silicon carbide crystal block 2;
the obtaining of the thickness of the silicon carbide crystal block 2 sequentially includes obtaining the weight of the silicon carbide crystal block 2 according to the leakage amount of the silicon carbide raw material 1 and the first preset relation, and obtaining the thickness of the silicon carbide crystal block 2 according to the weight of the silicon carbide crystal block 2.
Under the preferred scheme, after the leakage amount of the silicon carbide raw material is obtained in real time, according to the leakage amount of the silicon carbide raw material and a first preset relation, the weight of the real-time silicon carbide crystal block is obtained, as the density and the sectional area of the silicon carbide crystal block are known, and then the thickness of the real-time silicon carbide crystal block is obtained according to the weight of the silicon carbide crystal block, the inventor finds that the correlation between the leakage amount of the silicon carbide raw material and the weight of the silicon carbide crystal block grown by a resistance method is stronger, the accurate thickness of the silicon carbide crystal block is more beneficial to obtaining, and when the crucible position is adjusted according to the thickness of the silicon carbide crystal block, the best temperature of a silicon carbide growth surface is more beneficial to be kept, and the crystal quality is improved.
More preferably, the silicon carbide raw material 1 has a leakage amount ofM Leakage of The weight of the silicon carbide crystal block 2 isM Crystal block The first preset relation is thatM Crystal block =M Leakage of ×k 1 . Under the preferred scheme, the first preset relation is a linear relation, so that the weight of an accurate silicon carbide crystal block is more conveniently obtained, the thickness of the accurate silicon carbide crystal block is obtained, and when the position of the crucible is adjusted according to the thickness of the silicon carbide crystal block, the growth surface of the silicon carbide is further kept at the optimal temperature, and the crystal quality is improved.
In some preferred embodiments, the first preset relationship includes a third preset relationship that is a relationship of a leakage amount of the silicon carbide raw material 1 and a reaction amount of the silicon carbide raw material 1, and a fourth preset relationship that is a relationship of a reaction amount of the silicon carbide raw material 1 and a weight of the silicon carbide crystal block 2;
the obtaining of the thickness of the silicon carbide crystal block 2 sequentially includes obtaining a reaction amount of the silicon carbide raw material 1 according to the leakage amount of the silicon carbide raw material 1 and the third preset relation, obtaining a weight of the silicon carbide crystal block 2 according to the reaction amount of the silicon carbide raw material 1 and the fourth preset relation, and obtaining the thickness of the silicon carbide crystal block 2 according to the weight of the silicon carbide crystal block 2.
Under the preferred scheme, after the leakage amount of the silicon carbide raw material is obtained in real time, the reaction amount of the silicon carbide raw material is obtained according to the leakage amount of the silicon carbide raw material and a third preset relation, then the weight of the silicon carbide crystal block is obtained according to the reaction amount of the silicon carbide raw material and a fourth preset relation, as the density and the sectional area of the silicon carbide crystal block are known, and then the thickness of the real-time silicon carbide crystal block is obtained according to the weight of the silicon carbide crystal block, the inventor finds that the correlation between the leakage amount of the silicon carbide raw material and the reaction amount of the silicon carbide raw material is stronger, and meanwhile, the correlation between the reaction amount of the silicon carbide raw material and the weight of the silicon carbide crystal block is stronger, so that the accurate thickness of the silicon carbide crystal block is better obtained, the crucible position is adjusted in real time according to the thickness of the more accurate silicon carbide crystal block, the silicon carbide growth surface is better kept at the optimal temperature, and the crystal quality is improved.
More preferably, the silicon carbide raw material 1 has a leakage amount ofM Leakage of The reaction amount of the silicon carbide raw material 1 is thatM Reaction The weight of the silicon carbide crystal block 2 isM Crystal block The third preset relationship is thatM Reaction =M Leakage of ×k 3 The fourth preset relationship is thatM Crystal block =M Reaction ×k 4 . Under the preferred scheme, the third preset relation and the fourth preset relation are linear relations, so that the accurate real-time thickness of the silicon carbide crystal block is better obtained, the optimal temperature distribution of the silicon carbide growth surface is better kept when the crucible position is adjusted according to the thickness of the crystal block, the defects of polycrystal, polytype and the like of the crystal are restrained, and the crystal quality is improved.
More preferably, the silicon carbide growth furnace is charged with a weight ofM Total (S) The silicon carbide raw material 1 of (2) is reacted completely, and the leakage amount of the silicon carbide raw material 1 is measuredM Total leakage of Measuring the weight of the silicon carbide Crystal Block 2M Total crystal block The method comprises the steps of carrying out a first treatment on the surface of the Calculation ofM Total (S) /M Total leakage of Obtainingk 3 Calculation ofM Total crystal block /M Total (S) Obtainingk 4 The method comprises the steps of carrying out a first treatment on the surface of the Or, calculateM Total crystal block /M Total leakage of Obtainingk 1 . Under the preferred scheme, after the silicon carbide raw material is completely reacted, the total leakage of the silicon carbide raw material is measuredM Total leakage of And total weight of silicon carbide crystal massM Total crystal block Then calculate to obtaink 1 The method is more beneficial to obtaining the accurate thickness of the silicon carbide crystal block based on the correlation between the leakage amount of the silicon carbide raw material and the weight of the silicon carbide crystal block grown by a resistance method; after the silicon carbide raw material is completely reacted, adding carbonization in the initial stage of reactionWeight of silicon feedstockM Total (S) That is, the reaction amount of the silicon carbide raw material, by measuring the total leakage amount of the silicon carbide raw material after the reaction is completedM Total leakage of Calculated to obtaink 3 By measuring the total weight of the silicon carbide crystal mass after the reaction is completedM Total crystal block Calculated to obtaink 4 The thickness of the silicon carbide crystal block is accurately obtained based on the correlation between the leakage amount of the silicon carbide raw material and the reaction amount of the silicon carbide raw material and the correlation between the reaction amount of the silicon carbide raw material and the weight of the silicon carbide crystal block; therefore, according to the thickness of the more accurate silicon carbide crystal block, the position of the crucible is adjusted in real time, and the silicon carbide growth surface can be kept at the optimal temperature more conveniently.
In some preferred embodiments, the silicon carbide crystal block 2 has a thickness ofT Crystal block The initial height of the crucible 3 is 0, and the height of the crucible 3 after being moved up isH Crucible pot The second preset relationship is thatH Crucible pot =T Crystal block ×k 2 The saidk 2 0.9 to 1.1. In the preferred embodiment, the second preset relationship is thatH Crucible pot =T Crystal block ×k 2 The second preset relationship is a linear relationship, andk 2 the temperature of the silicon carbide growth surface is kept at the optimal temperature by adjusting the crucible to the optimal position according to the thickness of the silicon carbide crystal block, so that the error is reduced, and the crystal quality is improved. In the inventionk 2 Specifically, for example, 0.9, 0.95, 1, 1.05, and 1.1 are possible.
In a second aspect, the present invention provides a real-time adjustment system employing the real-time adjustment method of the first aspect, and referring to fig. 1, the system includes: the leakage detection module 4, the PLC logic control module and the mechanical driving module 5;
the leakage detection module 4 is used for detecting and outputting the leakage of the silicon carbide raw material 1 in the silicon carbide growth furnace; the PLC logic control system is used for receiving the leakage amount of the silicon carbide raw material 1, and calculating and outputting the height of the crucible 3 in the growth furnace after the crucible 3 moves upwards according to the leakage amount of the silicon carbide raw material 1, the first preset relation and the second preset relation; the mechanical driving module 5 is used for receiving the height of the crucible 3 after being moved up, and moving up the crucible 3 according to the height of the crucible 3 after being moved up.
According to the real-time regulating system, the leakage amount of the silicon carbide raw material can be detected and output in real time through the leakage amount detection module, the position of the silicon carbide growth interface relative to the graphite heating body can be calculated and output in real time according to the acquired leakage amount of the silicon carbide raw material through the PLC logic control system, the height of the crucible after the crucible is moved upwards can be adjusted in real time through the mechanical driving module, and the position of the silicon carbide growth interface relative to the graphite heating body can be maintained, so that the crystal quality is improved.
In some preferred embodiments, the leak detection module 4 comprises a weight sensor and the mechanical drive module 5 comprises a lift motor.
The leakage amount detection module can be a weight sensor arranged on the crucible, and detects the weight reduction amount of the crucible in the growth furnace, namely the leakage amount of the silicon carbide raw material in the silicon carbide growth furnace; the mechanical drive module may include a lift motor mounted on the crucible and other means of cooperating mounting and operation by which the crucible is moved up.
In some preferred embodiments, the PLC logic control system is configured to receive the leakage amount of the silicon carbide raw material, and calculate and output the height of the crucible in the growth furnace after the crucible has been moved up according to the leakage amount of the silicon carbide raw material, the third preset relationship, the fourth preset relationship, and the second preset relationship.
In a third aspect, the present invention provides a method for growing silicon carbide using the real-time conditioning method of the first aspect, the method comprising: and (3) heating: placing the crucible 3 filled with the silicon carbide raw material and the seed crystal into a silicon carbide growth furnace, vacuumizing, introducing nitrogen and argon into a furnace shell cavity, enabling the pressure in the furnace shell cavity to reach 10000 Pa-20000 Pa, enabling the flow of the nitrogen to be 0.45L/h-0.55L/h, enabling the flow of the argon to be 0.75L/h-0.85L/h, heating to the temperature of the crucible 3 to reach 2100 ℃ to 2300 ℃, and controlling the pressure in the furnace shell cavity to be reduced to 200 Pa-1000 Pa;
and (3) a growth stage: on the premise of keeping the pressure in the furnace shell cavity and the temperature of the crucible 3, the flow rate of the nitrogen is adjusted to be 0.04-0.07L/h, and the flow rate of the argon is adjusted to be 0.7-0.9L/h;
and (3) an annealing stage: the flow of the nitrogen is adjusted to be 0.25L/h-0.35L/h, the flow of the argon is adjusted to be 0.45L/h-0.55L/h, the pressure in the furnace shell cavity is increased to 50000 Pa-70000 Pa, the temperature of the crucible 3 is reduced to 800-900 ℃, and the temperature is kept for 3-5 h and then gradually reduced until the heating power of the graphite heating body 6 in the growing furnace is 0;
the real-time conditioning method of the first aspect is employed during the warming phase, the growing phase and the annealing phase.
The temperature of the crucible refers to the temperature of the top of the crucible.
Under the preferred scheme, in the growth stage, the pressure in the furnace shell cavity is 200 Pa-1000 Pa, the flow of nitrogen is adjusted to be 0.04-0.07L/h on the premise of keeping the pressure in the furnace shell cavity and the temperature of the crucible, and the flow of argon is adjusted to be 0.7L/h-0.9L/h, so that the leakage amount of the silicon carbide raw material can better reflect the thickness of a silicon carbide crystal block, the accuracy of the obtained thickness of the silicon carbide crystal block is improved, the temperature of a silicon carbide growth interface is better controlled, and the crystal quality is improved.
The invention will be further described in detail with reference to specific examples.
Example 1
The method for obtaining the third preset relationship and the fourth preset relationship comprises the following steps:
step one: placing a silicon carbide raw material into a silicon carbide raw material accommodating part of a crucible, wherein the weight of the silicon carbide raw material is as followsM Total (S) Placing a seed crystal into a seed crystal accommodating part of the crucible, wherein the seed crystal has the mass ofM Seed crystal Placing the crucible filled with the silicon carbide raw material and the seed crystal into a silicon carbide growth furnace, vacuumizing, introducing nitrogen into the furnace shell cavity at a flow rate of 0.5L/h, and introducing nitrogen into the furnace shell cavity at a flow rate of 0.8L/hArgon is introduced to ensure that the pressure in the furnace shell cavity reaches 15000Pa and then the pressure is maintained, and then the temperature of the crucible reaches 2200 ℃ through a graphite heating body outside the crucible;
step two: maintaining the pressure in the furnace shell cavity at 500pa, maintaining the temperature of the crucible at 2200 ℃, adjusting the flow of the nitrogen to 0.065L/h, and adjusting the flow of the argon to 0.8L/h, so that the silicon carbide raw materials are completely reacted;
step three: adjusting the flow of the nitrogen to 0.3L/h, adjusting the flow of the argon to 0.5L/h, increasing the pressure in the furnace shell cavity to 60000Pa, cooling to 850 ℃, and preserving heat for 3-5 h; then slowly cooling until the heating power of the graphite heating body 6 in the growth furnace is 0.
Step four: measuring the weight of the upper crystal block of the crucible, and subtracting the weight of the upper crystal blockM Seed crystal Obtaining the weight of the silicon carbide crystal block grown by the resistance methodM Total crystal block Measuring the weight of the raw material residue in the silicon carbide raw material containing portionM Residue of raw materials In the first stepM Total (S) Subtracting outM Total crystal block AndM residue of raw materials Obtaining leakage amount of silicon carbide raw materialM Total leakage of By usingM Total (S) /M Total leakage of Obtainingk 3 ，k 3 66, useM Total crystal block /M Total (S) Obtainingk 4 ，k 4 0.2.
The growth method of the silicon carbide comprises the following steps:
step one: placing silicon carbide raw materials into a silicon carbide raw material accommodating part of a crucible, placing seed crystals into a seed crystal accommodating part of the crucible, placing the crucible filled with the silicon carbide raw materials and the seed crystals into a silicon carbide growing furnace, vacuumizing, introducing nitrogen into a furnace shell cavity at a flow rate of 0.5L/h, introducing argon into the furnace shell cavity at a flow rate of 0.8L/h, maintaining the pressure after the pressure in the furnace shell cavity reaches 15000Pa, and then enabling the temperature of the crucible to reach 2200 ℃ through a graphite heating body outside the crucible;
step two: holding furnace shell cavityThe pressure in the crucible is 500pa, the temperature of the crucible is kept at 2200 ℃, the flow of the nitrogen is adjusted to be 0.065L/h, the flow of the argon is adjusted to be 0.8L/h, and the silicon carbide raw material sublimates and decomposes to generate gas which is transported to the surface of the seed crystal for recrystallization; during recrystallization, the weight reduction of the crucible, i.e., the leakage of the silicon carbide raw material, is obtained and outputted in real time by a leakage amount detection module 4 (weight sensor) mounted on the crucibleM Leakage of Real-time acquisition of PLC logic control systemM Leakage of And according toM Leakage of And a third preset relationshipM Reaction =M Leakage of X 66, calculating the reaction mass of silicon carbide raw material in real timeM Reaction According toM Reaction And a fourth preset relationshipM Crystal block =M Reaction X 0.2, weight of the grown silicon carbide crystal mass was calculated in real timeM Crystal block According toM Crystal block Calculating the thickness of the grown silicon carbide crystal block in real timeT Crystal block According toT Crystal block And a second preset relationshipH Crucible pot =T Crystal block X 1.0, calculating the height to which the crucible should be moved upwards in real time, outputting the height to which the crucible should be moved upwards in real time, and receiving the height to which the crucible 3 should be moved upwards in real time by a mechanical driving module 5 (a lifting motor) arranged on the crucible 3, and adjusting the height of the crucible 3 in real time until the silicon carbide raw material is completely reacted;
step three: adjusting the flow of the nitrogen to 0.3L/h, adjusting the flow of the argon to 0.5L/h, increasing the pressure in the furnace shell cavity to 60000Pa, cooling to 850 ℃, and preserving heat for 3-5 h; then slowly cooling until the heating power of the graphite heating body 6 in the growth furnace is 0.
In this example, the thickness of the silicon carbide crystal mass was calculated in real time when the silicon carbide raw material had reacted completelyT Crystal block The deviation from the actual thickness of the grown silicon carbide crystal mass measured after the removal of the silicon carbide after cooling was 5%, and polycrystalline and polytype defects were not found in the grown silicon carbide crystal. The detection of polycrystalline and polytype defects is in the purple lightUnder the irradiation of the lamp, the identification is carried out by naked eyes.
Example 2
Reference example 1 is performed, with the difference that in the growth method of silicon carbidek 2 0.85. The silicon carbide crystal grown in this example has fewer polytype defects.
Example 3
Reference example 1 is performed, with the difference that in the growth method of silicon carbidek 2 1.15. The silicon carbide crystal grown in this example has fewer polycrystalline defects.
Example 4
Reference example 1 was made, except that in the obtaining method of the third preset relationship and the fourth preset relationship and the growing method of silicon carbide, step two, the pressure in the furnace shell cavity was maintained at 1300Pa, the flow rate of nitrogen gas was 0.02L/h, and the flow rate of argon gas was 0.4L/h. In this example, when the silicon carbide raw material is completely reacted, the thickness of the obtained silicon carbide crystal block is calculated in real timeT Crystal block The deviation from the actual thickness of the grown silicon carbide crystal mass measured after cooling and removal of the silicon carbide was 12%, and fewer polycrystalline and polytype defects were present in the grown silicon carbide crystal.
Comparative example 1
The procedure was performed with reference to example 1, except that the elevation of the crucible as a whole was adjusted at a constant speed according to the intended growth rate setting program. The silicon carbide crystal grown in this comparative example had many polycrystalline and polytype defects.
As can be seen from comparative examples and comparative example 1, compared with the case where the setting program was adopted, the elevation of the crucible was adjusted, the leakage amount of the silicon carbide raw material in the silicon carbide growth furnace was obtained in real time, the thickness of the silicon carbide crystal mass grown by the resistance method was obtained from the leakage amount of the silicon carbide raw material, the height of the crucible after the crucible was moved up in the growth furnace was obtained from the thickness of the silicon carbide crystal mass, the position of the crucible was moved up from the height of the crucible after the crucible was moved up, the position of the silicon carbide growth interface relative to the graphite heating element was effectively controlled, and the formation of polycrystalline and polytype defects was reduced. Comparative examples 1 to 3 show that, in the second predetermined relationshipk 2 The temperature of the silicon carbide growth surface is more favorably kept at the optimal temperature and the formation of polycrystalline and polytype defects is reduced by 0.9-1.1. Comparing the embodiment 1 with the embodiment 4, it can be known that, in the growth stage, the pressure in the furnace shell cavity is 200 Pa-1000 Pa, the flow of nitrogen is adjusted to 0.04L/h-0.07L/h, the flow of argon is adjusted to 0.7L/h-0.9L/h, the leakage amount of the silicon carbide raw material can better reflect the thickness of the silicon carbide crystal block, the accuracy of the obtained thickness of the silicon carbide crystal block is improved, the temperature of the silicon carbide growth interface is better controlled, the formation of polycrystalline and polytype defects is reduced, and the quality of the crystal is improved.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (10)
1. The method for adjusting the temperature field in the silicon carbide growth furnace by the resistance method in real time is characterized by comprising the following steps of:
acquiring leakage amount of a silicon carbide raw material (1) in a silicon carbide growth furnace in real time, and acquiring thickness of a silicon carbide crystal block (2) grown by a resistance method according to the leakage amount of the silicon carbide raw material (1) and a first preset relation, wherein the leakage amount of the silicon carbide raw material (1) is weight reduction amount of materials in a crucible in the growth furnace;
and according to the thickness of the silicon carbide crystal block (2) and a second preset relation, acquiring the height of the crucible (3) in the growth furnace after the crucible (3) is moved upwards, and according to the height of the crucible (3) after the crucible is moved upwards, moving the position of the crucible (3) upwards.
2. The real-time adjustment method according to claim 1, characterized in that the first preset relationship is a relationship of the leakage amount of the silicon carbide raw material (1) and the weight of the silicon carbide crystal block (2);
the obtaining of the thickness of the silicon carbide crystal block (2) sequentially comprises obtaining the weight of the silicon carbide crystal block (2) according to the leakage amount of the silicon carbide raw material (1) and the first preset relation, and obtaining the thickness of the silicon carbide crystal block (2) according to the weight of the silicon carbide crystal block (2).
3. The real-time adjustment method according to claim 2, characterized in that the leakage amount of the silicon carbide raw material (1) isM Leakage of The weight of the silicon carbide crystal block (2) isM Crystal block The first preset relation is thatM Crystal block =M Leakage of ×k 1 。
4. The real-time adjustment method according to claim 1, characterized in that the first preset relationship includes a third preset relationship, which is a relationship of a leakage amount of the silicon carbide raw material (1) and a reaction amount of the silicon carbide raw material (1), and a fourth preset relationship, which is a relationship of a reaction amount of the silicon carbide raw material (1) and a weight of the silicon carbide crystal block (2);
the obtaining of the thickness of the silicon carbide crystal block (2) sequentially comprises obtaining the reaction quantity of the silicon carbide raw material (1) according to the leakage quantity of the silicon carbide raw material (1) and the third preset relation, obtaining the weight of the silicon carbide crystal block (2) according to the reaction quantity of the silicon carbide raw material (1) and the fourth preset relation, and obtaining the thickness of the silicon carbide crystal block (2) according to the weight of the silicon carbide crystal block (2).
5. The method according to claim 4, characterized in that the leakage of the silicon carbide raw material (1) isM Leakage of The reaction amount of the silicon carbide raw material (1) isM Reaction The weight of the silicon carbide crystal block (2) isM Crystal block The third preset relationship is thatM Reaction =M Leakage of ×k 3 The fourth preset relationship is thatM Crystal block =M Reaction ×k 4 。
6. The method of claim 3 or 5, wherein the silicon carbide growth furnace is charged with a weight ofM Total (S) The silicon carbide raw material (1) of the furnace is reacted completely, and the leakage amount of the silicon carbide raw material (1) is measuredM Total leakage of Measuring the weight of the silicon carbide crystal mass (2)M Total crystal block ；
Calculation ofM Total (S) /M Total leakage of Obtainingk 3 Calculation ofM Total crystal block /M Total (S) Obtainingk 4 ；
Or, calculateM Total crystal block /M Total leakage of Obtainingk 1 。
7. The real-time adjustment method according to claim 1, characterized in that the silicon carbide crystal block (2) has a thickness ofT Crystal block The initial height of the crucible (3) is 0, and the height of the crucible (3) after being moved up isH Crucible pot The second preset relationship is thatH Crucible pot =T Crystal block ×k 2 The saidk 2 0.9 to 1.1.
8. A real-time adjustment system employing the real-time adjustment method according to any one of claims 1-7, characterized in that the system comprises: the leakage detection module (4), the PLC logic control module and the mechanical driving module (5);
the leakage amount detection module (4) is used for detecting and outputting the leakage amount of the silicon carbide raw material (1) in the silicon carbide growth furnace; the PLC logic control module is used for receiving the leakage amount of the silicon carbide raw material (1), and calculating and outputting the height of the crucible (3) in the growth furnace after the crucible is moved upwards according to the leakage amount of the silicon carbide raw material (1), the first preset relation and the second preset relation; the mechanical driving module (5) is used for receiving the height of the crucible (3) after being moved upwards, and moving the crucible (3) upwards according to the height of the crucible (3) after being moved upwards.
9. Real-time adjustment system according to claim 8, characterized in that the leakage detection module (4) comprises a weight sensor and the mechanical drive module (5) comprises a lift motor.
10. A method for growing silicon carbide using the real-time adjustment method according to any one of claims 1 to 7, characterized in that the method comprises:
and (3) heating: placing a crucible (3) filled with a silicon carbide raw material and seed crystals into a silicon carbide growth furnace, vacuumizing, introducing nitrogen and argon into a furnace shell cavity, enabling the pressure in the furnace shell cavity to reach 10000 Pa-20000 Pa, enabling the flow of the nitrogen to be 0.45L/h-0.55L/h, enabling the flow of the argon to be 0.75L/h-0.85L/h, heating to the temperature of the crucible (3) to reach 2100-2300 ℃, and controlling the pressure in the furnace shell cavity to be reduced to 200 Pa-1000 Pa;
and (3) a growth stage: on the premise of keeping the pressure in the furnace shell cavity and the temperature of the crucible (3), the flow rate of the nitrogen is adjusted to be 0.04-0.07L/h, and the flow rate of the argon is adjusted to be 0.7-0.9L/h;
and (3) an annealing stage: the flow of the nitrogen is adjusted to be 0.25L/h-0.35L/h, the flow of the argon is adjusted to be 0.45L/h-0.55L/h, the pressure in the furnace shell cavity is increased to 50000 Pa-70000 Pa, the temperature of the crucible (3) is reduced to 800-900 ℃, and the temperature is kept for 3-5 h and then gradually reduced until the heating power of the graphite heating body (6) in the growing furnace is 0;
the real-time adjustment method according to any one of claims 1 to 7 is adopted in the temperature rising stage, the growth stage and the annealing stage.
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