CN115125613A - Growth device for preparing single crystal silicon carbide - Google Patents
Growth device for preparing single crystal silicon carbide Download PDFInfo
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- CN115125613A CN115125613A CN202210683987.6A CN202210683987A CN115125613A CN 115125613 A CN115125613 A CN 115125613A CN 202210683987 A CN202210683987 A CN 202210683987A CN 115125613 A CN115125613 A CN 115125613A
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- silicon carbide
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/002—Controlling or regulating
- C30B23/005—Controlling or regulating flux or flow of depositing species or vapour
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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
Abstract
The invention discloses a growth device for preparing single crystal silicon carbide, which comprises a growth crucible and an air inlet control assembly, wherein the growth crucible comprises a crucible body and a cover body, silicon carbide powder is contained in the crucible body, and the cover body is arranged on the crucible body; the gas inlet control assembly is positioned at the gas inlet end of the crucible body and used for controlling gas entering the crucible body according to the mass change of the silicon carbide powder. The invention can control the gas entering the crucible body according to the quality change of the silicon carbide powder in the crucible body, thereby regulating the airflow environment in the crucible body and improving the growth speed and the growth quality of crystals.
Description
Technical Field
The invention relates to the field of crystal growth, in particular to a growth device for preparing single crystal silicon carbide.
Background
Semiconductor silicon carbide single crystal materials have evolved through the last 30 years since their commercialization in the 90 s of the last century as the preferred substrate material for power electronics and microwave radio frequency devices. With the continuous development of downstream device technology and the continuous promotion of industrialization degree, the quality requirement of the silicon carbide single crystal substrate is more and more severe.
At present, the most mature technology for preparing silicon carbide single crystal is physical vapor transport method (abbreviated as PVT method), and its basic principle is that a graphite crucible placed in the center of a coil is heated by medium-frequency induction, and the wall of the graphite crucible generates heat by induction and then transfers the heat to the silicon carbide powder inside the graphite crucible and causes the silicon carbide powder to sublimate. In the growth process, the sublimation of the silicon carbide gas and the growth of the crystal are promoted mainly by the temperature gradient and the pressure gradient, but the sublimation speed is low, and the growth speed of the crystal needs to be improved; in different crystal growth periods, the internal atmosphere of the crucible is different, the early stage is rich in silicon, the later stage is rich in carbon, and uneven gas components easily cause crystal defects.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides a growth device for preparing single crystal silicon carbide, which can control gas entering a crucible body according to the quality change of silicon carbide powder in the crucible body, thereby regulating the airflow environment in the crucible body and improving the growth speed and growth quality of crystals.
The growth apparatus for producing single crystal silicon carbide according to the present invention comprises:
the growth crucible comprises a crucible body and a cover body, wherein silicon carbide powder is contained in the crucible body, and the cover body is arranged on the crucible body;
and the gas inlet control assembly is positioned at the gas inlet end of the crucible body and used for controlling gas entering the crucible body according to the mass change of the silicon carbide powder.
According to the growth device for preparing the single crystal silicon carbide, the sublimation of the silicon carbide powder can be promoted by utilizing the airflow formed by introducing the gas, and the sublimed silicon carbide vapor can be driven by utilizing the airflow to move towards the direction of the seed crystal, so that the growth speed of the crystal is accelerated. Simultaneously, along with the continuous growth of crystal, the inside air current component of crucible changes gradually, through the quality change that utilizes carborundum powder, automatic control lets in gas, thereby adjust the inside air current environment of crucible body, make the gas composition who lets in can be according to the difference of growth stage and automatic change, ensure that crucible body is inside all the time in the gas atmosphere that a suitable crystal grows, when accelerating crystal growth, can reduce dislocation and other flaws etc. that the crystal leads to because the component changes in the crucible body, the growth quality of crystal has been improved.
In some embodiments of the invention, the intake air control assembly comprises:
the raw material containing piece is arranged in the crucible body and is used for containing the silicon carbide powder;
the elastic piece is connected with the raw material containing piece and used for driving the raw material containing piece to move along the axial direction of the growth crucible according to the mass change of the silicon carbide powder;
and the gas flow control valve is positioned at the gas inlet end of the crucible body, is connected with a gas source and is used for controlling gas entering the crucible body according to the movement of the raw material containing piece.
In some embodiments of the invention, the raw material containing part is provided with an air inlet hole and an air outlet hole, the air inlet hole is communicated with the airflow control valve, and the air outlet hole is communicated with the air inlet hole and the inside of the crucible body; the venthole is equipped with a plurality ofly, and is a plurality of the venthole is evenly established the raw materials holds on placing the lateral wall of carborundum powder.
In some embodiments of the invention, the gas flow control valve is formed with a gas port, and is provided with a shield for shielding the gas port, the shield being connected to the raw material holder and adapted to shield the gas port to different degrees as the raw material holder moves.
In some embodiments of the present invention, the gas flow control valve is provided with three gas ports, the three gas ports are respectively connected with three different gas sources, the three different gas sources are respectively a silicon-rich gas, a carbon-rich gas and an inert gas, and the shielding member is adapted to change the shielding degree of the three gas ports along with the movement of the raw material containing member, so that the gas introduced into the crucible body meets the requirements of the growth of the crystal at each stage.
In some embodiments of the present invention, the crucible further comprises an air flow mixing bin, the air flow mixing bin is a hollow structure, the air flow mixing bin is provided with an air inlet end and an air outlet end, the air flow control valve is arranged at the air inlet end of the air flow mixing bin, and the air outlet end of the air flow mixing bin is used for introducing the air mixed by the air flow mixing bin into the crucible body.
In some embodiments of the invention, the crucible further comprises a transmission assembly connecting the raw material containing part and the gas flow control valve, the transmission assembly is a flexible transmission mechanism and comprises a guide wheel set arranged outside the crucible body, and the guide wheel set is connected with the raw material containing part and the gas flow control valve through transmission lines.
In some embodiments of the invention, the crucible further comprises a transmission assembly connecting the raw material containing part and the gas flow control valve, wherein the transmission assembly is a rigid transmission mechanism and comprises a guide connecting rod set arranged outside the crucible body, and the guide connecting rod set is connected with the raw material containing part and the gas flow control valve.
In some embodiments of the present invention, a seed crystal fixing member for fixing a seed crystal is disposed on an inner wall of the cover, the seed crystal fixing member has a cooling chamber, a cooling assembly is disposed in the cooling chamber, the cooling assembly includes an airflow pipeline and a blowing member, a cooling hole is disposed on the blowing member, the airflow pipeline is communicated with the blowing member, and a cooling gas flows into the blowing member through the airflow pipeline and enters the cooling chamber through the cooling hole.
In some embodiments of the invention, the inner wall of the crucible body and the seed crystal fixing piece jointly define a flow guide cavity, and the crucible body is provided with a first flow guide hole for communicating the flow guide cavity with the outside of the crucible body; and a second flow guide hole for communicating the cooling bin with the flow guide cavity is formed in the seed crystal fixing piece.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
FIG. 1 is a schematic view of a growth apparatus for producing single crystal silicon carbide in accordance with one embodiment of the present invention;
FIG. 2 is an enlarged schematic view of the intake control assembly of FIG. 1;
FIG. 3 is a schematic view of a growth apparatus for producing single crystal silicon carbide according to another embodiment of the present invention;
FIG. 4 is an enlarged schematic view of the intake control assembly of FIG. 3;
FIG. 5 is a schematic view of the construction of the material containment member of the present invention;
FIG. 6 is a top view of FIG. 5;
FIG. 7 is a schematic structural view of the cover of the present invention;
FIG. 8 is a bottom view of FIG. 7;
FIG. 9 is a schematic diagram of the configuration of the airflow passages in the airflow heating assembly according to one embodiment of the invention;
FIG. 10 is a schematic structural view of an airflow mixing bin according to one embodiment of the invention;
FIG. 11 is a schematic view of the construction of a shield in the airflow control valve according to an embodiment of the invention;
fig. 12 is a schematic view of the attachment of the elastic member to other structures according to the present invention.
Reference numerals:
an intake air control assembly 100;
a raw material container 10; a stone grinding disc 11; a graphite rod 12; an air intake hole 13; an air outlet 14; a cavity 15;
an elastic member 20;
an airflow heating assembly 30; a heater body 31; an air flow passage 311;
an air flow mixing bin 40; an air inlet end 41; an air outlet end 42;
an airflow control valve 50; gas ports 51; a shield 52; an elongated aperture 521; a baffle 522; a return spring 53;
a transmission assembly 60; a guide wheel group 61; a drive line 62; a first pulley 611; a second pulley 612; a third pulley 613; a reducing gear set 614; a guide link group 63; a fourth link 631; a third link 632; a sleeve 633; a second link 634; a first link 635;
a temperature reduction assembly 70; an air flow duct 71; a blowing member 72; a cooling hole 721; a gas flow rate control valve 73;
a growth crucible 200; a crucible body 201; a cover 202; a seed 203; a seed crystal holder 204; a cooling bin 205; a flow guide cavity 206; a first flow guide hole 207; second flow guide holes 208;
a first air port a; a second port b; and a third port c.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
The following disclosure provides many different embodiments, or examples, for implementing different features of the invention. To simplify the disclosure of the present invention, the components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit the present invention. Furthermore, the present invention may repeat reference numerals and/or letters in the various examples. This repetition is for the purpose of simplicity and clarity and does not in itself dictate a relationship between the various embodiments and/or configurations discussed. In addition, the present invention provides examples of various specific processes and materials, but one of ordinary skill in the art may recognize the applicability of other processes and/or the use of other materials.
A growth apparatus for producing single crystal silicon carbide according to an embodiment of the present invention is described below with reference to fig. 1 to 12, including: a growth crucible 200 and an inlet control assembly 100.
Referring to fig. 1 to 4, the growth crucible 200 includes a crucible body 201 and a cover 202, wherein silicon carbide powder is contained in the crucible body 201, the cover 202 is disposed on the crucible body 201, and a seed crystal 203 to be grown is mounted on the cover 202 and arranged opposite to the silicon carbide powder; the gas inlet control assembly 100 is located at the gas inlet end of the crucible body 201 and is used for controlling gas entering the crucible body 201 according to the mass change of the silicon carbide powder.
The crucible body 201 heats and transfers heat to the silicon carbide powder inside the crucible body and sublimates the silicon carbide powder, and the sublimated silicon carbide vapor moves to the seed crystal 203 to be grown on the cover body 202, so that crystal growth is realized on the seed crystal 203. Along with the introduction of the gas, the sublimation of the silicon carbide powder can be promoted by utilizing the airflow formed by the introduced gas, and the sublimed silicon carbide vapor can be driven by the airflow to move towards the direction of the seed crystal, so that the growth speed of the crystal is accelerated. Because in the growth process, the quality of carborundum powder can change, different carborundum powder quality shows different growth stages, so through the control to letting in gas, still can adjust the inside air current environment of crucible body 201, make the gaseous composition that lets in can be according to the different and nimble change in growth stage, ensure that crucible body 201 is inside all the time in the gaseous atmosphere that is fit for crystal growth, when accelerating crystal growth, can reduce dislocation and other flaws etc. that the crystal leads to because the composition changes in crucible body 201, the growth quality of crystal has been improved.
In the crystal growth process, the interior of the crucible body 201 is in a silicon-rich state firstly, and in the crystal growth later stage, due to the carbonization of the powder, the interior of the crucible body 201 is in a carbon-rich state, and the two states easily generate impurities such as silicon drops, carbon wrapping and the like, so that crystal defects are caused. Therefore, the gas introduced into the crucible body 201 is a mixture of one or more of a carbon-rich gas, an inert gas, and a silicon-rich gas. For example, when the inside of the crucible body 201 is in a silicon-rich state, the amount and time of introducing the carbon-rich gas can be controlled, and when the inside of the crucible body 201 is in a carbon-rich state, the amount and time of introducing the silicon-rich gas can be controlled, the specific introduction can be determined according to the growth stage, and the growth stage can be determined according to the change in the quality of the silicon carbide powder.
In some embodiments of the present invention, referring to fig. 1, the intake control assembly 100 includes a raw material container 10, an elastic member 20, and an airflow control valve 50. The raw material containing part 10 is movably arranged in the crucible body 201, is used for containing silicon carbide powder, and extends to the outside of the crucible body 201 through the side wall of the crucible body 201 at one side far away from the cover body 202; the raw material container 10 may be a graphite member so that the raw material container 10 has high temperature resistance. The elastic member 20 may be a spring, a leaf spring, or the like having a structure that is elastically stretchable and restorable. The elastic member 20 is connected to the end of the raw material container 10 extending out of the crucible body 201, the elastic member 20 is suitable for stretching or compressing when the mass of the silicon carbide powder changes, and when the mass of the silicon carbide powder changes, the elastic member 20 drives the raw material container 10 to move up and down along the axial direction of the growth crucible 200 (i.e. the sublimation direction of the silicon carbide powder or the growth direction of the seed crystal). The gas flow control valve 50 is located at the gas inlet end of the crucible body 201, is connected with a gas source, and is used for controlling the gas entering the crucible body 201 according to the movement of the raw material containing member 10.
It is understood that, in the initial stage of growth, the silicon carbide powder on the raw material holding member 10 is the heaviest in mass, and the elastic member 20 is in a compressed state. In the growth process, along with the continuous sublimation of carborundum powder, the weight of carborundum powder alleviates gradually on the raw materials holds 10, and elastic component 20 will constantly upwards extend to drive the raw materials and hold 10 and upwards remove, make the carborundum powder on the raw materials holds 10 remain on the high temperature line all the time, guaranteed the stability of carborundum powder sublimation rate, improved the growth quality of crystal. Meanwhile, along with the moving condition of the raw material containing part 10, the growth stage of the crystal can be reversely deduced, the airflow control valve 50 controls the opening and closing of different gas valves by combining different growth stages of the crystal, and adjusts the airflow environment inside the crucible body 201, so that the inside of the crucible body 201 is always in a gas atmosphere suitable for the growth of the crystal, and the growth quality of the crystal is ensured while the growth of the crystal is promoted. In addition, the gas flow control valve 50 controls the introduced gas to form gas flow, the formed gas flow can promote the sublimation of the silicon carbide powder, and can drive the sublimed silicon carbide vapor to move towards the direction of the seed crystal 203, so that the growth speed of the crystal is accelerated.
After growth is complete, the cover 202 may be opened to remove the final crystal. Then, the desired silicon carbide powder is added to the raw material container 10, the seed crystal 203 is arranged, and the lid body 201 is closed to proceed to the next preparation stage for seed crystal growth. At this time, the elastic member 20 is restored to the compressed state by the pressure due to the increase of the silicon carbide powder, and the above process is repeated.
In some embodiments of the present invention, referring to fig. 1, 5 and 6, the raw material container 10 is provided with an air inlet hole 13 and an air outlet hole 14, the air inlet hole 13 is communicated with the airflow control valve 50, and the air outlet hole 14 is communicated with the air inlet hole 13 and the inside of the crucible body 201; the air outlet holes 14 are provided with a plurality of air outlet holes 14 which are uniformly arranged on the side wall of the raw material containing piece 10 for placing the silicon carbide powder. For example, the whole raw material containing part 10 can be of a substantially T-shaped structure, and comprises a millstone 11 arranged in the crucible body 201 for placing silicon carbide and a graphite rod 12 arranged at the bottom of the millstone 11 and penetrating through the side wall of the crucible body 201, wherein the millstone 11 is provided with a hollow cavity 15, an air inlet 13 penetrates through the graphite rod 12, a plurality of air outlet holes 14 are all arranged on the upper wall of the millstone 11, and the air inlet hole 13 and the air outlet holes 14 are communicated with the cavity 15; the gaseous air current channel that forms through airflow control valve 50 via inlet port 13, cavity 15, venthole 14 reaches the bottom of carborundum powder, because venthole 14 evenly arranges, the homogeneity of increase gas that can the at utmost, make the air current evenly rise, guarantee the even atress of carborundum powder, promote the sublimation of carborundum powder, and accelerate sublimed carborundum vapour to the speed that the crystal removed, when promoting crystal growth efficiency, further reduced because of the crystal growth defect that carborundum powder sublimation is inhomogeneous and lead to, promote crystal growth quality.
In some embodiments of the present invention, as shown in fig. 1 and 2, the gas flow control valve 50 is formed with a gas port 51, and is provided with a shutter 52 for blocking the gas port 51, the shutter 52 being connected to the raw material container 10 and adapted to block the gas port 51 to various degrees in accordance with the movement of the raw material container 10. It can be understood that, along with the continuous reduction of carborundum powder in the growth process, under the effect of elastic component 20, raw materials holds piece 10 and will move upwards along the sublimed direction of carborundum powder, and simultaneously, the shielding piece 52 that links to each other with raw materials holds piece 10 will also move thereupon, realizes sheltering from gas port 51 not to the same extent to the realization is controlled the volume of letting in and the time of letting in of gas port 51 through the gas, so that the gaseous demand that can accord with the crystal growth stage that lets in. One or more air ports 51 can be arranged, a plurality of air ports 51 can pass through different gases, and shielding of the air ports 51 in different degrees can be shielding of one air port in different degrees, or shielding of different numbers of air ports 51.
In view of this, the gas flow control valve 50 according to the embodiment of the present invention, taking the carbon-rich gas as an example, can connect the carbon-rich gas to be introduced to the gas port 51, except that the inert gas is connected to the gas inlet end of the crucible body 201. In this embodiment, the gas flow control valve 50 may be provided with two gas ports 51, one gas port 51 for passing the carbon-rich gas and one gas port 51 for passing the inert gas; the gas flow control valve 50 may also be provided with only one gas port 51 for the passage of carbon rich gas, and the inert gas may additionally be channeled into the crucible body 201. For example, in the initial state, the shutter 52 does not shield the gas port 51, i.e. the gas port 51 is completely exposed, and the carbon-rich gas can be directly introduced into the crucible body 201 through the gas port 51. When the growth starts, because the melting point of silicon is low, the inside of the whole crucible body 201 is in a silicon-rich state, and the direct introduction of carbon-rich gas can adjust the gas flow environment inside the crucible body 201, so that the inside of the crucible body 201 is in a gas atmosphere suitable for crystal growth, thereby avoiding the generation of impurities such as silicon drops and the like, promoting the crystal growth and ensuring the growth quality of the crystal. Along with the rising of the raw material containing piece 10, the blocking piece 52 gradually blocks the gas port 51, the introduction amount of the carbon-rich gas is gradually reduced, when the first growth stage is finished, the gas port is just completely blocked by the blocking piece 52, and the carbon-rich gas stops being introduced into the crucible body 201.
Similarly, taking the silicon-rich gas as an example, the silicon-rich gas to be introduced can be connected to the gas port 51. Also, in the present embodiment, the gas flow control valve 50 may be provided with two gas ports 51, one gas port 51 for passing the silicon rich gas, and one gas port 51 for passing the inert gas; the gas flow control valve 50 may also be provided with only one gas port 51 for passing a silicon rich gas, and the inert gas may additionally be channeled into the crucible body 201. In the initial state, the shutter 52 completely blocks the air port 51. At the beginning of growth, the crucible body 201 is in a silicon-rich state, so that the gas port 51 is always shielded without introducing a silicon-rich gas. And at the crystal growth later stage, because the carbonization of carborundum powder, crucible body 201 is in rich carbon state, and shielding piece 52 will reduce gradually along with the rising of raw materials holding member 10 and shelter from gas port 51, and the gaseous input of rich silicon increases gradually to this air current environment of adjusting the crucible body 201 inside makes crucible body 201 inside be in a gas atmosphere that is fit for crystal growth, avoids the production of impurity such as carbon parcel, thereby promotes crystal growth, guarantees the growth quality of crystal.
Considering that the functional gases required by different growth stages of the crystal are different, in order to realize synchronous control of all introduced gases, the gas flow control valve 50 is provided with three gas ports 51, the three gas ports 51 are respectively connected with three different gas sources, the three different gas sources are respectively a silicon-rich gas, a carbon-rich gas and an inert gas, and the shielding piece 52 is suitable for changing the shielding degree of the three gas ports 51 along with the movement of the raw material containing piece, so that the gases introduced into the crucible body meet the growth requirements of the crystal at each stage. For example, referring to fig. 2, 4, 10 and 11, the three gas ports 51 are a first gas port a, a second gas port b and a third gas port c respectively, the carbon-rich gas is connected to the first gas port a, the inert gas is connected to the second gas port b, the silicon-rich gas is connected to the third gas port c, the shielding member 52 may be a baffle 522 with a strip-shaped hole 521 at the center, the strip-shaped hole 521 on the baffle 522 is located above the second gas port b, the shielding member 52 is connected to the raw material containing member 10, when the raw material containing member 10 moves up and down, the baffle 522 may move left and right along the parallel direction of the connecting lines of the three gas ports 51 above the three gas ports 51, so as to ensure that the third gas port c is completely covered by the baffle in the first growth stage of the crystal, and the gas introduced into the crucible body is the carbon-rich gas and the inert gas; in the second growth stage of the crystal, the first gas port a and the third gas port c are both shielded, and only inert gas is introduced; in the third growth stage of the crystal, the first gas port a is completely shielded by the baffle plate, and the silicon-rich gas and the inert gas are introduced.
It can be understood that, in the whole growth process of the crystal, the inert gas is always introduced, and whether the silicon-rich gas and the carbon-rich gas are introduced or not and the amount of the introduced gas can be controlled according to the quality change of the silicon carbide powder in different growth stages; for example, during the first growth phase, the first port a is gradually blocked as the baffle 522 is moved slowly, while the third port c is always completely blocked; in the second growth stage, only the second air port b is exposed, and the first air port a and the third air port c are always in a completely blocked state; in the third growth stage, the third port c is gradually exposed as the baffle 522 continues to move, and the first port a is always completely blocked in the process.
In other embodiments, the airflow control valve 50 may also be a valve body controlled by software, and the mass change of the silicon carbide powder is transmitted to the system, and after the system processes and analyzes the silicon carbide powder, the growth stage is determined, so that the opening and closing, the opening degree and the opening time of the airflow control valve 50 are controlled to realize the control of the introduced gas, and further the airflow environment inside the crucible body 201 is adjusted, so that the inside of the crucible body 201 is always in a gas atmosphere suitable for the growth of the crystal, the growth of the crystal is promoted, and the growth quality of the crystal is ensured.
In some embodiments of the present invention, referring to fig. 1, 2 and 10, the gas inlet control assembly 100 may further include a gas flow mixing bin 40, the gas flow mixing bin 40 is of a hollow structure, the gas flow mixing bin 40 is provided with a gas inlet end 41 and a gas outlet end 42, the gas flow control valve 50 is provided at the gas inlet end 41 of the gas flow mixing bin 40, and the gas outlet end 42 of the gas flow mixing bin 40 is used for introducing the gas mixed by the gas flow mixing bin 40 into the crucible body 201. The arrangement of the airflow mixing bin 40 can ensure that the gas to be introduced is mixed according to the required proportion and then enters the crucible body 201, so that the uniformity of the gas is ensured, the inside of the crucible body 201 is more favorably beaten into the gas atmosphere suitable for crystal growth, the growth of crystals is facilitated, and the growth quality of the crystals is ensured.
Considering that the temperature of the gas entering the crucible body 201 is directly related to the sublimation of the silicon carbide powder, and the sublimation of the silicon carbide powder is affected by the excessively low temperature, in some embodiments of the present invention, as shown in fig. 1, fig. 2 and fig. 9, the gas inlet control assembly 200 may further include a gas flow heating assembly 30 for heating the gas entering the crucible body 201, the gas flow heating assembly 30 includes a heater body 31, and the heater body 31 may be a graphite member, so that the heater body 31 has high temperature resistance; airflow channel 311 is opened in heater body 31, airflow channel 311 and airflow control valve 50, the inlet end intercommunication of crucible body 201, gaseous through airflow control valve 50, airflow channel 311, inside crucible body 201 was flowed into to the inlet end of crucible body 201, heater body 31 can preheat the gas in airflow channel 311, the gas after the heating can further promote the sublimation of carborundum powder after getting into crucible body 201, effectively improve the sublimation effect, and then improved crystal growth rate.
It can be understood that when the gas flow mixing bin 40 is provided, the gas flow heating assembly 30 may be disposed between the gas flow mixing bin 40 and the gas inlet end of the crucible body 201, and the mixed gas mixed by the gas flow mixing bin 40 enters the gas flow heating assembly 30 for heating before entering the crucible body 201, and the heated mixed gas may further promote sublimation of the silicon carbide powder. In other words, the combination of the airflow mixing bin 10 and the airflow heating assembly 30 can ensure that the airflow introduced from the bottom is fully mixed and heated firstly, and then enters the crucible body 201 after being uniformly mixed and heated, so that the problem that the silicon carbide powder is difficult to sublimate due to the direct introduction of low-temperature gas is avoided, and the sublimation effect is effectively improved; moreover, the uniformity of the gas entering can be ensured, and the crystal growth defects caused by non-uniform gas introduction can be reduced.
Alternatively, the gas flow channel 311 may be a spiral channel or an S-shaped channel, and the spiral channel or the S-shaped channel may increase the contact area and the contact duration between the gas and the graphite wall of the heater body 31, compared with a straight channel, so as to ensure the heating effect of the gas.
In other embodiments of the present invention, the airflow heating assembly 30 may also be an airflow heating pipe disposed in the sidewall of the crucible body 201, an inlet end of the airflow heating pipe is connected to an outlet of the airflow control valve/airflow mixing bin, and an outlet end of the airflow heating pipe is communicated with the inside of the crucible body 201. The airflow heating pipeline is arranged in the inner wall of the crucible body 201, when the crucible body 201 generates heat, the temperature of the airflow heating pipeline is increased, and the gas flowing through the airflow heating pipeline can be directly heated, so that the sublimation of the silicon carbide powder is further promoted by the gas entering the crucible body 201. Optionally, the airflow heating pipeline may be a curved pipeline, which can ensure that the gas is sufficiently heated in the sidewall of the crucible body 201, ensure that the gas entering the crucible body 201 is more beneficial to the sublimation of the silicon carbide powder, and further improve the growth rate of the crystal.
In some embodiments of the invention, as shown with reference to fig. 2 and 4, a transmission assembly 60 connecting the material containing member 10 and the airflow control valve 50 may be further included. The driving assembly 60 is used to drive the airflow control valve 50 to control the airflow by the movement of the material container 10, and the driving assembly 60 may be a flexible driving mechanism or a rigid driving mechanism. Where the airflow control valve 50 includes a shield 52, a drive assembly 60 connects the material holder 10 and the shield 52.
For example, referring to FIG. 2, the driving assembly 60 is a flexible driving mechanism, and includes a guide wheel set 61 disposed outside the crucible body, and the guide wheel set 61 is connected to the raw material containing member 10 and the gas flow control valve 50 by a driving wire 62. Specifically, the guide wheel set 61 includes a first pulley 611, a second pulley 612, a third pulley 613 and a reducing gear set 614, the first pulley 611, the third pulley 613 and the reducing gear set 614 are installed at the bottom of the outer wall of the crucible body 201, the reducing gear set 614 is disposed between the first pulley 611 and the third pulley 613, the second pulley 612 is disposed at one side of the gas flow control valve 50 and is located on an extension line of the moving range of the gas flow control valve 50, one end of the transmission line 62 is connected to the end of the raw material containing member 10 extending out of the crucible body 201, the other end passes through the first pulley 611, the reducing gear set 614, the third pulley 613 and the second pulley 612 in sequence and is connected to the shielding member 52 of the gas flow control valve 50, when the raw material containing member 10 moves upward under the action of the elastic member 20, one end of the transmission line 62 moves upward along with it, and the other end moves the shielding member 52 driving the gas flow control valve 50 in a horizontal direction, the realization is to the sheltering from of gas port 51 not equidimension, and then adjusts the inside air current environment of crucible body 201 to make crucible body 201 inside be in a suitable crystal growth's gas atmosphere all the time, promote crystal growth, guaranteed the growth quality of crystal. At this time, in order to ensure better restoration of the shutter 52 in the airflow control valve 50, a return spring 53 may be further added, and the return spring 53 is connected to an end of the shutter 52 away from the drive line 62.
In other embodiments of the present invention, referring to fig. 4, the driving assembly 60 may also be a rigid driving mechanism, including a guide linkage 63 disposed outside the crucible body 201, wherein the guide linkage 63 connects the raw material container 10 and the gas flow control valve 50. Specifically, the guiding linkage 63 includes four links hinged in sequence, which are a first link 635, a second link 634, a third link 632 and a fourth link 631 respectively; the head end of the first link 635 is connected to the end of the raw material container 10 extending out of the crucible body, and the tail end of the fourth link 631 is connected to the shutter 52 of the gas flow control valve 50; the second and fourth connecting rods 634, 631 are fixed along their respective rod axial directions, so that the second and fourth connecting rods 634, 631 can only reciprocate along their axial directions, and the second connecting rod 634 can be fixed by the sleeve 633 and can move up and down along the sleeve 633; the moving direction of the fourth link 631 coincides with the moving direction of the airflow control valve 50.
It is understood that when the material containing member 10 is moved upward by the elastic member 20, the second link 634 is moved upward in the axial direction thereof by the first link 635, and the connection end of the third link 632 and the second link 634 is moved upward and the other end is rotated; the fourth connecting rod 631 will drive the shielding piece 52 of the airflow control valve 50 to move, so as to shield the gas port 51 in different degrees, and further adjust the airflow environment inside the crucible body 201, so that the inside of the crucible body 201 is always in a gas atmosphere suitable for crystal growth, and the growth quality of crystals is ensured while the crystal growth is promoted.
In some embodiments of the present invention, referring to fig. 1, 7 and 8, a seed crystal fixing member 204 for fixing the seed crystal 203 may be disposed on an inner wall of the cover 202, the seed crystal fixing member 204 has a temperature reduction chamber 205, a temperature reduction assembly 70 is disposed in the temperature reduction chamber 205, the temperature reduction assembly 70 includes an airflow pipeline 71 and a blowing piece 72, a temperature reduction hole 721 is disposed on the blowing piece 72, the airflow pipeline 71 is communicated with the blowing piece 72, and the temperature reduction gas flows into the blowing piece 72 through the airflow pipeline 71 and enters the temperature reduction chamber 205 through the temperature reduction hole 721. The cooling gas can be used for reducing the temperature of the crystal part after reaching the cooling bin 205, and the gasification in the crystal growth process is reduced; simultaneously, make whole crystal growth face increase with the same speed to a face is produced at the growth face, the material that reduces in the post processing process and lead to because the crystal shape is unsmooth can not use the quantity, reduces extravagantly. With the continuous introduction of the cooling gas, the formation of an axial temperature gradient in the crucible body 201 can be promoted, the growth of the silicon carbide crystal is promoted, and the growth efficiency is improved.
Alternatively, as shown in FIG. 7, the blowing element 72 is a flow guide element with a gradually increasing diameter. For example, the blowing element 72 is a trumpet-shaped flow guide element, the cooling hole 721 is arranged at the outlet of the trumpet-shaped flow guide element, and the number of the cooling holes 721 may be one or more. When the cooling hole 721 is one, it may be a first through hole having a diameter smaller than the diameter of the outlet and larger than the diameter of the inlet. When there are a plurality of cooling holes 721, there may be a plurality of second through holes provided on the outlet sealing plate, and the diameter of the second through holes is smaller than that of the first through holes.
Optionally, there may be a plurality of cooling assemblies 70 in the cooling bin 205, a plurality of cooling assemblies 70 may be arranged in the cooling bin 205 according to cooling requirements to cool the crystal, each gas flow pipeline 71 of each cooling assembly 70 is provided with a gas flow control valve 73, and the gas flow in the corresponding gas flow pipeline 71 may be controlled by each gas flow control valve 73 to adjust the temperature of the corresponding crystal region, so as to control the growth speed of the crystal in different regions, thereby obtaining the crystal shape required by us, reducing the crystal loss caused by irregular shape due to different growth speeds, and reducing the crystal defects. For example, referring to fig. 7 and 8, four cooling assemblies 70 can be provided, and are uniformly distributed in the cooling chamber 205, and the outlet of the blower 72 in each cooling assembly 70 is opposite to the side wall of the seed crystal 203 mounted on the seed crystal holder 204.
In some embodiments of the present invention, the inner wall of the crucible body 201 and the seed crystal fixing member 204 together define a flow guiding cavity 206, and the crucible body 201 is provided with a first flow guiding hole 207 communicating the flow guiding cavity 206 and the outside of the crucible body 201; the seed crystal fixing piece 204 is provided with a second flow guiding hole 208 for communicating the cooling bin 205 with the flow guiding cavity 206. Specifically, a groove arranged in an annular shape is formed in the position, facing the seed crystal fixing piece 204, on the inner wall of the crucible body 201, and the flow guide cavity 206 is defined by the groove and the seed crystal fixing piece 204. In the growth process, because continuously let in gas in the crucible body 201, also increased the inside pressure of crucible body 201 when promoting carborundum powder sublimation to become gaseous upflow, so the setting of water conservancy diversion chamber 206 can supply to flow in the air current that flows in crucible body 201 through crucible body 201 inlet end along the crystal surface and flow in after the long brilliant end to reduce crucible body 201's internal pressure, and utilize the air current constantly to flow and take away impurities such as carbon parcel that produce in the growth process.
It can be understood that, after the waste gas (reacted gas in the crucible body 201) enters the diversion cavity 206, the waste gas will flow out of the crucible body 201 from the first diversion hole 207, so as to reduce the pressure at the growth part in the crucible body 201, and form a pressure gradient in cooperation with the lower portion, thereby keeping the pressure inside the crucible body 201 to be always high at the lower portion and low at the upper portion. Meanwhile, impurities of silicon carbide vapor are taken away by the continuous flow of the gas, and the purity of the crystal is improved. In addition, the used gas in the cooling bin 205 flows out through the second flow guide hole 208, and then flows into the flow guide cavity 206, and flows out together with the gas in the flow guide cavity 206.
Optionally, there may be a plurality of first guiding holes 207, and the plurality of first guiding holes 207 are uniformly formed around the guiding cavity 206 on the crucible body 207. It can be understood that the first flow guide holes 207 are uniformly formed, so that the gas in the flow guide cavity 206 can be better conveyed to the outside of the crucible body 201, uniform release is also more beneficial to ensuring that the pressure at the upper part of the crucible body 201 is in a stable state, and excessive accumulation of the gas at a certain position of the flow guide cavity 206 is avoided.
Optionally, there may be a plurality of second guiding holes 208, and the plurality of second guiding holes 208 are uniformly arranged around the cooling bin 205. It can be understood that the second flow guiding holes 208 formed uniformly are also more favorable for uniformly discharging the cooling gas used in the cooling bin 205 outward, so as to ensure that the cooling bin 205 is in a stable environment.
In some embodiments of the present invention, referring to fig. 1 and 3, the elastic member 20 may have a gas inlet and a gas outlet which are communicated with each other while having the functions of compressing and expanding, the gas entering the crucible body 201 passes through the elastic member 20 and then enters, and the gas transportation in the elastic member 20 is not affected when the elastic member 20 is compressed and expanded. Specifically, it can be directly connected between the air inlet 13 of the raw material container 10 and the outlet of the air flow passage 311 of the airflow heating unit 30. Of course, referring to fig. 12, the elastic member 20 may not have an air inlet and an air outlet, and accordingly, the air inlet 13 of the material container 10 is directly connected to the outlet of the air flow passage 311 of the air flow heating assembly 30.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are not to be considered limiting of the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; the connection can be mechanical connection, electrical connection or communication; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through an intermediate. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature "under," "beneath," and "under" a second feature may be directly under or obliquely under the second feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
While embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims (10)
1. A growth apparatus for producing single crystal silicon carbide, comprising:
the growth crucible comprises a crucible body and a cover body, wherein silicon carbide powder is contained in the crucible body, and the cover body is arranged on the crucible body;
and the gas inlet control assembly is positioned at the gas inlet end of the crucible body and used for controlling gas entering the crucible body according to the mass change of the silicon carbide powder.
2. A growth apparatus for producing single crystal silicon carbide according to claim 1, wherein the gas inlet control assembly includes:
the raw material containing piece is arranged in the crucible body and is used for containing the silicon carbide powder;
the elastic piece is connected with the raw material containing piece and used for driving the raw material containing piece to move along the axial direction of the growth crucible according to the mass change of the silicon carbide powder;
and the gas flow control valve is positioned at the gas inlet end of the crucible body, is connected with a gas source and is used for controlling gas entering the crucible body according to the movement of the raw material containing piece.
3. A growth apparatus for producing single crystal silicon carbide according to claim 2, wherein said raw material holding member is provided with an air inlet hole and an air outlet hole, said air inlet hole being communicated with said air flow control valve, said air outlet hole being communicated with said air inlet hole and an inside of said crucible body; the venthole is equipped with a plurality ofly, and is a plurality of the venthole is evenly established the raw materials holds on the lateral wall that the piece placed carborundum powder.
4. A growth apparatus for producing single crystal silicon carbide according to claim 2, wherein the gas flow control valve is formed with a gas port and is provided with a shielding member for shielding the gas port, the shielding member being connected to the raw material containing member and adapted to shield the gas port to different degrees in accordance with movement of the raw material containing member.
5. A growth apparatus for preparing single crystal silicon carbide according to claim 4 wherein said gas flow control valve is provided with three said gas ports, said three gas ports being connected to three different gas sources, respectively, said three different gas sources being a silicon-rich gas, a carbon-rich gas and an inert gas, said shield being adapted to vary the degree of shielding of said three gas ports with movement of said source material holder so that the gas introduced into said crucible body meets the requirements for growth at each stage of the crystal.
6. The growth device for preparing single crystal silicon carbide according to claim 2, further comprising a gas flow mixing bin, wherein the gas flow mixing bin is of a hollow structure, a gas inlet end and a gas outlet end are arranged on the gas flow mixing bin, the gas flow control valve is arranged at the gas inlet end of the gas flow mixing bin, and the gas outlet end of the gas flow mixing bin is used for introducing the gas mixed by the gas flow mixing bin into the crucible body.
7. The growth device for preparing single crystal silicon carbide according to claim 2, further comprising a transmission assembly connecting the raw material container and the gas flow control valve, wherein the transmission assembly is a flexible transmission mechanism and comprises a guide wheel set arranged outside the crucible body, and the guide wheel set is connected with the raw material container and the gas flow control valve through transmission lines.
8. A growth apparatus for producing single crystal silicon carbide according to claim 2, further comprising a transmission assembly connecting the raw material container and the gas flow control valve, wherein the transmission assembly is a rigid transmission mechanism comprising a guide linkage disposed outside the crucible body, the guide linkage connecting the raw material container and the gas flow control valve.
9. The growth device for preparing the single crystal silicon carbide as claimed in any one of claims 1 to 8, wherein a seed crystal fixing member for fixing the seed crystal is arranged on the inner wall of the cover body, the seed crystal fixing member is provided with a cooling bin, a cooling assembly is arranged in the cooling bin, the cooling assembly comprises an airflow pipeline and a blowing piece, a cooling hole is arranged on the blowing piece, the airflow pipeline is communicated with the blowing piece, and cooling gas flows into the blowing piece through the airflow pipeline and enters the cooling bin through the cooling hole.
10. The growth device for preparing single crystal silicon carbide according to claim 9, wherein the inner wall of the crucible body and the seed crystal fixing piece together define a flow guide cavity, and the crucible body is provided with a first flow guide hole for communicating the flow guide cavity and the outside of the crucible body; and a second flow guide hole for communicating the cooling bin with the flow guide cavity is formed in the seed crystal fixing piece.
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