CN113215654B

CN113215654B - Reactor assembly for preparing crystal by PVT method and use method and application thereof

Info

Publication number: CN113215654B
Application number: CN202110482795.4A
Authority: CN
Inventors: 刘鹏飞; 刘星; 刘家朋; 李加林
Original assignee: Shandong Tianyue Advanced Technology Co Ltd
Current assignee: Shandong Tianyue Advanced Technology Co Ltd
Priority date: 2021-04-30
Filing date: 2021-04-30
Publication date: 2022-04-12
Anticipated expiration: 2041-04-30
Also published as: CN113215654A

Abstract

The application discloses a reactor assembly for preparing crystals by a PVT method, and belongs to the field of semiconductor material preparation. The reactor assembly comprises: the reaction chamber comprises a raw material chamber and a waste material chamber, and the bottom end of the waste material chamber is lower than that of the raw material chamber; the heating mechanism is sleeved outside the raw material cavity and used for heating the raw material cavity; the crystal growth cavity is communicated with the raw material cavity through a gas phase transmission channel, and raw material gas generated by sublimation of raw materials in the raw material cavity is transmitted to seed crystals in the crystal growth cavity through the gas phase transmission channel for crystal growth; and the plug flow mechanism moves the waste materials generated in the crystal growth process in the raw material cavity to the waste material cavity. This reactor component can in time remove the waste material to the waste material chamber, improves the sublimation rate and the utilization ratio of raw materials to reduce the defect of crystal.

Description

Reactor assembly for preparing crystal by PVT method and use method and application thereof

Technical Field

The application relates to a reactor component for preparing crystals by a PVT method, belonging to the field of semiconductor material preparation.

Background

At present, in the preparation of silicon carbide crystal, physical vapor transport (abbreviated as PVT method) technology is mainly used, and the technology is used for sublimating and decomposing silicon carbide raw material into gas-phase component Si_mC_nAnd then, under the drive of the axial temperature gradient, the crystal is transmitted to the seed crystal to grow into a silicon carbide crystal. The PVT method is a complex process, and a plurality of parameters such as growth temperature, temperature gradient, direct distance between the seed crystal and the growth material, gas pressure, etc. must be comprehensively controlled, and any one of the parameters cannot be well controlled, and the stability of crystal growth will be damaged.

During the later growth period of silicon carbide crystal, the silicon carbide material is decomposed non-stoichiometrically, and more silicon atoms are in various gas phase components Si_mC_nIn the form of (1), when m > n, the gas-phase component Si_mC_nThe silicon-rich groups in the gas state can cause excessive carbon in the silicon carbide raw material, so that the graphitization phenomenon can occur, and waste materials can be formed. Graphitization of silicon carbide feedstock is a common instability factor that increases the likelihood of crystal graphitization and formation of other defects, such that the crystal growth rate is limited to a large extent.

The existing solution is that extra solid silicon is added into a graphite crucible, so that the loss of silicon in the growth raw material can be compensated, and the graphitization of the growth raw material is prevented to a certain extent, but the liquid silicon drops are formed and the multi-type structure is converted; and secondly, the tantalum crucible is used for creating an environment for adsorbing carbon, so that graphitization of the growth raw material can be obviously inhibited, but the tantalum crucible is too high in price and cannot be used in a large scale.

Disclosure of Invention

In order to solve the problems, the application provides a reactor component for preparing crystals by a PVT method, the reactor component transfers waste materials in a raw material cavity to a waste material cavity in time through a plug flow mechanism, so that the waste materials are not heated any more and participate in the growth of the crystals, the raw materials in the raw material cavity always keep the same carbonization degree, the uniformity of raw material gas components is improved, the sublimation rate and the utilization rate of the raw materials are further improved, and the preparation method is favorable for obtaining high-quality silicon carbide crystals.

The reactor component for preparing the crystal by the PVT method is characterized by comprising the following components:

the reaction chamber comprises a raw material chamber and a waste material chamber, and the bottom end of the waste material chamber is lower than that of the raw material chamber;

the heating mechanism is sleeved outside the raw material cavity and used for heating the raw material cavity;

the crystal growth cavity is communicated with the raw material cavity through a gas phase transmission channel, and raw material gas generated by sublimation of raw materials in the raw material cavity is transmitted to seed crystals in the crystal growth cavity through the gas phase transmission channel for crystal growth;

and the plug flow mechanism moves the waste materials generated in the crystal growth process in the raw material cavity to the waste material cavity.

Optionally, a seed crystal is arranged in the crystal growth cavity, and raw material gas obtained by sublimation of the raw material in the reaction cavity is transmitted to the seed crystal through the gas phase transmission channel to start crystal growth.

Optionally, the top opening of the feedstock chamber communicates with the top opening of the waste chamber, and the plug flow mechanism transfers the waste material to the waste chamber through the top opening of the feedstock chamber and the top opening of the waste chamber.

Optionally, the raw material cavity is sleeved on the periphery of the waste material cavity; or

The waste material cavity is sleeved on the periphery of the raw material cavity.

Optionally, the reaction chamber is formed by a reaction chamber inner cylinder and a reaction chamber outer cylinder, and the reaction chamber outer cylinder is sleeved outside the reaction chamber inner cylinder; and

the raw material cavity is formed between the reaction cavity outer cylinder and the reaction cavity inner cylinder, and the reaction cavity inner cylinder forms the waste cavity; or the waste material cavity is formed between the reaction cavity outer cylinder and the reaction cavity inner cylinder, and the raw material cavity is formed in the reaction cavity inner cylinder.

Optionally, the ratio of the diameter of the outer reaction chamber barrel 11 to the diameter of the inner reaction chamber barrel 12 is 1.5-3:1, preferably 2: 1.

Optionally, the distance D between the inner reaction chamber cylinder and the outer reaction chamber cylinder is 20-200 mm.

Optionally, the reaction cavity outer cylinder is higher than the reaction cavity inner cylinder, and the top of the reaction cavity outer cylinder is communicated with the crystal growth cavity.

Optionally, the reaction cavity inner barrel and the reaction cavity outer barrel are arranged on the same central axis.

Optionally, the gas phase conveying device further comprises a feeding mechanism, wherein the feeding mechanism comprises a material bearing table which is arranged in the raw material cavity and bears the raw material, and the feeding mechanism can control the material bearing table to drive the raw material to move towards the direction close to the gas phase conveying channel;

optionally, the horizontal plug flow mechanism comprises a pushing piece and a connecting rod connected with the pushing piece, the pushing piece is arranged in the gas phase transmission channel, and the connecting rod controls the pushing piece to push the raw material surface layer waste material with a target area and thickness into the waste material cavity.

Optionally, the material pushing part is a baffle plate, and the baffle plate is arranged at the top of the reaction chamber;

optionally, the ratio of the distance from the pushing member to the bottom end of the raw material cavity to the distance from the pushing member to the bottom end of the waste material cavity is 3-5: 7-10, preferably, the ratio of the distance from the pushing piece to the bottom end of the raw material cavity to the distance from the pushing piece to the bottom end of the waste material cavity is 3: 10.

Optionally, the distance between the pushing member and the top of the reaction chamber and the distance between the pushing member and the seed crystal are 3-10: 90-200, preferably, the distance between the pushing piece and the top of the reaction cavity is 3:200 to the distance between the pushing piece and the seed crystal.

The connecting rod can rotate to drive the baffle to rotate, and the raw material surface layer waste is pushed to the waste cavity.

Optionally, the link rotates clockwise or counterclockwise, and the rotation direction of the link is unchanged.

Optionally, the rotation speed of the connecting rod is 10-300r/h, preferably, the rotation speed is 10-100r/h, and more preferably, the rotation speed is 50r/h-70 r/h.

Optionally, the bearing table drives the raw material to move 0.1mm in the direction close to the gas phase transmission channel, and the connecting rod drives the baffle to rotate for 1-5 times;

preferably, the bearing table drives the raw materials to move 0.1mm in the direction close to the gas phase transmission channel, and the connecting rod drives the baffle to rotate for 1 time.

Optionally, the number of the baffles is at least two, the baffles are uniformly distributed on the circumference of the connecting rod, preferably, the number of the baffles is 3-5, the included angle between every two adjacent baffles is 40-120 °, and preferably, the angle between every two adjacent baffles is 60-90 °.

Optionally, the width of the baffle is 50-100mm, the height of the baffle is 2-10mm, preferably, the width of the baffle is 70-80mm, and the height of the baffle is 3-5 mm.

Optionally, the connecting rod is capable of stretching and contracting, and is used for controlling the baffle to move along the direction from the raw material cavity to the waste material cavity so as to push the raw material surface layer waste material to the waste material cavity.

Optionally, the device further comprises a first control mechanism for controlling the extension and contraction of the connecting rod or a second control mechanism for controlling the rotation of the connecting rod.

Optionally, a preformed hole is formed in the bottom of the waste material cavity, and the connecting rod penetrates through the preformed hole to be connected with the baffle so as to control the baffle to rotate.

Optionally, the preformed hole is arranged in the central position of the waste cavity, the baffle is positioned on the same plane with the top openings of the raw material cavity and the waste cavity, and the baffle can contact the inner side wall of the outer barrel of the reaction cavity.

Optionally, the feeding mechanism further comprises a push rod, the push rod penetrates through the bottom of the raw material cavity and is connected with the material bearing platform, and the push rod is used for pushing the material bearing platform to move towards the direction close to the gas phase transmission channel.

Optionally, a third control mechanism for controlling the movement of the push rod is further included.

Optionally, a porous graphite plate is arranged in the gas phase transmission channel, and the feed gas passes through the porous graphite plate and enters the crystal growth cavity.

According to another aspect of the present application, there is provided a method of using a reactor assembly as defined in any one of the preceding claims, the method comprising:

a preparation stage: charging the feedstock into the feedstock chamber;

crystal growth stage: controlling the crystal growth temperature and the crystal growth pressure of the raw material cavity, transmitting the raw material gas generated by heating and sublimating the raw material in the raw material cavity to the seed crystal through the gas phase transmission channel to start crystal growth, starting the plug flow mechanism to continuously move the waste material in the crystal growth process in the raw material cavity to the waste material cavity until the crystal growth is finished;

preferably, the crystal growth temperature is 2300-²Pa-2×10³And Pa, when the sublimation rate of the raw material in the raw material cavity reaches 0-5% in the crystal growth stage, starting the plug flow mechanism, and moving the waste material to the waste material cavity at a constant speed by the plug flow mechanism.

Optionally, after the sublimation rate of the silicon carbide raw material is greater than the first sublimation rate, the plug flow mechanism pushes the raw material surface layer waste material with the target area and the thickness into the waste material cavity at a constant speed, and the material removal frequency of the plug flow mechanism is 10-300 times/h; preferably, the material removing frequency is 10-100 times/h, and more preferably, the material removing frequency is 50-80 times/h.

Optionally, the first sublimation rate is 0-5%, and the crystal growth temperature in the crystal growth condition is 2300-; the crystal growth pressure is 5 multiplied by 10²Pa-2×10³Pa；

Preferably, the first sublimation rate is 0-2%, the crystal growth temperature is 2300K-2500K, and the crystal growth pressure is 5 × 10²Pa-1×10³Pa, more preferably, the first sublimation rate is 0%. The crystal growth temperature is 2450K.

Optionally, the method of using the reactor assembly comprises the steps of:

(1) placing a raw material cavity, a waste material cavity and a crystal growth cavity which are filled with silicon carbide raw materials in a crystal growth furnace and sealing, wherein the silicon carbide raw materials are flush with the raw material cavity;

(2) the furnace body is vacuumized to 10^-4Pa below, then introducing high-purity inert gas to 10⁴Pa, repeating the process for 2-3 times, and finally vacuumizing the furnace body to 10 degrees^-4Pa below;

(3) introducing high-purity inert gas into the furnace body, and increasing the pressure to 10 within 2-3h⁴Pa, continuously introducing high-purity inert gas and keeping the pressure unchanged, and increasing the temperature of the furnace body to 2100K-2300K within 5-10h, wherein the growth time is 5 h;

(4) crystal growth stage: reducing the pressure in the furnace body to 5 x 10²Pa-2×10³The temperature in the furnace body is increased to the crystal growth temperature 2300 and 2800K within 5-10 hours of Pa, and the growth time is 0-3 hours; when the sublimation rate of the silicon carbide raw material is not less than 0-5%, starting a plug flow mechanism, transferring waste materials generated after the raw material in the reaction cavity is sublimated to a waste material cavity through the plug flow mechanism, continuously sublimating the residual raw material in the raw material cavity for crystal growth, and removing the materials at a constant speed by the plug flow mechanism, wherein the material removing frequency is 1-100 times/h, and the growth time is 50-150 h;

(5) and after the crystal growth is finished, cooling the furnace body, filling high-purity inert gas into the furnace chamber to normal pressure, opening the furnace body, and taking out the crystal growth chamber to obtain the silicon carbide crystal with low defect density.

Preferably, the step (2) is to vacuumize the furnace body to 10 DEG^-5Pa below, then introducing high-purity inert gas to 10⁴Pa, repeating the process for 2-3 times, and finally vacuumizing the furnace body to 10 degrees^-5Pa or less.

According to another aspect of the present application, there is provided the use of a reactor assembly as defined in any one of the preceding claims in the preparation of a silicon carbide crystal.

Optionally, the reactor assembly is used to produce a silicon carbide single crystal.

Benefits that can be produced by the present application include, but are not limited to:

1. the utility model provides a reactor component, plug flow mechanism in time remove the waste material of raw materials intracavity to the waste material chamber for the waste material no longer continues to be heated and participates in the growth of crystal, and the raw materials of raw materials intracavity remains the same carbonization degree throughout, improves the homogeneity of feed gas component, and then improves the sublimation rate and the utilization ratio of raw materials, is favorable to obtaining high-quality silicon carbide crystal.

2. The application provides a reactor component, feeding mechanism's plummer can drive the raw materials of raw materials intracavity to moving near gaseous phase transmission channel direction, makes the continuous high temperature region of pushing of raw materials in the raw materials intracavity for the raw materials carbonization of raw materials intracavity is even, avoids partial raw materials at the central upper portion recrystallization of raw materials, improves the utilization ratio of raw materials, is favorable to growing out the heavier crystal of weight.

3. The application provides a reactor component, the bottom in waste material chamber is less than the bottom in raw materials chamber, makes the waste material keep away from the high temperature region, avoids the waste material sublimation to lead to the crystal defect to appear, improves the sublimation rate of raw materials and the growth rate of crystal, makes the feed gas of crystal growth intracavity keep unanimous in the growth process, is favorable to obtaining the even and no high quality silicon carbide crystal of small polytype in surface.

4. The application provides a reactor component, the thickness of the raw materials top layer waste material that connecting rod and baffle cooperation steerable will be got rid of to the volume of getting rid of the raw materials intracavity waste material is controlled, ensures to get rid of the waste material totally, and avoids getting rid of the even raw materials that distribute, guarantees that the gaseous phase component of raw materials is even, improves the growth quality of crystal, practices thrift manufacturing cost.

5. The utility model provides a reactor component, feed gas pass porous graphite plate and get into long brilliant chamber, and porous graphite plate can block the fine particle of doping in the feed gas, stabilizes the growth environment of crystal, avoids appearing defects such as polytype, dislocation, microtube, inclusion in the crystal production process.

6. The application provides a reactor component's application method, start plug flow mechanism when the first sublimation rate of control raw materials is less than 5% to in whole long brilliant, plug flow mechanism lasts even the waste material of getting rid of, and the component of ability effective control raw materials guarantees that the raw materials distribution in the raw materials intracavity is even, and the feed gas gaseous phase that further improves the growth matter production of crystal is stable, reduces the defect of crystal.

Drawings

The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:

FIG. 1 is a schematic view of the structure of a reactor module according to example 1 of the present application;

FIG. 2 is a schematic view of the structure of a reactor module according to example 1 of the present application;

FIG. 3 is an enlarged view of a portion A of FIG. 2;

FIG. 4 is a schematic view of the structure of a reactor module according to example 2 of the present application

List of parts and reference numerals:

1. a feedstock chamber; 11. an outer reaction chamber barrel; 12. an inner barrel of the reaction cavity; 2. a waste chamber; 3. a crystal growing cavity; 31. a porous graphite plate; 32. seed crystal; 41. pushing the material piece; 42. a connecting rod; 43. reserving a hole; 51. a bearing table; 52. a push rod.

Detailed Description

In order to more clearly explain the overall concept of the present application, the following detailed description is given by way of example in conjunction with the accompanying drawings.

In order that the above objects, features and advantages of the present application can be more clearly understood, the present application will be described in further detail with reference to the accompanying drawings and detailed description. It should be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflict.

In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present application, however, the present application may be practiced in other ways than those described herein, and therefore the scope of the present application is not limited by the specific embodiments disclosed below.

In addition, in the description of the present application, it is to be understood that the terms "center", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "axial", "radial", "circumferential", and the like, indicate orientations and positional relationships based on those shown in the drawings, are only for convenience of description and simplicity of description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present application.

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 application, "a plurality" means two or more unless specifically limited otherwise.

In this application, unless expressly stated or limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can include, for example, fixed connections, removable connections, or integral parts; 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 meaning of the above terms in the present application can be understood by those of ordinary skill in the art as appropriate.

In this application, unless expressly stated or limited otherwise, 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 intervening media. In the description herein, reference to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., means 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 application. 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.

The analysis method in the examples of the present application is as follows:

1. microscopic examination was carried out using a microscope model BX51 from OLYMPUS.

2. The polytype test used a model HR800 Raman spectrometer from HORIBA.

3. The dislocation test was carried out using a microscope model BX51 from OLYMPUS after etching with potassium hydroxide.

4. The inclusion test was performed using a microscope model BX51 from OLYMPUS.

Unless otherwise specified, the raw materials, catalysts and gases in the examples of the present application were all purchased commercially, wherein the purity of the silicon carbide raw material was 99.99%, and the purity of the high-purity inert gas (Ar or He) was more than 99.99%.

The reactor assembly for growing crystals of the present application can be used for growing silicon carbide crystals, but is not limited to growing silicon carbide crystals, and the structure and the using method of the reactor assembly are exemplified by silicon carbide crystals.

Example 1

Referring to fig. 1-3, embodiments of the present application disclose a reactor assembly for growing crystals, the reactor assembly comprising a reaction chamber, a growth chamber 3, and a plug flow mechanism; the reaction chamber includes raw materials chamber 1 and waste material chamber 2, and long brilliant chamber 3 communicates through gaseous phase transmission passageway with raw materials chamber 1, and the feed gas that raw materials sublimation in the raw materials chamber 1 produced passes through gaseous phase transmission passageway and transmits to long brilliant intracavity 3 and long brilliant, and the waste material that long brilliant in-process produced shifts waste material chamber 2 in with raw materials chamber 1 is flowed to the plug flow mechanism.

Specifically, former material chamber 1 and waste material chamber 2 are solitary cavity, and this solitary former material chamber 1 and waste material chamber 2 can be adjacent, can establish the form for the cover, and waste material chamber 2 can set up to fixed unchangeable, also can set up to the cavity that removes in the reaction chamber, as long as can realize depositing waste material in former material chamber 1 in waste material chamber 2 to the waste material can not continue to react in waste material chamber 2, do not injecing this.

Concretely, long brilliant chamber 3 and raw materials chamber 1 intercommunication, raw materials in the raw materials chamber 1 are heated and sublimated and produce the feed gas, this feed gas gaseous phase is transmitted to the seed crystal 32 department of long brilliant chamber 3 and is gone on long brilliant, long brilliant chamber 3 and raw materials chamber 1 can be a whole, also can middle baffle that exists, the route that the feed gas transmitted from raw materials chamber 1 to long brilliant chamber 3 is gaseous transmission passageway, the transmission mode of this gaseous phase transmission passageway depends on raw materials chamber 1 and long brilliant chamber 3's positional relationship, can be for upper and lower transmission, can control the transmission, also can transmit according to specific transmission route, consequently do not do the restriction to the positional relationship of long brilliant chamber 3 and raw materials chamber 1, as long as can realize that the feed gas transmits to long brilliant chamber 3.

Specifically, the plug flow mechanism transfers the waste material in the raw material cavity 1 to the waste material cavity 2, the plug flow mechanism removes the waste material by using a gripper, and the gripper timely grips the waste material in the raw material cavity 1 in the waste material cavity 2 in the crystal growth process; the waste material can also be removed by adopting a push plate, the waste material in the raw material cavity 1 is pushed to the waste material cavity 2 by utilizing the push plate, the waste material cavity 2 transfers the waste material to the outside of the reactor component after the reaction is finished, the form of a horizontal plug flow mechanism is not limited, and the waste material generated in the raw material cavity 1 can be transferred to the waste material cavity 2 only by realizing the purpose.

As an embodiment, still include heating mechanism, this heating mechanism sets up in raw materials chamber 1 outside for this raw materials chamber 1 of even heating, this heating mechanism's heating method is induction heating, and specific heating coil that utilizes heats, consequently can conveniently control the regional heating temperature in raw materials chamber 1, according to the position of raw materials, in time adjusts the regional heating temperature of raw materials, guarantees that the raw materials is continuously heated and sublimates, carries out the crystal growth.

Specifically, in the heating sublimation process of the raw material in the raw material cavity 1, the central material area with the highest temperature is firstly sublimated in a grading way to generate various forms of Si_mC_nThe gas phase component, along with the reaction continues, some raw materials have graphitization phenomenon, so that the sublimation rate of the raw materials is reduced, crystal defects such as polytype, dislocation, micro-pipeline and the like are easy to appear, and some raw materials are subjected to migration, bonding and sintering, and finally recrystallized into silicon carbide crystal grains which cannot be carbonized in a cooler area at the upper part of the center of the raw materials, namely the waste material. The waste material that in time shifts raw materials chamber 1 to waste material chamber 2 through the plug flow mechanism, the waste material that shifts to in waste material chamber 2 keeps away from the high temperature area, so the waste material no longer continues to participate in the reaction, thereby guarantee that the raw materials in long brilliant chamber 3 distributes evenly, improve the sublimation rate of raw materials and the growth rate of crystal, make the feed gas in long brilliant chamber 3 keep unanimous at the growth in-process, reduce the crystal defect, be favorable to obtaining the even and no little polytype high quality silicon carbide crystal in surface.

As an embodiment, the top opening of the material chamber 1 communicates with the top opening of the waste chamber 2, and the plug flow mechanism transfers waste material to the waste chamber 2 through the top opening of the material chamber 1 and the top opening of the waste chamber 2. When graphitization phenomenon produced the waste material appears in the raw materials in raw materials chamber 1, the waste material gathering is at the top of raw materials, consequently, the open-top of the raw materials chamber of smooth plug flow mechanism accessible is directly shifted the waste material to the open-top of waste material chamber 2, reduce the operating time of smooth plug flow mechanism, improve the efficiency of getting rid of the waste material, further open-top of raw materials chamber 1 communicates with the open-top of waste material chamber 2, be in the reaction chamber all the time among the waste material transfer process, reduce the interference of waste material transfer process to the feed gas, stabilize the growth environment of crystal, can produce the higher crystal of quality. Preferably, the top opening of the material chamber 1 is aligned with the top opening of the waste chamber 2, thereby further improving the waste removal efficiency.

As an implementation mode, the raw material cavity 1 is sleeved on the periphery of the waste material cavity 2, the reaction cavity is formed by a reaction cavity inner cylinder 12 and a reaction cavity outer cylinder 11, the reaction cavity outer cylinder 11 is sleeved outside the reaction cavity inner cylinder 12, the raw material cavity 1 is formed between the reaction cavity outer cylinder 11 and the reaction cavity inner cylinder 12, and the reaction cavity inner cylinder 12 forms the waste material cavity 2. During crystal growth, heating device heats this reactor subassembly, and the lateral wall of reaction chamber urceolus 11 is heated this moment, and reaction chamber inner tube 12 sets up in reaction chamber urceolus 11 for high temperature region is kept away from in waste material chamber 2, and the plug flow mechanism shifts waste material in 1 raw materials chamber to waste material chamber 2, and the reaction is stopped promptly to the waste material, improves the growth quality of crystal.

Specifically, the outer reaction cavity barrel 11 is higher than the inner reaction cavity barrel 12, and the top of the outer reaction cavity barrel 11 is communicated with the crystal growth cavity 3. The top of reaction chamber urceolus 11 communicates with long brilliant chamber 3, makes the feed gas that produces in the raw materials chamber 1 directly enter into long brilliant chamber 3 and carry out long brilliant, realizes the intercommunication in raw materials chamber 1 and waste material chamber 2 at the top opening part of reaction chamber inner tube 12, is favorable to transferring waste material chamber 2 from raw materials chamber 1 directly, guarantees feed gas smooth transfer to long brilliant chamber 3, accelerates the growth of crystal.

Specifically, the reaction chamber inner tube 12 with the setting of 11 coaxial centers on the axis of reaction chamber urceolus is favorable to heating device even to raw materials chamber 1, guarantees that the raw materials in raw materials chamber 1 is unanimous to be heated, improves the sublimation rate of raw materials, promotes the growth quality of crystal, and the graphitization degree of raw materials is unanimous in raw materials chamber 1, but the concordance of plug flow mechanism gets rid of the waste material, reduces the number of times of operation of plug flow mechanism.

As an implementation mode, the ratio of the diameter of the reaction cavity outer cylinder 11 to the diameter of the reaction cavity inner cylinder 12 is 1.5-3:1, preferably 2:1, when the diameter of the reaction cavity outer cylinder 11 and the diameter of the reaction cavity inner cylinder 12 are less than 1.5:1, the distance between the reaction cavity outer cylinder 11 and the reaction cavity inner cylinder 12 is too small, the carbonization speed of the raw material in the raw material cavity 1 is increased, the raw material is easily carbonized seriously, and the quality of crystals is influenced; when the diameter of the reaction cavity outer cylinder 11 and the diameter of the reaction cavity inner cylinder 12 are larger than 3:1, the distance between the reaction cavity outer cylinder 11 and the reaction cavity inner cylinder 13 is too large, so that the raw material in the raw material cavity 1 is heated unevenly, and the carbonization degree of the raw material close to the side wall of the raw material cavity 1 is larger than that of the raw material positioned in the middle of the raw material cavity 1, so that the carbonization degrees of the raw material are inconsistent, and the defects of crystals are increased.

As an implementation mode, the distance D between the inner reaction chamber cylinder 12 and the outer reaction chamber cylinder 11 is 20-200mm, preferably 50-100mm, and this arrangement mode is favorable for the heating mechanism to heat the raw material chamber 1, and ensures that the raw material in the raw material chamber 1 is heated uniformly and carbonized to a uniform extent, so that the generation rate of the generated waste material is relatively uniform, and the flat plug flow mechanism is favorable for uniformly removing the waste material.

As an implementation mode, the device further comprises a feeding mechanism, the feeding mechanism comprises a material bearing table 51 which is arranged in the raw material cavity 1 and bears the raw material, and the feeding mechanism can control the material bearing table 51 to drive the raw material to move towards the direction close to the gas phase transmission channel. The material bearing platform 51 can drive the raw material in the raw material cavity 1 to move towards the direction close to the gas phase transmission channel, and the horizontal plug flow mechanism can transfer the waste material to the waste material cavity 2 at the joint of the raw material cavity 1 and the crystal growth cavity 3.

As an implementation mode, long brilliant chamber 3 sets up in the reaction chamber top, the raw materials gas upwards transmits to long brilliant chamber 3 from the reaction chamber and carries out the crystal growth, the open-top department of raw materials chamber 1 is the high temperature region this moment, through holding platform 51 with the raw materials in the raw materials chamber 1 continuous push to the high temperature region, the raw materials that is located the high temperature region sublimate and carry out the crystal growth, and the plug flow mechanism constantly gets rid of the waste material totally, make the raw materials carbonization in raw materials chamber 1 even, avoid partial raw materials to recrystallize on raw materials center upper portion, improve the utilization ratio of raw materials, increase the raw materials volume of participating in the sublimation, be favorable to growing out the heavier crystal of weight. Specifically, the high temperature zone is the highest temperature zone in the reactor assembly, and the reaction chamber outer cylinder 11 is heated by an induction coil.

As an embodiment, the horizontal plug flow mechanism comprises a material pushing member 41 and a connecting rod 42 connected with the material pushing member 41, the material pushing member 41 is arranged in the gas phase transmission channel, and the connecting rod 42 controls the material pushing member 41 to push the raw material surface layer waste material with a target area and thickness into the waste material cavity 2. The material bearing platform 51 drives the raw materials to move towards the top opening of the raw material cavity 1, the waste materials in the raw material cavity 1 are moved out of the raw material cavity 1, the waste materials moved out of the raw material cavity 1 are raw material surface layer waste materials, and the movement of the material pushing piece 41 is controlled through the connecting rod 42, so that the raw material surface layer waste materials of a target area and a thickness are pushed into the waste material cavity 2. Through the relative position of adjustment pushing member 41 and raw materials chamber 1, the thickness of the raw materials top layer waste material that steerable will get rid of to the volume of getting rid of waste material in the control is to raw materials chamber 1, ensures to get rid of the waste material totally, and avoids getting rid of the even raw materials that distribute, guarantees that the gaseous phase component of raw materials is even, improves the growth quality of crystal.

As an embodiment, the pushing element 41 is a baffle, the baffle is disposed on the top of the crystal growth chamber 3, and the connecting rod 42 can rotate to drive the baffle to rotate, so as to push the raw material surface layer waste into the waste chamber 2. Specifically, the baffle setting is at the top opening part of reaction chamber inner tube 12, through the rotation of second control mechanism control connecting rod 42 to it is rotatory to drive the baffle, in order to promote the raw materials top layer waste material in raw materials chamber 1 to waste material chamber 2. According to the reaction cavity inner barrel 12 and the reaction cavity outer barrel 11 with different sizes, the movement speed of the material bearing platform 51 and the rotation speed of the connecting rod 42 are reasonably determined so as to ensure that waste materials in the raw material cavity 1 are removed completely. Connecting rod 42 drives the baffle and is in the rotation state always, can in time get rid of the waste material that raw materials chamber 1 produced totally, also can reduce the interference to the feed gas simultaneously, avoids influencing the gaseous phase transmission of feed gas, stabilizes the growth environment of crystal, further improves the quality of crystal.

As an implementation manner, the ratio of the distance from the pushing member 41 to the bottom end of the raw material chamber 1 to the distance from the pushing member 41 to the bottom end of the waste material chamber 2 is 3-5: 7-10, pushing material 41 removes the waste material to waste material chamber 2 after, in order to make the waste material keep away from the high temperature area, no longer continue to be heated and sublimate, consequently set up and push away the distance that material 41 will be greater than pushing away the distance that material 41 will be apart from raw materials chamber 1 from 2 bottoms in waste material chamber, and for the convenience of reactor subassembly, this distance ratio should not be too big yet, this distance can guarantee that the waste material shifts to waste material chamber 2 after can not continue to be heated and sublimate again, avoid waste material sublimation to influence the quality of crystal, if pushing away the distance overlength of material 41 distance waste material chamber 2, waste material chamber 2 keeps away from the high temperature area, waste material chamber 2 bottom temperature reduces, make the raw material gas sink to waste material chamber 2's bottom along with temperature gradient, lead to the raw material gas of seed crystal 32 department not enough, influence the crystal growth speed of crystal, still can lead to the crystal to appear serious dislocation, microtubule and polytype. But also can make the reactor assembly flexible and convenient and improve the universality of the reactor assembly. Preferably, the ratio of the distance from the pushing member 41 to the bottom end of the raw material cavity 1 to the distance from the pushing member 41 to the bottom end of the waste material cavity 2 is 3: 10.

As an implementation mode, the distance between the pushing piece 41 and the top of the reaction chamber and the distance between the pushing piece 41 and the seed crystal 32 are 3-10: 90-200, and the distance between the pushing piece 41 and the top of the reaction cavity and the distance between the pushing piece 41 and the seed crystal 32 are preferably 3: 200. The pushing piece 41 is far away from the seed crystal 32, so that the fine particles generated in the waste removing process can be ensured not to be directly transmitted to the seed crystal 32, the quality of the crystal is influenced, even a small amount of fine particles are generated in the waste removing process, the fine particles are doped in the feed gas, the fine particles are further heated and decomposed in the gas phase transmission channel, the fine particles are quickly transmitted to the seed crystal 32 in a gas phase form to start crystal growth, the transmission path of the fine particles is prolonged, the interference of the fine particles to the crystal growth process is reduced, and the formation of an inclusion is avoided.

Specifically, the fine particles refer to raw materials which are not carbonized and uniformly distributed, and because the particle size and weight of the waste are relatively large, the raw materials which are not carbonized inevitably come into contact with the waste materials in the process of removing the waste materials, and therefore the raw materials which are not carbonized may fly upward to become fine particles to be doped in the raw material gas.

In one embodiment, the number of the baffles is at least two, at least two baffles are uniformly distributed on the circumference of the connecting rod 42, the included angle between two adjacent baffles is 40-120 degrees, and preferably, the angle between two adjacent baffles is 60-90 degrees. If the number of the baffles is too large, the angle between two adjacent baffles is too small, so that waste materials are easy to fly in material removal, and gas flow of raw material gas is caused to influence a crystal growth environment; if the number of the baffles is too small, the angle between every two adjacent baffles is too large, the material removing effect is poor, and the crystal defects are increased. The angle can ensure that the waste in the raw material cavity is smoothly and cleanly removed, the gas phase transmission of the raw material gas cannot be influenced, the growth environment of the crystal is stabilized, and the growth quality of the crystal is further improved.

Optionally, the width of the baffle is 50-100mm, the height of the baffle is 2-10mm, the width of the baffle can ensure that the waste can be completely moved to the waste cavity to the maximum extent, and the baffle cannot scratch the inner side wall of the outer cylinder 11 of the reaction cavity, the width of the baffle is too wide, the reactor is easily scratched, the long-term use of the reactor is not facilitated, and the long-crystal environment can be stabilized; the height of baffle can guarantee to scrape into waste material chamber 2 completely with the waste material, avoids the waste material too much, causes the waste material to get rid of unclean to lead to the waste material to mix in the feed gas, and then influence the quality of crystal. Preferably, the width of the baffle is 70-80mm, the height of the baffle is 3-5mm, the baffle is too narrow, waste materials are prone to being removed incompletely, the baffle is too wide, gas flow is prone to being generated in material removal, the growth environment of crystals is disturbed, and the growth quality of the crystals can be optimal due to the width of the baffle of 3-5 mm.

As an implementation mode, a preformed hole 43 is formed at the bottom of the waste material cavity 2, and the connecting rod 42 penetrates through the preformed hole 43 to be connected with the baffle so as to control the baffle to rotate. Set up the preformed hole 43 that supplies connecting rod 42 to pass in the bottom of reaction chamber inner tube 12, connecting rod 42 is connected with the baffle through preformed hole 43, the size of preformed hole 43 and connecting rod 42's shape looks adaptation, can restrict connecting rod 42's motion through preformed hole 43, avoid connecting rod 42 to appear driving the baffle and appear squinting, ensure that the baffle only promotes the waste material of target area and thickness when promoting the waste material and promote to waste material chamber 2, avoid the waste of raw materials, further practice thrift manufacturing cost.

As an embodiment, the preformed hole 43 is arranged at the center of the waste material chamber 2, the baffle is positioned on the same plane with the top openings of the raw material chamber 1 and the waste material chamber 2, and the baffle can contact the inner side wall of the reaction chamber outer barrel 11. Preformed hole 43 sets up the central point at reaction chamber inner tube 12 and puts to baffle and waste material chamber 2 flush with the open-top of former feed chamber 1, are convenient for promote the waste material at 1 top of former feed chamber to waste material chamber 2, and the length of baffle extends to reaction chamber urceolus 11 from reaction chamber inner tube 12, can guarantee to get rid of the waste material completely.

Specifically, the number of baffles can be one, can be a plurality of, in order to improve the efficiency of removing material of plug flow mechanism, the preferred number of baffles sets up to 2-5, and the connecting rod 42 is rotatory to drive a plurality of baffles rotatory, and high efficiency gets rid of the waste material totally.

Referring to fig. 2-3, as an embodiment, the pushing element 41 is a baffle plate, the baffle plate is disposed at the top of the reaction chamber, and the connecting rod 42 is capable of extending and contracting, and is configured to control the baffle plate to move along the direction from the raw material chamber 1 to the waste material chamber 2, so as to push the raw material surface layer waste material into the waste material chamber 2. Specifically, the baffle setting is on the inside wall of reaction chamber urceolus 11 to be located the open-top portion of former feed chamber 1, connecting rod 42 is flexible, drives the baffle and moves to waste material chamber 2 from the inside wall of reaction chamber urceolus 11, promotes the raw materials top layer waste material in 1 former feed chamber to waste material chamber 2. The number of times of extension and contraction of the link 42 is determined according to the moving speed of the material-receiving table 51 to control the removal speed of the scrap. In the arrangement mode, after the material bearing platform 51 drives the raw material in the raw material cavity 1 to move for a certain distance, the first control mechanism controls the connecting rod 42 to extend out, the connecting rod 42 drives the baffle plate to push the waste material to the waste material cavity 2, and after the waste material is removed, the first control mechanism controls the connecting rod 42 to retract to drive the baffle plate to reset; after the material bearing table 51 drives the raw material in the raw material chamber 1 to move continuously to a certain distance, the connecting rod 42 continues to drive the push plate to repeat the above movement.

In a preferred embodiment, the shape of the baffle is matched with the shape of the outer reaction chamber cylinder 11, the shapes of the outer reaction chamber cylinder 11 and the inner reaction chamber cylinder 12 are circular, and the baffle is provided in the shape of an arc plate, and the arc plate has the same radian as the outer reaction chamber cylinder 11. In order to guarantee to get rid of raw materials top layer waste material totally, the baffle is that quantity sets up to a plurality ofly, and the quantity of connecting rod 42 is the same with the quantity of baffle, and when the baffle promoted waste material to waste material chamber 2, a plurality of baffles alternately promoted, guarantee to push away to waste material chamber 2 with the waste material at raw materials chamber 1 top is whole.

As a preferred embodiment, the connecting rod 42 can rotate horizontally to drive the baffle to rotate a certain angle in the horizontal direction, so that the baffle can push more waste materials, and the number of the baffles can be reduced, and when a plurality of baffles are reset, gaps can exist between the baffles, and the baffles can push the waste materials to the waste material cavity 2 at the same time.

As an implementation mode, the feeding mechanism further comprises a push rod 52, the push rod 52 penetrates through the bottom of the raw material cavity 1 to be connected with the material bearing platform 51, and the push rod 52 is used for pushing the material bearing platform 51 to move towards the direction close to the gas phase transmission channel. The push rod 52 is arranged between the reaction cavity inner cylinder 12 and the reaction cavity outer cylinder 11, the third control mechanism controls the movement of the push rod 52, and the push rod 52 pushes the material bearing platform 51 to move towards the direction close to the gas phase transmission direction, so that the raw materials can be pushed smoothly. Preferably, the distance between the push rod 52 and the inner barrel 12 or the outer barrel 11 of the reaction chamber is equal, so that the balance of the material bearing platform 51 is maintained in the pushing process, the raw materials are uniformly distributed, and the quality of the crystal is improved.

As an embodiment, the bottom in waste material chamber 2 is less than the bottom in former feed chamber 1, and under this mode of setting, the waste material enters into waste material chamber 2, and the top in former feed chamber 1 is the high temperature area, is heated at the high temperature area raw materials and sublimates and carries out the long crystal, and the bottom in waste material chamber 2 will be less than the bottom in former feed chamber 1 for the high temperature area is kept away from to the waste material, can not continue to be heated again and participate in the long crystal reaction, avoids the waste material sublimation to lead to the crystal defect to appear, improves the growth quality of crystal.

As an implementation mode, the porous graphite plate 31 is arranged in the gas phase transmission channel, the feed gas passes through the porous graphite plate 31 and enters the crystal growth cavity 3, part of fine particles enter the crystal growth cavity 3 along with the feed gas in the sublimation of the feed gas, the fine particles can cause the crystal to have defects, the plug flow mechanism is used for removing the material, the arrangement of the porous graphite plate 31 can prevent the fine particles in the waste from being driven by the feed gas to the seed crystal in the crystal growth cavity 3 to grow the crystal, the growth environment of the crystal is stabilized, the defects of polytype, dislocation, microtubes, inclusion bodies and the like in the production process of the crystal are avoided, and the quality of the crystal is further improved.

Example 2

Referring to fig. 4, the present embodiment is different from embodiment 1 in that a waste chamber 2 is sleeved on the periphery of the raw material chamber 1, the waste chamber 2 is formed between a reaction chamber outer cylinder 11 and a reaction chamber inner cylinder 12, and the reaction chamber inner cylinder 12 forms the raw material chamber 1. Under this setting mode, 1 top in raw materials chamber is the high temperature area, and the raw materials sublimation is long brilliant, and the plug flow mechanism in time gets rid of the waste material in the raw materials chamber 1 for the waste material falls into the bottom in waste materials chamber 2, and the high temperature area is kept away from to the waste material this moment, can't continue to be heated and sublimate, avoids the waste material to cause crystal defect, further improves the growth quality of crystal.

As an embodiment, the material bearing platform 51 pushes the raw material in the raw material chamber 1 to a direction close to the gas phase transmission channel, the outer cylinder 11 of the reaction chamber is higher than the inner cylinder 12 of the reaction chamber, and the baffle timely pushes the waste material on the surface layer of the raw material in the raw material chamber 1 to the waste material chamber 2.

Specifically, the link 42 may also drive the baffle to move by rotating or stretching, and when the link 42 stretches and stretches to drive the baffle to move, the baffle and the link 42 may be arranged in the same manner as in embodiment 1. When the connecting rod 42 rotates to drive the baffle to move, the connecting rod 42 can be arranged at the top of the reaction chamber inner cylinder 12, at this time, the length of the baffle at least extends from the connecting rod 42 to the outer side wall of the reaction chamber inner cylinder 12, preferably, the length of the baffle extends from the connecting rod 42 to the opening at the top of the waste material chamber 2, so that the waste material can be completely pushed to the waste material chamber 2; the connecting rod 42 can also be arranged at the bottom of the reaction cavity outer cylinder 11, when the number of the connecting rod 42 and the baffle is one, the length of the baffle at least contacts with the upper end surface of the whole reaction cavity inner cylinder 12, when the number of the connecting rod 42 and the baffle is a plurality of, the length of the baffle at least can extend to the central axis of the reaction cavity inner cylinder 12 from the connecting rod 42, and the two arrangement modes are beneficial to removing the waste materials at the top of the reaction cavity completely and further improving the growth quality of crystals.

Example 3

In an embodiment which is not shown, a raw material cavity 1 is formed between a reaction cavity outer barrel 11 and a reaction cavity inner barrel 12, a waste material cavity 2 is arranged at the bottom, the top or the outer side of the raw material cavity 1, the porosity of the surface of the reaction cavity inner barrel 12 is higher than that of the surface of the reaction cavity outer barrel 11, a seed crystal is arranged in the reaction cavity inner barrel 12 in a column mode, the extending direction of the central axis of the seed crystal is approximately the same as that of the reaction cavity inner barrel 12, a crystal growing cavity 3 is formed between the seed crystal and the inner side wall of the reaction cavity inner barrel 12, and a heating device is arranged at the outer side of the reaction cavity outer barrel 11, so that raw material gas in the raw material cavity 1 passes through the reaction cavity inner barrel 12 to reach the crystal growing cavity 3 for crystal growing. The seed crystal is arranged in the inner barrel 12 of the reaction cavity, which is favorable for preparing the crystal with larger thickness, and the waste material in the reaction cavity is timely and cleanly removed through the plug flow mechanism, thereby being favorable for improving the quality of the crystal, reducing the defects of the silicon carbide crystal and being favorable for the large-scale production of the silicon carbide crystal.

Example 4

A method of preparing a silicon carbide crystal, comprising:

providing a reaction cavity, a crystal growth cavity and a plug flow mechanism, wherein the reaction cavity comprises a raw material cavity and a waste material cavity, and silicon carbide raw materials are filled into the raw material cavity;

crystal growth stage: the control is grown brilliant the condition, the feed gas that the raw materials sublimation in the raw materials intracavity produced is transmitted to growing brilliant chamber through gaseous phase transmission passageway and is grown the brilliant, when carborundum raw materials sublimation rate is first sublimation rate, starts the plug flow mechanism, the plug flow mechanism will the waste material that produces after the reaction intracavity raw materials sublimation shifts to the waste material chamber, the surplus raw materials of raw materials intracavity continues to sublimate under this long brilliant condition and carries out the growth brilliant, and the plug flow mechanism is continuously removed the material and is ended to growing brilliant, makes promptly carborundum crystal.

Preferably, a method for preparing silicon carbide crystals comprises the following steps:

(1) the reactor assembly of example 1 was used to prepare crystals by placing the feedstock chamber, the waste chamber, and the growth chamber into which the silicon carbide feedstock was charged in a crystal growth furnace flush with the feedstock chamber and sealed; the ratio of the distance from the pushing piece to the bottom end of the raw material cavity to the distance from the bottom end of the waste material cavity is 3:10, and the ratio of the distance from the pushing piece to the top of the reaction cavity to the distance from the seed crystal is 3: 200; the diameter ratio of the outer barrel of the reaction cavity to the inner barrel of the reaction cavity is 2:1, the angle between two adjacent baffles is 60 degrees, the width of each baffle is 75mm, and the height of each baffle is 5 mm.

(4) crystal growth stage: reducing the pressure in the furnace body to 5 x 10²Pa-2×10³The temperature in the furnace body is increased to 2300-2800K within Pa, 5-10h, and the growth time is 0-3 h; when the sublimation rate of the silicon carbide raw material is not less than 0-5%, starting a plug flow mechanism, transferring waste materials generated after the raw material in the reaction cavity is sublimated to a waste material cavity through the plug flow mechanism, continuously sublimating the residual raw material in the raw material cavity for crystal growth, and removing the materials at a constant speed by the plug flow mechanism, wherein the material removing frequency is 1-100 times/h, and the growth time is 50-150 h;

The reactor used in the preparation method is a preferred embodiment among embodiments of the present application, with reference to fig. 1.

The differences between the specific preparation method of 2200g of silicon carbide raw material used for preparing silicon carbide single crystal # 1-4 and the comparative silicon carbide single crystal # D1-D5 according to the above method are shown in Table 1.

TABLE 1

Structural defects such as crystal micropipes, polytypes, dislocations, inclusions and the like of the prepared silicon carbide single crystal 1# -4# and the comparative silicon carbide single crystal D1# -D5# were detected, and the weights thereof were weighed, and the detection results are shown in table 2.

TABLE 2

From the results of tables 1 and 2, it can be seen that:

1. the preparation condition of the silicon carbide single crystal 1# is that the silicon carbide single crystal obtained by growth after a group of crystal growth parameters are optimized and combined, the quality of the single crystal is best, and the defects of the crystal are least.

2. The silicon carbide single crystals 2# and 3# and the comparative silicon carbide single crystal D1# improve the first sublimation rate of the silicon carbide raw material on the basis of the silicon carbide single crystal 1#, the higher the first sublimation rate is, the higher the initial carbonization degree of the raw material is increased, and therefore a part of waste materials can affect the crystals, and related defects are correspondingly increased.

3. On the basis of the silicon carbide single crystal 1#, the moving speed of the bearing table of the silicon carbide single crystal 4# is adjusted to 1cm/h from 0.2cm/h, the defects of the produced crystal are increased, and the weight of the crystal is reduced, because the moving speed of the bearing table driving the raw material is increased, the amount of waste materials removed by the plug flow mechanism is increased, and a part of the carbonized raw material is moved to a waste material cavity, so that the weight of the crystal is reduced; meanwhile, the amount of the removed waste materials is increased, so that tiny waste material particles are easily doped in the gas phase transmission channel in the material removing process of the plug flow mechanism, and the crystal defects are increased.

4. Compared with the silicon carbide single crystal D2#, on the basis of the silicon carbide single crystal 1#, the bearing table is not used for driving the raw material to move, and the material removal is not carried out by using a plug flow mechanism, so that the quality of the grown single crystal is obviously deteriorated, and the corresponding defects are obviously increased; compared with the silicon carbide single crystal D3#, on the basis of the silicon carbide single crystal 1#, only the bearing table is used for driving the raw material to move, the material is not removed by the plug flow mechanism, and partial waste material can automatically fall into the waste material cavity in the moving process of the raw material, so that the crystal quality of the D3# is slightly higher than that of the D2# but still lower than that of the silicon carbide single crystal 1# -4 #.

5. Compared with the silicon carbide single crystal D4#, on the basis of the silicon carbide single crystal 1#, the rotating speed of the connecting rod is adjusted from 50 revolutions per hour to 400 revolutions per hour, the material removing frequency of the plug flow mechanism is increased, and the faster the material removing frequency is, the more waste material particles in a gas phase transmission channel are increased, so that the crystal growing environment of the crystal is unstable, and the defects of the crystal are increased.

6. Compared with the silicon carbide single crystal D5#, on the basis of the silicon carbide single crystal 1#, the growth temperature of the crystal is adjusted from 2450K to 2300K, the moving speed and the material removing frequency of the raw material are not changed, so that a part of the raw material still exists in the waste material, the utilization rate of the raw material is reduced, and the weight of the crystal is reduced; further, the particle size of the waste material particles is generally larger than that of the uniform silicon carbide raw material, so that the removal of the raw material in the presence of the raw material in the waste material results in that a part of the raw material is doped in the form of particles in the raw material gas, thereby causing a significant increase in crystal defects.

Example 5

The silicon carbide single crystal was produced by changing the parameters of the reactor components in accordance with the above-mentioned method # 1 for producing a silicon carbide single crystal, using 2200g of the specific parameters of the reactor components as the silicon carbide raw material, except as shown in Table 3.

TABLE 3

Structural defects such as micropipes, polytypes, dislocations, inclusions and the like of the prepared silicon carbide single crystals 1#, 5#, 6# and comparative silicon carbide single crystals D6# -D10# were detected, and the weights thereof were weighed, and the detection results are shown in table 4.

TABLE 4

From the results of tables 3 and 4, it can be seen that:

2. The ratio of the distance from the pushing piece to the bottom end of the raw material cavity to the distance from the pushing piece to the bottom end of the waste material cavity is too small, and after the waste materials are transferred to the waste material cavity, a part of the waste materials still can be sublimated to participate in crystal growth, so that the quality of crystals is reduced; the ratio is too large, which causes insufficient atmosphere of raw material gas at the seed crystal, influences the crystal growth speed of the crystal and causes defects of the crystal.

3. When the pushing piece is close to the seed crystal, fine particles in a part of waste materials participate in crystal growth along with the feed gas in the material removing process, and the fine particles participate in crystal growth without further thermal decomposition due to the fact that the fine particles are short along with the transmission path of the feed gas, so that the quality of crystals is reduced.

4. The ratio of the diameter of the outer barrel of the reaction cavity to the diameter of the inner barrel of the reaction cavity is too large, so that the distance between the raw material cavities is too large, the carbonization degree of the raw materials in the raw material cavities is inconsistent, and the defects of crystals are increased.

The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments. In particular, for the system embodiment, since it is substantially similar to the method embodiment, the description is simple, and for the relevant points, reference may be made to the partial description of the method embodiment.

The above description is only an example of the present application and is not intended to limit the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.

Claims

1. A reactor assembly for PVT process crystal production comprising:

2. The reactor assembly as claimed in claim 1, wherein the plug flow mechanism comprises a pushing member and a connecting rod connected with the pushing member, the pushing member is arranged in the gas phase transmission channel, and the connecting rod controls the pushing member to move the raw material surface layer waste material with a target area and thickness into the waste material cavity.

3. The reactor assembly of claim 2, wherein the pusher is disposed at a top of the reaction chamber,

the ratio of the distance from the pushing piece to the bottom end of the raw material cavity to the distance from the pushing piece to the bottom end of the waste material cavity is 3-5: 7-10; and/or

The distance between the pushing piece and the top of the reaction cavity and the distance between the pushing piece and the seed crystal are 3-10: 90-200.

4. The reactor assembly as set forth in claim 2 wherein the pusher is a baffle;

5. The reactor assembly as set forth in claim 4 wherein the tie rod rotates clockwise or counterclockwise and the direction of rotation of the tie rod is unchanged.

6. The reactor assembly as set forth in claim 4 wherein the number of baffles is at least two, at least two of the baffles being evenly distributed along the circumference of the tie rod, the angle between adjacent two of the baffles being 40-120 °.

7. The reactor assembly as set forth in claim 6 wherein the angle between adjacent two of the baffles is between 60 ° and 90 °.

8. The reactor assembly as claimed in claim 6, wherein the width of the baffle is 50-100mm and the height of the baffle is 2-10 mm.

9. The reactor assembly as claimed in claim 8, wherein the width of the baffle is 70-80mm and the height of the baffle is 3-5 mm.

10. The reactor assembly as claimed in claim 1, further comprising a feeding mechanism, wherein the feeding mechanism comprises a material supporting platform disposed in the material chamber and supporting the material, and the feeding mechanism is capable of controlling the material supporting platform to move the material toward the gas phase transport channel.

11. The reactor assembly of claim 10, wherein the feeding mechanism further comprises a push rod, the push rod penetrates through the bottom of the raw material chamber to be connected with the material bearing platform, and the push rod is used for pushing the material bearing platform to move towards the direction close to the gas phase transmission channel.

12. The reactor assembly of any one of claims 1-11, wherein the top opening of the feedstock chamber is in communication with the top opening of the waste chamber, and the plug flow mechanism pushes the waste material to the waste chamber through the top opening of the feedstock chamber and the top opening of the waste chamber.

13. The reactor assembly as set forth in claim 12 wherein the feed material chamber is disposed about the periphery of the waste chamber.

14. The reactor assembly as claimed in claim 12, wherein the reaction chamber is formed by an inner reaction chamber cylinder and an outer reaction chamber cylinder, and the outer reaction chamber cylinder is sleeved outside the inner reaction chamber cylinder;

the raw material cavity is formed between the reaction cavity outer cylinder and the reaction cavity inner cylinder, and the reaction cavity inner cylinder forms the waste cavity.

15. The reactor assembly as set forth in claim 14 wherein the inner reaction chamber cylinder is disposed coaxially with the outer reaction chamber cylinder, the outer reaction chamber cylinder being higher than the inner reaction chamber cylinder;

the crystal growth cavity is connected with the top of the reaction cavity outer barrel.

16. A method of using the reactor assembly of any of claims 1-15, comprising:

a preparation stage: charging the feedstock into the feedstock chamber;

crystal growth stage: and controlling the crystal growth temperature and the crystal growth pressure of the raw material cavity, transmitting the raw material gas generated by heating and sublimating the raw material in the raw material cavity to the seed crystal through the gas phase transmission channel to start crystal growth, starting the plug flow mechanism to continuously move the waste materials in the crystal growth process in the raw material cavity to the waste material cavity until the crystal growth is finished.

17. The method as claimed in claim 16, wherein the crystallization temperature is 2300-²Pa-2×10³And Pa, when the sublimation rate of the raw material in the raw material cavity reaches 0-5% in the crystal growth stage, starting the plug flow mechanism, and moving the waste material to the waste material cavity at a constant speed by the plug flow mechanism.

18. Use of a reactor assembly as defined in any one of claims 1 to 15 in the preparation of silicon carbide crystals.