CN114561693A - Single crystal growing apparatus - Google Patents

Single crystal growing apparatus Download PDF

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Publication number
CN114561693A
CN114561693A CN202210136243.2A CN202210136243A CN114561693A CN 114561693 A CN114561693 A CN 114561693A CN 202210136243 A CN202210136243 A CN 202210136243A CN 114561693 A CN114561693 A CN 114561693A
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China
Prior art keywords
crucible
inner crucible
atmosphere
single crystal
side wall
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Granted
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CN202210136243.2A
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Chinese (zh)
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CN114561693B (en
Inventor
李远田
陈俊宏
吴亚娟
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Jiangsu Jixin Advanced Materials Co ltd
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Jiangsu Jixin Semiconductor Silicon Research Institute Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/36Carbides
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B23/00Single-crystal growth by condensing evaporated or sublimed materials
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B23/00Single-crystal growth by condensing evaporated or sublimed materials
    • C30B23/002Controlling or regulating
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention discloses a single crystal growing apparatus, comprising: the outer crucible defines a growth cavity, and the top wall of the growth cavity is provided with seed crystals; the first inner crucible is arranged in the growth cavity, the first inner crucible and the seed crystal are arranged oppositely along the axial direction, one end of the first inner crucible, facing the seed crystal, is open, the outer side wall of the first inner crucible is spaced from the inner side wall of the outer crucible to define an air outlet flow channel, and the first inner crucible is used for containing silicon carbide raw materials; the second inner crucible is arranged in the growth cavity and located on one side, away from the seed crystal, of the first inner crucible, one end, facing the first inner crucible, of the second inner crucible is open, the second inner crucible is suitable for containing silicon materials used for generating compensation atmosphere or doping agents used for generating doping atmosphere, and the second inner crucible is suitable for moving between the first position and the second position to communicate or separate the gas flow channel and the inner cavity of the second inner crucible. According to the single crystal growing apparatus of the present invention, the continuity of the silicon carbide crystal growing process can be improved.

Description

Single crystal growing apparatus
Technical Field
The invention relates to the technical field of silicon carbide crystal growth, in particular to a single crystal growth device.
Background
In a process for preparing a silicon carbide crystal by a PVT (physical vapor transport) method, a compensation atmosphere or a doping atmosphere is generally required to be provided for the crystal according to the kind of the crystal to be prepared and the growth process of the crystal, but in the existing process, because the structure of single crystal growth equipment is complex, the growth continuity of the crystal is easily reduced for realizing atmosphere compensation, and the growth efficiency of the crystal is low.
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 single crystal growing device which can realize the compensation of growing atmosphere in the growing process, thereby realizing the continuity of the growing process of the silicon carbide crystal and improving the crystal quality.
The single crystal growing apparatus according to the present invention comprises: the outer crucible defines a growth cavity, and the top wall of the growth cavity is provided with seed crystals; the first inner crucible is arranged in the growth cavity and is opposite to the seed crystal in the axial direction, one end of the first inner crucible facing the seed crystal is open, the outer side wall of the first inner crucible is spaced from the inner side wall of the outer crucible to define a gas flow channel, and the first inner crucible is used for containing silicon carbide raw materials; the second inner crucible is arranged in the growth cavity and is arranged on one side of the first inner crucible, which is far away from the seed crystal, the end of the second inner crucible facing the first inner crucible is open, the second inner crucible is suitable for containing silicon material for generating compensation atmosphere or dopant for generating doping atmosphere, wherein the second inner crucible is adapted to be moved between a first position and a second position, wherein, in the first position, at least part of the side wall of the second inner crucible is embedded in the gas flow channel so as to separate the inner cavity of the second inner crucible from the gas flow channel, in the second position, the second inner crucible is axially spaced from the first inner crucible, so that the inner cavity of the second inner crucible is communicated with the gas flow channel, and the compensation atmosphere or the doping atmosphere flows to the seed crystal through the gas flow channel.
According to the single crystal growing device, the first inner crucible suitable for containing the silicon carbide raw material and the second inner crucible suitable for containing the silicon material or the doping agent are arranged in the outer crucible, and the air outlet channel is defined between the first inner crucible and the outer crucible, so that when the silicon carbide atmosphere or doping is required to be supplemented in the growing process of the seed crystal, the air flow channel can be controlled to be communicated with the inner cavity of the second inner crucible, the compensation atmosphere or the doping atmosphere generated by the second inner crucible is transferred to the seed crystal through the air flow channel, the compensation of the growing atmosphere in the growing process is realized, the continuity of the growing process of the silicon carbide crystal is improved, and the silicon carbide crystal with qualified quality and variety is prepared.
Further, the single crystal growing apparatus further includes: the connecting piece, the connecting piece is located airflow channel, the connecting piece forms to follow the cyclic annular that the circumference of first interior crucible extends, the inner wall of connecting piece with the outer wall of first interior crucible links to each other, the outer wall of connecting piece with the inner wall of outer crucible links to each other, be formed with a plurality of blow vents that run through along the thickness direction on the connecting piece, it is a plurality of the blow vent with airflow channel intercommunication and edge the circumference interval arrangement of connecting piece.
In some embodiments, a portion of the side wall of the second inner crucible adjacent to the top end is formed with a blocking portion, the blocking portion is formed in a ring shape extending along the circumferential direction of the first inner crucible, the width of the blocking portion in the radial direction is adapted to the width of the gas flow passage, and when the second inner crucible is in the first position, the blocking portion is positioned in the gas flow passage to block the gas flow passage and the inner cavity of the second inner crucible.
Further, a heat conducting portion is formed at the bottom end of the first inner crucible, the heat conducting portion is in a circular truncated cone shape, the diameter of the heat conducting portion is matched with the inner diameter of the blocking portion, and when the second inner crucible is located at the first position, the inner side wall of the blocking portion is in sealing fit with the outer side wall of the heat conducting portion.
In a specific example, the thickness of the stopper portion in the axial direction of the outer crucible is not more than the thickness of the heat conductive portion.
According to some embodiments of the invention, a portion of the side wall of the second inner crucible located below the stopper is spaced from the inner side wall of the outer crucible to form a filling cavity adapted to be filled with insulation.
According to some embodiments of the invention, the bottom end of the outer crucible is open to form a mounting opening, and the second inner crucible is adapted to close off the mounting opening.
Further, the second inner crucible includes: the material containing part is positioned on the inner side of the outer crucible, the material containing part is formed into a cylinder with an open top end, the material containing part is used for containing the silicon material or the dopant, when the second inner crucible is at the first position, at least part of the side wall of the material containing part is embedded in the airflow channel, the inner cavity of the material containing part is isolated from the airflow channel, when the second inner crucible is at the second position, the material containing part is axially spaced from the first inner crucible, the inner cavity of the material containing part is communicated with the airflow channel, and the compensation atmosphere or the doping atmosphere flows to the seed crystal through the airflow channel; the supporting platform is located at the bottom end of the material containing portion, the outer diameter of the supporting platform is larger than that of the material containing portion, and when the material containing portion is located on the inner side of the outer crucible, the bottom end of the outer crucible is suitable for being supported on the supporting platform.
Still further, the outer diameter of the supporting platform is larger than that of the outer crucible, a matching part is further formed on the supporting platform, the matching part extends along the circumferential direction of the supporting platform and is spaced from the material containing part along the radial direction to form a slot, and the part, close to the bottom end, of the outer crucible is suitable for being inserted into the slot.
According to some embodiments of the invention, the single crystal growing apparatus further comprises: a drive device; one end of the first transmission shaft penetrates through the second inner crucible to be connected with the bottom of the first inner crucible, and the other end of the first transmission shaft is connected with the driving device; one end of the second transmission shaft is connected with the bottom of the second inner crucible, the other end of the second inner crucible is connected with the driving device, and the second transmission shaft is sleeved on the outer side of the first transmission shaft; the driving device is suitable for driving the first transmission shaft to drive the first inner crucible to move along the axial direction of the outer crucible, and the driving device is also suitable for driving the second transmission shaft to drive the second inner crucible to move between the first position and the second position.
According to some embodiments of the invention, the single crystal growing apparatus further comprises: and the flow guide piece is arranged on the first inner crucible and/or the connecting piece so as to guide the atmosphere in the airflow channel to the seed crystal.
Further, the baffle is formed as a baffle comprising: the first plate section is formed into a cylindrical shape with two open ends along the axial direction, one end of the first plate section in the axial direction is supported at the top end of the first inner crucible or the inner end of the connecting piece, a plurality of flow guide holes penetrating along the radial direction of the first inner crucible are formed in the first plate section, and the flow guide holes are communicated with the airflow channel; and the upper end of the second plate section is connected with the upper end of the first plate section, and the lower end of the second plate section is abutted against the inner side wall of the outer crucible and/or the outer end of the connecting piece.
According to some embodiments of the invention, the single crystal growing apparatus further comprises: a first heating element for heating the silicon carbide feedstock in the first inner crucible to cause sublimation of the silicon carbide feedstock by heating to produce a silicon carbide atmosphere, the silicon carbide atmosphere being adapted to migrate to the seed crystal; a second heating member for heating the silicon material or dopant in the second inner crucible to create a compensating atmosphere or a doping atmosphere adapted to migrate to the seed crystal through the gas flow channel.
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 one embodiment of a single crystal growing apparatus according to the present invention;
FIG. 2 is a cross-sectional view of the single crystal growing apparatus shown in FIG. 1;
FIG. 3 is a schematic view of another embodiment of a single crystal growing apparatus according to the present invention;
FIG. 4 is a cross-sectional view of the single crystal growing apparatus shown in FIG. 3;
FIG. 5 is a schematic view of yet another embodiment of a single crystal growing apparatus according to the present invention;
FIG. 6 is a cross-sectional view of the single crystal growing apparatus shown in FIG. 5;
FIG. 7 is a schematic view of yet another embodiment of a single crystal growing apparatus according to the present invention;
FIG. 8 is a schematic view of the assembly of the first inner crucible and the connecting piece according to an embodiment of the invention;
FIG. 9 is a schematic view of a second inner crucible of the single crystal growing apparatus shown in FIG. 5;
FIG. 10 is a schematic view of a second inner crucible of the single crystal growing apparatus shown in FIG. 7.
Reference numerals:
single crystal growth apparatus 100:
an outer crucible 1, a crucible body 11, a crucible cover 12, a graphite felt layer 121,
a first inner crucible 2, a heat conducting portion 21, a first transmission shaft 22, an air flow passage 23,
the connecting member 3, the vent port 31, the first fitting screw thread 32, the second fitting screw thread 33,
the flow guide member 4, the first plate section 41, the flow guide hole 411, the second plate section 42,
a second inner crucible 5, a blocking part 51, a third assembling thread 511, a material containing part 52, a supporting platform 53, a matching part 531, a slot 532, a second transmission shaft 54, a fourth assembling thread 55,
a first heating member 6, a second heating member 7, and a seed crystal 200.
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.
A single crystal growing apparatus 100 according to an embodiment of the present invention is described below with reference to fig. 1 to 10.
Referring to fig. 1 to 7, a single crystal growing apparatus 100 according to an embodiment of the present invention includes: an outer crucible 1, a first inner crucible 2 and a second inner crucible 5.
Wherein, outer crucible 1 prescribes a limit to the growth chamber, the roof in growth chamber is provided with seed crystal 200, first interior crucible 2 locates the growth intracavity of outer crucible 1, first interior crucible 2 and seed crystal 200 are along the axial relative arrangement of outer crucible 1, the one end of first interior crucible 2 towards seed crystal 200 opens in order to form first open mouth, be suitable for in the first interior crucible 2 to hold the carborundum raw materials, the carborundum raw materials is heated the sublimation and is in order to produce the carborundum atmosphere that supplies seed crystal 200 to grow, carborundum atmosphere flows to seed crystal 200 via first open mouth, the lateral wall of first interior crucible 2 is spaced apart in order to prescribe a limit to airflow channel 23 with the inside wall of outer crucible 1.
The second inner crucible 5 is arranged in the growth chamber, the second inner crucible 5 is arranged on the side of the first inner crucible 2 facing away from the seed crystal 200, one end of the second inner crucible 5 facing the first inner crucible 2 is open to form a second open mouth, the second inner crucible 5 is adapted to contain a silicon material or a dopant, wherein the silicon material can be used for generating a compensation atmosphere and the dopant can be used for generating a doping atmosphere. The second inner crucible 5 is adapted to move axially relative to the first inner crucible 2 between a first position and a second position, wherein at least a portion of the sidewall of the second inner crucible 5 is embedded in the gas flow channel 23 when the second inner crucible 5 is in the first position, for example, a portion of the sidewall of the second inner crucible 5 adjacent to the top end may be embedded in the gas flow channel 23, and the inner cavity of the second inner crucible 5 is isolated from the gas flow channel 23. In the second position, the second inner crucible 5 is axially spaced from the first inner crucible 2, the inner cavity of the second inner crucible 5 is communicated with the gas flow channel 23, and the compensation atmosphere or the doping atmosphere generated in the second inner crucible 5 flows to the seed crystal 200 through the gas flow channel 23 so as to facilitate the growth of the seed crystal 200, so that the movement form of the second inner crucible 5 is simple, the circulation of the compensation atmosphere or the doping atmosphere can be controlled by controlling the movement of the second inner crucible 5, and the quality of the silicon carbide crystal can be better controlled.
For example, as shown in FIGS. 2, 4, 6 and 7, a seed crystal 200 is provided on a top cover of an outer crucible 1 at a central axis of the outer crucible 1, a first inner crucible 2 is provided in an inner cavity of the outer crucible 1 and at a lower side of the seed crystal 200, the first inner crucible 2 and the seed crystal 200 are spaced apart in an up-down direction, an upper side of the first inner crucible 2 is formed with a first open mouth, silicon carbide raw material is contained in the first inner crucible 2, an outer sidewall of the first inner crucible 2 is spaced apart from an inner sidewall of the outer crucible 1 in a radial direction of the outer crucible 1 to form an annular gas flow channel 23 extending in a circumferential direction of the first inner crucible 2, a second inner crucible 5 is provided at a lower side of the first inner crucible 2, an upper end of the second inner crucible 5 is opened and axially opposite to the first inner crucible 2, the second inner crucible 5 is adapted to contain silicon material or dopant, wherein the silicon material atmosphere is used to generate a compensating atmosphere, i.e., silicon carbide, the doping agent can be used to create a doping atmosphere and the second inner crucible 5 can be moved relative to the first inner crucible 2 in the axial direction of the outer crucible 1.
When the seed crystal 200 needs to be supplemented with the silicon carbide atmosphere or needs to be doped in the growth process, the second inner crucible 5 can move towards the direction away from the first inner crucible 2 and reach the second position, so that the gas flow channel 23 is communicated with the inner cavity of the second inner crucible 5, and the silicon carbide compensation atmosphere or the doping atmosphere generated in the second inner crucible 5 can flow towards the seed crystal 200; when the silicon carbide raw material in the first inner crucible 2 is sufficient and does not need to be doped during the growth of the seed crystal 200, the second inner crucible 5 is moved towards the first inner crucible 2 to reach the first position so as to block the inner cavity of the second inner crucible 5 and the air flow passage 23.
According to the single crystal growing device 100 provided by the embodiment of the invention, the first inner crucible 2 suitable for containing silicon carbide raw materials and the second inner crucible 5 suitable for containing silicon materials or doping agents are arranged in the outer crucible 1, and the gas flow channel 23 is defined between the first inner crucible 2 and the outer crucible 1, so that when the seed crystal 200 needs to be supplemented with silicon carbide atmosphere or doped in the growing process, the compensation atmosphere or doped atmosphere generated by the second inner crucible 5 can be transferred to the seed crystal 200 through the gas flow channel 23 by communicating the gas flow channel 23 with the inner cavity of the second inner crucible 5, and thus, the compensation of the growing atmosphere can be realized, the continuity of the growing process of the silicon carbide crystal is improved, and the silicon carbide crystal with qualified quality and variety is prepared.
Alternatively, in other embodiments, it is possible for only the second inner crucible 5 to be moved relative to the first inner crucible 2, for only the first inner crucible 2 to be moved relative to the second inner crucible 5, and for both the first inner crucible 2 and the second inner crucible 5 to be moved relative to one another.
According to some embodiments of the present invention, referring to fig. 1 to 7, the outer crucible 1 may include a crucible main body 11 and a crucible cover 12, wherein at least a top of the crucible main body 11 is open, the crucible cover 12 is covered on the crucible main body 11, the seed crystal 200 may be attached to an inner side surface of the crucible cover 12, and an upper surface of the crucible cover 12 may be provided with a graphite felt layer 121, thereby improving a heat insulating effect of the crucible cover 12.
Alternatively, referring to fig. 2, 4, 6 and 7, a graphite felt may be disposed in the gas flow channel 23, and the graphite felt may be a porous graphite felt, so that the heat preservation effect of the single crystal growth apparatus 100 may be improved, and meanwhile, the porous graphite felt has high gas permeability and does not affect the flow of the silicon carbide atmosphere or the doping atmosphere in the gas flow channel 23.
Further, referring to fig. 1 to 8, the single crystal growing apparatus 100 may further include: a connecting piece 3. Specifically, the connecting member 3 is provided in the air flow channel 23, for example, the connecting member 3 may be provided in the middle or upper part of the air flow channel 23, and of course, the position where the connecting member 3 is provided may be reasonably selected according to actual needs. The connecting member 3 is formed in a ring shape extending in the circumferential direction of the first inner crucible 2, the inner sidewall of the connecting member 3 is connected to the outer sidewall of the first inner crucible 2, and the outer sidewall of the connecting member 3 is connected to the inner sidewall of the outer crucible 1, so that the first inner crucible 2 is connected to the outer crucible 1 through the connecting member 3, thereby improving the stability of the first inner crucible 2. Be formed with a plurality of blow vents 31 that run through along the thickness direction on the connecting piece 3, a plurality of blow vents 31 and air current passageway 23 intercommunication, so, set up connecting piece 3 to be provided with a plurality of blow vents 31 on the connecting piece 3, both can conveniently fix first interior crucible 2, can not influence again and carry out the flow of atmosphere when atmosphere compensation or doping to the crystal. The plurality of air vents 31 are arranged at intervals along the circumferential direction of the connecting piece 3, so that the uniformity of the distribution of the compensation atmosphere or the doping atmosphere in the space can be improved, and the prepared silicon carbide crystal has a good and uniform growth interface.
Further, referring to FIG. 8, the outer sidewall of the connecting member 3 is screw-fitted to the inner sidewall of the outer crucible 1, the inner sidewall of the connecting member 3 is screw-fitted to the outer sidewall of the first inner crucible 2, for example, the outer sidewall of the connecting member 3 may be formed with a first fitting thread 32, the inner sidewall of the outer crucible 1 may be formed with a first mating thread, the first fitting thread 32 and the first mating thread cooperate with each other to achieve the connection of the connecting member 3 with the outer crucible 1, the inner sidewall of the connecting member 3 may be formed with a second fitting thread 33, the outer sidewall of the first inner crucible 2 may be formed with a second mating thread, the second fitting thread 33 and the second mating thread cooperate with each other to achieve the connection of the connecting member 3 with the first inner crucible 2, and further, by means of threaded fit, the tightness of the joints of the connecting piece 3 and the outer crucible 1 and the connecting piece 3 and the first inner crucible 2 can also be improved.
In some embodiments, the portion of the side wall of the second inner crucible 5 adjacent to the tip end is formed with a blocking portion 51, the blocking portion 51 is formed in a ring shape extending along the circumferential direction of the first inner crucible 2, the width of the blocking portion 51 in the radial direction is adapted to the width of the gas flow channel 23, and the thickness of the blocking portion 51 is greater than the thickness of the remaining portion of the second inner crucible 5 except for the blocking portion 51, so that, when the second inner crucible 5 is in the first position, the blocking portion 51 is located inside the gas flow channel 23 to block the gas flow channel 23 and the inner cavity of the second inner crucible 5, and when the second inner crucible 5 is in the second position, the blocking portion 51 is located on the lower side of the gas flow channel 23 and is spaced from the first inner crucible 2 in the up-down direction, at which the gas flow channel 23 and the inner cavity of the second inner crucible 5 communicate with each other.
Further, a heat conducting portion 21 is formed at the bottom end of the first inner crucible 2, the heat conducting portion 21 may be formed in a circular truncated cone shape, the diameter of the heat conducting portion 21 is adapted to the inner diameter of the blocking portion 51, when the second inner crucible 5 is at the first position, the inner side wall of the blocking portion 51 is in sealing fit with the outer side wall of the heat conducting portion 21, so that on one hand, the sealing property of the inner cavity of the second inner crucible 5 is improved when the second inner crucible 5 is at the first position, and on the other hand, by arranging the heat conducting portion 21 at the bottom of the first inner crucible 2, it is not only beneficial to receive heat from a heat source through the heat conducting portion 21, but also beneficial to increase the temperature of the silicon carbide raw material in the first inner crucible 2, so as to generate a silicon carbide atmosphere through sublimation, and further, the top center position of the second inner crucible 2 is kept at a higher temperature, so as to promote the compensation atmosphere or doping atmosphere in the second inner crucible 5 to diffuse to the outer edge, thereby entering the gas flow channel 23 and finally migrating to the seed crystal 200 under the influence of the temperature gradient, besides, the waste of raw materials caused by the deposition or crystallization of the compensation atmosphere or doping atmosphere in the second inner crucible 5 directly at the bottom of the first inner crucible 2 can be avoided.
In a specific example, referring to fig. 1 to 7, the heat conducting portion 21 is a graphite platform, so that the heat conducting portion 21 has good heat conductivity, and optionally, the heat conducting portion 21 and the first inner crucible 2 may be integrally formed or may be connected by bonding or the like.
Further, referring to fig. 1-7 and fig. 9 and 10, the inner sidewall of the blocking portion 51 is in threaded engagement with the outer sidewall of the heat conducting portion 21, and the outer sidewall of the blocking portion 51 is in threaded engagement with the inner sidewall of the outer crucible 1, for example, the inner sidewall of the blocking portion 51 may be formed with a third assembling thread 511, the outer sidewall of the heat conducting portion 21 is formed with a third assembling thread, the third assembling thread 511 and the third assembling thread cooperate with each other to achieve the sealing engagement of the second inner crucible 5 with the first inner crucible 2 at the first position, the outer sidewall of the blocking portion 51 may be formed with a fourth assembling thread 55, and the inner sidewall of the outer crucible 1 may be formed with a fourth assembling thread, so that the fourth assembling thread 55 and the fourth assembling thread cooperate with each other to facilitate the fixing of the second inner crucible 5 and the improvement of the sealing between the second inner crucible 5 and the outer crucible 1.
In a specific example, the thickness of the blocking portion 51 in the axial direction of the outer crucible 1 is not greater than the thickness of the heat conducting portion 21, so that the blocking platform is prevented from being too high and entering the crystal production area during lifting, and influencing the thermal field inside the first inner crucible 2.
According to some embodiments of the invention, a part of the side wall of the second inner crucible 5 located at the lower side of the blocking portion 51 is spaced from the inner side wall of the outer crucible 1 to form a filling cavity, which is suitable for filling with a thermal insulation member, for example, the thermal insulation member may be a graphite thermal insulation felt, and of course, the filling cavity may be selected according to the thermal field requirements as to whether to fill the thermal insulation member and what kind of material to fill the thermal insulation member.
In some embodiments, the bottom end of the outer crucible 1 is open to form a receiving opening, and the second inner crucible 5 is adapted to close the receiving opening, i.e., the second inner crucible 5 can close the receiving opening of the outer crucible 1 in both the first position and the second position, so that the convenience of mounting and dismounting the second inner crucible 5 and the outer crucible 1 can be improved because the second inner crucible 5 is located at the lower side of the first inner crucible 2 and the bottom end of the outer crucible 1 forms the receiving opening, thereby improving the efficiency of loading the material into the second inner crucible 5.
Further, with reference to fig. 5, 6 and 9, the second inner crucible 5 may comprise: a holding portion 52 and a support platform 53. Wherein the material containing part 52 is located at the inner side of the outer crucible 1, for example, the material containing part 52 is located at the inner side of the outer crucible 1 in the radial direction, the material containing part 52 is formed in a cylindrical shape with an open top end, the material containing part 52 is used for containing silicon material or dopant, when the second inner crucible 5 is at the first position, at least part of the side wall of the material containing part 52 is embedded in the gas flow channel 23, the inner cavity of the material containing part 52 is isolated from the gas flow channel 23, when the second inner crucible 5 is at the second position, the material containing part 52 is axially spaced from the first inner crucible 2, the inner cavity of the material containing part 52 is communicated with the gas flow channel 23, and the compensation atmosphere or the doping atmosphere flows to the seed crystal 200 through the gas flow channel 23. The supporting platform 53 is located at the bottom end of the material containing part 52, the outer diameter of the supporting platform 53 is larger than that of the material containing part 52, when the material containing part 52 is located at the inner side of the outer crucible 1, the bottom end of the outer crucible 1 is suitable for being supported on the supporting platform 53, so that when the material containing part 52 is located at the inner side of the outer crucible 1, the supporting platform 53 can be matched with the end face of one end of the mounting opening of the outer crucible 1, and the sealing performance of the single crystal growing device 100 can be improved on the basis of conveniently assembling and disassembling the second inner crucible 5.
The blocking part 51 is formed at the top end of the side wall of the material containing part 52, when the second inner crucible 5 is at the first position, the blocking part 51 of the material containing part 52 is embedded in the airflow channel 23, the inner cavity of the material containing part 52 is blocked from the airflow channel 23, when the second inner crucible 5 is at the second position, the blocking part 51 of the material containing part 52 is axially spaced from the first inner crucible 2, the inner cavity of the material containing part 52 is communicated with the airflow channel 23, and the compensation atmosphere or the doping atmosphere flows to the seed crystal 200 through the airflow channel 23.
Still further, referring to fig. 7 and 10, the outer diameter of the supporting platform 53 is larger than that of the outer crucible 1, the supporting platform 53 is further formed with a fitting portion 531, the fitting portion 531 extends along the circumferential direction of the supporting platform 53, the fitting portion 531 is spaced apart from the holding portion 52 in the radial direction to form a slot 532, that is, the opening of the slot 532 is upward, and the portion of the outer crucible 1 adjacent to the bottom end is adapted to be inserted into the slot 532, so that the sealing performance of the silicon carbide growth apparatus 100 can be further improved.
According to some embodiments of the invention, the single crystal growing apparatus 100 may further comprise: a drive means (not shown), a first drive shaft 22 and a second drive shaft 54. Wherein, the driving device can be arranged at the lower side of the single crystal growing device 100, one end of the first transmission shaft 22 passes through the second inner crucible 5 to be connected with the bottom of the first inner crucible 2, the other end of the first transmission shaft 22 is connected with the driving device, one end of the second transmission shaft 54 is connected with the bottom of the second inner crucible 5, the other end of the second inner crucible 5 is connected with the driving device, and the second transmission shaft 54 is sleeved at the outer side of the first transmission shaft 22. The driving device is suitable for driving the first transmission shaft 22 to drive the first inner crucible 2 to move along the axial direction of the outer crucible 1, so that the position of the first inner crucible 2 in the axial direction of the outer crucible 1 can be adjusted, and the distance between the seed crystal 200 and the thermal field can be adjusted; the drive means are also adapted to drive the second drive shaft 54 to move the second inner crucible 5 between the first position and the second position, so that the position of the second inner crucible 5 in the axial direction of the outer crucible 1 can be controlled, thereby adjusting the interruption or continuation of the circulation of the compensation atmosphere or doping atmosphere in the second inner crucible 5.
According to some embodiments of the present invention, referring to fig. 3 and 4, the single crystal growing apparatus 100 may further include: a flow guide 4. The guiding element 4 may be disposed on the first inner crucible 2 and/or the connecting element 3 to guide the atmosphere in the gas flow channel 23 to the seed crystal 200, for example, the guiding element 4 may be supported on the top end of the first inner crucible 2, or the guiding element 4 may be disposed on the connecting element 3, or a part of the guiding element 4 may be engaged with the first inner crucible 2 and another part of the guiding element 4 may be engaged with the connecting element 3, so as to achieve the assembling of the guiding element 4.
Further, with reference to fig. 3 and 4, the flow guide 4 is formed as a flow guide which may comprise: a first plate section 41 and a second plate section 42. The first plate section 41 is formed into a cylindrical shape with two open ends along the axial direction, one end of the first plate section 41 in the axial direction is supported at the top end of the first inner crucible 2 or the inner end of the connecting piece 3, the first plate section 41 is formed with a plurality of flow guide holes 411 which penetrate along the radial direction of the first inner crucible 2, and the flow guide holes 411 are communicated with the airflow channel 23. The upper end of the second plate section 42 is connected to the upper end of the first plate section 41, and the lower end of the second plate section 42 abuts against the inner side wall of the outer crucible 1 and/or the outer end of the connecting member 3, so that the compensating atmosphere or the doping atmosphere can be better guided to the seed crystal 200.
For example, as shown in fig. 3, the flow guide member 4 may be formed in a substantially V-shaped cross section, wherein the lower end of the first plate section 41 may be supported on the upper end of the first inner crucible 2, or the lower end of the first plate section 41 may be supported on the inner end edge of the upper surface of the connecting member 3, and a plurality of flow guide holes 411 are formed on the first plate section 41 and extend in the radial direction. The upper end of the second plate section 42 is connected to the upper end of the first plate section 41, and the lower end of the second plate section 42 abuts against the side wall of the outer crucible 1, or the lower end of the second plate section 42 is supported on the outer end edge of the upper surface of the connecting member 3. Thus, the flow guide member 4 can change the flow direction of the atmosphere in the gas flow channel 23 from the axial direction to the radial direction to enter the upper side of the first inner crucible 2, and the gas flow direction is fully mixed with the atmosphere in the first inner crucible 2 and then transferred to the seed crystal 200, so that the prepared silicon carbide crystal has higher quality and more uniform doping. Alternatively, the second plate section 42 may be formed to have a cross section in an upwardly curved arc shape in a direction from the lower end to the upper end, which is advantageous in reducing atmospheric resistance.
According to some embodiments of the present invention, referring to fig. 1-7, single crystal growing apparatus 100, further comprises: a first heating member 6 and a second heating member 7. Wherein the first heating member 6 is used for heating the silicon carbide raw material in the first inner crucible 2 so that the silicon carbide raw material is heated and sublimated to generate a silicon carbide atmosphere, and the silicon carbide atmosphere is suitable for being migrated to the seed crystal 200. For example, the first heating member 6 may be a first induction coil circumferentially disposed on the outside of the outer crucible 1, the first induction coil being disposed opposite the first inner crucible 2 in the inside-outside direction.
The second heating member 7 is used for heating the silicon material or dopant in the second inner crucible 5 to generate a compensation atmosphere or a doping atmosphere, and the compensation atmosphere or the doping atmosphere is suitable for moving to the seed crystal 200 through the gas flow passage, for example, the second heating member 7 can be a second induction coil surrounding the outer side of the outer crucible 1, the second induction coil and the second inner crucible 5 are oppositely arranged along the inner and outer directions, and the first induction coil and the second induction coil can be arranged along the axial direction of the outer crucible 1 at intervals, and the first induction coil and the second induction coil can respectively and independently control the temperature.
In a specific embodiment, the outer crucible 1, the first inner crucible 2 and the second inner crucible 5 are graphite crucibles, so that the outer crucible 1, the first inner crucible 2 and the second inner crucible 5 can withstand higher temperatures, thereby ensuring stable growth of the silicon carbide crystal.
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 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 (13)

1. A single crystal growing apparatus, comprising:
the outer crucible defines a growth cavity, and the top wall of the growth cavity is provided with seed crystals;
the first inner crucible is arranged in the growth cavity and is opposite to the seed crystal in the axial direction, one end of the first inner crucible facing the seed crystal is open, the outer side wall of the first inner crucible is spaced from the inner side wall of the outer crucible to define a gas flow channel, and the first inner crucible is used for containing silicon carbide raw materials;
a second inner crucible arranged in the growth chamber and positioned on the side of the first inner crucible facing away from the seed crystal, wherein one end of the second inner crucible facing the first inner crucible is open, the second inner crucible is suitable for containing silicon materials used for generating compensation atmosphere or doping agents used for generating doping atmosphere,
wherein the second inner crucible is adapted to move between a first position in which at least a portion of a sidewall of the second inner crucible is embedded within the gas flow passage to separate the inner cavity of the second inner crucible from the gas flow passage and a second position in which the second inner crucible is axially spaced from the first inner crucible to place the inner cavity of the second inner crucible in communication with the gas flow passage, the compensating atmosphere or the doping atmosphere flowing through the gas flow passage toward the seed crystal.
2. A single crystal growing apparatus according to claim 1, comprising: a connecting piece arranged on the airflow channel, the connecting piece is formed into a ring shape extending along the circumferential direction of the first inner crucible, the inner side wall of the connecting piece is connected with the outer side wall of the first inner crucible, the outer side wall of the connecting piece is connected with the inner side wall of the outer crucible,
the connecting piece is provided with a plurality of vent holes penetrating along the thickness direction, and the vent holes are communicated with the airflow channel and are arranged along the circumferential interval of the connecting piece.
3. The single crystal growth apparatus according to claim 1, wherein a portion of the side wall of the second inner crucible adjacent to the tip end is formed with a stopper portion formed in a ring shape extending in the circumferential direction of the first inner crucible, the stopper portion having a width in the radial direction adapted to the width of the gas flow channel,
when the second inner crucible is positioned at the first position, the blocking part is positioned in the gas flow passage to block the gas flow passage and the inner cavity of the second inner crucible.
4. The single crystal growth apparatus according to claim 3, wherein a bottom end of the first inner crucible is formed with a heat-conducting portion formed in a circular truncated cone shape, a diameter of the heat-conducting portion is adapted to an inner diameter of the stopper portion,
when the second inner crucible is located at the first position, the inner side wall of the blocking part is in sealing fit with the outer side wall of the heat conducting part.
5. The single crystal growth apparatus according to claim 4, wherein a thickness of the stopper portion in an axial direction of the outer crucible is not more than a thickness of the heat conductive portion.
6. A single crystal growth apparatus according to claim 3, wherein a portion of the side wall of the second inner crucible located below the seal is spaced from the inner side wall of the outer crucible to form a filled cavity, the filled cavity being adapted to be filled with a thermal insulator.
7. A single crystal growing apparatus according to any one of claims 1 to 6 wherein the bottom end of the outer crucible is open to form a mounting opening, the second inner crucible being adapted to close off the mounting opening.
8. The single crystal growing apparatus of claim 7 wherein the second inner crucible comprises:
the material containing part is positioned on the inner side of the outer crucible, the material containing part is formed into a cylinder with an open top end, the material containing part is used for containing the silicon material or the dopant, when the second inner crucible is at the first position, at least part of the side wall of the material containing part is embedded in the airflow channel, the inner cavity of the material containing part is isolated from the airflow channel, when the second inner crucible is at the second position, the material containing part is axially spaced from the first inner crucible, the inner cavity of the material containing part is communicated with the airflow channel, and the compensation atmosphere or the doping atmosphere flows to the seed crystal through the airflow channel;
the supporting platform is located at the bottom end of the material containing portion, the outer diameter of the supporting platform is larger than that of the material containing portion, and when the material containing portion is located on the inner side of the outer crucible, the bottom end of the outer crucible is suitable for being supported on the supporting platform.
9. A single crystal growing apparatus according to claim 8 wherein the outer diameter of the support platform is greater than the outer diameter of the outer crucible, the support platform further having formed thereon a mating portion extending circumferentially of the support platform and spaced radially from the receptacle to form a slot into which a portion of the outer crucible adjacent the bottom end is adapted to be inserted.
10. The single crystal growing apparatus of claim 1, further comprising:
a drive device;
one end of the first transmission shaft penetrates through the second inner crucible to be connected with the bottom of the first inner crucible, and the other end of the first transmission shaft is connected with the driving device;
one end of the second transmission shaft is connected with the bottom of the second inner crucible, the other end of the second inner crucible is connected with the driving device, and the second transmission shaft is sleeved on the outer side of the first transmission shaft;
the driving device is suitable for driving the first transmission shaft to drive the first inner crucible to move along the axial direction of the outer crucible, and the driving device is also suitable for driving the second transmission shaft to drive the second inner crucible to move between the first position and the second position.
11. The single crystal growing apparatus of claim 2, further comprising: and the flow guide piece is arranged on the first inner crucible and/or the connecting piece, and is used for guiding the atmosphere in the airflow channel to the seed crystal.
12. A single crystal growing apparatus according to claim 11 wherein the flow guide is formed as a flow guide comprising:
the first plate section is formed into a cylindrical shape with two open ends along the axial direction, one end of the first plate section in the axial direction is supported at the top end of the first inner crucible or the inner end of the connecting piece, a plurality of flow guide holes penetrating along the radial direction of the first inner crucible are formed in the first plate section, and the flow guide holes are communicated with the airflow channel;
and the upper end of the second plate section is connected with the upper end of the first plate section, and the lower end of the second plate section is abutted against the inner side wall of the outer crucible and/or the outer end of the connecting piece.
13. The single crystal growing apparatus of claim 1, further comprising:
a first heating element for heating the silicon carbide feedstock in the first inner crucible to cause sublimation of the silicon carbide feedstock by heating to produce a silicon carbide atmosphere, the silicon carbide atmosphere being adapted to migrate to the seed crystal;
a second heating element for heating the silicon material or dopant in the second inner crucible to create a compensating atmosphere or a doping atmosphere adapted to migrate to the seed crystal through the gas flow passage when the second inner crucible is in the second position.
CN202210136243.2A 2022-02-14 2022-02-14 Single crystal growing apparatus Active CN114561693B (en)

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Publication number Priority date Publication date Assignee Title
JP2012201584A (en) * 2011-03-28 2012-10-22 Showa Denko Kk Apparatus and method for producing silicon carbide single crystal, and growth method thereof
JP2015229608A (en) * 2014-06-04 2015-12-21 株式会社フジクラ Apparatus for producing single crystal
CN111041553A (en) * 2019-12-04 2020-04-21 山东天岳先进材料科技有限公司 Crystal growth device and method
CN212560515U (en) * 2020-04-30 2021-02-19 山东天岳先进科技股份有限公司 Growth device of silicon carbide single crystal
CN113249792A (en) * 2021-06-22 2021-08-13 苏州优晶光电科技有限公司 Silicon carbide crystal growth method and equipment for adjusting component balance
CN113862789A (en) * 2021-12-01 2021-12-31 浙江大学杭州国际科创中心 Crucible structure, device and method for preparing p-type 4H-SiC single crystal

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012201584A (en) * 2011-03-28 2012-10-22 Showa Denko Kk Apparatus and method for producing silicon carbide single crystal, and growth method thereof
JP2015229608A (en) * 2014-06-04 2015-12-21 株式会社フジクラ Apparatus for producing single crystal
CN111041553A (en) * 2019-12-04 2020-04-21 山东天岳先进材料科技有限公司 Crystal growth device and method
CN212560515U (en) * 2020-04-30 2021-02-19 山东天岳先进科技股份有限公司 Growth device of silicon carbide single crystal
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