CN114481291A - Method for automatically stabilizing seed crystals to stick slag - Google Patents
Method for automatically stabilizing seed crystals to stick slag Download PDFInfo
- Publication number
- CN114481291A CN114481291A CN202011258169.9A CN202011258169A CN114481291A CN 114481291 A CN114481291 A CN 114481291A CN 202011258169 A CN202011258169 A CN 202011258169A CN 114481291 A CN114481291 A CN 114481291A
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- Prior art keywords
- slag
- steel wire
- seed crystals
- main chamber
- automatically
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- 239000013078 crystal Substances 0.000 title claims abstract description 56
- 239000002893 slag Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 32
- 230000000087 stabilizing effect Effects 0.000 title claims abstract description 31
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 53
- 239000010959 steel Substances 0.000 claims abstract description 53
- 239000007788 liquid Substances 0.000 claims abstract description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000010453 quartz Substances 0.000 claims abstract description 10
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 10
- 239000010703 silicon Substances 0.000 claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- 229910052786 argon Inorganic materials 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 8
- 210000000078 claw Anatomy 0.000 claims description 5
- 238000010926 purge Methods 0.000 claims description 4
- 238000012544 monitoring process Methods 0.000 claims description 3
- 238000009835 boiling Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides a method for automatically stabilizing seed crystals to stick slag, which comprises the following steps: and under the set thermal field power, enclosing the pulling steel wire in a certain space, operating the pulling steel wire and lowering the seed crystal to a set position, and starting to stick slag when the lower end surface of the seed crystal corresponds to the central point of the liquid level of the silicon melt in the quartz crucible. The method provided by the invention has the advantages that the whole slag adhering process can be automatically controlled, the intervention of personnel operation is not needed, the human error is reduced, the contact accuracy of the seed crystal and the slag at the center of the molten silicon liquid level is improved by 5-8%, the slag adhering quality is ensured, and the working efficiency is improved.
Description
Technical Field
The invention belongs to the technical field of Czochralski single crystal manufacturing, and particularly relates to a method for automatically stabilizing seed crystals to adhere slag.
Background
In the existing slag bonding process, the position of the guide shell and the alignment of the seed crystal and the center of the silicon melt surface cannot be accurately controlled, and the control is manually operated and judged by experience. If the operator is unskilled in skill and power is not reduced in time, liquid level boiling occurs during slag bonding, and slag bonding cannot be performed; or the guide shell is not lowered in time, slag can be fried, and abnormal production can be caused; in addition, if the operating personnel do not stick the slag in time, the slag head can be melted, the slag can not be stuck, and the crystallization and quality conditions can be influenced. Moreover, the accuracy of slag adhesion is very unstable due to the shaking of seed crystals and the boiling of the liquid level of the molten silicon, so that the situation of front and back inconsistency often occurs, and the tracing and judgment of quality problems are seriously influenced.
Disclosure of Invention
The invention provides a method for automatically stabilizing seed crystals to stick slag, which solves the technical problem that the seed crystals cannot be automatically stabilized to stick slag in the prior art.
In order to solve the technical problems, the invention adopts the technical scheme that:
a method for automatically stabilizing seed crystals for slag adhesion comprises the following steps: and under the set thermal field power, enclosing the pulling steel wire in a certain space, operating the pulling steel wire and lowering the seed crystal to a set position, and starting to stick slag when the lower end surface of the seed crystal corresponds to the central point of the liquid level of the silicon melt in the quartz crucible.
Further, before the seed crystal descends to a set position, the power of a main heater in the thermal field is not more than 80kW, and the power of a bottom heater in the thermal field is not more than 10 kW.
Further, before the seed crystal descends to a set position, after the power of the thermal field is set, the method also comprises the step of operating the guide shell to descend for a certain distance.
Further, the descending distance of the guide shell is 30-100 mm.
Further, after the guide cylinder is set to descend for a set distance, the method further comprises the step of introducing argon into the main chamber of the single crystal furnace for purging, wherein the argon is closed after being introduced for a certain time.
Further, the argon gas is introduced for 8-12 min.
Further, before the argon gas is introduced, the method also comprises the steps of closing the main chamber pressure control ring and opening the argon gas quick-filling valve.
Furthermore, the lifting steel wire is arranged in a manner that the stabilizing device in the main chamber is surrounded, and the stabilizing device is positioned above the guide cylinder and arranged in a staggered manner with the CCD camera in the main chamber.
Furthermore, the stabilizing device comprises telescopic rods which are oppositely arranged, one end of each telescopic rod is fixedly arranged on the inner side wall of the main chamber, the other end of each telescopic rod is arranged in a suspended manner, and a clamping jaw is arranged on one side of each telescopic rod, which is far away from the inner wall of the main chamber; the space formed by the alignment of the two clamping jaws is penetrated by the lifting steel wire and is not contacted with the lifting steel wire.
Further, the axis of the telescopic rod is perpendicular to the lifting steel wire; and a position sensor for monitoring the lifting steel wire is arranged on the inner side of the clamping jaw.
Compared with the prior art, by adopting the technical scheme, the whole slag adhering process can be automatically controlled, the operation intervention of personnel is not needed, the human error is reduced, the accuracy of the contact between the seed crystal and the slag at the center of the molten silicon liquid level is improved by 5-8%, the slag adhering quality is ensured, and the working efficiency is improved.
Drawings
FIG. 1 is a schematic structural diagram of a seed crystal sticking slag according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a fixing device according to an embodiment of the present invention.
In the figure:
10. main chamber 20, guide cylinder 30, quartz crucible
40. Lifting steel wire 50, seed crystal 60 and stabilizing device
61. Telescopic link 62, manipulator
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
The embodiment provides a method for automatically stabilizing seed crystals to stick slag, which is mainly applied to the precise contact between the seed crystals and central slag charge in a quartz crucible 30 in the slag sticking process, the structure of the method is shown in figure 1, in the slag sticking process, a heavy hammer at the lower end part of a lifting steel wire 40 is connected with the seed crystals 50 and is positioned in a main chamber 10 of a single crystal furnace; a stabilizing device 60 for preventing the lifting steel wire 40 from shaking, namely improving the stable downward movement of the seed crystal 50 and accurately contacting with the slag charge block of the quartz crucible 30 is arranged above the guide cylinder 20; and a system controller disposed outside the single crystal furnace for controlling the up and down displacement and speed of the steel wire 40, the magnitude of the thermal field power, the rotational speed of the quartz crucible 30, the height of the seed crystal 50, and the operation of the stabilizing device 60. The stabilizing device 60 is arranged in the main chamber 10, has a large adjustable space range and is easy to install and observe; simultaneously, crystal drawing is not influenced; the fixing device 60 is arranged in a staggered manner with the CCD camera in the main chamber 10, so as to avoid affecting the observation sight of the CCD camera on the slag sticking process of the seed crystal 50.
Wherein, securing device 60 is as shown in fig. 2, including the telescopic link 61 that the symmetry set up, the one end of telescopic link 61 sets firmly in the inside wall of main chamber 10, and the unsettled level of the other end sets up, telescopic link 61 axis horizontal perpendicular to the inside wall of main chamber 10, and the vertical setting of perpendicular to carries steel wire 40. The telescopic rod 61 can be controlled by the controller to automatically move toward the steel wire 40 or away from the steel wire 40 in the horizontal direction. The manipulator 62 is arranged on one side of the inner wall of the telescopic rod 61 far away from the main chamber 10, and the upper end face of the manipulator 62 is horizontally arranged.
Further, the manipulator 62 includes jaws which are oppositely arranged and hinged, the jaws are arc-shaped structures, that is, the inner and outer walls of the symmetrically arranged jaws are hinged to each other to form an arc-shaped structure, when the manipulator starts to approach the lifting steel wire 40, the opening of the jaws is large, so that the lifting steel wire 40 enters the space enclosed by the jaws, and the inner wall of the clamping jaw is not contacted with the lifting steel wire 40; when the pull steel wire 40 is inserted into the space, the jaw opening is reduced to reduce the area of the space surrounded by the pull steel wire 40, thereby reducing the shaking range.
The two manipulators 62 are aligned to form a space which can be expanded or reduced, and the space surrounded by the two manipulators 62 is penetrated by the steel wire 40 and is not contacted with the steel wire 40. When the steel wire 40 is close to the lifting steel wire, the enclosed space is larger, and as the telescopic rod 61 slowly extends forwards, the space enclosed by the mechanical arm 62 is gradually reduced, so that the lifting steel wire 40 swings in a relatively small annular space, and the centering and calibrating time of the lifting steel wire 40 and the calibrating piece 50 is shortened.
Further, in order to ensure the accuracy of the start-up of the robot arm 62, a position sensor (not shown) for monitoring the lifting of the steel wire 40 is provided inside the robot arm 62. In the present embodiment, only one of the robots 62 may be provided with a position sensor. The position of the position sensor is preferably set at the middle axis of the manipulator 62 parallel to the steel wire 40, the position sensor monitors the steel wire 40 and sends a signal to the controller, and the controller controls the telescopic rod 61 to move towards the side close to the steel wire 40 until the center position of the arc horizontal plane of the manipulator 62 is matched with the position of the steel wire 40.
The shortest radial distance between the mechanical arm 40 and the inner wall of the main chamber 10 is not more than the radial distance between the outer wall of the upper end surface of the guide cylinder 20 and the inner wall of the main chamber 10. The purpose is to prevent stabilizer 60 from affecting the drawing of the crystal, especially the argon flow, when stabilizer 60 is not needed to enclose the drawn steel wire 40.
The two side telescopic rods 61 can be controlled by the same cylinder device, and can also be respectively controlled by two synchronous cylinders, and the control is not particularly limited. During operation, when the position sensor monitors that the steel wire 40 is lifted, a signal is transmitted to the controller, the controller controls the pneumatic device to enable the telescopic rods 61 on the two sides to synchronously move towards one side of the steel wire 40, in the moving process, the openings of the clamping jaws in the mechanical arm 62 are outwards expanded, after the steel wire 40 is lifted and arranged in an enclosing mode, the clamping jaws shrink gradually, the clamping jaws on the two sides are in end-to-end contact and form a closed space, and the steel wire is lifted and arranged in an enclosing mode completely and is not in contact with the clamping jaws on the two sides. When the enclosure is not needed, the telescopic rods 61 on the two sides of the clamping jaw move towards one side away from the lifting steel wire 40 and retract outwards until the clamping jaw is completely retracted to the initial position.
Specifically, the method for automatically stabilizing the seed crystal 50 for slag adhesion comprises the following steps:
s1: the power of the thermal field is reduced and the thermal field is within the set power, namely the power of the main heater in the thermal field is not more than 80kW and the power of the bottom heater is not more than 10kW before the seed crystal 50 is lowered to the set position.
S2: the guide shell 20 descends a certain distance, and preferably, the guide shell 20 descends a distance of 30-100 mm.
S3: the system controller controls the starting of the trigger position of the heat shield, automatically closes the pressure control ring of the main chamber 10 and then opens the fast argon filling fast filling valve. It is also required that argon is introduced for 8-12min, preferably 10min, in the main chamber 10, and the purging of the silicon material in the quartz crucible 30 is completed.
S4: after the argon purging is finished for 4-6min, the controller controls the pulling steel wire 40 to drive the seed crystal 50 to move towards the side close to the quartz crucible 30, and the seed crystal 50 is stopped when the seed crystal 50 descends to a position 500mm away from the liquid level 400-5. At this time, the position sensor in the stabilizing device 10 is controlled to start working, when the position sensor monitors the lifting steel wire 40, the signal is transmitted to the controller, the controller controls the pneumatic device to enable the telescopic rods 61 on the two sides to synchronously and relatively move towards one side of the lifting steel wire 40, in the moving process, the openings of the claws in the manipulator 62 are outwards expanded, after the lifting steel wire 40 is enclosed, the claws gradually contract, the claws on the two sides contact end to form a closed space, and the lifting steel wire 40 is completely enclosed and does not contact with the claws on the two sides.
After the lifting steel wire 50 is completely surrounded by the stabilizing device 60, the controller is controlled to directly control the seed crystal to automatically move downwards along the space surrounded by the two mechanical arms 62 of the stabilizing device 60, the lifting steel wire 40 is a flexible part and is easy to deform, and when the lifting steel wire 40 is surrounded in a certain space and moves downwards along the space, the seed crystal 50 can be kept to be stably and vertically arranged in the certain space, so that the seed crystal 50 can be automatically controlled to descend to the position of the liquid level of the molten silicon and start to contact with a slag block arranged in the middle of the quartz crucible 30 to stick slag. The arrangement of the stabilizing device 60 can stably strengthen the contact between the seed crystal 50 and the slag block, and further improve the accuracy of slag adhesion.
The whole slag adhering process can be automatically controlled, personnel operation intervention is not needed, human errors are reduced, the accuracy of contact between seed crystals and slag at the center of the molten silicon liquid level is improved, the accuracy of contact between the seed crystals and the slag at the center of the molten silicon liquid level is improved by 5-8%, the slag adhering quality is ensured, and the working efficiency is improved.
The embodiments of the present invention have been described in detail, and the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (10)
1. A method for automatically stabilizing seed crystals for slag adhesion is characterized by comprising the following steps: and under the set thermal field power, enclosing the pulling steel wire in a certain space, operating the pulling steel wire and lowering the seed crystal to a set position, and starting to stick slag when the lower end surface of the seed crystal corresponds to the central point of the liquid level of the silicon melt in the quartz crucible.
2. A method for automatically stabilizing seed crystals for sticking slag as claimed in claim 1, wherein the power of the main heater in the thermal field is not more than 80kW and the power of the bottom heater is not more than 10kW before the seed crystals descend to the set position.
3. The method for automatically stabilizing seed crystals for slag adhesion as claimed in claim 1 or 2, further comprising the step of operating the guide cylinder to descend for a certain distance before the seed crystals descend to the set position and after the power of the thermal field is set.
4. The method for automatically stabilizing seed crystals for sticking slag as claimed in claim 3, wherein the descending distance of the guide shell is 30-100 mm.
5. The method for automatically stabilizing seed crystals for sticking slag as claimed in claim 4, further comprising the step of introducing argon gas into the main chamber of the single crystal furnace for purging after the guide cylinder is set to descend for a set distance, wherein the argon gas is closed after being introduced for a certain time.
6. A method for automatically stabilizing seed crystals for sticking slag as claimed in claim 5, wherein the argon gas is introduced for 8-12 min.
7. A method for automatically stabilizing seed crystals for slag adhesion as claimed in claim 5 or 6, further comprising the steps of closing the main chamber pressure control loop and opening the quick argon gas filling valve before the argon gas is introduced.
8. The method for automatically stabilizing seed crystals for sticking slag as claimed in claim 7, wherein the steel wire is surrounded by a stabilizing device arranged in the main chamber, and the stabilizing device is positioned above the guide shell and is arranged in a staggered manner with the CCD camera in the main chamber.
9. The method as claimed in claim 8, wherein the stabilizing means comprises opposite telescopic rods, one end of the telescopic rod is fixed on the inner wall of the main chamber, the other end is suspended, and a claw is arranged on the side of the telescopic rod away from the inner wall of the main chamber; the space formed by the alignment of the two clamping jaws is penetrated by the lifting steel wire and is not contacted with the lifting steel wire.
10. The method for automatically stabilizing seed crystals for sticking slag as claimed in claim 9, wherein the axis of the telescopic rod is arranged perpendicular to the pulling steel wire; and a position sensor for monitoring the lifting steel wire is arranged on the inner side of the clamping jaw.
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CN202011258169.9A CN114481291B (en) | 2020-11-12 | 2020-11-12 | Method for automatically stabilizing seed crystal to adhere slag |
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CN202011258169.9A CN114481291B (en) | 2020-11-12 | 2020-11-12 | Method for automatically stabilizing seed crystal to adhere slag |
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CN114481291B CN114481291B (en) | 2023-12-01 |
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CH632300A5 (en) * | 1978-01-04 | 1982-09-30 | Vnii Monokristallov | System for growing single crystals from a melt |
US5888299A (en) * | 1995-12-27 | 1999-03-30 | Shin-Etsu Handotai Co., Ltd. | Apparatus for adjusting initial position of melt surface |
CN111809237A (en) * | 2020-06-03 | 2020-10-23 | 有研光电新材料有限责任公司 | Method for sticking dirty material in growth process of germanium crystal |
-
2020
- 2020-11-12 CN CN202011258169.9A patent/CN114481291B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CH632300A5 (en) * | 1978-01-04 | 1982-09-30 | Vnii Monokristallov | System for growing single crystals from a melt |
US5888299A (en) * | 1995-12-27 | 1999-03-30 | Shin-Etsu Handotai Co., Ltd. | Apparatus for adjusting initial position of melt surface |
CN111809237A (en) * | 2020-06-03 | 2020-10-23 | 有研光电新材料有限责任公司 | Method for sticking dirty material in growth process of germanium crystal |
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Address after: No.19, Amur South Street, Saihan District, Hohhot, Inner Mongolia Autonomous Region Applicant after: Inner Mongolia Zhonghuan Crystal Materials Co.,Ltd. Address before: No.19, Amur South Street, Saihan District, Hohhot, Inner Mongolia Autonomous Region Applicant before: INNER MONGOLIA ZHONGHUAN XIEXIN PHOTOVOLTAIC MATERIAL Co.,Ltd. |
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