CN113913922B - Method for setting liquid gap of single crystal furnace - Google Patents
Method for setting liquid gap of single crystal furnace Download PDFInfo
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- CN113913922B CN113913922B CN202111266358.5A CN202111266358A CN113913922B CN 113913922 B CN113913922 B CN 113913922B CN 202111266358 A CN202111266358 A CN 202111266358A CN 113913922 B CN113913922 B CN 113913922B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
Abstract
The invention discloses a method for setting liquid gap of a single crystal furnace, which comprises the following steps: the method comprises the following steps of (1) descending a heat shield provided with a positioning device to a preset position of a single crystal furnace, wherein the positioning device is used for positioning a first descending position of seed crystals, and the distance between the first descending position and the lower edge of the heat shield is a; lowering the seed crystal to a first lowered position; continuously descending the seed crystal from the first descending position to a second descending position, wherein the second descending position is located below the lower edge of the heat shield, the distance between the second descending position and the first descending position is L, L = H + a, and H is the distance between liquid ports; and lifting the crucible to the liquid level of the silicon material in the crucible to be in contact with the lower end of the seed crystal positioned at the second descending position, and stopping lifting the crucible. According to the method for setting the liquid opening distance of the single crystal furnace, the seed crystal is lowered to the liquid opening distance required by the process in advance through the positioning device, and then the crucible is lifted to enable the liquid level of the silicon material to be in contact with the seed crystal, so that the accuracy and the consistency of the liquid opening distance setting are improved.
Description
Technical Field
The invention relates to the technical field of monocrystalline silicon production, in particular to a method for setting liquid gap distance of a monocrystalline furnace.
Background
In the process of pulling a single crystal by Czochralski method, the guide cylinder is used for controlling the flow form of protective gas (such as argon), weakening the temperature difference between the upper part and the lower part and reducing the influence of the gas flow on the growth of the single crystal silicon. The distance from the lower edge of the draft tube to the surface of the molten silicon (referred to herein as the gap) greatly affects the growth of the silicon single crystal. Therefore, accurate measurement of the liquid gap is required. The temperature in the single crystal furnace is very high, and the requirement on the cleanness of the environment in the single crystal furnace is higher, and the direct measurement of the distance of a liquid opening in the single crystal furnace is difficult to realize by the existing material technology.
At present, the liquid gap is mostly set by depending on the observation and judgment of human eyes, and a real numerical value of the liquid gap is not actually measured. On one hand, different people have different judgment methods for the actual liquid opening distance in the single crystal furnace, and on the other hand, the liquid opening distance is judged by the same person twice. And the liquid port distances of various enterprises in the industry are judged and controlled by different methods in process regulations, so that many production operators with abundant experience are difficult to adapt quickly due to different processes when setting the liquid port distances in different enterprises.
Therefore, how to realize the accurate setting of the liquid gap is a technical problem that needs to be solved by those skilled in the art.
Disclosure of Invention
In view of the above, the present invention provides a method for setting a liquid gap of a single crystal furnace, so as to replace the setting of the liquid gap by human eye observation and judgment, and realize the accurate setting of the liquid gap.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for setting liquid gap distance of a single crystal furnace comprises the following steps:
a heat shield descending step: the method comprises the following steps of (1) lowering a heat shield to a preset position of a single crystal furnace, wherein the heat shield is provided with a positioning device for positioning a first lowering position of seed crystals, and the distance between the first lowering position and the lower edge of the heat shield is a;
a seed crystal first descending step: lowering the seed crystal to a first lowered position;
a second descending step of the seed crystal: continuously descending the seed crystal from the first descending position to a second descending position, wherein the second descending position is located below the lower edge of the heat shield, the distance between the second descending position and the first descending position is L, L = H + a, and H is the distance between liquid ports;
a crucible lifting step: and (4) lifting the crucible to the liquid level of the silicon material in the crucible to contact with the lower end of the seed crystal positioned at the second descending position, and stopping lifting the crucible.
Preferably, in the heat shield descending step in the method for setting the liquid gap distance of the single crystal furnace, the positioning device is a heat shield cover plate horizontally arranged at the lower edge of the heat shield, and the distance a is 0.
Preferably, in the method for setting the liquid gap of the single crystal furnace, the heat shield cover plate is made of a conductive material and is in contact with the heat shield, and a hoisting device for hoisting the seed crystal and a heat shield passage are realized when the seed crystal contacts the heat shield cover plate, so that the seed crystal is controlled to descend to the first descending position and stop descending.
Preferably, in the method for setting the liquid gap distance of the single crystal furnace, the first step of lowering the seed crystal is specifically: and detecting the voltage value on the hoisting equipment for hoisting the seed crystal, and when the voltage value is reduced from the first preset voltage value to the second preset voltage value, reducing the seed crystal to the first reduction position.
Preferably, in the method for setting the liquid gap distance of the single crystal furnace, the first preset voltage value is 7-9V, and the second preset voltage value is 0-3V.
Preferably, in the method for setting the liquid gap distance of the single crystal furnace, a step of lowering the seed crystal first and a step of lowering the seed crystal second further comprise,
taking down the heat shield cover plate: taking down the heat shield cover plate positioned at the lower edge of the heat shield;
seed crystal replacement: the seed crystal is removed and replaced with a new seed crystal, and the new seed crystal is lowered to the first lowered position.
Optionally, in the heat shield descending step in the method for setting the liquid gap distance of the single crystal furnace, the positioning device is a correlation sensor, and when the seed crystal descends to the first descending position, the correlation sensor generates a signal change to stop the descending action of the seed crystal by the feedback controller.
Preferably, in the method for setting the liquid gap distance of the single crystal furnace, the positioning device is arranged at the lower edge of the heat shield, wherein the distance a is 0.
Preferably, in the above method for setting the liquid gap of the single crystal furnace, H is in the range of 20 to 40mm.
Preferably, in the method for setting the liquid gap distance of the single crystal furnace, the crucible raising step specifically comprises:
the crucible is lifted, when the voltage value of the liquid level is reduced from a third preset voltage value to a fourth preset voltage value, the liquid level of the silicon material in the crucible is contacted with the lower end of the seed crystal positioned at a second descending position, and the crucible is stopped to be lifted; the liquid level voltage value is a voltage value on hoisting equipment for hoisting seed crystals, the third preset voltage value is 7-9V, and the fourth preset voltage value is 0-3V.
The technical scheme is different from the prior art in that the liquid mouth distance is set in a measuring and calculating mode instead of a human eye observation mode, and the liquid mouth distance is accurately set. According to the scheme, a first descending position of the seed crystal is positioned through a positioning device arranged on a heat shield, a second descending position of the seed crystal is obtained through the distance a between the first descending position and the lower edge of the heat shield and the liquid opening distance H required to be arranged, the distance L between the second descending position and the first descending position is set, then L = H + a, the crucible is lifted until the liquid level of the silicon material in the crucible is contacted with the lower end of the seed crystal positioned at the second descending position, the crucible is stopped to ascend, and the liquid opening distance at the moment is the liquid opening distance H required by the process.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of a method for setting a liquid gap of a single crystal furnace according to an embodiment of the present invention;
FIG. 2 is a schematic view of a seed crystal lowered position using a heat shield cover according to an embodiment of the present invention;
wherein, 10 heat shield cover plates, 20 heat shields, 30 silicon material liquid level, 40 seed crystals, P1 is a first descending position, and P2 is a second descending position.
Detailed Description
The core of the invention is to disclose a method for setting the liquid mouth distance of the single crystal furnace, so as to replace the setting of the liquid mouth distance by human eye observation and judgment and realize the accurate setting of the liquid mouth distance.
In order that those skilled in the art will better understand the solution of the present invention, embodiments of the present invention will be described below with reference to the accompanying drawings. The embodiments described below do not limit the contents of the invention described in the claims. The entire contents of the configurations shown in the following embodiments are not limited to those required as solutions of the inventions described in the claims.
In the existing Czochralski pulling single crystal process, the temperature in the single crystal furnace is very high, the requirement on the cleanness of the environment in the single crystal furnace is high, and the existing material technology cannot support the direct measurement of the liquid mouth distance in the single crystal furnace, so the arrangement of the liquid mouth distance depends on the observation and judgment of human eyes. However, different people have different judgment methods for the actual liquid opening distance in the single crystal furnace, and the liquid opening distance judged by the same person twice can generate errors, so that the liquid opening distance is not accurately set.
In order to overcome the technical problem, the inventor designs a method for setting the liquid opening distance of the single crystal furnace by ingenious conception, the method comprises the steps of positioning a first descending position of a seed crystal through a positioning device arranged on a heat shield, obtaining a second descending position of the seed crystal through the distance a between the first descending position and the lower edge of the heat shield and the liquid opening distance H required to be set, enabling the distance between the second descending position and the first descending position to be L, enabling L = H + a, then ascending the crucible until the liquid level of silicon materials in the crucible is contacted with the lower end of the seed crystal positioned at the second descending position, and stopping ascending the crucible, wherein the liquid opening distance at the moment is the liquid opening distance H required by the process. The method can realize the accurate setting of the liquid mouth distance without depending on the judgment of human eyes. For details, see the detailed description below.
As shown in FIG. 1 and FIG. 2, the embodiment of the invention discloses a method for setting the liquid gap distance of a single crystal furnace, which comprises the following steps:
step S01: the heat shield 20 is descended to the preset position of the single crystal furnace
The heat shield 20 is lowered to a preset position of the single crystal furnace, and the preset position should be used for lowering the heat shield 20 to a proper position in the single crystal furnace according to the actual requirements of the monocrystalline silicon growth process, in this embodiment, the heat shield 20 may be lowered to a lower limit position of a lifting device for driving the heat shield 20 to be lowered.
It should be noted that the difference between the heat shield 20 of the present embodiment and the heat shield 20 of the prior art is that the heat shield 20 is provided with a positioning device for positioning the first lowered position of the seed crystal 40 at least in this step, and the configuration of the positioning device is not limited as long as the positioning of the seed crystal 40 can be achieved, and the positional relationship between the seed crystal 40 and the heat shield 20 in the single crystal furnace can be specified by the positioning device. The fixed position of the positioning device in the heat shield 20 is not limited, for example, the distance between the first descending position and the lower edge of the heat shield 20 is a, and in order to determine the liquid outlet distance, it is preferable to set the distance a to 0, and it should be noted that a may also be greater than 0.
Step S02: lowering the seed crystal 40 to a first lowered position
The seed crystal 40 is lowered to the first lowered position, and since the heat shield 20 is provided with a positioning means for positioning the first lowered position, when the seed crystal 40 is lowered, the seed crystal 40 is stopped from being further lowered when the seed crystal is lowered to the first lowered position determined by the positioning means.
Step S03: lowering the seed crystal 40 to a second lowered position
And continuously descending the seed crystal 40 from the first descending position to a second descending position, wherein the second descending position is positioned below the lower edge of the heat shield 20, the distance between the second descending position and the first descending position is L, L = H + a, H is the distance between liquid ports, and the seed crystal 40 can reach the second descending position by setting the lifting device on the upper part of the seed crystal 40 to lower the seed crystal 40 by the height of L.
It should be noted that the second descending position of the seed crystal 40, that is, the position of the seed crystal 40 at the liquid-gap distance H meeting the process requirement, at this time, the height of the seed crystal 40 beyond the lower edge of the heat shield 20 is L-a, that is, the liquid-gap distance H.
Step S04: the crucible is lifted to ensure that the liquid level 30 of the silicon material in the crucible is contacted with the lower end of the seed crystal 40
And after the seed crystal 40 reaches the second descending position, the silicon material liquid level 30 in the crucible is contacted with the lower end of the seed crystal 40 positioned at the second descending position, and the crucible is stopped to ascend, at the moment, the distance from the lower edge of the heat shield 20 to the silicon material liquid level 30 in the crucible is the height of the seed crystal 40 exceeding the lower edge of the heat shield 20, namely the liquid opening distance H.
According to the method for setting the liquid mouth distance of the single crystal furnace, provided by the invention, the position of the seed crystal 40 is calibrated by carrying out a first descending process on the seed crystal 40, the distance a between the seed crystal 40 and the lower edge of the heat shield 20, namely the relative position between the seed crystal 40 and the heat shield 20, is determined, then the seed crystal 40 reaches a second descending position through a second descending process, the lower end of the seed crystal 40 is controlled to exceed the liquid mouth distance H required by a process at the lower edge of the heat shield 20, and then the liquid mouth distance is set by enabling the liquid level 30 of silicon materials in the crucible to be in contact with the lower end of the seed crystal 40 through the action of ascending the crucible. The method for setting the liquid gap of the single crystal furnace accurately mechanizes the calibration and descending processes, avoids the process of setting the liquid gap by means of human eye observation and judgment, and realizes the accurate setting of the liquid gap.
In another embodiment of the present invention, as shown in fig. 2, the positioning device in step S01 is a heat shield cover horizontally disposed on the lower edge of the heat shield 20, the upper plane of the heat shield cover is closely attached to the lower edge of the heat shield 20, the first lowered position is the lower edge of the heat shield 20, and the distance between the first lowered position and the lower edge of the heat shield 20 is a, where a is 0.
It should be noted that the heat shield cover plate is made of a conductive material and is arranged in contact with the heat shield 20, the heat shield cover plate is used as a positioning device to determine the working principle of the first descending position of the seed crystal 40, when the seed crystal 40 contacts the upper plane of the heat shield cover plate in the descending process, a hoisting device for hoisting the seed crystal 40 forms a passage with the heat shield 20, a voltage sensor arranged on the hoisting device detects that the value changes, the controller controls the hoisting device to stop descending, and at this time, the seed crystal 40 is located at the first descending position.
It should be further noted that the step of lowering the seed crystal 40 to the first lowering position specifically includes: the voltage sensor is arranged on the seed crystal 40 hoisting equipment, the voltage value on the hoisting equipment is detected, when the voltage value is reduced from the first preset voltage value to the second preset voltage value, the seed crystal 40 is judged to be reduced to the first reduction position, and the controller controls the hoisting equipment to stop the reduction action. In the above steps, the first preset voltage value is 7-9V, and the second preset voltage value is 0-3V.
In order to further optimize the above solution, in this embodiment, when the heat shield cover plate is used as the positioning device, between step S02 and step S03, the method further includes:
step of taking down heat shield cover plate
After the seed crystal 40 is lowered to the first lowered position by using the heat shield, the heat shield needs to be removed and then the subsequent lowering operation of the seed crystal 40 is performed in order to allow the seed crystal 40 to continue to be lowered to the second lowered position.
When the heat shield cover plate is used as a positioning device, the descending action is stopped through the voltage change when the seed crystal 40 contacts the upper plane of the heat shield cover plate, the contact between the lower end of the seed crystal 40 and the upper plane of the heat shield cover plate can cause the lower end of the seed crystal 40 to be damaged, and the subsequent growth speed of monocrystalline silicon is influenced, so the stroke of descending the seed crystal 40 to the first descending position needs to be recorded, and after the seed crystal 40 is replaced, a new seed crystal is descended to the first descending position according to the stroke, and then the subsequent descending action is carried out.
In another embodiment of the present invention, in the step S01, the positioning device is a correlation sensor, the correlation sensor can detect whether there is an object block therebetween, and when there is an object block therebetween, the correlation sensor signal is interrupted. When the seed crystal 40 descends, the signal of the correlation sensor is changed from on to off, and at the moment, the seed crystal 40 is judged to descend to the first descending position, then the correlation sensor feeds back the signal, and the controller controls the hoisting equipment of the seed crystal 40 to stop descending, so that the action of descending the seed crystal 40 to the first descending position is completed.
It should be noted that the positioning device can be disposed at any position of the heat shield 20 to determine the descending position of the seed crystal 40 to the first descending position, but since the first descending motion of the seed crystal 40 is substantially to determine the relative position of the seed crystal 40 and the heat shield 20, i.e. to calibrate the position of the seed crystal 40, the first descending position is approximately close to the lower edge of the heat shield 20, and the error generated when the liquid gap is subsequently set is smaller. In the present embodiment, the positioning device is preferably disposed at the lower edge of the heat shield 20, i.e., the distance a =0 between the first lowering position and the lower edge of the heat shield 20.
In the above embodiment provided by the present invention, the setting height of the liquid gap required by the process is 20-40mm, and in the above embodiment, the setting height of the liquid gap is preferably 30mm.
In order to further optimize the above solution, the specific operation of raising the crucible in step S04 in the above embodiment is: and (3) lifting the crucible, and when the voltage value of the liquid level is reduced from the third preset voltage value to the fourth preset voltage value, the liquid level 30 of the silicon material in the crucible is contacted with the lower end of the seed crystal 40 at the second descending position, and the lifting of the crucible is stopped.
It should be noted that the liquid level voltage value in step S04 is a voltage value on a hoisting device for hoisting the seed crystal 40, the third preset voltage value is 7-9V, and the fourth preset voltage value is 0-3V.
The above steps are provided only for helping to understand the structure, method and core idea of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the principles of the invention, and these changes and modifications also fall within the scope of the appended claims.
Claims (4)
1. A method for setting liquid gap distance of a single crystal furnace is characterized by comprising the following steps:
a heat shield descending step: the method comprises the following steps of (1) lowering a heat shield to a preset position of a single crystal furnace, wherein the heat shield is provided with a positioning device for positioning a first lowering position (P1) of seed crystals, and the distance between the first lowering position (P1) and the lower edge of the heat shield is a;
a seed crystal first descending step: lowering the seed crystal to the first lowered position (P1);
taking down the positioning device: taking down the positioning device positioned at the lower edge of the heat shield;
seed crystal replacement: taking down the seed crystal and replacing the seed crystal with a new seed crystal, and descending the new seed crystal to a first descending position (P1);
a second descending step of the seed crystal: continuing to lower the seed crystal from the first lowered position (P1) to a second lowered position (P2), the second lowered position (P2) being located below the lower edge of the heat shield, the second lowered position (P2) being spaced from the first lowered position (P1) by a distance L, wherein L = H + a, and H is the liquid gap;
a crucible lifting step: the crucible is lifted to the liquid level of the silicon material in the crucible and is contacted with the lower end of the seed crystal positioned at the second descending position (P2), and the crucible is stopped to be lifted;
the positioning device is a heat shield cover plate (10), the heat shield cover plate (10) is made of a conductor material and is in contact with the heat shield, and a hoisting device for hoisting the seed crystal and a heat shield passage are realized when the seed crystal is in contact with the heat shield cover plate (10) so as to control the seed crystal to descend to a first descending position (P1) and stop descending;
the positioning device can also be a correlation sensor, and when the seed crystal descends to a first descending position (P1), the correlation sensor generates signal change to stop the descending action of the seed crystal by a feedback controller;
the seed crystal first descending step specifically comprises the following steps: detecting a voltage value on hoisting equipment for hoisting seed crystals, and when the voltage value is reduced from a first preset voltage value to a second preset voltage value, lowering the seed crystals to a first reduction position (P1), wherein the first preset voltage value is 7-9V, and the second preset voltage value is 0-3V;
the crucible lifting step specifically comprises the following steps: the crucible is lifted, when the voltage value of the liquid level is reduced from a third preset voltage value to a fourth preset voltage value, the liquid level of the silicon material in the crucible is contacted with the lower end of the seed crystal positioned at a second descending position (P2), and the crucible is stopped to be lifted; the liquid level voltage value is a voltage value on hoisting equipment for hoisting seed crystals, the third preset voltage value is 7-9V, and the fourth preset voltage value is 0-3V.
2. The method for setting the liquid gap distance of the single crystal furnace according to claim 1, wherein in the heat shield descending step, the positioning means is a heat shield cover plate (10) horizontally disposed at a lower edge of the heat shield, and wherein the distance a is 0.
3. The method for setting the liquid gap distance of the single crystal furnace according to claim 1, wherein the correlation sensor is disposed at the lower edge of the heat shield, and the distance a is 0.
4. A method of setting a liquid gap of a single crystal furnace according to any one of claims 1 to 3, wherein H is in a range of 20 to 40mm.
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| CN114543728A (en) * | 2022-01-26 | 2022-05-27 | 弘元新材料(包头)有限公司 | Novel liquid gap calibration method |
| CN114808115B (en) * | 2022-04-28 | 2023-08-15 | 晶科能源股份有限公司 | Liquid mouth distance measuring method and liquid mouth distance testing device |
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| JPWO2016038817A1 (en) * | 2014-09-12 | 2017-06-01 | 信越半導体株式会社 | Single crystal manufacturing method |
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| CN110552059A (en) * | 2019-09-19 | 2019-12-10 | 宁夏隆基硅材料有限公司 | Liquid gap positioning device and method and single crystal furnace |
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| JPWO2016038817A1 (en) * | 2014-09-12 | 2017-06-01 | 信越半導体株式会社 | Single crystal manufacturing method |
| CN106435714A (en) * | 2015-08-07 | 2017-02-22 | 特变电工新疆新能源股份有限公司 | Polycrystalline silicon solution liquid level distance positioning method |
| CN207862479U (en) * | 2017-11-07 | 2018-09-14 | 宁夏隆基硅材料有限公司 | A kind of single crystal growing furnace is with automatic crystal pulling liquid mouth away from accurate-location device |
| CN110552059A (en) * | 2019-09-19 | 2019-12-10 | 宁夏隆基硅材料有限公司 | Liquid gap positioning device and method and single crystal furnace |
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Effective date of registration: 20230829 Address after: 014020 No. 18 Chuangye Street, Binhe New Area, Baotou Rare Earth High tech Industrial Development Zone, Baotou City, Inner Mongolia Autonomous Region Patentee after: Shuangliang Xinneng Technology (Baotou) Co.,Ltd. Address before: 014062 No. 35, Cuihu Road, Binhe new area, Rare Earth Development Zone, Baotou City, Inner Mongolia Autonomous Region Patentee before: Shuangliang silicon material (Baotou) Co.,Ltd. |