CN112725884A - Device and method for detecting liquid level distance of molten silicon in Czochralski single crystal growth process - Google Patents
Device and method for detecting liquid level distance of molten silicon in Czochralski single crystal growth process Download PDFInfo
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- CN112725884A CN112725884A CN202011515946.3A CN202011515946A CN112725884A CN 112725884 A CN112725884 A CN 112725884A CN 202011515946 A CN202011515946 A CN 202011515946A CN 112725884 A CN112725884 A CN 112725884A
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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
- C30B15/22—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal
- C30B15/26—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal using television detectors; using photo or X-ray detectors
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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
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a device and a method for detecting the liquid level distance of molten silicon in the growth process of czochralski single crystal, wherein the device comprises a quartz pin and a heat shield, the quartz pin comprises a horizontal part and a main body part, the horizontal part is arranged above the main body part and is mutually vertical to form a T-shaped structure, and the outer vertical surface of the main body part is provided with a reflecting material; the heat shield comprises a guide cylinder, a stepped through hole is formed in the bottom of the guide cylinder, the stepped through hole is composed of a first through hole and a second through hole, a main body part of the quartz pin penetrates through the second through hole and extends out of the bottom of the guide cylinder, and a horizontal part of the quartz pin is arranged in the first through hole; the main body part of the quartz pin vertically extends downwards out of the lower edge of the guide shell to be used as a ruler for measuring distance. The method adopts an inversion method, because the inner edge of the heat shield in the Czochralski crystal growing furnace generates an inversion on the liquid level of the silicon melt, the inversion method utilizes a camera to collect the inversion on the liquid level, and then the position of the inversion edge at the position of the liquid level of the silicon melt in an image is detected.
Description
Technical Field
The invention relates to a distance measuring device for the molten silicon liquid level of a czochralski crystal growing furnace, belonging to the technical field of semiconductor material detection.
Background
Monocrystalline silicon is a good semiconductor material, is the most basic raw material in the electronic information industry and the new energy photovoltaic power generation industry, and is widely applied to the production and manufacture of products such as power rectifiers, high-power transistors, diodes, switching devices, solar cells and the like.
The current methods for producing single crystal silicon mainly include a czochralski method (CZ), a float zone method (FZ), an epitaxial method, a hydrothermal method, and the like. Of which the czochralski method is the most common method in the production of single crystal silicon. During the growth of the Czochralski single crystal, as the pulling apparatus rotationally pulls the single crystal rod upward, the silicon melt volume decreases and the position of the liquid level of the silicon melt continuously lowers. The variation of the surface level of the molten silicon in the crucible is closely related to the temperature gradient in the crystal melt, and according to the Voronkov defect theory, the variation of the temperature gradient at the crystal melt interface is an important factor affecting the quality and yield of the crystal. Therefore, accurate measurement of the molten silicon level distance is very important for producing high quality crystals.
Because the czochralski crystal growing furnace is always in a severe environment with high-temperature sealing and negative pressure in work, the detection of the liquid level position of the silicon melt can only adopt a non-contact measurement method. In the past, when the position of the melt is controlled, a crucible random method, a laser method, an inverted image method and the like are often adopted.
The crucible following method, which is a method in which the crucible lifting rate varies with the crystal lifting during the crystal equal-diameter growth, has a disadvantage of extremely poor accuracy because the actual crystal diameter at the growth stage cannot be accurately measured, and thus cannot meet the requirements of modern material manufacturing. Another common method is to control the position of the melt with a laser. The apparatus comprises a laser generator and a laser receiver, which form an angle and intersect at the surface of the molten silicon, and the position of the melt is controlled by measuring the variation of the intensity of the laser light. It has the disadvantage that it is expensive, the calibration process of the system is too complicated, the requirements on the thermal field design are high, because the thermal field components cannot block the optical path of the laser, otherwise the system will not work.
Disclosure of Invention
The invention aims to provide a device and a method for detecting the liquid level distance of molten silicon in the growth process of a czochralski single crystal so as to measure the height change of the liquid level of the molten silicon during the operation of the czochralski single crystal.
In order to achieve the purpose, the invention adopts the technical scheme that:
an apparatus for detecting a distance of a liquid level of a molten silicon in a growth process of a czochralski single crystal, comprising a quartz pin and a heat shield, wherein:
the quartz pin comprises a horizontal part and a main body part, wherein the horizontal part is arranged above the main body part and is vertical to the main body part to form a T shape, and a reflecting material is arranged on the outer vertical surface of the main body part;
the heat shield comprises a guide cylinder, a stepped through hole is formed in the bottom of the guide cylinder, the stepped through hole is composed of a first through hole located on the inner side of the guide cylinder and a second through hole located on the outer side of the guide cylinder, and the inner diameter of the first through hole is larger than that of the second through hole; the main part of the quartz pin penetrates through the second through hole and extends out of the bottom of the guide shell, and the horizontal part of the quartz pin is arranged in the first through hole; the main body part of the quartz pin vertically extends downwards out of the lower edge of the guide shell to be used as a ruler for measuring distance.
A graphite plate is placed on the horizontal portion of the quartz pin.
The thickness of the horizontal part of the quartz pin is uniform, the verticality of the upper end face of the horizontal part is less than 0.01 by taking the axis of the quartz pin as a benchmark A, the verticality of the horizontal part is less than 0.01 by taking the lower end face of the horizontal part as a benchmark B.
The thickness of the horizontal portion of the quartz pin is greater than the depth of the first through hole by 0.01 mm.
The reflective material is a molybdenum strip or a silicon strip.
The periphery of the reflecting material is wrapped by quartz.
The difference between the distance between the stepped through hole and the center of the crystal bar in the single crystal furnace and the maximum radius of the crystal bar is not less than 30 mm.
A method for measuring the liquid level distance of molten silicon in a single crystal furnace comprises the following steps:
will the device is placed in single crystal growing furnace silicon melt liquid level top, and the record quartz round pin stretches out in the fixed length L of draft tube bottom, rises through the operation crucible, makes the liquid level promote gradually to just contacting the quartz round pin bottom, records the crucible position this moment, then descends crucible position to target liquid level, measures the liquid level of two crucible positions apart from H, and the distance of silicon melt liquid level and draft tube bottom this moment is: s ═ L + H.
Has the advantages that:
the method adopts an inversion method, because the inner edge of the heat shield in the Czochralski crystal growing furnace generates an inversion on the liquid level of the silicon melt, the inversion method utilizes a camera to collect the inversion on the liquid level, and then the position of the inversion edge at the position of the liquid level of the silicon melt in an image is detected. Has the following advantages:
(1) a clearer reflection point is generated;
(2) the influence of crystal diameter change or over-large diameter of monocrystalline silicon on reflection quality in the growth process; the quartz pin is prevented from falling into the melt in the actual production process;
(3) and the liquid level distance measurement error caused by unstable fixation of the quartz pin is reduced.
Drawings
FIG. 1 is a schematic structural view of a quartz pin;
FIG. 2 is a schematic view of a heat shield;
fig. 3 is a schematic structural diagram of the device of the present invention.
Detailed Description
As shown in FIGS. 1 to 3, an apparatus for detecting a liquid level distance of molten silicon in a Czochralski single crystal growing process of the present invention comprises a quartz pin and a heat shield, wherein:
the quartz pin comprises a horizontal part 1 and a main body part 2, wherein the horizontal part 1 is arranged above the main body part 2 and is mutually vertical to form a T shape, and a reflecting material 3 is arranged on the outer vertical surface of the main body part 2;
the heat shield comprises a guide shell 4, a stepped through hole is formed in the bottom of the guide shell 4, the stepped through hole is composed of a first through hole 5 located on the inner side of the guide shell 4 and a second through hole 6 located on the outer side of the guide shell 4, the inner diameter of the first through hole 5 is larger than that of the second through hole 6, the inner diameter of the first through hole 5 is slightly larger than the outer diameter of the horizontal part 1, the inner diameter of the second through hole 6 is slightly larger than that of the main part 2, and the inner diameter of the second through hole 6 is smaller than that of the horizontal part 1; the main body part 2 of the quartz pin passes through the second through hole 6 and extends out of the bottom of the guide shell 4, and the horizontal part 1 of the quartz pin is arranged in the first through hole 5; the main body part 2 of the quartz pin vertically extends downwards out of the lower edge of the guide cylinder 4 to be used as a ruler for measuring distance.
The graphite plate 7 is placed on the horizontal part 1 of the quartz pin and fixed in the vertical direction.
The thickness of the horizontal part 1 of the quartz pin is uniform, the verticality of the upper end surface of the horizontal part 1 is less than 0.01 by taking the axis of the quartz pin as a benchmark A, and the verticality of the horizontal part 1 is less than 0.01 by taking the lower end surface of the horizontal part 1 as a benchmark B.
In order to ensure a firm vertical hold during the measurement, the horizontal part 1 of the quartz pin has a thickness greater than 0.01mm of the depth of the first through hole 5.
The reflecting material 3 is a molybdenum strip or a silicon strip, or other materials with high reflecting performance, and is wrapped by quartz around the reflecting material.
The difference between the distance between the stepped through hole and the center of the crystal bar in the single crystal furnace and the maximum radius of the crystal bar is not less than 30 mm.
Based on the device, the invention provides a method for measuring the liquid level distance of the molten silicon in the single crystal furnace, which comprises the following steps:
place the device in single crystal growing furnace silicon melt liquid level top, record the quartz round pin and stretch out in the fixed length L of draft tube bottom, rise through the operation crucible, make the liquid level promote gradually to just contacting the quartz round pin bottom, record the crucible position this moment, then descend the crucible position to the target liquid level, measure the liquid level of two crucible positions apart from H, the distance of silicon melt liquid level and draft tube bottom this moment is: s ═ L + H.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (8)
1. A device for detecting the liquid level distance of molten silicon in the growth process of Czochralski single crystal is characterized in that: including quartz pin and heat shield, wherein:
the quartz pin comprises a horizontal part (1) and a main body part (2), wherein the horizontal part (1) is arranged above the main body part (2) and is mutually vertical to form a T shape, and a reflecting material (3) is arranged on the outer vertical surface of the main body part (2);
the heat shield comprises a guide shell (4), a step-type through hole is formed in the bottom of the guide shell (4), the step-type through hole is composed of a first through hole (5) located on the inner side of the guide shell (4) and a second through hole (6) located on the outer side of the guide shell (4), and the inner diameter of the first through hole (5) is larger than that of the second through hole (6); the main body part (2) of the quartz pin penetrates through the second through hole (6) and extends out of the bottom of the guide cylinder (4), and the horizontal part (1) of the quartz pin is arranged in the first through hole (5); the main body part (2) of the quartz pin vertically extends downwards out of the lower edge of the guide shell (4) to be used as a ruler for measuring distance.
2. The apparatus as set forth in claim 1, wherein the apparatus comprises: and a graphite plate (7) is placed on the horizontal part (1) of the quartz pin.
3. The apparatus as set forth in claim 1, wherein the apparatus comprises: the thickness of the horizontal part (1) of the quartz pin is uniform, the verticality of the upper end face of the horizontal part (1) is less than 0.01 by taking the axis of the quartz pin as a benchmark A, and the verticality of the horizontal part (1) is less than 0.01 by taking the lower end face of the horizontal part (1) as a benchmark B.
4. The apparatus as set forth in claim 1, wherein the apparatus comprises: the thickness of the horizontal part (1) of the quartz pin is 0.01mm greater than the depth of the first through hole (5).
5. The apparatus as set forth in claim 1, wherein the apparatus comprises: the reflective material (3) is a molybdenum strip or a silicon strip.
6. The apparatus for detecting the liquid surface distance of the silicon melt in the growth of the Czochralski single crystal according to claim 1 or 5, wherein: the periphery of the reflecting material (3) is wrapped by quartz.
7. The apparatus as set forth in claim 1, wherein the apparatus comprises: the difference between the distance between the stepped through hole and the center of the crystal bar in the single crystal furnace and the maximum radius of the crystal bar is not less than 30 mm.
8. A method for detecting a distance of a liquid surface of a molten silicon during a growth of a Czochralski single crystal based on the apparatus of claim 1, characterized in that: the method comprises the following steps:
will the device is placed in single crystal growing furnace silicon melt liquid level top, and the record quartz round pin stretches out in the fixed length L of draft tube bottom, rises through the operation crucible, makes the liquid level promote gradually to just contacting the quartz round pin bottom, records the crucible position this moment, then descends crucible position to target liquid level, measures the liquid level of two crucible positions apart from H, and the distance of silicon melt liquid level and draft tube bottom this moment is: s ═ L + H.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011515946.3A CN112725884A (en) | 2020-12-21 | 2020-12-21 | Device and method for detecting liquid level distance of molten silicon in Czochralski single crystal growth process |
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| CN202011515946.3A CN112725884A (en) | 2020-12-21 | 2020-12-21 | Device and method for detecting liquid level distance of molten silicon in Czochralski single crystal growth process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114808115A (en) * | 2022-04-28 | 2022-07-29 | 晶科能源股份有限公司 | Liquid gap measuring method and liquid gap testing device |
| CN116288662A (en) * | 2023-05-18 | 2023-06-23 | 内蒙古中环领先半导体材料有限公司 | Method for controlling surface distance of Czochralski single crystal liquid |
| WO2023142507A1 (en) * | 2022-01-27 | 2023-08-03 | 中环领先半导体材料有限公司 | Single crystal growth device |
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| WO2023142507A1 (en) * | 2022-01-27 | 2023-08-03 | 中环领先半导体材料有限公司 | Single crystal growth device |
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