CN116200817A - Power pulse seeding method - Google Patents
Power pulse seeding method Download PDFInfo
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- CN116200817A CN116200817A CN202310069824.3A CN202310069824A CN116200817A CN 116200817 A CN116200817 A CN 116200817A CN 202310069824 A CN202310069824 A CN 202310069824A CN 116200817 A CN116200817 A CN 116200817A
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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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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/14—Measures for saving energy, e.g. in green houses
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- Crystallography & Structural Chemistry (AREA)
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- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention belongs to the technical field of monocrystalline silicon manufacture, and relates to a power pulse seeding method; the seeding process is divided into three stages, in the third stage of seeding, the actual seeding liquid level brightness value is compared with the target seeding liquid level brightness value, if the actual seeding liquid level brightness value is not in the range of the target seeding liquid level brightness value, the seeding power adjustment quantity is calculated according to the deviation of the target seeding liquid level brightness value and the actual seeding liquid level brightness value, if the actual seeding liquid level brightness value is greater than the target seeding liquid level brightness value, the seeding temperature is higher, and the power pulse adjustment is reduced; if the actual seeding liquid level brightness value is less than the target seeding liquid level brightness value, the seeding temperature is lower, and the power pulse is adjusted and increased; according to the invention, the power adjustment amount is obtained by monitoring the liquid level brightness deviation amount and calculating, and the power adjustment is realized through a plurality of adjustment periods, so that the temperature is controlled within the process requirement range, the technical difficulty of seeding is greatly reduced, the seeding survival rate is improved, the invalid working hours are reduced, and the single crystal yield is improved.
Description
Technical Field
The invention belongs to the technical field of monocrystalline silicon manufacturing, and particularly relates to a power pulse seeding method.
Background
In the single crystal silicon rod pulling industry, along with the technical development and iteration for years, the automation degree of a single crystal furnace is remarkably improved, and the automatic pulling can be basically realized at present. The temperature-regulating seeding process in the single crystal pulling process is used as a heavy center of single crystal growth, a key step of single crystal growth is determined, the optimal interval range is required for single crystal seeding temperature in the prior art, but the proportion of the interval range is controlled to be 80%, so that partial seeding does not meet the process requirement, the temperature-regulating seeding is performed again, the working efficiency is greatly reduced, the labor burden is caused for operators, and the labor and working hour cost of a company are greatly wasted.
The key point of seeding is the control of seeding temperature, which directly relates to the success or failure of seeding and the stability of crystal pulling. At present, the seeding temperature adjustment process cannot realize absolute temperature measurement, and meanwhile, the liquid level temperature measurement value is inaccurate due to the rotation of the liquid level in the temperature adjustment seeding process, so that the seeding temperature cannot realize an accurate value. In addition, in the prior art, the seeding temperature is judged whether to be suitable by measuring the pulling speed data of the seeding target, but the large-size thermal field has large inertia and hysteresis due to slower temperature reaction. According to the pulling speed judgment and adjustment in the seeding process, excessive adjustment phenomenon often occurs, and precise control on seeding temperature adjustment cannot be realized. The crystal formation rate can be greatly improved only by matching the design of the parameters of the Czochralski single crystal pulling process with the optimal seeding temperature interval, and the prior art cannot reach the optimal temperature adjustment interval by 100 percent, so that the success rate of subsequent shoulder-release and constant diameter links is low, the crystal formation rate of the single crystal is affected, and the temperature adjustment seeding becomes a technological difficulty.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a power pulse seeding method, which solves the problem that the temperature adjustment cannot achieve 100% of precision to reach a target temperature adjustment interval, monitors the liquid level brightness deviation in the seeding process, obtains the power adjustment amount by calculation, and controls the target temperature to be within a process requirement range by power adjustment in a plurality of adjustment periods, thereby greatly reducing the technical difficulty of seeding, improving the seeding survival rate, reducing invalid working hours and improving the single crystal yield.
The aim of the invention is realized by the following technical scheme: a power pulse seeding method, the method comprising:
the first stage of seeding: a coarse crystal extension stage, namely extending the coarse crystal on the basis of the original seed crystal to reach the target growth length and the target diameter of the coarse crystal;
and (3) seeding a second stage: in the diameter reduction stage, gradually and continuously reducing the coarse crystal into a target diameter reduction diameter and a target diameter reduction length, and adjusting the seeding pulling speed to achieve the target diameter reduction diameter through the deviation between the actual measured diameter and the target diameter reduction diameter;
and a third stage of seeding: in the fine crystal constant diameter stage, the seeding diameter continuously grows according to the target diameter, the seeding liquid level brightness value is monitored from 1-150mm from the seeding start in the third stage, the actual seeding liquid level brightness value is measured through a camera, the actual seeding liquid level brightness value is compared with the target seeding liquid level brightness value, if the actual seeding liquid level brightness value is not in the target seeding liquid level brightness value range, the seeding power adjustment amount is calculated according to the deviation of the target seeding liquid level brightness value and the actual seeding liquid level brightness value, if the actual seeding liquid level brightness value is larger than the target seeding liquid level brightness value, the seeding temperature is higher, and the power pulse adjustment is reduced; if the actual seeding liquid level brightness value is less than the target seeding liquid level brightness value, the seeding temperature is lower, and the power pulse is adjusted and increased.
The first stage of seeding aims to prolong coarse grains on the basis of the original seed crystals and improve the use times of the seed crystals; the camera of the first stage of seeding uses an industrial high-definition CCD camera, a camera bracket is adopted to be fixed on a CCD observation window of the single crystal furnace, and the installation angle positions of the cameras are uniformly fixed; in the third stage of seeding, judging whether the actual seeding liquid level brightness value is within the range of the target seeding liquid level brightness value, and if not, obtaining the seeding power adjustment quantity through a seeding power adjustment quantity formula; setting an adjustment period and a power adjustment duration. And adjusting the interval period, obtaining the power pulse adjusting amplitude through a formula, and performing pulse power adjustment.
Preferably, the camera exposure is uniformly set to 15000; the camera picture adopts fixed coordinates, the picture is internally provided with a coordinate axis, the brightness acquisition point is fixed with coordinates, and the coordinates of the brightness acquisition position of the camera are (x, y): (550,500).
Preferably, in the third stage of seeding, the brightness value of the target seeding liquid level is 50Pit, and the brightness value range of the target seeding liquid level is 50+/-0.5 Pit.
Preferably, the calculation formula of the seeding power adjustment amount is Δpower=Δv×d;
wherein Δpower is the seeding power adjustment; deltaV is the deviation between the brightness value of the target seeding liquid level and the brightness value of the actual seeding liquid level; d is the power adjustment coefficient of 0.1-0.15.
Preferably, the power pulse adjustment amplitude calculation formula is P- (x×n/5);
wherein P is the primary seeding power; absolute value of the X seeding power adjustment; n adjustment periods.
Preferably, the single power pulse in the third seeding stage has an adjustment amplitude of 5-8kw; the power adjustment duration is 5-10s; the interval period is regulated to be the seeding length, and the period length is set to be 10-20mm.
Preferably, the seeding third stage comprises 5 periods; in the third stage of seeding, the power amplitude is regulated to 8kw by a single pulse; the adjusting period is that the seeding length is 20mm; the power adjustment duration was 10s.
Preferably, the first stage of seeding uses a fixed pulling rate of 150mm/hr to prolong the coarse crystals, and the target growth length of the coarse crystals is 20-30mm; the target diameter of the coarse crystals is 16+/-2 mm.
Preferably, the target diameter reduction diameter of the seeding second stage is 5+/-0.5 mm; the target reducing length is 50mm.
The invention has the following beneficial effects: (1) The seeding is divided into 3 stages, and in the third stage of seeding, the deviation between the brightness value of the target seeding liquid surface and the brightness value of the actual seeding liquid surface is adopted, the seeding power adjustment quantity is obtained through calculation, and the power adjustment is completed through 5 power pulses, so that the problem of inaccurate temperature in the seeding temperature adjustment process is corrected; the method solves the problems that absolute temperature measurement cannot be realized in the current seeding temperature adjusting process, and meanwhile, the liquid level temperature measurement value is inaccurate due to the rotation of the liquid level in the temperature adjusting seeding process, so that the seeding temperature cannot realize an accurate value; solves the problem that excessive adjustment frequently occurs in the conventional seeding process of judging and adjusting the pulling speed.
(2) According to the invention, the liquid level brightness deviation is monitored in the seeding process, the power adjustment amount is obtained by calculation, and the power adjustment is realized through a plurality of adjustment periods, so that the temperature is controlled within the process requirement range, the technical difficulty of seeding is greatly reduced, the seeding survival rate is improved, the invalid working hours are reduced, and the single crystal yield is improved.
(3) The invention is more suitable for the actual application scene of the prior large-size thermal field, and can effectively improve the large inertia of the large-size thermal field. Slow temperature reaction and the like.
Drawings
FIG. 1 is a schematic diagram of a power pulse seeding process according to the present invention;
fig. 2 is a schematic diagram of pulse power adjustment related to a power pulse seeding method according to the present invention.
In the figure: 11 coarse grain extension stage, 12 diameter reduction stage and 13 fine grain isodiametric stage.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to be limiting.
As shown in fig. 1-2, a power pulse seeding method is provided, which comprises the following steps:
the first stage of seeding: a coarse crystal extension stage 11 for extending the coarse crystal on the basis of the original seed crystal to reach the target growth length and the target diameter of the coarse crystal; the main purpose of the stage is to prolong coarse crystals on the basis of the original seed crystals and improve the use times of the seed crystals; the fixed pulling rate is used for growing coarse crystals at 150mm/hr, and the target growth length of the coarse crystals is 20-30mm; the target diameter of the coarse crystals is 16+/-2 mm;
and (3) seeding a second stage: the diameter reduction stage 12 is to continuously reduce the coarse crystal into a target diameter reduction diameter of 5+/-0.5 mm and a target diameter reduction length of 50mm step by step, and adjust the seeding pulling speed to achieve the target diameter reduction diameter through the deviation between the actual measured diameter and the target diameter reduction diameter;
and a third stage of seeding: the fine crystal constant diameter stage 13, the seeding diameter continuously grows according to the target diameter reduction diameter of 5+/-0.5 mm, and the power pulse seeding is adjusted for the seeding stage of 1-150 mm;
starting to monitor the brightness value of the seeding liquid level from 1-150mm from the seeding in the third stage, and setting the brightness value of the target seeding liquid level to be 50+/-0.5 Pit; measuring an actual seeding liquid level brightness value through a camera, comparing the actual seeding liquid level brightness value with a target seeding liquid level brightness value, and calculating a seeding power adjustment quantity according to the deviation between the target seeding liquid level brightness value and the actual seeding liquid level brightness value if the actual seeding liquid level brightness value is not in the target seeding liquid level brightness value range; if the actual seeding liquid level brightness value is larger than the target seeding liquid level brightness value, the seeding temperature is higher, and the power pulse adjustment is reduced; if the actual seeding liquid level brightness value is less than the target seeding liquid level brightness value, the seeding temperature is lower, and the power pulse is adjusted and increased.
The camera uses an industrial high-definition camera CCD camera, a camera bracket is adopted to be fixed on a CCD observation window of the single crystal furnace, the installation angle positions of the cameras are uniformly fixed, the picture of the camera is fixed by adopting coordinates, the picture is internally provided with coordinate axes, the brightness is fixed by adopting coordinates, and the brightness acquisition position coordinates of the camera are (x, y): (550,500).
The calculation formula of the seeding power adjustment quantity is delta power=delta v×d;
wherein Δpower is the seeding power adjustment; deltaV is the deviation between the brightness value of the actual seeding liquid level and the brightness value of the target seeding liquid level; d is the power adjustment coefficient of 0.1-0.15;
the power pulse adjusting amplitude calculation formula is P- (X n/5);
wherein P is the primary seeding power; absolute value of the X seeding power adjustment; n adjustment periods.
Setting the single power pulse adjusting amplitude in the third seeding stage to be 5-8kw; the power adjustment duration is 5-10s; the interval period is regulated to be the seeding length, and the period length is set to be 10-20mm.
Example 1
The first stage of seeding: a coarse crystal extension stage 11, in which the coarse crystal is obtained by extending 30mm on the basis of the original seed crystal, and the coarse crystal is grown at a fixed pulling rate of 150mm/hr, and the target diameter of the coarse crystal is 16mm;
and (3) seeding a second stage: a diameter reduction stage 12, in which the coarse crystals are gradually and continuously reduced to a target diameter reduction diameter of 5+/-0.5 mm and a target diameter reduction length of 50mm, and the pulling speed is adjusted to achieve the target diameter reduction diameter by actually measuring the deviation between the diameter and the target diameter reduction diameter;
and a third stage of seeding: the fine crystal constant diameter stage 13, the seeding diameter continuously grows according to the target diameter reduction diameter of 5+/-0.5 mm, and the power pulse seeding is adjusted for the seeding stage of 1-150 mm; monitoring the average value of the brightness of the seeding liquid level from 1-150mm from the third stage, measuring the brightness of the actual seeding liquid level by a camera,
setting the brightness value of the liquid level of the target seeding as 50Pit, wherein the brightness value range of the liquid level of the target seeding is 50+/-0.5 Pit, and the actual seeding liquid level brightness is measured as 55Pit by a seeding starting system to obtain the deviation delta V= -5Pit of the brightness value of the liquid level of the target seeding and the brightness value of the actual seeding liquid level; if the deviation is within the 50+/-0.5 Pit range of the brightness value of the target seeding liquid level, no adjustment is needed;
obtaining a seeding power adjustment quantity of-0.5 kw through a calculation formula delta power=delta V x d= -5 x 0.1= -0.5 (kw) of the seeding power adjustment quantity;
setting the seeding third stage to comprise 5 periods, and adjusting the power to be-0.5 kw altogether, namely, setting the seeding length to be 100mm; the power amplitude of the single pulse is regulated to 8kw; the adjusting period is that the seeding length is 20mm; the power adjustment duration is 10s;
seeding power pulse adjustment as shown in fig. 2, the initial seeding power is 60kw; the brightness value of the actual seeding liquid level is 55Pit
The first power adjustment, the initial seeding power is reduced by 8kw, the continuous 10s is finished, the formula P- (X X n/5) =60- (0.5X 1/5) =59.9 kw is calculated according to the power pulse adjustment amplitude, the power pulse adjustment amplitude is 59.9kw, then the seeding power is quickly restored to 59.9kw, when the second adjustment starting node is 20mm longer than the seeding length, the adjustment is started, and the 5 pulse adjustment is completed by analogy;
when the seeding length reaches 70mm, the power of the first pulse is reduced to 52kw, the duration is 10s, and the power is adjusted back to 59.9kw;
when the seeding length reaches 90mm, the power of the second pulse is reduced to 53kw for 10 seconds, and the power is adjusted back to 59.8 kw;
when the seeding length reaches 110mm, the power of the third pulse is reduced to 54kw for 10 seconds, and the power is adjusted back to 59.7 kw;
when the seeding length reaches 130mm, the fourth pulse power is reduced to 55kw, the duration is 10s, and the power is adjusted back to 59.6kw;
when the seeding length reached 150mm, the fifth pulse power was reduced to 56kw for a duration of 10s and the power was adjusted back to 59.5kw. And (5) finishing the power cooling amount by adjusting the power pulse of 5 periods. The seeding power of the later stage is kept constant at 59.5kw until the seeding is completed.
The foregoing has outlined and described the basic principles, features, and advantages of the present invention. However, the foregoing is merely specific examples of the present invention, and the technical features of the present invention are not limited thereto, and any other embodiments that are derived by those skilled in the art without departing from the technical solution of the present invention are included in the scope of the present invention.
Claims (9)
1. A power pulse seeding method, characterized in that the method comprises the following steps:
the first stage of seeding: a coarse crystal extension stage (11) for extending the coarse crystal on the basis of the original seed crystal to reach the target growth length and the target diameter of the coarse crystal;
and (3) seeding a second stage: a diameter reduction stage (12) for gradually and continuously reducing the coarse crystal into a target diameter reduction diameter and a target diameter reduction length, and adjusting the pulling speed to achieve the target diameter reduction diameter through the deviation between the actual measured diameter and the target diameter reduction diameter;
and a third stage of seeding: a fine crystal constant diameter stage (13) in which the seeding diameter continuously grows according to the target diameter, the seeding liquid level brightness value is monitored from 1-150mm from the seeding start in the third stage, the actual seeding liquid level brightness value is measured by a camera, the actual seeding liquid level brightness value is compared with the target seeding liquid level brightness value, if the actual seeding liquid level brightness value is not in the target seeding liquid level brightness value range, the seeding power adjustment amount is calculated according to the deviation of the target seeding liquid level brightness value and the actual seeding liquid level brightness value, if the actual seeding liquid level brightness value is greater than the target seeding liquid level brightness value, the seeding temperature is higher, and the power pulse adjustment is reduced; if the actual seeding liquid level brightness value is less than the target seeding liquid level brightness value, the seeding temperature is lower, and the power pulse is adjusted and increased.
2. The power pulse seeding method according to claim 1, wherein the camera exposure is uniformly set to 15000; the camera picture adopts fixed coordinates, the picture is internally provided with a coordinate axis, the brightness acquisition point is fixed with coordinates, and the coordinates of the brightness acquisition position of the camera are (x, y): (550,500).
3. The method of claim 1, wherein the target seeding level brightness value in the third stage of seeding is 50Pit, and the range of target seeding level brightness values is 50±0.5Pit.
4. The power pulse seeding method according to claim 1, wherein the calculation formula of the seeding power adjustment amount is Δpower=Δv×d;
wherein Δpower is the seeding power adjustment; deltaV is the deviation between the brightness value of the target seeding liquid level and the brightness value of the actual seeding liquid level; d is the power adjustment coefficient of 0.1-0.15.
5. The power pulse seeding method according to claim 1, wherein the power pulse adjustment amplitude calculation formula is P- (X n/5);
wherein P is the primary seeding power; absolute value of the X seeding power adjustment; n adjustment periods.
6. The power pulse seeding method according to claim 4, wherein the single power pulse in the third seeding stage has an adjustment amplitude of 5-8kw; the power adjustment duration is 5-10s; the interval period is regulated to be the seeding length, and the period length is set to be 10-20mm.
7. The power pulse seeding method according to claim 4, wherein the third stage of seeding comprises 5 periods; in the third stage of seeding, the power amplitude is regulated to 8kw by a single pulse; the adjusting period is that the seeding length is 20mm; the power adjustment duration was 10s.
8. The power pulse seeding method according to claim 1, wherein the seeding first stage uses a fixed pull rate of 150mm/hr to lengthen the coarse crystals, and the target growth length of the coarse crystals is 20-30mm; the target diameter of the coarse crystals is 16+/-2 mm.
9. The power pulse seeding method according to claim 1, wherein the target diameter reduction diameter of the second seeding stage is 5+ -0.5 mm; the target reducing length is 50mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310069824.3A CN116200817A (en) | 2023-02-07 | 2023-02-07 | Power pulse seeding method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310069824.3A CN116200817A (en) | 2023-02-07 | 2023-02-07 | Power pulse seeding method |
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| CN116200817A true CN116200817A (en) | 2023-06-02 |
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| CN202310069824.3A Pending CN116200817A (en) | 2023-02-07 | 2023-02-07 | Power pulse seeding method |
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- 2023-02-07 CN CN202310069824.3A patent/CN116200817A/en active Pending
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