CN117488396A - Pulse power temperature regulating method - Google Patents
Pulse power temperature regulating method Download PDFInfo
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- CN117488396A CN117488396A CN202311478547.8A CN202311478547A CN117488396A CN 117488396 A CN117488396 A CN 117488396A CN 202311478547 A CN202311478547 A CN 202311478547A CN 117488396 A CN117488396 A CN 117488396A
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- 238000000034 method Methods 0.000 title claims abstract description 45
- 230000001105 regulatory effect Effects 0.000 title claims abstract description 33
- 239000013078 crystal Substances 0.000 claims abstract description 99
- 239000007788 liquid Substances 0.000 claims abstract description 43
- 238000010899 nucleation Methods 0.000 claims abstract description 37
- 238000002844 melting Methods 0.000 claims abstract description 22
- 230000008018 melting Effects 0.000 claims abstract description 22
- 238000004140 cleaning Methods 0.000 claims abstract description 12
- 230000000087 stabilizing effect Effects 0.000 claims abstract description 11
- 238000003466 welding Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims description 15
- 238000000746 purification Methods 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 230000006641 stabilisation Effects 0.000 claims description 4
- 238000011105 stabilization Methods 0.000 claims description 4
- 230000033228 biological regulation Effects 0.000 abstract description 8
- 230000007363 regulatory process Effects 0.000 abstract description 8
- 230000004083 survival effect Effects 0.000 abstract description 2
- 238000005259 measurement Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
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
- C30B15/20—Controlling or regulating
-
- 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 discloses a pulse power temperature regulating method, which relates to the field of single crystal furnace temperature regulation and is used for judging a solid-liquid ratio value in a full melting stage and obtaining a power regulating quantity through calculation. The temperature regulating process is divided into 3 stages, wherein the first stage is the last feeding stage and the third full melting stage, the second stage is the valve bin and auxiliary chamber cleaning and purifying, welding and temperature stabilizing stage, and the third stage is the automatic temperature regulating stage. The problem that 100% of temperature adjustment cannot reach a target temperature interval accurately is solved, the change of the solid-liquid ratio is judged in the temperature adjustment process, the power adjustment amount is obtained through calculation, the target temperature is controlled to be within the process requirement range through power adjustment of a plurality of adjustment periods, the temperature adjustment accuracy is greatly improved, the melting time is reduced, the temperature adjustment seeding survival rate is improved, and the invalid working hours are reduced.
Description
Technical Field
The invention relates to the field of single crystal furnace temperature regulation, in particular to a pulse power temperature regulation method.
Background
In the single crystal silicon rod pulling industry, with the technical development of many years, the automation degree of a single crystal furnace is remarkably improved, and the automatic crystal pulling can be basically realized at present. The temperature adjusting process in the single crystal pulling process is used as a key point of single crystal growth, is a key step of single crystal growth, requires optimal time for single crystal temperature adjustment in the prior art, but is controlled to be only 80% in interval range proportion, so that partial seeding does not meet the process requirement, the influence on the subsequent processes such as seeding is large, the seeding is re-adjusted for multiple times, the working efficiency is greatly reduced, the labor burden is also caused for operators, and the labor and working hour cost of a company are greatly wasted.
In the prior art, whether the temperature is proper or not is judged by measuring the liquid level brightness data, but the absolute measurement temperature cannot be realized at present, the measured temperature is a relative temperature value, and the final temperature is different due to the difference of calibration values; the measured data is deviated due to problems of reflection points on the liquid surface, dust adhesion on the camera lens, and the like. The liquid level temperature difference is caused, so that the final temperature regulation temperature has deviation and cannot reach the standard temperature interval range. The parameter design of the Czochralski single crystal drawing process needs to be matched with an optimal temperature interval, so that the crystallization rate can be greatly improved, and the temperature adjustment becomes a technical difficulty because the optimal temperature interval cannot be achieved in the prior art.
Disclosure of Invention
The invention aims to solve the technical problems of the prior art, and provides a pulse power temperature regulating method, which solves the technical problems that the measurement data are inaccurate, the temperature regulating working hours are increased due to temperature regulating failure in the current temperature regulating process, the temperature regulating temperature reaches the target range by regulating the power pulse in the temperature regulating process, the uncertainty in the temperature regulating process is greatly reduced, and the stability of the monocrystalline temperature regulating process is improved.
In order to solve the technical problems, the invention adopts the following technical scheme:
a pulse power temperature regulating method is used for regulating the power of a single crystal pulling process in a single crystal furnace and comprises the following steps of: temperature adjustment first stage, step 2: temperature adjustment second stage and step 3: a third stage of temperature adjustment; step 1 specifically comprises the following steps; step 1: temperature adjustment first stage: the method comprises a final feeding stage and a three-time total melting stage, wherein the solid-liquid ratio value is judged in the total melting stage, and then power adjustment is carried out; step 1.1: the last feeding stage: adding the last batch of material into a single crystal furnace; step 1.2: a first full melting stage: when the last batch of material is added into the single crystal furnace, the full melting is started for the first time, the power of a main heater of the single crystal furnace is regulated to 95kw, and the power of a bottom heater of the single crystal furnace is regulated to 60kw; step 1.3: and (3) a second full melting stage: when the solid-liquid ratio value in the single crystal furnace is detected to be approximately equal to 3, starting the single crystal furnace for the second time, adjusting the power of a main heater of the single crystal furnace to be 1.45 times of the power of the seeding power of the previous section, and adjusting the power of a bottom heater of the single crystal furnace to be 50kw; when the solid-to-liquid ratio value in the single crystal furnace is detected to be less than or equal to 1.25, the power of a main heater of the single crystal furnace is regulated to be 1.42 times of the seeding power of the previous section, and the power of a bottom heater of the single crystal furnace is regulated to be 20kw; step 1.4: and a third full melting stage: when the solid-liquid ratio value in the single crystal furnace is detected to be less than or equal to 0.05 and less than or equal to 0.6, starting the single crystal furnace for the third time, adjusting the power of a main heater of the single crystal furnace to be 1.38 times of the power of the previous section of seeding, adjusting the power of a bottom heater of the single crystal furnace to be 0kw, and adjusting the crucible rotation of the single crystal furnace to be 3.5rpm; when the solid-liquid ratio value is detected to be less than or equal to 0.05, namely after the material is completely melted, the heat shield of the single crystal furnace is reduced to 50mm when the liquid temperature is 1520-1560 ℃. The temperature of the heat shield is lower, and the heat shield is lowered to adjust the temperature of the heat field so as to reach the target liquid temperature.
As a further preferred aspect of the present invention, step 2 specifically includes the steps of: step 2: and a second temperature adjustment stage: comprises a valve bin and auxiliary chamber cleaning stage and a purification welding stable temperature starting stage; step 2.1: valve cabin and auxiliary chamber cleaning stage: after the step 1.1 is completed, cleaning the valve bin and the auxiliary chamber to be sanitary immediately, and hanging seed crystals; after the cleaning is finished, a seed crystal rotating step is executed, and after the seed crystal rotating step is finished, seed crystal stabilizing operation is carried out; step 2.2: and (3) a purification welding stable temperature starting stage: and clicking a purification welding temperature stabilizing button of the single crystal furnace after the seed crystal stabilizing operation is finished.
As a further preferred aspect of the present invention, the step 2 further includes a step 2.3: the following preparation stage: and 2.2, connecting a lifting crucible position to place the crucible position of the section, enabling the display value of the liquid port distance pixel value to be consistent with the standard of a card, continuing to refer to the previous section of crystal pulling growth record, selecting the crystal pulling power of the successful equal-diameter section as a reference, adjusting the power according to the residual weight, the crucible position difference and the crystal pulling speed, setting the crystal pulling power value of the section, and finishing the preparation work.
As a further preferred aspect of the present invention, step 3: and a third temperature adjustment stage: the stage is an automatic temperature adjustment stage; step 3.1, firstly, the single crystal furnace system automatically adjusts the main heating power to 0.65 times of seeding power, simultaneously the crucible rotation is restored to the seeding setting crucible rotation, the system gradually restores the main heater power of the single crystal furnace to the setting seeding power value according to the brightness change condition, and the main heater power enters a temperature stabilizing stage, and the stabilizing time is more than or equal to 20 minutes.
As a further preferred aspect of the present invention, the method further comprises step 3.2: and (3) seeding: and 3.1, firstly confirming that the deviation value between the actual liquid level temperature in the single crystal furnace and the target liquid level temperature is less than or equal to 0 ℃ and less than or equal to minus 2 ℃, then judging whether the temperature in the single crystal furnace meets the seeding condition, and clicking a seeding button of the single crystal furnace if the temperature meets the seeding condition.
As a further preferable aspect of the present invention, the seeding condition is that the aperture of the liquid surface is bright and four points are protruded.
As a further preferred aspect of the present invention, the range adjustment in step 2 is less than or equal to 0.8kw.
As a further preference of the invention, the addition amount of the last material in the step 1.1 is more than or equal to 50kg, and the time of the last feeding is when the linear size of the unmelted block in the single crystal furnace is consistent with the size of the flow guide cylinder opening.
According to the power pulse temperature regulating method, the power regulating quantity is calculated by the change of the solid-liquid ratio, so that the problem of inaccurate temperature in the temperature regulating process is corrected. The problem that measurement data in the current temperature adjusting process are inaccurate, temperature adjusting time is increased due to temperature adjusting failure, 100% of temperature adjusting temperature reaches a target range through power pulse adjustment in the temperature adjusting process is solved, the technical problem that uncertainty exists in the temperature adjusting process is greatly reduced, and the stability of a monocrystalline temperature adjusting process is improved.
The invention has the following beneficial effects:
1. the invention aims at the problems and provides a power pulse temperature regulating method. The problem that temperature adjustment can not achieve the target temperature interval accurately is solved, and the accuracy of controlling the target temperature interval is effectively improved. The change of the solid-liquid ratio is judged in the temperature adjusting process, the power adjustment amount is obtained through calculation, and the target temperature is controlled to be within the process requirement range through power adjustment of a plurality of adjustment periods, so that the temperature adjusting accuracy is greatly improved, the melting time is reduced, the temperature adjusting seeding survival rate is improved, and the invalid working hours are reduced.
2. The invention can realize positive and negative power regulation, and the temperature regulation is rapidly fed back to the target range through multiple pulse regulation and multiple period regulation.
Drawings
Fig. 1 is a schematic diagram of pulse power adjustment related to a power pulse attemperation method.
Detailed Description
The invention will be described in further detail with reference to the accompanying drawings and specific preferred embodiments.
In the description of the present invention, it should be understood that the terms "left", "right", "upper", "lower", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the apparatus or element being referred to must have a specific orientation, be configured and operated in a specific orientation, and "first", "second", etc. do not indicate the importance of the components, and thus are not to be construed as limiting the present invention. The specific dimensions adopted in the present embodiment are only for illustrating the technical solution, and do not limit the protection scope of the present invention.
As shown in FIG. 1, the invention provides a temperature adjustment method for power pulses of a Czochralski crystal. The temperature regulating method of the Czochralski silicon single crystal judges the solid-liquid ratio value in the full melting stage, and the power regulating quantity is obtained through calculation. The temperature regulating method of the power pulse of the Czochralski silicon single crystal comprises the following steps: the temperature regulating process is divided into 3 stages, wherein the first stage is the last feeding stage and the third full melting stage, the second stage is the valve bin and auxiliary chamber cleaning and purifying, welding and temperature stabilizing stage, and the third stage is the automatic temperature regulating stage. The power pulse temperature adjustment implementation stage is a first stage and a second stage.
Temperature adjustment first stage: a last feeding stage and three full melting stages, wherein the main purpose of the stage is to melt the residual material blocks rapidly and control the temperature within a temperature range capable of being welded. Before the last barrel of material is added, confirming that the feeding weight is more than or equal to 50kg; when the feeding time of the last barrel is that the linear size of the unmelted block is the same as the size of the flow guide cylinder opening, the last barrel of material can be added. When the system detects that the last barrel of material is lifted, the full melting is started for the first time, and the power of the main heater of the single crystal furnace is automatically adjusted to be fixed, so that the power of the bottom heater of the single crystal furnace is increased to 95kw, and the power of the bottom heater of the single crystal furnace is reduced to 60kw.
Further, the system detects the solid-liquid ratio value in real time, when the solid-liquid ratio value is about equal to 3, the full melting is started for the second time, the power is automatically regulated, the power of the main heater of the single crystal furnace is 1.45 times of the power of the last section of seeding, the power of the bottom heater of the single crystal furnace is reduced to 50kw, meanwhile, the system detects the solid-liquid ratio value in real time, and according to the change of the solid-liquid ratio value, when the solid-liquid ratio value is less than or equal to 1.25, the power of the main heater of the single crystal furnace is 1.42 times of the power of the last section of seeding, and the power of the bottom heater of the single crystal furnace is reduced to 20kw. The seeding power is a floating value, and the seeding power of each section is different, and the previous section is used as a reference value.
Further, when the solid-liquid ratio value is less than or equal to 0.6, starting the whole melting for the third time, so that the power of a main heater of the single crystal furnace is 1.38 times of the power of the previous section of seeding, the power of a bottom heater of the single crystal furnace is reduced to 0kw, and meanwhile, the rotation of a 3.5ramp crucible is given; meanwhile, the system detects the solid-liquid ratio value in real time, and according to the change of the solid-liquid ratio value, when the solid-liquid ratio value is less than or equal to 0.05, namely after the material block is completely melted, the single crystal furnace system automatically reduces the position of the heat shield to 50mm when the liquid temperature is 1520-1560 ℃.
And a second temperature adjustment stage: the valve bin and auxiliary chamber cleaning and purifying welding stable temperature starting stage mainly aims at tightly connecting the first stage, immediately starting to clean the auxiliary chamber and the valve bin and clean/hang the chuck and seed crystal before the material block is not melted, namely after the last feeding stage is finished, executing a seed crystal rotating step after the cleaning is finished, executing a seed crystal stabilizing operation after the working step is finished, and continuously executing a purifying welding stable temperature step before the temperature regulating first stage is finished; and then the crucible position is lifted and lowered to place the crucible position, so that the display value of the liquid port distance pixel value is consistent with the standard of the card, namely the deviation is less than or equal to +/-1, the previous section of crystal pulling growth record is continuously referred, the crystal pulling power of the successful equal-diameter section is selected as a reference, small-range adjustment is carried out according to the factors such as the weight of the residual materials, the difference of the crucible position, the crystal pulling speed and the like, the adjustment range is less than or equal to 0.8kw, and the crystal pulling power value of the section is set, so that the preparation work is completed. After step 1.1 is completed, step 1.2 and step 2.1 are performed synchronously without mutual influence. Step 2.2 is started after step 1.3, while step 2.1 is already completed.
And a third temperature adjustment stage: and in the automatic temperature adjustment stage, the system automatically adjusts the main heating power to 0.65 times of the seeding power, the crucible rotation is restored to the seeding setting crucible rotation, the main heating power is gradually restored to the setting seeding power value according to the brightness change condition, the system enters the temperature stabilization stage, the stabilization time is more than or equal to 20 minutes, the deviation value between the actual liquid level temperature and the target liquid level temperature is less than or equal to 0 and less than or equal to-2 is confirmed, the temperature in the furnace meets the seeding condition, namely the aperture is bright, four points are protruded, and the process step of seeding is entered.
According to the power pulse temperature regulating method, the power regulating quantity is calculated by the change of the solid-liquid ratio, so that the problem of inaccurate temperature in the temperature regulating process is corrected. The technical problems that measurement data are inaccurate in the current temperature adjusting process, temperature adjusting time is increased due to temperature adjusting failure, the temperature adjusting temperature reaches a target range through adjusting power pulses in the temperature adjusting process, uncertainty in the temperature adjusting process is greatly reduced, and the stability of the monocrystalline temperature adjusting process is improved are solved.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various equivalent changes can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the equivalent changes belong to the protection scope of the present invention.
Claims (8)
1. A pulse power temperature regulating method is used for regulating the power of a single crystal pulling process in a single crystal furnace and comprises the following steps of: temperature adjustment first stage, step 2: temperature adjustment second stage and step 3: a third stage of temperature adjustment; the method is characterized in that: step 1 specifically comprises the following steps;
step 1: temperature adjustment first stage: the method comprises a final feeding stage and a three-time total melting stage, wherein the solid-liquid ratio value is judged in the total melting stage, and then power adjustment is carried out;
step 1.1: the last feeding stage: adding the last batch of material into a single crystal furnace;
step 1.2: a first full melting stage: when the last batch of material is added into the single crystal furnace, the full melting is started for the first time, the power of a main heater of the single crystal furnace is regulated to 95kw, and the power of a bottom heater of the single crystal furnace is regulated to 60kw;
step 1.3: and (3) a second full melting stage: when the solid-liquid ratio value in the single crystal furnace is less than or equal to 2.98 and less than or equal to 3.02, starting the single crystal furnace for the second time, adjusting the power of a main heater of the single crystal furnace to be 1.45 times of the power of the previous section of seeding, and adjusting the power of a bottom heater of the single crystal furnace to be 50kw; when the solid-to-liquid ratio value in the single crystal furnace is detected to be less than or equal to 1.25, the power of a main heater of the single crystal furnace is regulated to be 1.42 times of the seeding power of the previous section, and the power of a bottom heater of the single crystal furnace is regulated to be 20kw;
step 1.4: and a third full melting stage: when the solid-liquid ratio value in the single crystal furnace is detected to be less than or equal to 0.05 and less than or equal to 0.6, starting the single crystal furnace for the third time, adjusting the power of a main heater of the single crystal furnace to be 1.38 times of the power of the previous section of seeding, adjusting the power of a bottom heater of the single crystal furnace to be 0kw, and adjusting the crucible rotation of the single crystal furnace to be 3.5ramp; when the solid-liquid ratio value is detected to be less than or equal to 0.05, namely after the material is completely melted, the heat shield of the single crystal furnace is reduced to 50mm when the liquid temperature is 1520-1560 ℃.
2. The pulse power temperature control method according to claim 1, wherein: the step 2 specifically comprises the following steps:
step 2: and a second temperature adjustment stage: comprises a valve bin and auxiliary chamber cleaning stage and a purification welding stable temperature starting stage;
step 2.1: valve cabin and auxiliary chamber cleaning stage: after the step 1.1 is completed, cleaning the valve bin and the auxiliary chamber to be sanitary immediately, and hanging seed crystals; after the cleaning is finished, a seed crystal rotating step is executed, and after the seed crystal rotating step is finished, seed crystal stabilizing operation is carried out;
step 2.2: and (3) a purification welding stable temperature starting stage: and clicking a purification welding temperature stabilizing button of the single crystal furnace after the seed crystal stabilizing operation is finished.
3. The pulse power temperature control method according to claim 2, wherein: the step 2 further comprises a step 2.3: the following preparation stage: and 2.2, connecting a lifting crucible position to place the crucible position of the section, enabling the display value of the liquid port distance pixel value to be consistent with the standard of a card, continuing to refer to the previous section of crystal pulling growth record, selecting the crystal pulling power of the successful equal-diameter section as a reference, adjusting the power according to the residual weight, the crucible position difference and the crystal pulling speed, setting the crystal pulling power value of the section, and finishing the preparation work.
4. A pulse power attemperation method as defined in claim 3, wherein:
step 3: and a third temperature adjustment stage: the stage is an automatic temperature adjustment stage;
step 3.1, firstly, the single crystal furnace system automatically adjusts the main heating power to 0.65 times of the seeding power of the previous section, simultaneously the crucible rotation is restored to the seeding setting crucible rotation, the system gradually restores the main heater power of the single crystal furnace to the setting seeding power value according to the brightness change condition, and the stabilization time is more than or equal to 20 minutes after entering the temperature stabilization stage.
5. The pulse power temperature control method according to claim 4, wherein: further comprising the step 3.2: and (3) seeding: and 3.1, firstly confirming that the deviation value between the actual liquid level temperature in the single crystal furnace and the target liquid level temperature is less than or equal to 0 ℃ and less than or equal to minus 2 ℃, then judging whether the temperature in the single crystal furnace meets the seeding condition, and clicking a seeding button of the single crystal furnace if the temperature meets the seeding condition.
6. The pulse power temperature control method according to claim 5, wherein: the seeding condition is that the aperture of the liquid level is bright and four points are prominent.
7. A pulse power attemperation method as defined in claim 3, wherein: the range adjustment in the step 2 is less than or equal to 0.8kw.
8. The pulse power temperature control method according to claim 1, wherein: in the step 1.1, the addition amount of the last material is more than or equal to 50kg, and the time of the last feeding is when the linear size of the unmelted block in the single crystal furnace is consistent with the size of the guide cylinder opening.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311478547.8A CN117488396A (en) | 2023-11-08 | 2023-11-08 | Pulse power temperature regulating method |
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| CN202311478547.8A CN117488396A (en) | 2023-11-08 | 2023-11-08 | Pulse power temperature regulating method |
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