CN117702259A - Method for quickly cooling PVT furnace - Google Patents
Method for quickly cooling PVT furnace Download PDFInfo
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- CN117702259A CN117702259A CN202410167161.3A CN202410167161A CN117702259A CN 117702259 A CN117702259 A CN 117702259A CN 202410167161 A CN202410167161 A CN 202410167161A CN 117702259 A CN117702259 A CN 117702259A
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- 238000001816 cooling Methods 0.000 title claims abstract description 95
- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000000112 cooling gas Substances 0.000 claims abstract description 47
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 239000011261 inert gas Substances 0.000 claims abstract description 21
- 239000001307 helium Substances 0.000 claims abstract description 13
- 229910052734 helium Inorganic materials 0.000 claims abstract description 13
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims abstract description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 66
- 229910052786 argon Inorganic materials 0.000 claims description 33
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 30
- 229910002804 graphite Inorganic materials 0.000 description 29
- 239000010439 graphite Substances 0.000 description 29
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 9
- 229910010271 silicon carbide Inorganic materials 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 230000006698 induction Effects 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
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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
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The application discloses a method for quickly cooling a PVT furnace, which comprises the following steps: s1: stopping heating the PVT furnace, and filling cooling gas into the PVT furnace, wherein the cooling gas is helium, and controlling the pressure in the PVT furnace until the temperature of the PVT furnace is not more than 50 ℃; s2: and (3) cooling is completed, inert gas is filled into the PVT furnace until the pressure in the PVT furnace reaches atmospheric pressure, and the crucible is taken out. The method for quickly cooling the PVT furnace can greatly shorten the time for cooling the PVT furnace to normal temperature, thereby improving the production efficiency.
Description
Technical Field
The application relates to the technical field of semiconductor growth, in particular to a method for quickly cooling a PVT furnace.
Background
Silicon carbide (SiC) is a popular material for third generation semiconductors, and is widely used in industries such as 5G communication, new energy automobiles, photovoltaic inverters, and the like, due to its excellent characteristics of wide forbidden band, high saturated electron mobility, high breakdown electric field, high thermal conductivity, and the like.
The third generation of semiconductor silicon carbide single crystal production methods mainly include a physical vapor transport method (PVT), a top seed solution growth method (TSSG), and a high temperature chemical vapor deposition method (HT-CVD), wherein the PVT method is a main technical route of current commercialization.
The method for synthesizing the high-purity silicon carbide powder for the growth of the third-generation semiconductor silicon carbide single crystal comprises the following steps: liquid phase, solid phase and gas phase processes. The solid phase method (improving the self-propagating method to synthesize the silicon carbide is also called PVT method) is used for preparing the high-purity silicon carbide, and has the characteristics of high purity, high yield, good particle crystallinity and the like, and is widely popularized.
Currently, the most commonly used preparation methods of third-generation semiconductor silicon carbide single crystals and high-purity powder materials are all prepared by a PVT furnace. The PVT furnace is equipment for realizing a PVT method, and adopts induction heating to heat a graphite crucible to 2000-2300 ℃, and grows high-purity SiC crystals and high-purity SiC powder in a quartz tube/stainless steel cavity by a physical vapor transport method (PVT). PVT stove tolerates temperature height, intensification speed is fast and thermal insulation performance characteristics such as good.
The PVT stove has good heat preservation performance, so that the cooling speed is low. Only 5-10 hours are needed for the PVT furnace to be heated from room temperature to 2200 ℃, but 30-40 hours are needed for the PVT furnace to be cooled from 2200 ℃ to room temperature. The PVT furnace has low cooling speed, so that the cycle recycling efficiency is greatly reduced, and the optimal production efficiency cannot be achieved. Therefore, an economic and efficient way for accelerating the cooling speed of the PVT furnace needs to be developed.
Disclosure of Invention
The purpose of this application is to accelerate the cooling rate of PVT stove.
In order to achieve the above purpose, the technical scheme adopted in the application is as follows: a method for quickly cooling a PVT furnace comprises the following steps: s1: stopping heating the PVT furnace, and filling cooling gas into the PVT furnace, wherein the cooling gas is helium, and controlling the pressure in the PVT furnace until the temperature of the PVT furnace is not more than 50 ℃; s2: and (3) cooling is completed, inert gas is filled into the PVT furnace until the pressure in the PVT furnace reaches atmospheric pressure, and the crucible is taken out.
Preferably, the purity of the cooling gas and the inert gas is greater than 99.9999%.
In another preferred embodiment, in the step S1, the pressure of the PVT furnace is controlled to be 600-800 mbar.
As another preferable, the inert gas is argon.
As another preferable aspect, the step S1 specifically includes: and stopping heating the PVT furnace, filling cooling gas which is helium into the PVT furnace, opening a valve of a forced cooling system, starting a fan of the forced cooling system, and performing heat exchange and cooling on the cooling gas by using a heat exchanger until the temperature of the PVT furnace is not more than 50 ℃.
A method for quickly cooling a PVT furnace comprises the following steps: a1: stopping heating the PVT furnace, and filling a first cooling gas into the PVT furnace, wherein the first cooling gas is argon or helium, and controlling the pressure in the PVT furnace until the temperature of the PVT furnace is not more than 1000 ℃; a2: extracting the first cooling gas in the PVT furnace, and filling a second cooling gas which is hydrogen until the temperature of the PVT furnace is not more than 50 ℃; a3: and (3) cooling is completed, inert gas is filled into the PVT furnace until the pressure in the PVT furnace reaches atmospheric pressure, and the crucible is taken out.
As another preference, the purity of the first cooling gas, the second cooling gas and the inert gas is greater than 99.9999%.
In another preferred embodiment, in the step A1, the pressure of the PVT furnace is controlled to be 600-800 mbar.
As another preferable, the inert gas is argon.
Further preferably, the step A2 specifically includes: and (3) extracting the first cooling gas, filling the second cooling gas, opening a valve of the forced cooling system, starting a fan of the forced cooling system, and performing heat exchange and cooling on the second cooling gas by using a heat exchanger until the temperature of the PVT furnace is not more than 50 ℃.
Compared with the prior art, the beneficial effect of this application lies in:
(1) The method for quickly cooling the PVT furnace can greatly shorten the time for cooling the PVT furnace to normal temperature, thereby improving the production efficiency;
(2) According to the PVT furnace rapid cooling method, new impurities are prevented from being introduced into the PVT furnace, and meanwhile cooling cost is reduced.
Drawings
FIG. 1 is a device for rapidly cooling a PVT furnace according to one embodiment of the present application;
in the figure: 1. a graphite crucible; 2. a thermal field; 3. a PVT furnace; 4. a forced cooling system; 41. a blower; 42. a heat exchanger; 43. and (3) a valve.
Detailed Description
The present application will be further described with reference to the specific embodiments, and it should be noted that, on the premise of no conflict, new embodiments may be formed by any combination of the embodiments or technical features described below.
The terms "comprises" and "comprising," along with any variations thereof, in the description and claims of the present application are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements that are expressly listed or inherent to such process, method, article, or apparatus.
The application provides a method for quickly cooling a PVT furnace, which comprises the following steps:
s1: stopping heating the PVT furnace, and filling cooling gas into the PVT furnace, wherein the cooling gas is helium, and controlling the pressure in the PVT furnace until the temperature of the PVT furnace is not more than 50 ℃;
s2: and (5) filling inert gas into the PVT furnace until the pressure in the PVT furnace reaches atmospheric pressure, and completing cooling.
In some embodiments, the PVT furnace is connected to a forced cooling system, and the forced cooling system is provided with a heat exchanger or a fan and other cooling devices, so that the cooling rate of the PVT furnace is improved, and the time is saved. Through the arrangement of the heat exchanger in the forced cooling system, the gas in the PVT furnace flows and is fully contacted with the heat exchanger, so that the temperature in the furnace can be taken away rapidly, and the cooling speed is further improved.
In some embodiments, step S1 is specifically: and stopping heating the PVT furnace, filling cooling gas which is helium into the PVT furnace, opening a valve of the forced cooling system, starting a fan of the forced cooling system, and performing heat exchange and cooling on the cooling gas by using a heat exchanger until the temperature of the PVT furnace is not more than 50 ℃.
In some embodiments, in step S1, the pressure in the PVT furnace is controlled to be 600-800 mbar.
In some embodiments, the inert gas is selected from the group consisting of low cost argon.
In some embodiments, to avoid introducing impurities into the PVT furnace, the cooling gas and inert gas are selected from high purity gases having a purity greater than 99.9999%.
The application also provides a method for quickly cooling the PVT furnace, which comprises the following steps:
a1: stopping heating the PVT furnace, and filling a first cooling gas into the PVT furnace, wherein the first cooling gas is argon or helium, and controlling the pressure in the PVT furnace until the temperature of the PVT furnace is not more than 1000 ℃;
a2: extracting the first cooling gas in the PVT furnace, and filling the second cooling gas which is hydrogen until the temperature of the PVT furnace is not more than 50 ℃;
a3: and (5) filling inert gas into the PVT furnace until the pressure in the PVT furnace reaches atmospheric pressure, and completing cooling.
In some preferred embodiments, the PVT furnace is connected to the forced cooling system, and in step A2, after the PVT furnace is filled with the second cooling gas, a valve of the forced cooling system is opened, a fan of the forced cooling system is started, and heat exchange is performed by using a heat exchanger until the temperature in the PVT furnace does not exceed 50 ℃.
In some embodiments, the A1 step controls the pressure in the PVT furnace to be 600-800 mbar.
In some embodiments, the inert gas is relatively inexpensive argon.
In some preferred embodiments, the first cooling gas, the second cooling gas, and the inert gas are all highly pure gases, with a purity greater than 99.9999%, to ensure that the PVT oven is not contaminated with impurities and to ensure safe operation of the cooling system.
The PVT furnace is internally provided with a closed environment, and heat conduction is mainly carried out by gas transmission, wherein the heat conduction speed of cooling gases with different heat conduction coefficients determines the cooling speed. The thermal conductivity of argon is 0.016W/(m.K), the thermal conductivity of helium is 0.15W/(m.K), and the thermal conductivity of hydrogen is 0.1805W/(m.K), so that the thermal conductivity of hydrogen is highest in three cooling gases, and the cooling rate can be accelerated by using hydrogen when the PVT furnace is cooled.
The temperature reduction of the PVT furnace is divided into two stages, different cooling gases are filled into the two stages, argon is filled into the A1 stage for temperature reduction, the argon in the PVT furnace is pumped out when the PVT furnace is cooled to below 1000 ℃, and hydrogen is filled into the PVT furnace.
The hydrogen will react with carbon in the PVT furnace at high temperature to pollute the furnace, so that after the temperature is reduced by using argon, the PVT furnace gas is replaced by hydrogen, and the cooling time is shortened.
Under the standard state, the thermal conductivity of argon is 0.016W/(m.K), and the capability of the argon in the thermal conduction process is limited, but the argon has low cost compared with other inert gases, so that the argon is filled into the PVT furnace after the temperature is reduced in the step A2, and the internal and external air pressure of the PVT furnace is kept consistent.
When the cooling gas is filled into the furnace, the PVT furnace is filled with the cooling gas rapidly at a high flow rate, and a low flow rate is maintained in the cooling process so that the inert gas can perform heat exchange fully.
The application also provides a PVT furnace rapid cooling device, which comprises a graphite crucible 1, a thermal field 2, a PVT furnace 3 and a forced cooling system 4, wherein the thermal field 2 is internally provided with the graphite crucible 1, the thermal field 2 is loaded in the PVT furnace 3, and the PVT furnace 3 is connected with the forced cooling system 4, as shown in figure 1.
The forced cooling system 4 comprises a fan 41, a heat exchanger 42 and a valve 43, wherein the valve 43 is used for controlling whether a pipeline of the forced cooling system 4 is communicated with the PVT furnace 3.
The heat exchanger 42 is a conventional art, and heat exchange is illustrated by using cooling circulating water.
The PVT furnace 3 is provided with an induction heating system and a vacuum pressure system, wherein the induction heating system consists of an induction power supply and an induction coil, and the vacuum pressure system in the PVT furnace 3 consists of a mechanical pump, a molecular pump, a proportional valve, a flowmeter and other components. The cavity of the PVT furnace 3 consists of a quartz tube, a metal flange and other parts.
The thermal field 2 is internally provided with a graphite barrel, the outer side of the graphite barrel is wound by 3-5 layers of graphite soft felts, the top of the graphite barrel is covered with a plurality of layers of graphite soft felts, and the bottom of the graphite barrel is provided with a graphite hard felt. The graphite soft felt and the graphite hard felt have heat preservation effect, and the graphite hard felt arranged at the bottom of the graphite barrel also has the effect of supporting the graphite barrel. The purity of the graphite soft felt and the graphite hard felt is more than 99.998 percent.
The graphite crucible 1 is suitable for being placed in a graphite barrel of the thermal field 2 in an embedded mode, and the graphite crucible 1 comprises a graphite body, a graphite upper cover and a graphite lower cover which are connected with the graphite body through graphite bolts respectively. Wherein the purity of the graphite crucible is more than 99.9999%.
Example 1
In order to test the method for rapidly cooling the PVT furnace, a cooling device shown in fig. 1 is used, and the PVT furnace is heated first and then is kept for a period of time. Simulating actual PVT furnace production scene in heating and heat preservation steps
And (3) heating: placing a thermal field 2 filled with a graphite crucible 1 into a cavity of a PVT furnace 3, and setting the pressure in the PVT furnace 3 to be 1 x 10 -3 Below mbar and PVT furnace 3 was heated to 2200 ℃.
And (3) heat preservation: when the PVT furnace 3 reached 2200 ℃, argon was introduced into the PVT furnace 3, the internal pressure of the furnace was set at 600.+ -.2 mbar, the internal temperature of the furnace was maintained at 2200.+ -.10 ℃, and the PVT furnace 3 was kept for 10 hours.
And (3) a cooling stage: s1: stopping heating and starting timing of the PVT furnace 3, evacuating argon in the furnace, charging helium into the PVT furnace 3, and controlling the pressure in the furnace to be about 800+/-2 mbar until the temperature of the PVT furnace 3 is reduced to below 50 ℃;
s2: argon is filled into the PVT furnace 3, and the timing is stopped after the pressure in the furnace reaches the atmospheric pressure.
Example 2
The temperature rising stage and the temperature keeping stage of example 2 remain the same as those of example 1.
And (3) a cooling stage: s10: stopping heating and starting timing the PVT furnace 3, and controlling the pressure in the furnace to be 800+/-2 mbar until the temperature of the PVT furnace 3 is reduced to 1000 ℃;
s11: evacuating argon in the PVT furnace 3 and charging hydrogen, and controlling the pressure in the furnace to be 800+/-2 mbar until the temperature of the PVT furnace 3 is reduced to below 50 ℃;
s2: the PVT furnace 3 was evacuated of hydrogen and argon was introduced into the furnace until the pressure in the furnace reached atmospheric pressure, and the time was stopped.
Example 3
And (3) heating: the thermal field 2 with the graphite crucible 1 was placed in the cavity of the PVT furnace 3, the valve 43 of the forced cooling system 4 was opened, the pressure in the PVT furnace 3 was set below 1 x 10 "3 mbar, the air valve 43 was closed, and the PVT furnace 3 was heated to 2200 ℃.
And (3) heat preservation: when the PVT furnace 3 reached 2200 ℃, argon was introduced into the PVT furnace 3, the internal pressure of the furnace was set at 600.+ -.2 mbar, the internal temperature of the furnace was maintained at 2200.+ -.10 ℃, and the PVT furnace 3 was kept for 10 hours.
And (3) cooling: s10: stopping heating and starting timing of the PVT furnace 3, evacuating argon in the PVT furnace 3, and charging helium, wherein the pressure in the furnace is controlled at 800+/-2 mbar until the temperature of the PVT furnace 3 is reduced to 1500 ℃;
s11: opening a valve 43 of the forced cooling system 4, starting a fan 41, controlling the pressure in the furnace to be 800+/-2 mbar, and controlling the water inlet temperature in the heat exchanger 42 to be within 28 ℃ until the temperature of the PVT furnace 3 is reduced to be lower than 50 ℃;
s2: argon is filled into the furnace until the pressure in the furnace reaches atmospheric pressure, and the timing is stopped.
Example 4
The procedure for the warm-up phase and cool-down phase in example 4 was consistent with that in example 3.
And (3) cooling: s10: stopping heating the PVT furnace 3, starting timing, filling argon into the PVT furnace 3, and controlling the pressure in the furnace to be 800+/-2 mbar until the temperature of the PVT furnace 3 is reduced to 1000 ℃;
s11: evacuating argon in the PVT furnace 3, filling hydrogen, opening a valve 43 of the forced cooling system 4, starting a fan 41, controlling the pressure in the furnace to be 800+/-2 mbar, and controlling the water inlet temperature in the heat exchanger 42 to be within 28 ℃ until the temperature of the PVT furnace 3 is reduced to be below 50 ℃;
s2: argon is filled into the furnace until the pressure in the furnace reaches atmospheric pressure, and the timing is stopped.
Comparative example 1
The temperature rising stage and the heat retaining stage of comparative example 1 were kept identical to those of example 1.
And (3) a cooling stage: stopping heating and starting timing the PVT furnace 3, charging argon into the furnace, and controlling the pressure in the furnace to be about 800+/-2 mbar until the temperature of the PVT furnace 3 is reduced to below 50 ℃;
s2: argon is filled into the PVT furnace 3, and the timing is stopped after the pressure in the furnace reaches the atmospheric pressure.
Comparative example 2
The procedure of the temperature increasing stage and the temperature decreasing stage in comparative example 2 was kept the same as in example 3.
And (3) a cooling stage: s10: stopping heating and starting timing the PVT furnace 3, charging argon into the furnace, and controlling the pressure in the furnace to be 800+/-2 mbar until the temperature of the PVT furnace 3 is reduced to 1500 ℃;
s11: opening a valve 43 of the forced cooling system 4, starting a fan 41, controlling the pressure in the furnace to be 800+/-2 mbar, and controlling the water inlet temperature in the heat exchanger 42 to be within 28 ℃ until the temperature of the PVT furnace 3 is reduced to be lower than 50 ℃;
s2: argon is filled into the furnace until the pressure in the furnace reaches atmospheric pressure, and the timing is stopped.
The test times of examples 1 to 4 and comparative examples 1 to 2 are recorded in table 1 below.
Table 1 cooling time used in each of examples and comparative examples
The comparison result analysis of the embodiment 1-4 and the comparison example 1-2 shows that the PVT furnace rapid cooling method can shorten the cooling time of the PVT furnace, thereby improving the production efficiency. In the optimal cooling scheme, the cooling time can be shortened by about 60%, namely, the cooling rate can be improved by 60% at maximum.
In addition, the problem of cooling cost is also considered in the application, the cooling rate is improved by using the heat exchanger and the fan under the condition of not remarkably increasing the cost, and the pressure of the PVT furnace is enabled to reach the atmospheric pressure by using the relatively low argon filling PVT furnace.
The PVT furnace cooling method and device have good cooling effect, can greatly shorten cooling link time and improve production efficiency.
The foregoing has outlined the basic principles, main features and advantages of the present application. It will be appreciated by persons skilled in the art that the present application is not limited to the embodiments described above, and that the embodiments and descriptions described herein are merely illustrative of the principles of the present application, and that various changes and modifications may be made therein without departing from the spirit and scope of the application, which is defined by the appended claims. The scope of protection of the present application is defined by the appended claims and equivalents thereof.
Claims (10)
1. The method for quickly cooling the PVT furnace is characterized by comprising the following steps of:
s1: stopping heating the PVT furnace, and filling cooling gas into the PVT furnace, wherein the cooling gas is helium, and controlling the pressure in the PVT furnace until the temperature of the PVT furnace is not more than 50 ℃;
s2: and (3) cooling is completed, inert gas is filled into the PVT furnace until the pressure in the PVT furnace reaches atmospheric pressure, and the crucible is taken out.
2. The method of rapid cooling of a PVT oven according to claim 1, wherein the purity of the cooling gas and the inert gas is greater than 99.9999%.
3. The method for rapidly cooling a PVT furnace according to claim 1, wherein in the step S1, the pressure of the PVT furnace is controlled to be 600-800 mbar.
4. The method for rapidly cooling a PVT furnace according to claim 1, wherein the inert gas is argon.
5. The method for rapidly cooling a PVT furnace according to any one of claims 1 to 4, wherein S1 specifically comprises: and stopping heating the PVT furnace, filling cooling gas which is helium into the PVT furnace, opening a valve of a forced cooling system, starting a fan of the forced cooling system, and performing heat exchange and cooling on the cooling gas by using a heat exchanger until the temperature of the PVT furnace is not more than 50 ℃.
6. The method for quickly cooling the PVT furnace is characterized by comprising the following steps of:
a1: stopping heating the PVT furnace, and filling a first cooling gas into the PVT furnace, wherein the first cooling gas is argon or helium, and controlling the pressure in the PVT furnace until the temperature of the PVT furnace is not more than 1000 ℃;
a2: extracting the first cooling gas in the PVT furnace, and filling a second cooling gas which is hydrogen until the temperature of the PVT furnace is not more than 50 ℃;
a3: and (3) cooling is completed, inert gas is filled into the PVT furnace until the pressure in the PVT furnace reaches atmospheric pressure, and the crucible is taken out.
7. The method of rapid cooling of a PVT furnace according to claim 6 wherein the purity of the first cooling gas, the second cooling gas, and the inert gas is greater than 99.9999%.
8. The method for rapidly cooling a PVT furnace according to claim 6, wherein in the step A1, the pressure of the PVT furnace is controlled to be 600-800 mbar.
9. The method for rapidly cooling a PVT furnace according to claim 6, wherein the inert gas is argon.
10. The method for rapidly cooling a PVT furnace according to any one of claims 6 to 9, wherein the step A2 specifically comprises: and (3) extracting the first cooling gas, filling the second cooling gas, opening a valve of the forced cooling system, starting a fan of the forced cooling system, and performing heat exchange and cooling on the second cooling gas by using a heat exchanger until the temperature of the PVT furnace is not more than 50 ℃.
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