CN111485289A - Heating device and heating method - Google Patents
Heating device and heating method Download PDFInfo
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- CN111485289A CN111485289A CN202010284703.7A CN202010284703A CN111485289A CN 111485289 A CN111485289 A CN 111485289A CN 202010284703 A CN202010284703 A CN 202010284703A CN 111485289 A CN111485289 A CN 111485289A
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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
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
- C30B29/406—Gallium nitride
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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
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
- C30B7/105—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes using ammonia as solvent, i.e. ammonothermal processes
Abstract
The invention relates to a heating device and a heating method, wherein the heating device comprises: a container; the heating part is positioned outside the container and used for heating the container; and the cooling layer is positioned outside the container and is isolated from the container through the heating component and the heat insulation layer. The heating device comprises the cooling layer, so that the temperature outside the container is constant, the influence of the change of the ambient temperature on the temperature in the container is reduced, the axial temperature difference in the container can be accurately controlled, and the cost is reduced.
Description
Technical Field
The invention relates to the field of semiconductor manufacturing equipment, in particular to a heating device and a heating method.
Background
Generally, a medium has a low viscosity in a supercritical state and is more easily diffused than a liquid but has the same solvating power as the liquid, and a subcritical state refers to a liquid state having a density substantially the same as a critical density in the vicinity of a critical temperature. The ammonothermal method is a method for growing GaN single crystal in supercritical environment, in the device for growing GaN single crystal by ammonothermal method, a raw material area and a crystallization area are arranged, and the raw material is dissolved by heating to make the raw material area in supercritical state; the crystallization zone is made to be in a subcritical state, and crystal growth is performed by utilizing the solubility difference between the supercritical state and the subcritical state. In the existing device technology for growing GaN single crystals by an ammonothermal method, the change of ambient temperature has certain influence on the temperature in the device, and is not beneficial to the accurate control of the temperature.
Disclosure of Invention
In view of the above, the present invention provides a heating apparatus and a heating method.
The present invention provides a heating device comprising: a container; a heating member located outside the container; and the cooling layer is positioned outside the container and is isolated from the container through the heating component and the heat insulating layer.
The heating device comprises the cooling layer, so that the temperature outside the container is constant, the influence of the change of the ambient temperature on the temperature in the container is reduced, the axial temperature difference in the container can be accurately controlled, and the cost is reduced.
In one embodiment, the vessel comprises an autoclave, which is a vessel for ammonothermal growth of gallium nitride single crystals.
In one embodiment, the container includes a first region and a second region located below the first region, and the heating means includes a first heating unit and a second heating unit whose temperatures are independently controllable from each other, the first heating unit being located at a periphery of the first region, and the second heating unit being located at a periphery of the second region.
In one embodiment, the heating member and the heat insulating layer coat the container together, the first heating unit and the second heating unit have a distance therebetween, the size of the distance is greater than or equal to 50mm, the heat insulating layer includes a top heat insulating layer, an upper heat insulating layer, a middle heat insulating layer, a lower heat insulating layer, and a bottom heat insulating layer, the top heat insulating layer is located at the top of the container, the upper heat insulating layer is located outside the first zone, the middle heat insulating layer is located between the first heating unit and the second heating unit, the lower heat insulating layer is located outside the second zone, and the bottom heat insulating layer is located at the bottom of the container.
In one embodiment, the heating component comprises a heating wire and a support body for supporting the heating wire, and the support body is made of one or a combination of aluminum silicate, zirconium oxide, aluminum nitride and aluminum oxide, so that the heat insulation performance of the support body is good, and the cost is reduced.
In one embodiment, the material of the heat insulating layer comprises one or a combination of aluminum silicate, zirconium oxide, aluminum nitride and aluminum oxide, so that the heat insulating performance of the heat insulating layer is improved, and the cost is reduced.
In one embodiment, the cooling layer covers the container and is isolated from the container by the heating component and the heat insulating layer, the cooling layer comprises a top cooling layer, a middle cooling layer and a bottom cooling layer, the top cooling layer is positioned at the top of the container, the middle cooling layer is positioned at the periphery of the container, and the bottom cooling layer is positioned at the bottom of the container.
In one embodiment, a cooling liquid or a cooling gas is introduced into the cooling layer.
In one embodiment, the temperature of the cooling layer is less than 100 ℃.
In one embodiment, the cooling layer comprises a jacket structure or a coiled tube structure.
The invention also provides a heating method, comprising the following steps: providing the heating device, and heating the container by adopting the heating device; when the lowest temperature in the container is lower than a first temperature, heating the container to the first temperature at a first heating speed and controlling the pressure in the container to be lower than a first pressure; when the lowest temperature in the container is higher than the first temperature and lower than a second temperature, heating the container to the second temperature at a second heating speed and controlling the pressure in the container to be lower than a second pressure, wherein the first heating speed is higher than the second heating speed; when the lowest temperature in the container is equal to the second temperature, the temperature change in the container is accurately controlled to control the growth of the gallium nitride single crystal in the container.
The heating device adopted by the heating method comprises the cooling layer, so that the temperature outside the container is constant, the influence of ambient temperature change on the temperature in the container is reduced, the accurate control of the axial temperature difference in the container is facilitated, and the cost is reduced; in the heating method, the container is heated at the first heating speed and the second heating speed in different time periods, so that the temperature rise process in the container is safer, and the temperature and the pressure can be controlled more accurately.
In one embodiment, the container comprises a first region and a second region, the temperature difference between the temperature of the first region and the temperature of the second region is controlled to be equal to or less than a first temperature difference during heating at the first heating rate, the temperature difference between the temperature of the first region and the temperature of the second region is controlled to be equal to or less than a second temperature difference during heating at the second heating rate, the temperature difference between the temperature of the first region and the temperature of the second region is controlled to be equal to or less than the second temperature difference and equal to or more than a third temperature difference during precise control of the change of the temperature in the container, the first temperature difference and the second temperature difference are used for ensuring the safety of the container, and the third temperature difference is used for controlling the growth of gallium nitride single crystal in the container.
Drawings
Fig. 1 is a cross-sectional view of a heating device of the present invention.
FIG. 2 is a flow chart of a heating method of the present invention.
In the figure: 10. a container; 1011. a first region; 1012. a second region; 1021. an upper end cover of the container; 1022. a container wall; 1023. a container lower end cap; 20. a heating member; 2011. a first heating unit; 2012. a second heating unit; 2021. heating wires; 2022. a support body; 30. a heat insulating layer; 301. a top insulating layer; 302. an upper thermal insulation layer; 303. a middle heat insulating layer; 304. a lower heat insulating layer; 305. a bottom thermal insulation layer; 40. a cooling layer; 404. a coolant line; 50. a separator.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "vertical", "horizontal", "inner", "outer", etc. indicate orientations or positional relationships based on methods or positional relationships shown in the drawings, and are only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the referred devices or elements must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
One embodiment, as shown in fig. 1, provides a heating apparatus comprising: a container 10; a heating part 20 located outside the container 10 for heating the container 10; and a cooling layer 40 located outside the container 10 and isolated from the container 10 by the heating member 20 and the heat insulating layer 30.
In this embodiment, the cooling layer 40 is included in the heating device, so that the temperature outside the container 10 is constant, the influence of ambient temperature change on the temperature in the container 10 is reduced, the axial temperature difference in the container 10 can be controlled accurately, the stability and consistency of the growth process are ensured, the yield and the performance are improved, and the product cost is reduced.
In one embodiment, the vessel 10 includes a vessel wall 1022, a vessel upper end cap 1021, and a vessel lower end cap 1023. The container wall 1022 may be cylindrical.
In one embodiment, the heating member 20 comprises a furnace, preferably a resistance furnace.
In one embodiment, the vessel comprises an autoclave, which is a vessel for ammonothermal growth of gallium nitride single crystals.
In a specific embodiment, the heating device is used for ammonothermal growth of gallium nitride single crystal, wherein the container 10 is an autoclave, the container 10 comprises a first region 1011 and a second region 1012 located below the first region 1011, wherein the first region 1011 is a crystallization region, the second region 1012 is a raw material region, the heating component 20 makes ammonia filled in the autoclave in a supercritical state, the heating component 20 comprises a first heating unit 2011 and a second heating unit 2012, the temperatures of which can be independently controlled, the first heating unit 2011 is located at the periphery of the first region 1011, and the second heating unit 2012 is located at the periphery of the second region 1012, so that the first region 1011 and the second region 1012 can form a temperature difference, thereby being more beneficial to growth of gallium nitride single crystal.
Wherein, the crystallization zone can be below the raw material zone or above the raw material zone. When an acidic mineralizer is used, the temperature in the feed zone is higher than the temperature in the crystallization zone; when a basic mineralizer is used, the temperature in the crystallization zone is higher than the temperature in the feed zone.
In this embodiment, during the growth of the gallium nitride single crystal, the pressure in the container 10 is 100MPa to 300MPa, and the temperature in the container 10 is 450 ℃ to 650 ℃.
In one embodiment, the container 10 includes a first zone 1011 and a second zone 1012, and the heating component 20 includes a first heating unit 2011 and a second heating unit 2012 that are temperature controllable independently of each other, the first heating unit 2011 being configured to heat the first zone 1011 and the second heating unit 2012 being configured to heat the second zone 1012.
In one embodiment, the first heating unit 2011 and the second heating unit 2012 have a spacing therebetween, and preferably, the spacing between the first heating unit 2011 and the second heating unit 2012 is greater than or equal to 50mm, for example, the spacing between the first heating unit 2011 and the second heating unit 2012 may be 50mm, 55mm, 60mm, 70mm, or 80 mm.
In one embodiment, the first heating unit 2011 and the second heating unit 2012 are assembled by at least 1 heating element, for example, the first heating unit 2011 and the second heating unit 2012 are assembled by 3 heating elements. Each heating element comprises a plurality of heating wires 2021, preferably, the heating wires 2021 are heating resistance wires.
In one embodiment, the vessel 10 further includes a partition 50 with a through hole therein for separating the first region 1011 from the second region 1012. The partition plate 50 is beneficial to forming a step temperature difference in the container 10, and can also enable the respective environments of the first area 1011 and the second area 1012 to be relatively stable, thereby effectively controlling the crystal growth speed.
In one embodiment, heating component 20 and thermal insulation 30 together encase container 10, first heating unit 2011 and second heating unit 2012 have a gap therebetween, thermal insulation 30 includes top thermal insulation layer 301, upper thermal insulation layer 302, middle thermal insulation layer 303, lower thermal insulation layer 304, and bottom thermal insulation layer 305, top thermal insulation layer 301 is located at the top of container 10, upper thermal insulation layer 302 is located outside first zone 1011, middle thermal insulation layer 303 is located between first heating unit 2011 and second heating unit 2012, lower thermal insulation layer 304 is located outside second zone 1012, and bottom thermal insulation layer 305 is located at the bottom of container 10.
In one embodiment, the heating member 20 includes a heating wire 2021 and a supporting body 2022 for supporting the heating wire 2021, and the material of the supporting body 2022 includes one or a combination of aluminum silicate, zirconium oxide, aluminum nitride and aluminum oxide, so that the heat insulation performance of the supporting body 2022 is good, and the cost is reduced.
In this embodiment, the heating member 20 is cylindrical, the heating wires 2021 are located inside the heating member 20 and are uniformly distributed along the circumference, and the supporting member 2022 is used for supporting the heating wires 2021, so that a certain heat insulation effect can be achieved.
In one of the embodiments, the heating wire 2021 is vertically disposed.
In another embodiment, the heating wire 2021 may also be horizontally disposed.
In one embodiment, the material of the thermal insulation layer 30 includes one or a combination of aluminum silicate, zirconium oxide, aluminum nitride and aluminum oxide, which improves the thermal insulation performance of the thermal insulation layer 30 and reduces the cost.
In one embodiment, the cooling layer 40 surrounds the container 10 and is isolated from the container 10 by the heating element 20 and the insulating layer 30, the cooling layer 40 comprising a top cooling layer located at the top of the container 10, a middle cooling layer located at the periphery of the container 10, and a bottom cooling layer located at the bottom of the container 10.
In this embodiment, the middle cooling layer is cylindrical.
In one embodiment, the cooling layer 40 is filled with a cooling fluid or a cooling gas.
In one embodiment, the cooling fluid may be water at ambient temperature.
In one embodiment, the temperature of the cooling layer 40 is less than 100 ℃, for example, the temperature of the cooling layer 40 may be 60 ℃ or less.
In one embodiment, the cooling layer 40 comprises a jacket structure or a wound tube structure.
Jacket means an outer jacket applied to the outside of the vessel wall (or pipe wall).
In a specific embodiment, the cooling layer 40 comprises a coiled pipe structure, the cooling layer 40 has cooling fluid pipes 404 distributed therein, and the cooling layer 40 comprises a top cooling layer, a middle cooling layer and a bottom cooling layer, wherein the middle cooling layer is cylindrical, the cooling layer 40 has a cooling fluid inlet and a cooling fluid outlet, in this embodiment, the cooling fluid inlet of the middle cooling layer is located at the lower part of the middle cooling layer, and the cooling fluid outlet is located at the upper part of the middle cooling layer.
In one embodiment, more than 2 thermocouples are included to measure the temperature of the first region 1011 and the second region 1012 within the vessel 10.
In one embodiment, the vessel 10 is provided with temperature sensing holes that mate with thermocouples that pass through gaps between the heating wires 2021 in the heating member 20 and through the temperature sensing holes to measure the temperature within the vessel 10.
In one embodiment, a pressure sensor is included for sensing pressure within the container 10.
In one embodiment, a system of pipes is included, including a pipe for charging the vessel 10 with ammonia, a pipe for cleaning the vessel 10, and a pipe for connecting the press.
One embodiment, as shown in fig. 2, provides a heating method comprising: providing the heating device, and heating the container 10 by using the heating device; wherein, when the lowest temperature in the container 10 is lower than the first temperature, the container 10 is heated to the first temperature at a first heating speed and the pressure in the container 10 is controlled to be lower than the first pressure; when the lowest temperature in the container 10 is higher than the first temperature and lower than the second temperature, heating the container 10 to the second temperature at a second heating speed and controlling the pressure in the container 10 to be lower than the second pressure, wherein the first heating speed is higher than the second heating speed; when the minimum temperature in vessel 10 is equal to the second temperature, the temperature variation in vessel 10 is precisely controlled to control the growth of the gallium nitride single crystal in vessel 10.
In this embodiment, the heating device used in the above heating method includes the cooling layer 40, so that the temperature outside the container 10 is constant, the influence of ambient temperature change on the temperature inside the container 10 is reduced, the precise control of the axial temperature difference inside the container 10 is facilitated, and the cost is reduced; in the above heating method, the heating is performed at the first heating rate and the second heating rate in different time periods, so that the temperature rise process in the container 10 is safer, and the temperature and the pressure can be controlled more accurately.
In a specific embodiment, the above heating method is used for ammonothermal growth of gallium nitride single crystals.
S10: providing the heating device, and heating the container 10 by using the heating device; wherein, when the lowest temperature in the container 10 is lower than the first temperature, the container 10 is heated to the first temperature at a first heating speed and the pressure in the container 10 is controlled to be lower than the first pressure.
In one embodiment, after step S10, the method further includes:
s11: when the temperature inside the vessel 10 is equal to the first temperature, the temperature inside the vessel 10 is maintained and calibration of the temperature and pressure inside the vessel 10 is performed.
The calibration of the temperature and pressure in the container 10 can more accurately control the content of ammonia in the container 10, so that the process is safer.
S20: when the lowest temperature in the container 10 is higher than the first temperature and lower than the second temperature, the container 10 is heated to the second temperature at a second heating speed, and the pressure in the container 10 is controlled to be lower than the second pressure, wherein the first heating speed is higher than the second heating speed.
In one embodiment, the second temperature is an initial temperature for growth of a gallium nitride single crystal.
In one embodiment, the second temperature is 450 ℃ or higher, for example, the second temperature may be 450 ℃, 500 ℃, 600 ℃, 650 ℃.
In one embodiment, the second pressure is the design pressure of the vessel 10.
S30: when the minimum temperature in vessel 10 is equal to the second temperature, the temperature variation in vessel 10 is precisely controlled to control the growth of the gallium nitride single crystal in vessel 10.
In one embodiment, when the first zone temperature or the second zone temperature is less than the first temperature, the first zone is heated at a first zone first heating rate and the second zone is heated at a second zone first heating rate within vessel 10; when the first zone temperature and the second zone temperature are greater than the first temperature and the first zone temperature or the second zone temperature is less than the second temperature, the first zone is heated in the container 10 at the first zone second heating rate and the second zone is heated at the second zone second heating rate.
In one embodiment, the container 10 includes a first region 1011 and a second region 1012, a temperature difference between a temperature of the first region and a temperature of the second region is controlled to be equal to or less than a first temperature difference during heating at a first heating rate, a temperature difference between a temperature of the first region and a temperature of the second region is controlled to be equal to or less than a second temperature difference during heating at a second heating rate, a temperature difference between a temperature of the first region and a temperature of the second region is controlled to be equal to or less than the second temperature difference and equal to or more than a third temperature difference during precise control of a change in temperature within the container 10, the first temperature difference and the second temperature difference are used to ensure safety of the container 10, and the third temperature difference is used to control growth of a gallium nitride single crystal within the container 10.
In one embodiment, the temperature fluctuation range of the first zone temperature and the second zone temperature is controlled to be less than or equal to 5 ℃ and the temperature difference between the first zone temperature and the second zone temperature, namely the third temperature difference is greater than 0 ℃ in the growth process of the gallium nitride single crystal.
In one embodiment, the temperature difference between the first zone temperature and the second zone temperature is controlled to be equal to or less than a first temperature difference, preferably, the first temperature difference is 80 ℃ during heating at the first heating rate.
In one embodiment, the second temperature difference is 50 ℃ or less, preferably, the second temperature difference is 25 ℃.
In one specific embodiment, the heating method is for ammonothermal growth of a gallium nitride single crystal, wherein the first region 1011 is a crystallization region and the second region 1012 is a source material region.
In one embodiment, after growth of the gallium nitride single crystal is complete, heating member 20 is turned off and vessel 10 is cooled by cooling layer 40.
The technical features of the above embodiments can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above embodiments are not described, but should be considered as the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above examples only show some embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (12)
1. A heating device, comprising:
a container;
a heating member located outside the container;
and the cooling layer is positioned outside the container and is isolated from the container through the heating component and the heat insulating layer.
2. The heating device according to claim 1, wherein the container comprises an autoclave, and the autoclave is a container for ammonothermally growing a gallium nitride single crystal.
3. The heating device of claim 1, wherein the container comprises a first zone and a second zone located below the first zone, and the heating means comprises a first heating unit and a second heating unit that are temperature controllable independently of each other, the first heating unit being located at a periphery of the first zone and the second heating unit being located at a periphery of the second zone.
4. The heating apparatus according to claim 3, wherein the heating member and the heat insulating layer together cover the container, a space is provided between the first heating unit and the second heating unit, the space has a size of 50mm or more, the heat insulating layers include a top heat insulating layer, an upper heat insulating layer, a middle heat insulating layer, a lower heat insulating layer, and a bottom heat insulating layer, the top heat insulating layer is located at the top of the container, the upper heat insulating layer is located outside the first zone, the middle heat insulating layer is located between the first heating unit and the second heating unit, the lower heat insulating layer is located outside the second zone, and the bottom heat insulating layer is located at the bottom of the container.
5. The heating device as claimed in claim 1, wherein the heating member comprises a heating wire and a supporting body for supporting the heating wire, and the material of the supporting body comprises one or more of aluminum silicate, zirconium oxide, aluminum nitride and aluminum oxide.
6. The heating device of claim 1, wherein the material of the heat insulating layer comprises one or more of aluminum silicate, zirconium oxide, aluminum nitride and aluminum oxide.
7. The heating device of claim 1, wherein the cooling layer surrounds the container and is isolated from the container by the heating element and the insulating layer, the cooling layer comprising a top cooling layer, a middle cooling layer, and a bottom cooling layer, the top cooling layer being located at the top of the container, the middle cooling layer being located at the periphery of the container, and the bottom cooling layer being located at the bottom of the container.
8. The heating device of claim 1, wherein a cooling liquid or a cooling gas is passed through the cooling layer.
9. The heating device of claim 1, wherein the temperature of the cooling layer is less than 100 ℃.
10. The heating device of claim 1, wherein the cooling layer comprises a jacket structure or a coiled tube structure.
11. A method of heating, comprising:
providing a heating device according to any one of claims 1 to 10, wherein the heating device is used for heating the container; wherein the content of the first and second substances,
when the lowest temperature in the container is lower than a first temperature, rapidly heating the container to the first temperature and controlling the pressure in the container to be lower than a first pressure;
when the lowest temperature in the container is higher than the first temperature and lower than a second temperature, slowly heating the container to the second temperature and controlling the pressure in the container to be lower than a second pressure;
when the lowest temperature in the container is equal to the second temperature, the temperature change in the container is accurately controlled to control the growth of the gallium nitride single crystal in the container.
12. The heating method according to claim 11, wherein the container includes a first zone and a second zone, a temperature difference between a temperature of the first zone and a temperature of the second zone is controlled to be equal to or less than a first temperature difference during the rapid heating, a temperature difference between a temperature of the first zone and a temperature of the second zone is controlled to be equal to or less than a second temperature difference during the slow heating, and a temperature difference between a temperature of the first zone and a temperature of the second zone is controlled to be equal to or less than the second temperature difference and equal to or more than a third temperature difference while precisely controlling a change in temperature within the container.
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