CN111962155B - Preparation method of dielectric layer assisted thick periodically poled ferroelectric crystal - Google Patents

Preparation method of dielectric layer assisted thick periodically poled ferroelectric crystal Download PDF

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CN111962155B
CN111962155B CN202010784697.1A CN202010784697A CN111962155B CN 111962155 B CN111962155 B CN 111962155B CN 202010784697 A CN202010784697 A CN 202010784697A CN 111962155 B CN111962155 B CN 111962155B
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ferroelectric crystal
dielectric layer
periodically poled
bonding
lithium niobate
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CN111962155A (en
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王东周
桑元华
孙德辉
刘齐鲁
王孚雷
周飞
刘宏
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Shandong University
University of Jinan
Jinan Institute of Quantum Technology
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University of Jinan
Jinan Institute of Quantum Technology
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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
    • C30B30/00—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions
    • C30B30/02—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions using electric fields, e.g. electrolysis
    • 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
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    • C30B29/30—Niobates; Vanadates; Tantalates

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Abstract

The invention discloses a method for preparing a thick periodically poled ferroelectric crystal based on the assistance of a dielectric layer, wherein the dielectric layer is firstly prepared on the polished surface of a periodically poled ferroelectric crystal material. The dielectric layer is an isotropic transparent material and then the transparent dielectric layer is polished. Due to the existence of the dielectric layer, a particularly flat surface can be obtained, and the formation of high-quality bonded crystals is facilitated. The thickness of the dielectric layer is almost negligible relative to the thickness of the crystal, and the performance of the crystal, particularly the nonlinear optical performance, is not influenced.

Description

Preparation method of dielectric layer assisted thick periodically poled ferroelectric crystal
Technical Field
The invention relates to the field of materials, in particular to a preparation method of a dielectric layer assisted thick periodically poled ferroelectric crystal.
Background
Periodically Poled Lithium Niobate (PPLN) crystals based on quasi-phase matching technology become an important nonlinear optical material due to the fact that the periodically poled lithium niobate crystals have very large nonlinear coefficients, flexible design and wide light transmission range. However, the damage resistance of lithium niobate crystal is relatively low, and even through doping/near stoichiometric ratio growth and other technologies, the requirement of high-power density nonlinear optical frequency conversion still cannot be met. The existing solution is to achieve high power laser generation through a large clear aperture. However, the preparation of the periodically poled lithium niobate crystal with large thickness is difficult, the maximum preparation thickness of the periodically poled lithium niobate with high quality is only 2mm at present, the preparation is only mastered in a few units, and the foreign high-quality crystal is blocked domestically.
In the prior art, to prepare PPLN crystals of large thickness, for example, "Periodicpoling in 3-mm-thick-brick MgO: LiNbO3crystals "[ Ishizuki, Hideki et al, Japanese journal of applied physics 42.2A (2003): L108.]，"Half-joule output optical-parametric oscillation by using10-mm-thick periodically poled Mg-doped congruentLiNbO3"[ Ishizuki, Hideki and Takunrori Taira, Optics Express 20.18(2012):20002-]And "High-energy quasi-phase-matched catalytic catalysis in a polydicalcium poled MgO" LiNbO3device with a 5mm by 5mm alert "[ Ishizuki Hideki and Takuori Taira, Optics letters 30.21(2005):2918-]Et al, however, the quality of the large thickness PPLN crystals prepared based on these prior solutions is not high, and the performance is affected by the inability to form a complete periodic domain structure.
Another prior art approach for obtaining large thickness periodically poled lithium niobate crystals is to obtain large thickness wafer materials by bonding two thin periodically poled lithium niobate wafers. Because the periodically poled lithium niobate crystal less than 2mm can obtain high-quality samples by a mature technology, especially periodically poled lithium niobate crystals with the thickness of 1mm or less, high-quality large-size samples can be obtained relatively simply. By bonding two lithium niobate crystals with small thickness, the periodically poled lithium niobate crystal with large thickness can be finally obtained. For example, similar reports are found in the documents of "Difsion-bonded tables of ferroelectric poled crystals" [ Missey M J et al Optics letters,1998,23(9):664 ], "Fabric of piezoelectric-poled ferroelectric crystals by solid state poled field poling and direct tboding" [ Kim B J et al Journal of the Optical Society of Korea,2010,14(4):420 423], Chinese patent application No. 201110241438.5 entitled "method for preparing a periodically poled ferroelectric crystal material with large thickness".
However, it has been found in practice that these techniques, which are currently based on bonding techniques, do not allow to obtain periodically poled lithium niobate crystals of large thickness with satisfactory quality. The inventor of the present invention has found through extensive research that, in the prior art, bonding is performed after periodically poled lithium niobate crystals are directly polished, and due to the influence of the internal structure of the periodically poled lithium niobate crystals, periodic stripes are generated when the periodically poled lithium niobate crystals are finely polished, which seriously affects the polishing precision of the surfaces thereof, that is, planes with high flatness cannot be formed, as shown in fig. 1. Since such a plane with high flatness cannot be formed in the current preparation scheme based on the bonding technology, bubbles and defects are easily formed in the bonding process, and the defect of high stress exists, which finally has adverse effect on the quality of the prepared crystal.
In addition, another method for preparing a large-thickness periodically poled ferroelectric crystal material is disclosed in the prior art, for example, see chinese patent application No. 201110431555.8, in which a transparent electrode is provided on the + Z plane of two ferroelectric crystal materials, then the two ferroelectric crystal materials are bonded on the + Z plane to obtain a composite ferroelectric crystal, and then the composite ferroelectric crystal is poled to obtain a large-thickness periodically poled ferroelectric crystal material. As can be seen from analysis, in this scheme, the flatness of the bonding surface cannot be controlled, which makes the bonding effect unpredictable and the quality not guaranteed; meanwhile, in this scheme, a connection operation between the transparent electrode on the bonding surface and the pulse power source is required, which makes the entire preparation operation very complicated and difficult to implement industrially.
Disclosure of Invention
The inventor discloses the root cause of poor effect of the existing preparation method of the large-thickness periodic polarization ferroelectric crystal material by carrying out deep research on the prior art, and pertinently provides a preparation method of the thick periodic polarization ferroelectric crystal based on the assistance of the dielectric layer, so that the high-quality thick periodic polarization ferroelectric crystal, such as a lithium niobate crystal, a lithium tantalate crystal and the like, can be prepared and obtained in a simple manner.
In the preparation method of the thick periodically poled ferroelectric crystal based on the dielectric layer assistance, the dielectric layer is firstly prepared on the polished surface of the periodically poled ferroelectric crystal material. The dielectric layer is an isotropic transparent material and then the transparent dielectric layer is polished. Due to the existence of the dielectric layer, a particularly flat surface can be obtained, and the formation of high-quality bonded crystals is facilitated. The thickness of the dielectric layer is almost negligible relative to the thickness of the crystal, and does not affect the performance of the crystal, particularly the nonlinear optical performance.
Specifically, the invention relates to a preparation method of a dielectric layer assisted thick periodically poled ferroelectric crystal, which comprises a dielectric layer forming step, a bonding preparation step and a bonding step, wherein:
in the dielectric layer forming step, forming a transparent dielectric layer with a preset thickness on the surfaces of the first periodic polarized ferroelectric crystal material and the second periodic polarized ferroelectric crystal material, and polishing the surface of the transparent dielectric layer to form a polished surface;
aligning the polished surfaces of the transparent dielectric layers on the first and second periodically poled ferroelectric crystal materials and bonding the aligned polished surfaces together in the bonding preparation step; and the number of the first and second groups,
in the bonding step, pressure is applied to two sides of the first and second periodically poled ferroelectric crystal materials to enable the two materials to be in close contact, and bonding is carried out at a first preset temperature to form a thick periodically poled ferroelectric crystal.
Further, the manufacturing method of the present invention further includes a preparation step for providing the first periodically poled ferroelectric crystal material and the second periodically poled ferroelectric crystal material. Wherein in the preparing step, the surfaces of the first and second periodically poled ferroelectric crystal materials are further subjected to polishing treatment to form polished surfaces; and/or preparing the first and second periodically poled ferroelectric crystal materials by an applied electric field poling method.
Further, the periodically poled ferroelectric crystal material is one of lithium niobate crystal with the same composition, magnesium-doped lithium niobate crystal with the same composition, lithium niobate crystal with near stoichiometric ratio doped with magnesium, lithium tantalate crystal, potassium titanyl phosphate, rubidium titanyl phosphate and potassium titanyl arsenate.
Further, the periodically poled ferroelectric crystal material has a thickness of 0.5mm to 3 mm; and/or the transparent medium layer is formed by isotropic transparent materials; and/or the thickness of the transparent medium layer is 10-500 nm; and/or the polished surface of the transparent dielectric layer has a flatness of less than 5nm and/or the transparent dielectric layer is formed by magnetron sputtering, physical vapor deposition, chemical vapor deposition, plasma-enhanced chemical vapor deposition, or electron beam evaporation.
Preferably, the transparent dielectric layer is SiO2A dielectric layer or a dielectric layer with the same composition as the periodically poled ferroelectric crystal material.
Preferably, in the bonding preparation step, the alignment accuracy is less than or equal to ± 2 μm.
Preferably, in the bonding step, the pressure is between 10 and 100N/m2To (c) to (d); and/or the maximum temperature of the first preset temperature is between 400 and 800 ℃.
Further, the preparation method of the invention further comprises a post-processing step, which is used for annealing the thick periodically polarized ferroelectric crystal provided by the bonding step at a second preset temperature and polishing the light-passing surface of the annealed thick periodically polarized ferroelectric crystal.
Preferably, the second preset temperature is 300 ℃.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 shows the surface morphology of a crystal obtained by a method for preparing a large-thickness periodically poled lithium niobate crystal based on bonding in the prior art;
FIG. 2 schematically illustrates the steps of a dielectric layer assisted thick-film periodically poled ferroelectric (e.g., lithium niobate) crystal fabrication method of the present invention.
In the drawings:
c1 and C2 are first and second periodic poled ferroelectric (e.g., lithium niobate) crystals, respectively, which may be prepared, for example, by an applied electric field poling process;
d1 and D2 are first and second dielectric layers formed on the first and second ferroelectric crystals C1 and C2, respectively;
B-C are thick periodically poled ferroelectric (e.g. lithium niobate) crystals that are finally formed by bonding.
Detailed Description
Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings. The following examples are provided by way of illustration in order to fully convey the spirit of the invention to those skilled in the art to which the invention pertains. Accordingly, the present invention is not limited to the embodiments disclosed herein.
FIG. 2 is a schematic flow chart of the preparation method of the dielectric layer assisted thick periodically poled ferroelectric crystal of the present invention.
In the present invention, the method for producing a thick periodically poled ferroelectric crystal may comprise a preparation step.
In the preparing step, a first periodically poled ferroelectric crystal material and a second periodically poled ferroelectric crystal material may be provided.
As an example, a periodically poled ferroelectric crystal material may be prepared using an applied electric field poling method. For example, the prepared periodically poled ferroelectric crystal material may have a thickness of 0.5mm to 3 mm.
In the present invention, the ferroelectric crystal material may be (but is not limited to) a homomorphic lithium niobate crystal, a magnesium-doped homomorphic lithium niobate crystal, a near stoichiometric lithium niobate crystal, a magnesium-doped near stoichiometric lithium niobate crystal, a lithium tantalate crystal, potassium titanyl phosphate, rubidium titanyl phosphate, potassium titanyl arsenate, or other ferroelectric crystal material.
In this preparation step, the surfaces of the first and second periodically poled ferroelectric crystal materials may also be subjected to polishing treatment to form polished surfaces. For example, a polished surface may be formed on the bonding surface of the crystalline material. Further, the first and second periodically poled ferroelectric crystal materials may be cut to the same size as needed.
The preparation method of the thick periodically poled ferroelectric crystal can also comprise a dielectric layer forming step.
In the dielectric layer forming step, a transparent dielectric layer of a predetermined thickness may be formed on the polished surfaces of the poled ferroelectric crystal material in the first and second periods, and the surface of the dielectric layer may be subjected to a fine polishing process.
The transparent dielectric layer may be formed of an isotropic transparent material. For example, the transparent dielectric layer may be SiO2Dielectric layer, or LiNbO3A dielectric layer.
The transparent dielectric layer may be formed on the polished surfaces of the first and second period poled ferroelectric crystal materials by means of magnetron sputtering, physical vapor deposition, chemical vapor deposition, plasma-enhanced chemical vapor deposition, electron beam evaporation, or the like.
The thickness of the transparent dielectric layer can be controlled in the nanometer level. Preferably, the thickness of the transparent dielectric layer may be controlled to be between 10-500 nm.
In a preferred example, the transparent dielectric layer may be finely polished to have a flatness of less than 5 nm.
The method for preparing the thick periodically poled ferroelectric crystal can also comprise a bonding preparation step.
In the bonding preparation step, the polished surfaces of the transparent dielectric layers on the first and second periodically poled ferroelectric crystal materials may be accurately aligned by means of a high-precision alignment technique, and the aligned polished surfaces may be brought together. Preferably, the alignment accuracy may be less than or equal to ± 2 μm.
The preparation method of the thick periodically poled ferroelectric crystal can also comprise a bonding step.
In the bonding step, pressure may be applied to both sides of the polarized ferroelectric crystal material in the first and second periods to bring the two into close contact, and bonding may be performed at a first preset temperature.
In a preferred example, the applied pressure may be between 10-100N/m2In the meantime. The maximum temperature of the first predetermined temperature may be between 400 and 800 ℃.
Finally, the method for preparing the thick periodically poled ferroelectric crystal of the present invention may comprise a post-processing step.
In the post-processing step, annealing treatment may be performed on the bonded periodically poled ferroelectric crystal material at a second preset temperature, and polishing treatment may be performed on a light-passing surface of the annealed periodically poled ferroelectric crystal material.
Thereby, a high quality thick periodically poled ferroelectric crystal material can be obtained from the first and second periodically poled ferroelectric crystal materials by means of the dielectric layer based on the bonding technique. At this time, the thick periodically poled ferroelectric crystal material can be suitably used for manufacturing an optical device.
The method for the preparation of the dielectric layer assisted thick-film periodically poled ferroelectric crystal according to the invention will be further described below with the aid of several exemplary embodiments.
(example 1)
In the preparation step, the first and second Z-cut congruent lithium niobate crystals are prepared by an external electric field polarization method, and the periods of the first and second Z-cut congruent lithium niobate crystals are 30 micrometers, the thicknesses of the first and second Z-cut congruent lithium niobate crystals are 1mm, the lengths of the first and second Z-cut congruent lithium niobate crystals are 30mm, and the widths of the first and second Z-cut congruent lithium niobate crystals are 10 mm. And, the surfaces to be bonded (the dimensions of which are 30mm × 10mm) of the first and second homoconstituent lithium niobate crystals are polished, thereby forming polished surfaces.
In the dielectric layer forming step, SiO of 30nm is formed on the polished surfaces of the first and second lithium niobate crystals of the same composition by magnetron sputtering, respectively2And finely polishing the surface of the dielectric layer.
In the bonding preparation step, the surfaces of the polished dielectric layers on the first and second congruent lithium niobate crystals are precisely aligned and bonded together.
In the bonding step, 50N/m is used2The force of (a) causes the first and second congruent lithium niobate crystals to be tightly held together and heated at 500 c for 4 hours to effect bonding.
In the post-treatment step, the bonded first and second congruent lithium niobate crystals were annealed at 300 ℃ and the light-passing surfaces of the bonded crystals were polished, thereby obtaining thick periodically polarized congruent lithium niobate crystals having a thickness of 2mm and a size of 30mm × 10 mm.
(example 2)
In the preparation step, the first Z-cut magnesium-doped congruent lithium niobate crystal and the second Z-cut magnesium-doped congruent lithium niobate crystal are prepared by adopting an external electric field polarization method. Wherein the period of the first Z-cut magnesium-doped congruent lithium niobate crystal is 20 microns, the thickness of the first Z-cut magnesium-doped congruent lithium niobate crystal is 1mm, the length of the first Z-cut magnesium-doped congruent lithium niobate crystal is 40mm, the width of the first Z-cut magnesium-doped congruent lithium niobate crystal is 10mm, and the period of the second Z-cut magnesium-doped congruent lithium niobate crystal is 20 microns, the thickness of the second Z-cut magnesium-doped congruent lithium niobate crystal is 2mm, the length of the second Z-cut magnesium-doped congruent lithium niobate crystal is 40mm, and the width of the second Z-cut magnesium-doped congruent lithium niobate crystal is 10 mm.
And, the surfaces to be bonded (the size of which is 40mm × 10mm) of the first and second magnesium-doped homoconstituent lithium niobate crystals are polished, thereby forming polished surfaces.
In the step of forming the dielectric layer, 50nm SiO is formed on the polished surfaces of the first and second magnesium-doped lithium niobate crystals with the same composition by magnetron sputtering2And finely polishing the surface of the dielectric layer.
In the bonding preparation step, the surfaces of the polished dielectric layers on the first and second magnesium-doped congruent lithium niobate crystals are precisely aligned and bonded together.
In the bonding step, 30N/m is used2The forces of (a) and (b) are such that the first and second magnesium-doped congruent lithium niobate crystals are held together tightly and bonded by heating at 750 c for 2 hours.
In the post-treatment step, the bonded first and second magnesium-doped congruent lithium niobate crystals are annealed at 300 ℃, and the light-passing surfaces of the bonded crystals are polished, thereby obtaining thick-piece periodically polarized magnesium-doped congruent lithium niobate crystals with a thickness of 3mm and a size of 40mm × 10 mm.
Example 3:
in the preparation step, the first and second Z-cut near-stoichiometric lithium niobate crystals are prepared by an external electric field polarization method, wherein the period is 20 microns, the thickness is 1mm, and the diameter is 50 mm. And, the surfaces to be bonded (the diameter thereof is 50mm) of the first and second near-stoichiometric lithium niobate crystals are polished to form polished surfaces.
In the dielectric layer forming step, LiNbO of 25nm is formed on the polished surfaces of the first and second near-stoichiometric lithium niobate crystals by magnetron sputtering, respectively3And finely polishing the surface of the dielectric layer.
In the bonding preparation step, the surfaces of the polished dielectric layers on the first and second near-stoichiometric lithium niobate crystals are precisely aligned and bonded together.
In the bonding step, 75N/m is used2The first and second near stoichiometric lithium niobate crystals are brought into close proximity and bonded by heating at 400 c for 6 hours.
In the post-treatment step, the bonded first and second near-stoichiometric lithium niobate crystals are annealed at 300 ℃, and the light-passing surfaces of the bonded crystals are polished, thereby obtaining a periodically poled near-stoichiometric lithium niobate crystal having a thickness of 2mm and a diameter of 50 mm.
In the invention, through the unique design of the dielectric layer, a particularly smooth bonding surface can be obtained, which is beneficial to forming high-quality bonding crystals. Meanwhile, the thickness of the dielectric layer is almost negligible relative to the thickness of the crystal, and the performance of the crystal, particularly the nonlinear optical performance, is not affected.
Although the present invention has been described in connection with the embodiments illustrated in the accompanying drawings, it will be understood by those skilled in the art that the embodiments described above are merely exemplary for illustrating the principles of the present invention and are not intended to limit the scope of the present invention, and that various combinations, modifications and equivalents of the above-described embodiments may be made by those skilled in the art without departing from the spirit and scope of the present invention.

Claims (9)

1. A preparation method of a dielectric layer assisted thick periodically poled ferroelectric crystal comprises a dielectric layer forming step, a bonding preparation step and a bonding step, wherein:
in the dielectric layer forming step, forming a transparent dielectric layer with a preset thickness on the surfaces of the first periodic polarized ferroelectric crystal material and the second periodic polarized ferroelectric crystal material, and polishing the surface of the transparent dielectric layer to form a polished surface;
aligning the polished surfaces of the transparent dielectric layers on the first and second periodically poled ferroelectric crystal materials and bonding the aligned polished surfaces together in the bonding preparation step; and the number of the first and second groups,
in the bonding step, pressure is applied to two sides of the first periodic polarization ferroelectric crystal material and the second periodic polarization ferroelectric crystal material to enable the two sides to be in close contact, and bonding is carried out at a first preset temperature to form a thick periodic polarization ferroelectric crystal;
the transparent medium layer is made of isotropic transparent material and is made of SiO2A dielectric layer or a dielectric layer with the same composition as the periodically poled ferroelectric crystal material.
2. The method of manufacturing of claim 1, further comprising a preparatory step for providing the first periodically poled ferroelectric crystal material and the second periodically poled ferroelectric crystal material.
3. The manufacturing method according to claim 2, wherein in the preparing step, the surfaces of the first and second periodically poled ferroelectric crystal materials are further subjected to polishing treatment to form polished surfaces;
and/or preparing the first and second periodically poled ferroelectric crystal materials by an applied electric field poling method.
4. The method of claim 1, wherein the periodically poled ferroelectric crystal material is one of a lithium niobate crystal of homogeneous composition, a lithium niobate crystal of homogeneous composition doped with magnesium, a lithium niobate crystal of near stoichiometric ratio doped with magnesium, a lithium tantalate crystal, potassium titanyl phosphate, rubidium titanyl phosphate, potassium titanyl arsenate.
5. The production process according to claim 1, wherein,
the periodically poled ferroelectric crystal material has a thickness of 0.5mm to 3 mm;
and/or the thickness of the transparent medium layer is 10-500 nm;
and/or the polished surface of the transparent dielectric layer has a flatness of less than 5nm
And/or the transparent medium layer is formed by a magnetron sputtering method, a physical vapor deposition method, a chemical vapor deposition method, a plasma enhanced chemical vapor deposition method or an electron beam evaporation method.
6. The production method according to claim 1, wherein in the bonding preparation step, the alignment accuracy is less than or equal to ± 2 μm.
7. The production method according to claim 1, wherein, in the bonding step, the pressure is between 10 and 100N/m2To (c) to (d);
and/or the maximum temperature in the first preset temperature is between 400 ℃ and 800 ℃.
8. The manufacturing method according to claim 1, further comprising a post-processing step of annealing the thick periodically poled ferroelectric crystal provided in the bonding step at a second predetermined temperature and polishing a light-passing surface of the annealed thick periodically poled ferroelectric crystal.
9. The method of claim 8, wherein the second predetermined temperature is 300 ℃.
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