CN117867638A - Method for preparing SiC by raising temperature of Si-based solution through aluminothermic reaction - Google Patents
Method for preparing SiC by raising temperature of Si-based solution through aluminothermic reaction Download PDFInfo
- Publication number
- CN117867638A CN117867638A CN202410004428.7A CN202410004428A CN117867638A CN 117867638 A CN117867638 A CN 117867638A CN 202410004428 A CN202410004428 A CN 202410004428A CN 117867638 A CN117867638 A CN 117867638A
- Authority
- CN
- China
- Prior art keywords
- sic
- temperature
- based solution
- thermite
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000007133 aluminothermic reaction Methods 0.000 title abstract description 9
- 239000013078 crystal Substances 0.000 claims abstract description 38
- 239000003832 thermite Substances 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 7
- 239000010439 graphite Substances 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 230000003028 elevating effect Effects 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000006184 cosolvent Substances 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 7
- 230000001276 controlling effect Effects 0.000 abstract description 6
- 239000000843 powder Substances 0.000 abstract description 6
- 230000001105 regulatory effect Effects 0.000 abstract description 4
- 239000007790 solid phase Substances 0.000 abstract description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 39
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 35
- 239000000758 substrate Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000007792 addition Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B27/00—Single-crystal growth under a protective fluid
- C30B27/02—Single-crystal growth under a protective fluid by pulling from a melt
-
- 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
- C30B29/36—Carbides
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for preparing SiC by raising the temperature of a Si-based solution through thermite reaction, which comprises the steps of uniformly mixing a high-purity Si material and a thermite, placing the mixture in a graphite crucible, and controlling heating of a thermal field to enable the upper temperature of the solution to be lower than the lower temperature; and slowly reducing the seed crystal to be in contact with the Si-based solution system after the thermal field is stabilized, starting the rotary pulling system to start crystal growth, and obtaining the SiC monocrystal. The invention heats powder by utilizing heat generated by aluminothermic reaction, and utilizes Ti, cr or Fe elements generated by the reaction as cosolvent to dissolve C element, and the P-type SiC crystal is prepared by regulating and controlling the proportion of A1 element to ensure that the Al remains after the complete reaction. Al produced by the reaction 2 O 3 In solid phase in Si-based solutionThe SiC crystal growth is not affected, the time for heating is reduced, the problem of overhigh energy consumption in the SiC crystal growth process is solved, and the production cost is reduced.
Description
Technical Field
The invention belongs to the technical field of silicon carbide production, relates to SiC preparation, and in particular relates to a method for preparing SiC by increasing the temperature of a Si-based solution through aluminothermic reaction, which reduces the time required for heating, solves the problem of overhigh energy consumption in the SiC crystal growth process and reduces the production cost.
Background
SiC is a wide bandgap semiconductor material that stands out in a large number of semiconductor materials due to its high thermal conductivity, high breakdown field and large electron mobility. Typically, siC single crystals are prepared by Physical Vapor Transport (PVT), which requires high temperatures (about 2500K), and the dislocation density of the SiC substrate produced is still high, and the production of P-type SiC substrates by PVT is still difficult, limiting its further use.
The solution method attracts attention as a method for producing high-quality SiC single crystal, and the growth interface is almost in an equilibrium state during the growth process, so that grown crystal micropipes and dislocation defects are very few.
Solution growth generally requires placing a co-solvent and a high purity Si material together in a graphite crucible as the C source, and transporting the solution in a molten state to the upper seed crystal of the collapse with internal convection for crystal growth. Since the solubility of C in Si is very low at high temperatures, the addition of a co-solvent is generally required to promote the dissolution of C in Si. As the cosolvent, fe, ti, cr, etc. can be generally used. In recent decades, researchers have investigated the effect of various solution systems on crystal growth. For example, by using Si-Ti-C or Si-Cr-C solvents, a growth rate of about 0.3mm/h at relatively low temperatures (about 1800 ℃ C.) can be achieved.
The SiC crystal growth requires extremely high temperatures and the temperature rise process consumes a large amount of electrical energy. SiC substrates occupy 60% of the cost of the entire industry chain, and SiC can only be used in large-scale applications if the cost of the substrate is reduced.
Thermite reactions are a classical and practical chemical reaction. As shown in the following formula,
the aluminum simple substance can be combined with Fe at high temperature 2 O 3 、TiO 2 、Cr 2 O 3 The metal oxides react to generate a large amount of heat.
Disclosure of Invention
In order to solve the defects of overlarge energy consumption and high cost in the existing preparation of SiC, the invention provides a method for preparing SiC by raising the temperature of a Si-based solution through aluminothermic reaction. Because the temperature of SiC crystal prepared by the solution method is about 1800 ℃, al generated by the reaction 2 O 3 The melting point is 2054 ℃, the boiling point is 2980 ℃, and the SiC crystal growth is not affected by the solid phase in the Si-based solution.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the invention provides a method for preparing SiC by raising the temperature of a Si-based solution through aluminothermic reaction, which comprises the following steps:
1) Uniformly mixing a high-purity Si material and a thermite, then placing the mixture in a graphite crucible, and controlling heating by a thermal field to ensure that the upper temperature of the solution is lower than the lower temperature;
2) Slowly reducing seed crystal to contact with the Si-based solution system after the thermal field is stable, starting a rotary pulling system to start crystal growth, and obtaining SiC monocrystal;
the prepared P-type SiC monocrystal is P-type 4H-SiC or P-type 6H-SiC.
According to the invention, the powder is heated by utilizing heat generated by aluminothermic reaction, ti, cr or Fe elements generated by the reaction are used as cosolvent to dissolve C element, and the proportion of A1 element is regulated and controlled to ensure that Al balance is remained after the complete reaction to prepare the P-type SiC crystal, so that the electric energy loss in the heating process of growing the SiC crystal by a solution method is effectively reduced by 20% -30%, and the cost reduction and synergy of the SiC industry are promoted.
As a preferred embodiment of the present invention, in the step 1), the purity of the high purity Si material is 99.99%.
As a preferred embodiment of the invention, in step 1), the upper temperature of the solution is 5-30K lower than the lower temperature.
As a preferable scheme of the invention, the thermite consists of two materials, namely A and B, wherein A is aluminum powder, B is Fe 2 O 3 、TiO 2 、Cr 2 O 3 One of them.
As a preferable scheme of the invention, the element content of the material A in the thermite is more than 30-50% of the stoichiometric ratio of the material B compound.
As a preferable scheme of the invention, the mol ratio of the high-purity Si material to the thermite is 1:1-9:1.
As a preferable scheme of the invention, in the step 2), the growth condition is 2000K-2400K, the growth atmosphere is 100% argon, the pressure is 150KPa, and the growth time is 30-100h.
As a preferable mode of the invention, in the step 2), the rotation speed of the seed crystal is 10rpm, the rotation speed of the crucible is 5rpm, and the stretching rate is 0.1-0.8mm/h.
Compared with the prior art, the invention has the following beneficial effects:
1) The invention innovatively utilizes high-purity Si material and thermite to grow SiC crystal by a solution method, heats powder by heat generated by thermite reaction, dissolves C element by taking Ti, cr or Fe element generated by the reaction as cosolvent, and prepares P-type SiC crystal by regulating and controlling the proportion of A1 element to ensure that the thermite still has A1 balance after complete reaction.
2) The invention effectively reduces the electric energy loss by 20% -30% in the heating process of growing SiC crystals by a solution method, and promotes the cost reduction and synergy of the SiC industry.
3) The method reduces the time required by heating by the heat released by the aluminothermic reaction, solves the problem of overhigh energy consumption in the SiC crystal growth process, and reduces the production cost.
Drawings
Fig. 1 is a flow chart of the present invention.
Detailed Description
In order to facilitate understanding of the technical means, the creation characteristics, the achievement of the objects and the effects achieved by the present invention, the present invention is further described below with reference to specific examples, but the following examples are only preferred examples of the present invention, not all of which are described in detail below. Based on the examples in the embodiments, those skilled in the art can obtain other examples without making any inventive effort, which fall within the scope of the invention. The experimental methods in the following examples are conventional methods unless otherwise specified, and materials, reagents, etc. used in the following examples are commercially available unless otherwise specified.
Referring to fig. 1, the present invention provides a method for preparing SiC by elevating the temperature of a Si-based solution by means of a thermite reaction, the method comprising the steps of:
1) Uniformly mixing a high-purity Si material and a thermite, then placing the mixture in a graphite crucible, and controlling heating by a thermal field to ensure that the upper temperature of the solution is lower than the lower temperature;
2) Slowly reducing seed crystal to contact with the Si-based solution system after the thermal field is stable, starting a rotary pulling system to start crystal growth, and obtaining SiC monocrystal;
the prepared P-type SiC monocrystal is P-type 4H-SiC or P-type 6H-SiC.
Example 1
The embodiment provides a method for preparing SiC by rapidly increasing the temperature of a Si-based solution by means of aluminothermic reaction, which comprises the following steps:
the high-purity Si material and the thermite are uniformly mixed and then placed in a graphite crucible. The thermite is prepared from aluminum powder and Fe 2 O 3 Composition, aluminum powder content is greater than Fe 2 O 3 30% of the stoichiometric ratio of the chemical reaction. The mol ratio of the high-purity Si material to the thermite is 1:1. the heating by the thermal field is controlled to make the upper temperature of the solution lower than the lower temperature by about 5K.
After the thermal field is stable, the seed crystal slowly descends to be contacted with the Si-based solution system, and the rotary pulling system is started to start crystal growth. The growth temperature is 2000K, the growth atmosphere is 100% argon, the pressure is 150KPa, the growth time is 100h, the rotation speed of seed crystal is 10rpm, the rotation speed of crucible is 5rpm, and the stretching rate is 0.5mm/h.
Comparative example 1
And uniformly mixing the high-purity Si material and Fe powder, and then placing the mixture in a graphite crucible. The molar ratio of the high-purity Si material to the Fe powder is 1:1. the heating by the thermal field is controlled to make the upper temperature of the solution lower than the lower temperature by about 5K.
After the thermal field is stable, the seed crystal slowly descends to be contacted with the Si-based solution system, and the rotary pulling system is started to start crystal growth. The growth temperature is 2000K, the growth atmosphere is 100% argon, the pressure is 150KPa, the growth time is 100h, the rotation speed of seed crystal is 10rpm, the rotation speed of crucible is 5rpm, and the stretching rate is 0.5mm/h.
The effect on energy consumption using thermite is shown in table 1.
TABLE 1 influence of energy consumption
| Total energy consumption of growth | |
| Example 1 | 4129KWh |
| Comparative example 1 | 3256KWh |
As can be seen from Table 1, the invention uses high purity Si material and thermite to grow SiC crystal by solution method, uses heat generated by thermite reaction to heat powder, uses Ti, cr or Fe element generated by reaction as cosolvent to dissolve C element, and makes thermite still have A1 balance after complete reaction to prepare P-type SiC crystal by regulating and controlling A1 element proportion, thereby effectively reducing electric energy loss by 20% -30% in heating process of SiC crystal grown by solution method, and promoting SiC industry to reduce cost and increase efficiency.
While the invention has been described with respect to preferred embodiments thereof, it will be understood by those skilled in the art that various modifications and additions may be made without departing from the scope of the invention. Equivalent embodiments of the present invention will be apparent to those skilled in the art having the benefit of the teachings disclosed herein, when considered in the light of the foregoing disclosure, and without departing from the spirit and scope of the invention; meanwhile, any equivalent changes, modifications and evolution of the above embodiments according to the essential technology of the present invention still fall within the scope of the technical solution of the present invention.
Claims (8)
1. A method for preparing SiC by elevating the temperature of a Si-based solution by means of thermite reaction, comprising the steps of:
1) Uniformly mixing a high-purity Si material and a thermite, then placing the mixture in a graphite crucible, and controlling heating by a thermal field to ensure that the upper temperature of the solution is lower than the lower temperature;
2) Slowly reducing seed crystal to contact with the Si-based solution system after the thermal field is stable, starting a rotary pulling system to start crystal growth, and obtaining SiC monocrystal;
the prepared P-type SiC monocrystal is P-type 4H-SiC or P-type 6H-SiC.
2. The method for preparing SiC by elevating the temperature of a Si based solution according to claim 1, wherein in step 1), the purity of the high purity Si material is 99.99%.
3. The method for producing SiC by raising the temperature of a Si based solution by thermite reaction according to claim 1, wherein in step 1), the upper temperature of the solution is 5-30K lower than the lower temperature.
4. The method for preparing SiC by raising the temperature of a Si-based solution by thermite reaction according to claim 1, wherein the thermite is composed of two materials A and B, wherein A is aluminum powder and B is Fe 2 O 3 、TiO 2 、Cr 2 O 3 One of them.
5. The method for preparing SiC by elevating the temperature of a Si based solution according to claim 4, wherein the content of the element of the a material in the thermite is greater than 30% to 50% of the stoichiometric ratio of the compound of the B material.
6. The method for preparing SiC by elevating the temperature of a Si based solution by thermite reaction according to claim 1, wherein the molar ratio of high purity Si material to thermite is 1:1-9:1.
7. The method for preparing SiC by elevating the temperature of a Si based solution according to claim 1, wherein in step 2), the growth conditions are 2000K to 2400K, 100% argon, 150KPa, and 30 to 100h.
8. The method for preparing SiC by elevating the temperature of a Si based solution according to claim 1, wherein in step 2), the rotation speed of the seed crystal is 10rpm, the rotation speed of the crucible is 5rpm, and the stretching rate is 0.1-0.8mm/h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410004428.7A CN117867638A (en) | 2024-01-03 | 2024-01-03 | Method for preparing SiC by raising temperature of Si-based solution through aluminothermic reaction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410004428.7A CN117867638A (en) | 2024-01-03 | 2024-01-03 | Method for preparing SiC by raising temperature of Si-based solution through aluminothermic reaction |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117867638A true CN117867638A (en) | 2024-04-12 |
Family
ID=90587728
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202410004428.7A Pending CN117867638A (en) | 2024-01-03 | 2024-01-03 | Method for preparing SiC by raising temperature of Si-based solution through aluminothermic reaction |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117867638A (en) |
-
2024
- 2024-01-03 CN CN202410004428.7A patent/CN117867638A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP2004883B1 (en) | Method of manufacturing a silicon carbide single crystal | |
| CN103305903B (en) | A kind of high nitrogen pressure fusing assistant-falling crucible method prepares the method for GaN crystal | |
| CN109553105B (en) | High-purity silicon carbide powder and preparation method thereof | |
| CN102732953A (en) | Technology and apparatus for growing single silicon carbide crystals through double seed crystal-assisted vapor transport method | |
| WO2003078703A1 (en) | CdTe SINGLE CRYSTAL AND CdTe POLYCRYSTAL, AND METHOD FOR PREPARATION THEREOF | |
| CN108118394B (en) | Method for reducing nitrogen impurity content in silicon carbide single crystal | |
| CN116121870A (en) | Method for growing SiC monocrystal by solution method | |
| TW202346661A (en) | Semi-insulating gallium arsenide single crystal and a preparation method and growth device thereof | |
| CN109629003B (en) | Preparation method of low-concentration P-type indium phosphide single crystal | |
| CN115124040A (en) | Solid-phase synthesis method for improving material ratio of large-particle-size silicon carbide powder | |
| JP7235318B2 (en) | SEMI-INSULATING SILICON CARBIDE SINGLE CRYSTAL DOPED WITH MINOR VANADIUM, SUBSTRATE AND MANUFACTURING METHOD | |
| CN110284195A (en) | Boron phosphide single crystal and preparation method and application thereof | |
| CN108560053A (en) | The yttrium luetcium silicate scintillation material and its growing method that a kind of lanthanum, dysprosium, cerium are co-doped with | |
| JP2002249376A (en) | Low nitrogen concentration carbonaceous material and method for producing the same | |
| US5211801A (en) | Method for manufacturing single-crystal silicon carbide | |
| CN117867638A (en) | Method for preparing SiC by raising temperature of Si-based solution through aluminothermic reaction | |
| CN102094236B (en) | Czochralski method for growing long-lifetime P-type boron-doped silicon single crystal | |
| CN116145258A (en) | Method for growing SiC crystal by low-temperature solution method | |
| JPS6350399A (en) | Method for growing p-type sic single crystal | |
| JP5419116B2 (en) | Bulk crystal growth method | |
| CN112919914A (en) | Preparation method of AlN ceramic powder | |
| CN113106547A (en) | Preparation method of large-size high-resistivity gallium-lanthanum tantalate crystal | |
| CN111394781B (en) | Method for growing uranium dioxide crystal by using borate fluxing agent | |
| CN113913920B (en) | AlGaAs single crystal preparation method and preparation device | |
| CN114182350B (en) | Method for preparing FePbSeTe monocrystal superconducting material by suspension smelting method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |