CN116487113A - Preparation method of iron-based superconducting material - Google Patents
Preparation method of iron-based superconducting material Download PDFInfo
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- CN116487113A CN116487113A CN202310672919.4A CN202310672919A CN116487113A CN 116487113 A CN116487113 A CN 116487113A CN 202310672919 A CN202310672919 A CN 202310672919A CN 116487113 A CN116487113 A CN 116487113A
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 36
- 239000000463 material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 52
- 239000000126 substance Substances 0.000 claims abstract description 25
- 238000005245 sintering Methods 0.000 claims abstract description 24
- 239000012298 atmosphere Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 21
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 15
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 13
- 238000000137 annealing Methods 0.000 claims abstract description 12
- 238000003825 pressing Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 6
- 150000001342 alkaline earth metals Chemical group 0.000 claims abstract description 6
- 238000012545 processing Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 14
- 229910052785 arsenic Inorganic materials 0.000 claims description 9
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 8
- 229910052788 barium Inorganic materials 0.000 claims description 7
- 238000011049 filling Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 229910052792 caesium Inorganic materials 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 11
- 238000005204 segregation Methods 0.000 abstract description 10
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 239000013589 supplement Substances 0.000 abstract description 2
- 239000012300 argon atmosphere Substances 0.000 description 11
- 239000000523 sample Substances 0.000 description 11
- 238000012360 testing method Methods 0.000 description 10
- 239000012299 nitrogen atmosphere Substances 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 6
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- KWLSQQRRSAWBOQ-UHFFFAOYSA-N dipotassioarsanylpotassium Chemical compound [K][As]([K])[K] KWLSQQRRSAWBOQ-UHFFFAOYSA-N 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 239000012467 final product Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- VETKVGYBAMGARK-UHFFFAOYSA-N arsanylidyneiron Chemical compound [As]#[Fe] VETKVGYBAMGARK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- FDKAYGUKROYPRO-UHFFFAOYSA-N iron arsenide Chemical compound [Fe].[As]=[Fe] FDKAYGUKROYPRO-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001683 neutron diffraction Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B12/00—Superconductive or hyperconductive conductors, cables, or transmission lines
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E40/00—Technologies for an efficient electrical power generation, transmission or distribution
- Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a preparation method of an iron-based superconducting material, which comprises the following steps: according to the chemical formula Ae 1‑x A x+a Fe 2‑b As 2+c Mixing uniformly to obtain unreacted raw powder, wherein Ae is alkaline earth metal element, A is alkali metal element, x is more than or equal to 0.15 and less than or equal to 0.8,0<c<a is less than or equal to 0.4x, b is less than or equal to 0 and less than or equal to 0.1; pressing and forming the raw powder in an inert atmosphere; sintering the raw powder at high temperature in an inert atmosphere or a vacuum environment to prepare a block; processing the sintered block material into powder again, and placing the powder into a container; and (5) carrying out annealing treatment on the processed powder. The invention can supplement the alkali metal element and As element loss in the high-temperature sintering process, eliminate the impurity phase and element segregation, and after the first sintering, the superconducting bulk contains superconducting main phase and impurity phase, wherein the impurity phase exists between main phase grains; the second annealing adopts inert atmosphere or low-pressure inert atmosphere, which is favorable for volatilizing partial hetero-phase, thereby further reducing the arsenide hetero-phase.
Description
Technical Field
The invention relates to a preparation method of an iron-based superconducting material, which is a method for preparing the iron-based superconducting material with high purity and high uniformity, and belongs to the technical field of material preparation.
Background
The iron-based superconducting material has excellent high-field properties. However, since the iron-based superconducting material contains volatile alkali metal elements and arsenic elements, element loss is liable to occur during high-temperature sintering. The existing internationally widely adopted nominal components have poor element content matching, so that the problems of element segregation, serious deviation from target chemical components, high impurity phase content and the like exist in the final product, and the improvement of the performance of the iron-based superconducting material is restricted. Therefore, development of a novel preparation process of the iron-based superconducting material is needed, element segregation and impurity phase generation are inhibited, and purity and uniformity of the iron-based superconducting material are improved.
Conventional iron-based superconducting material fabrication processes typically employ nominal compositions with an excess of K and a non-excess of As, and no adjustments to the iron content are made (e.g., reference iScience 25,103992,2022). The final product prepared according to the nominal composition is easy to generate element segregation, contains a large amount of residual second phases such as iron-arsenic mixed phases, iron particles, barium arsenide, potassium arsenide and the like, and severely restricts the performance improvement. Furthermore, conventional processes typically employ only one sintering process (e.g., reference Supercond. Sci. Technology. 33,065001, 2020), with impurities remaining in the sample. And the hot isostatic pressing process is partially adopted for secondary sintering, the pressure is up to 190MPa, the final product is a block (for example, reference Scientific Reports 11,3143,2021), the removal of the impurity phases is not facilitated under the high pressure environment, the process is seriously dependent on expensive high-pressure equipment, the preparation cost is high, and the large-scale production is not facilitated.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides a preparation method of an iron-based superconducting material.
The invention adopts the following technical scheme:
a method for preparing an iron-based superconducting material, the method comprising the following process steps:
(1) The raw materials are subjected to the following chemical formula Ae in an inert atmosphere 1-x A x+a Fe 2-b As 2+c Mixing uniformly to obtain unreacted raw powder, wherein Ae is alkaline earth metal element, A is alkali metal, x is more than or equal to 0.15 and less than or equal to 0.8,0<c<a≤0.4x，0≤b≤0.1；
(2) Pressing the raw powder in the step (1) in an inert atmosphere to form;
(3) At the position ofPressure of 10 -3 Sintering the pressed raw powder in the step (2) at a high temperature in an inert atmosphere or a vacuum environment with the pressure of Pa-0.1MPa to prepare a block;
(4) Re-processing the sintered block into powder in inert atmosphere, placing the powder into a container, and filling the powder with a density of 0.1g/cm 3 -3 g/cm 3 ；
(5) At a pressure of 10 -3 Annealing the powder in step (4) in an inert atmosphere or vacuum atmosphere of Pa-0.1MPa or in a flowing inert atmosphere.
Further, in the step (1), 0.15.ltoreq.x.ltoreq.0.8, for example, x is 0.15, 0.17, 0.19, 0.21, 0.23, 0.25, 0.27, 0.29, 0.3, 0.32, 0.34, 0.36, 0.38, 0.40, 0.42, 0.44, 0.46, 0.48, 0.5, 0.52, 0.54, 0.56, 0.58, 0.6, 0.62, 0.64, 0.66, 0.68, 0.7, 0.72, 0.74, 0.76, 0.78 or 0.8. B.ltoreq.b.ltoreq.0.1, e.g.b is 0, 0.01, 0.02, 0.03, 0.04, 0.05, 0.06, 0.07, 0.08, 0.09 or 0.1.
Further, ae in the step (1) is Ca, sr or Ba, and a is Na, K, rb or Cs.
Further, the raw materials mentioned in the step (1) are respectively: an alkaline earth metal simple substance or compound, an alkali metal simple substance or compound, an iron simple substance or compound, and an arsenic simple substance.
Further, b is more than or equal to 0.001 and less than or equal to 0.1 in the step (1).
Further, the pressure used for pressing in the step (2) is 0.1MPa-1GPa, for example, the pressure used for pressing is 0.1MPa, 10MPa, 30MPa, 500MPa or 1GPa, and the shape of the molded sample comprises a cylinder, a cuboid or a sphere.
Further, the sintering procedure in the step (3) is as follows: heating to 400-700 ℃ (e.g., 400 ℃, 450 ℃, 500 ℃, 550 ℃, 1150 ℃ or 1200 ℃) at a rate of 100-1000 ℃/h (e.g., at a rate of 100 ℃/h, 200 ℃/h, 300 ℃/h, 400 ℃/h, 500 ℃/h, 600 ℃/h, 700 ℃/h, 800 ℃/h, 900 ℃/h or 1000 ℃/h) and incubating for 1-12 hours, and heating to 800-1200 ℃ (e.g., 800 ℃, 850 ℃, 900 ℃, 950 ℃, 1000 ℃, 1050 ℃, 1100 ℃, 1150 ℃ or 1200 ℃) at a rate of 100-600 ℃/h (e.g., at a rate of 100 ℃/h, 150 ℃/h, 200 ℃/h, 250 ℃/h, 300 ℃/h, 350 ℃/h, 400 ℃/h, 450 ℃/h, 500 ℃/h, 550 ℃/h or 600 ℃/h) and incubating for 1-100 hours.
Further, in the step (4), the powder packing density was 0.1g/cm 3 、0.5g/cm 3 、1g/cm 3 、1.5g/cm 3 、2g/cm 3 、2.5g/cm 3 Or 3g/cm 3 。
Further, the annealing temperature in the step (5) is 40-400 ℃ and the annealing time is 0.01-24 hours. For example, the annealing temperature is 40 ℃, 90 ℃, 100 ℃, 150 ℃, 200 ℃, 250 ℃, 300 ℃, 350 ℃, or 400 ℃, and the annealing time is 0.01 hour, 0.5 hour, 1 hour, 2 hours, 3 hours, 4 hours, 5 hours, 6 hours, 7 hours, 8 hours, 9 hours, 10 hours, 11 hours, 12 hours, 13 hours, 14 hours, 20 hours, or 24 hours.
The invention has the beneficial effects that:
(1) The optimized chemical components are adopted: ae 1-x A x+a Fe 2-b As 2+c Defining the relationship between an alkali metal excess value of a and an As element excess value of c: 0<c<a is less than or equal to 0.4x. The nominal composition can supplement the loss of alkali metal elements and As elements in the high-temperature sintering process. The upper limit a of the content of excessive alkali metal is less than or equal to 0.4x, so that excessive alkali metal impurity phase or alkali metal arsenide impurity phase residue is prevented. Since alkali metal A is more volatile and lost during high-temperature sintering, the content c of the excessive As element is set<and a, enabling excessive alkali metal A element to react with excessive As element, reducing the consumption of the As element in a main phase, preventing Fe element segregation, and inhibiting the generation of mixed phases such As barium arsenide and the like. The content of iron element is moderately reduced, and the reduction value is more than or equal to 0.001 and less than or equal to 0.1, so as to achieve the aim of eliminating excessive iron.
(2) After the first sintering, the superconducting bulk contains a superconducting main phase and a hetero-phase, wherein the hetero-phase exists between main phase grains. Crushing the block after the first sintering into powder, and exposing alkali metal, alkaline earth metal or arsenide impurity phases among superconducting grains; the second annealing adopts flowing inert atmosphere or low-pressure inert atmosphere, which is favorable for volatilizing partial hetero-phase, thereby further reducing the arsenide hetero-phase.
(3) The method only sinters in vacuum or normal pressure, and does not need high-pressure equipment to assist, thereby greatly reducing the preparation cost.
Drawings
FIG. 1 shows an X-ray diffraction pattern and a fitting result of an iron-based superconducting material prepared by the method of the invention, wherein the difference between the X-ray diffraction pattern and the fitting result is small, and the iron-based superconducting material does not contain a hetero-phase peak, so that the superconducting material has high purity.
Detailed Description
The invention will now be described in detail with reference to the accompanying drawings and specific embodiments thereof. The following examples are intended to be illustrative only and the scope of the invention is to be construed as including the full breadth of the claims and by the recitation of the following examples, the full breadth of the claims can be fully set forth by those skilled in the art.
Example 1:
(1) Barium arsenide, potassium arsenide, iron arsenide and arsenic simple substance are processed according to chemical formula Ba in argon atmosphere 0.6 K 0.5 Fe 1.95 As 2.03 Proportioning and uniformly mixing to obtain unreacted raw powder;
(2) Pressing the raw powder in the step (1) into a rectangular parallelepiped shape under an argon atmosphere by using a pressure of 30 MPa;
(3) Sintering the green powder pressed in the step (2) into a block material at a high temperature in a vacuum atmosphere with the pressure of 1Pa, wherein the sintering procedure is as follows: heating to 500 ℃ at the speed of 200 ℃/h and preserving heat for 10 hours, and heating to 900 ℃ at the speed of 200 ℃/h and preserving heat for 50 hours;
(4) In an argon atmosphere, the sintered block is reprocessed into powder and placed in a container, and the powder filling density is 1g/cm 3 ；
(5) The powder in step (4) was annealed at 40℃for 24 hours in a vacuum atmosphere at a pressure of 1 Pa.
The obtained iron-based superconducting material is subjected to X-ray diffraction test, and is found to contain no impurity phase, and the purity is as high as 99.5 percent, as shown in figure 1; test hair by scanning electronic probeAt present, the elements in the sample are uniformly distributed, no segregation phenomenon exists, and the actual chemical component is measured to be Ba 0.593 K 0.407 Fe 2.003 As 2.013 。
Example 2:
(1) The simple substances of strontium, sodium, iron and arsenic are treated in nitrogen atmosphere according to chemical formula Sr 0.85 Na 0.21 Fe 1.999 As 2.04 Proportioning and uniformly mixing to obtain unreacted raw powder;
(2) Pressing the raw powder in the step (1) into a cylinder shape by using a pressure of 0.1MPa in a nitrogen atmosphere;
(3) At a pressure of 10 -3 Sintering the raw powder pressed in the step (2) into a block at a high temperature under the vacuum of MPa, wherein the sintering process is as follows: heating to 400 ℃ at the speed of 100 ℃/h and preserving heat for 12 hours, and heating to 800 ℃ at the speed of 100 ℃/h and preserving heat for 100 hours;
(4) In a nitrogen atmosphere, the sintered block is reprocessed into powder and placed in a container, and the powder filling density is 0.1g/cm 3 ；
(5) The powder in step (4) was annealed at 100 ℃ for 10 hours under flowing argon.
The obtained iron-based superconducting material is subjected to synchronous X-ray diffraction test, the purity of superconducting phase is up to 99.8%, the scanning electron probe test shows that segregation phenomenon does not exist in the sample, and the actual chemical component is Sr 0.853 Na 0.147 Fe 2.021 As 2.013 。
Example 3:
(1) Strontium, potassium arsenide, iron and arsenic are mixed according to chemical formula Sr in argon atmosphere 0.5 K 0.7 Fe 1.9 As 2.12 Proportioning and uniformly mixing to obtain unreacted raw powder;
(2) Pressing the raw powder in the step (1) into a cylinder shape by using 500MPa pressure in an argon atmosphere;
(3) Sintering the green powder pressed in the step (2) into a block material at a high temperature in a nitrogen atmosphere with the pressure of 0.1MPa, wherein the sintering procedure is as follows: heating to 600 ℃ at the speed of 500 ℃/h and preserving heat for 8 hours, and heating to 1000 ℃ at the speed of 300 ℃/h and preserving heat for 24 hours;
(4) In an argon atmosphere, the sintered block is reprocessed into powder and placed in a container, and the powder filling density is 2g/cm 3 ；
(5) The powder in step (4) was annealed at 300℃for 1 hour in a nitrogen atmosphere of 0.1 MPa.
The obtained iron-based superconducting material is subjected to X-ray diffraction test, the purity of the superconducting phase is up to 99.3%, the scanning electron probe test shows that segregation phenomenon does not exist in a sample, and the actual chemical component is measured to be Sr 0.503 K 0.497 Fe 1.995 As 2.003 。
Example 4:
(1) The simple substances of barium, rubidium, iron and arsenic are processed according to the chemical formula Ba in nitrogen atmosphere 0.2 Rb 0.9 Fe 1.99 As 2.08 Proportioning and uniformly mixing to obtain unreacted raw powder;
(2) Pressing the raw powder in the step (1) into spheres by using a pressure of 1GPa in a nitrogen atmosphere;
(3) Sintering the green powder pressed in the step (2) into a block material at a high temperature in an argon atmosphere with the pressure of 0.05MPa, wherein the sintering procedure is as follows: heating to 700 ℃ at a speed of 1000 ℃/h and preserving heat for 1 hour, and heating to 1200 ℃ at a speed of 600 ℃/h and preserving heat for 1 hour;
(4) In a nitrogen atmosphere, the sintered block is reprocessed into powder and placed in a container, and the powder filling density is 3g/cm 3 ；
(5) The powder in step (4) was annealed at 400℃for 0.01 hours in an argon atmosphere of 0.1 MPa.
The obtained iron-based superconducting material is subjected to X-ray diffraction test, the purity of the superconducting phase is up to 99.5%, the scanning electron probe test shows that elements in a sample are uniformly distributed and have no segregation phenomenon, and the actual chemical component is Ba 0.211 Rb 0.789 Fe 2.013 As 2.016 。
Example 5:
(1) Barium arsenide, potassium arsenide, iron and arsenic are mixed in argon atmosphereChemical formula Ba 0.7 K 0.4 Fe 1.999 As 2.01 Proportioning and uniformly mixing to obtain unreacted raw powder;
(2) Pressing the raw powder in the step (1) into a cylinder shape by using 10MPa pressure in an argon atmosphere;
(3) Sintering the green powder pressed in the step (2) into a block material at a high temperature in an argon atmosphere with the pressure of 0.1MPa, wherein the sintering procedure is as follows: heating to 500 ℃ at the speed of 700 ℃/h and preserving heat for 9 hours, and heating to 880 ℃ at the speed of 400 ℃/h and preserving heat for 48 hours;
(4) In an argon atmosphere, the sintered block is reprocessed into powder and placed in a container, and the powder filling density is 0.5g/cm 3 ；
(5) At 10 -2 Annealing the powder in step (4) at 120℃for 0.03 hours in a vacuum atmosphere of Pa.
The obtained iron-based superconducting material is subjected to neutron diffraction test, the purity of superconducting phase is up to 99.9%, the scanning electron probe test shows that elements in a sample are uniformly distributed and segregation phenomenon does not exist, and the actual chemical component is measured to be Ba 0.691 K 0.309 Fe 1.993 As 2.011 。
The present invention is not described in detail in part as being well known to those skilled in the art. The above examples are merely illustrative of preferred embodiments of the invention, which are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Various modifications and improvements of the technical scheme of the present invention will fall within the protection scope of the present invention as defined in the claims without departing from the design spirit of the present invention.
Claims (7)
1. The preparation method of the iron-based superconducting material is characterized by comprising the following process steps of:
(1) The raw materials are subjected to the following chemical formula Ae in an inert atmosphere 1-x A x+a Fe 2-b As 2+c Proportioning and mixing uniformly to obtain unreacted raw powder, whereinAe is alkaline earth metal element, A is alkali metal element, x is more than or equal to 0.15 and less than or equal to 0.8,0<c<a≤0.4x，0≤b≤0.1；
(2) Pressing the raw powder in the step (1) in an inert atmosphere to form;
(3) At a pressure of 10 -3 Sintering the pressed raw powder in the step (2) at a high temperature in an inert atmosphere or a vacuum environment with the pressure of Pa-0.1MPa to prepare a block;
(4) Re-processing the sintered block into powder in inert atmosphere, placing the powder into a container, and filling the powder with a density of 0.1g/cm 3 -3g/cm 3 ；
(5) And (3) annealing the powder in the step (4) under an inert atmosphere or a vacuum environment with the pressure of 10 < -3 > Pa to 0.1MPa or in a flowing inert atmosphere.
2. The method for producing an iron-based superconducting material according to claim 1, wherein: and (2) in the step (1), ae is Ca, sr or Ba, and A is Na, K, rb or Cs.
3. The method for producing an iron-based superconducting material according to claim 1, wherein: the raw materials mentioned in the step (1) are respectively: an alkaline earth metal simple substance or compound, an alkali metal simple substance or compound, an iron simple substance or compound, and an arsenic simple substance.
4. The method for producing an iron-based superconducting material according to claim 1, wherein: b is more than or equal to 0.001 and less than or equal to 0.1 in the step (1).
5. The method for producing an iron-based superconducting material according to claim 1, wherein: the pressure used for pressing in the step (2) is 0.1MPa-1GPa, and the formed sample shape comprises a cylinder shape, a cuboid shape or a sphere shape.
6. The method for producing an iron-based superconducting material according to claim 1, wherein: the sintering procedure in the step (3) is as follows: heating to 400-700 ℃ at the rate of 100-1000 ℃ per hour, preserving heat for 1-12 hours, heating to 800-1200 ℃ at the rate of 100-600 ℃ per hour, and preserving heat for 1-100 hours.
7. The method for producing an iron-based superconducting material according to claim 1, wherein: the annealing temperature in the step (5) is 40 ℃ to 400 ℃ and the annealing time is 0.01 hour to 24 hours.
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