CN113643853B - Application of KF as raw material in preparation of 122-series iron-based superconductor and preparation method of 122-series iron-based superconductor - Google Patents
Application of KF as raw material in preparation of 122-series iron-based superconductor and preparation method of 122-series iron-based superconductor Download PDFInfo
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- CN113643853B CN113643853B CN202110934020.6A CN202110934020A CN113643853B CN 113643853 B CN113643853 B CN 113643853B CN 202110934020 A CN202110934020 A CN 202110934020A CN 113643853 B CN113643853 B CN 113643853B
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Abstract
The present invention belongs toIn the technical field of iron-based superconducting materials, in particular to application of KF as a raw material in preparing an iron-based superconductor and a preparation method of the iron-based superconductor. The invention provides Ae 1‑ x K x Fe 2 As 2 A method of preparing a superconductor comprising the steps of: in a protective atmosphere, according to the mass ratio of 1-x: x:2:2, performing ball milling on the Ae, the KF, the Fe and the As to obtain a mixture; calcining the mixture to obtain the Ae 1‑x K x Fe 2 As 2 A superconductor; the calcining temperature is 600-1000 ℃. The preparation method using KF to replace K as the raw material improves the safety and the practicability of the preparation and is beneficial to batch production.
Description
Technical Field
The invention belongs to the technical field of iron-based superconducting materials, and particularly relates to application of KF (KF) as a raw material in preparation of a 122-series iron-based superconductor and a preparation method of the 122-series superconductor.
Background
A novel Iron-based high-temperature superconductor (Iron-based layered superconductor LaO) was discovered in 2008 by Tokyo university of Japan 1-x F x FeAs(x＝0.05-0.12)with T c =26k.j.am.chem.sco.130,3296-3297,2008), the superconducting transition temperature of which reaches 26K, and the method has attracted extensive attention in the field of superconducting research. Iron-based superconductors are mainly classified into four types according to the difference of matrix structures: 1111 systems, 122 systems, 11 systems, and 111 systems. In the 122-series superconductor, ae 1-x K x Fe 2 As 2 (x is more than 0 and less than 1) has the characteristics of high critical current density, high upper critical field, small anisotropy, small dependence of critical current on a strong magnetic field and the like, has wide application prospect in the aspects of medium-low temperature and strong magnetic fields, and is expected to be widely applied in the fields of medical treatment, energy, traffic, national defense and the like.
At present, ae 1-x K x Fe 2 As 2 The superconductor is mainly synthesized by a solid-phase reaction method, and is obtained by utilizing the solid-phase reaction of the preparation raw materials during high-temperature heat treatment, but in the preparation raw materials of the superconductor, a K simple substance is very active and can be rapidly oxidized in the air and explode when meeting water, and spontaneous combustion can easily occur even in a humid environment. This makes the entire manufacturing process dangerous and spontaneous ignition or explosion may occur once the raw materials are exposed to air.
Disclosure of Invention
In view of the above, the present invention provides an Ae 1-x K x Fe 2 As 2 The preparation method of the superconductor, provided by the invention, has safety and practicability and is beneficial to batch production.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for preparing Ae by using KF as a raw material 1-x K x Fe 2 As 2 Application in superconductors.
Preferably, the purity of the KF is more than or equal to 99 percent.
The invention provides an Ae 1-x K x Fe 2 As 2 A method of preparing a superconductor comprising the steps of:
in a protective atmosphere, according to the mass ratio of 1-x: x:2:2, performing ball milling on the Ae, the KF, the Fe and the As to obtain a mixture;
calcining the mixture to obtain the Ae 1-x K x Fe 2 As 2 A superconductor;
the calcining temperature is 600-1000 ℃.
Preferably, ae is Ba, sr, ca or Eu.
Preferably, the calcination time is 10 to 100 hours.
Preferably, the rate of temperature increase to the calcination temperature is 1 to 50 ℃/min.
Preferably, the ball milling time is 2-10 h, and the rotation speed of the ball milling is 200-500 r/min.
Preferably, the purity of Ae, fe and As is independently more than or equal to 99%.
Preferably, the KF is dried before the ball milling;
the drying temperature is 150-200 ℃, and the drying time is 10-100 h.
Preferably, during the calcination, the mixture is compressed into a block, and the compression pressure is 10-200 MPa.
The invention provides an Ae 1-x K x Fe 2 As 2 A method of preparing a superconductor comprising the steps of: in a protective atmosphere, according to the mass ratio of 1-x: x:2:2, performing ball milling on the Ae, the KF, the Fe and the As to obtain a mixture; calcining the mixture to obtain the Ae 1-x K x Fe 2 As 2 A superconductor; the calcining temperature is 600-1000 ℃. The preparation method provided by the invention adopts a solid-phase reaction method to prepare the Ae 1-x K x Fe 2 As 2 The superconductor adopts KF to replace K as one of the raw materials, and the calcination temperature is 600-1000 ℃, thereby ensuring that F element is removed while the phase reaction is carried out to obtain Ae 1-x K x Fe 2 As 2 Superconductors with stable KF chemistry, easy storage, ability to reduce Ae 1-x K x Fe 2 As 2 The results of the examples show that the Ae prepared by the preparation method using KF as the raw material instead of K provided by the invention is beneficial to batch production 1-x K x Fe 2 As 2 The superconductor has a structure of 122 and a transition temperature of 37K.
Drawings
FIG. 1 shows Ba prepared in example 1 of the present invention 1-x K x Fe 2 As 2 XRD pattern of superconductor;
FIG. 2 shows Ba prepared in example 1 of the present invention 1-x K x Fe 2 As 2 M-T plot of superconductor.
Detailed Description
The invention provides a method for preparing Ae by using KF as a raw material 1-x K x Fe 2 As 2 Application in superconductors.
In the present invention, the purity of KF is preferably 99% or more, more preferably 99.5% or more.
The invention provides an Ae 1-x K x Fe 2 As 2 A method of preparing a superconductor comprising the steps of:
in a protective atmosphere, according to the mass ratio of 1-x: x:2:2, performing ball milling on the Ae, the KF, the Fe and the As to obtain a mixture;
calcining the mixture to obtain the Ae 1-x K x Fe 2 As 2 A superconductor;
the calcining temperature is 600-1000 ℃.
In the present invention, the starting materials are all commercially available products well known to those skilled in the art, unless otherwise specified.
In a protective atmosphere, the invention comprises the following components in a mass ratio of 1-x: x:2:2, carrying out ball milling on the Ae, the KF, the Fe and the As to obtain a mixture.
In the present invention, the Ae is preferably Ba, sr, ca or Eu, and in a specific embodiment of the present invention, the Ae is preferably Ba or Sr. In the present invention, the purity of Ae is preferably 99% or more, more preferably 99.5% or more.
In the present invention, the purity of KF is preferably 99% or more, more preferably 99.5% or more.
In the invention, before the ball milling, the KF is preferably dried; in the present invention, the drying temperature is preferably 150 to 200 ℃, more preferably 160 to 180 ℃, and the drying time is preferably 10 to 100 hours, more preferably 15 to 50 hours, most preferably 20 to 30 hours, more preferably 24 hours. The invention removes the moisture on the KF surface by drying.
In the present invention, the purity of Fe is preferably 99% or more, more preferably 99.5% or more.
In the present invention, the purity of As is preferably 99% or more, more preferably 99.5% or more.
In the present invention, 0 < x < 1, more preferably 0.4. Ltoreq. X.ltoreq.0.8, and in particular embodiments of the invention, x is preferably 0.4 or 0.5.
In a specific embodiment of the present invention, said Ae 1-x K x Fe 2 As 2 The superconductor is preferably Ba 0.6 K 0.4 Fe 2 As 2 Superconductor, sr 0.6 K 0.4 Fe 2 As 2 Superconductors or Ba 0.5 K 0.5 Fe 2 As 2 A superconductor.
In the present invention, the time for ball milling is preferably 2 to 10 hours, more preferably 4 to 8 hours; the rotation speed of the ball milling is preferably 150-550 r/min, more preferably 200-500 r/min, and most preferably 250-350 r/min; in the present invention, the ball milling preferably comprises dry milling or wet milling, more preferably dry milling; in the present invention, when wet milling is employed, the wet milling medium is preferably a lower alcohol, and the lower alcohol is preferably ethanol, and after wet milling, the wet milling medium is preferably removed cleanly. The invention has no special requirements on the specific implementation process of the ball milling; in the present invention, the ball milling is performed in a protective atmosphere, which is preferably a nitrogen atmosphere or an inert gas atmosphere, more preferably an inert gas atmosphere, and most preferably an argon atmosphere; in a specific embodiment of the invention, the ball milling is performed in a glove box.
In a particular embodiment of the invention, the ball milling preferably comprises the following steps: carrying out pre-ball milling on the Ae, the KF, the Fe and the As to obtain a premix; and carrying out secondary ball milling on the premix.
In the invention, the Ae, KF, fe and As are subjected to pre-ball milling to obtain the premix, the pre-ball milling time is preferably 1-1.5 h, and the rotation speed of the pre-ball milling is preferably 200-250 r/min.
In a specific embodiment of the present invention, the pre-ball milling is preferably performed in a ball mill, and after the pre-ball milling is completed, the ball milling tank is taken out from the ball mill, the ball milling tank is opened in a protective atmosphere, and the premix adhered to the inner wall of the ball milling tank is scraped off, and then the secondary ball milling is performed.
After the premix is obtained, the premix is subjected to secondary ball milling. In the present invention, the time of the secondary ball milling is preferably 1 to 9 hours, more preferably 3 to 7 hours, and the rotation speed of the secondary ball milling is preferably 500 to 550r/min.
In the specific embodiment of the invention, the secondary ball milling is preferably carried out in a ball mill, and the invention preferably continuously takes out the ball milling tank from the ball mill in the secondary ball milling process, opens the ball milling tank in a protective atmosphere, scrapes off the mixed material attached to the inner wall of the ball milling tank, and then continues to carry out the secondary ball milling; in the present invention, the interval between two times of taking out the ball milling jar is preferably 1 to 2 hours.
In the invention, ae, KF, fe and As are uniformly mixed by ball milling, and the raw materials are ball milled into powder, wherein the particle size of the mixture is preferably 0.1-50 μm, and more preferably 10-40 μm.
The invention improves the mixing uniformity of Ae, KF, fe and As by ball milling in stages.
After the mixture is obtained, the mixture is calcined to obtain the Ae 1-x K x Fe 2 As 2 A superconductor.
In the invention, the calcining temperature is 600-1000 ℃, preferably 650-950 ℃; the calcination time is preferably 10 to 100 hours, and more preferably 15 to 80 hours; in the present invention, the rate of temperature rise to the calcination temperature is preferably 1 to 50 ℃/min, more preferably 3 to 30 ℃/min, and most preferably 4 to 10 ℃/min. In a particular embodiment of the invention, the calcination is preferably carried out in a tube furnace; in the present invention, the calcination is performed in a protective atmosphere, which is preferably a nitrogen atmosphere or an inert gas atmosphere, more preferably an inert gas atmosphere, and most preferably an argon atmosphere.
In the invention, during calcination, the mixture is compressed into blocks, and the compression pressure is 10-200 MPa. In a specific embodiment of the present invention, when the mixture is calcined, the mixture is preferably placed in a cylindrical mold, the inner diameter of the cylindrical mold is preferably 12mm, and the cylindrical mold containing the mixture is pressurized to compress the mixture into a block; in the present invention, the pressure of the compression is preferably 10 to 200MPa, more preferably 20 to 150MPa; in the invention, the block is preferably put into a crucible, and then the crucible is packaged into an iron pipe and then calcined, wherein the crucible has an inner diameter of preferably 13mm and an outer diameter of preferably 16mm, the length of the iron pipe is preferably 18cm, the outer diameter of the iron pipe is preferably 22mm, and the inner diameter of preferably 18mm; when the mixture is filled into a cylindrical die, the process is preferably carried out in a protective atmosphere; when the crucible containing the sheet product is sealed in an iron tube, the sealing is preferably carried out in a protective atmosphere; in the present invention, the protective range of the protective atmosphere is preferably the same as that of the protective atmosphere described above.
The invention adopts a solid-phase reaction method to prepare the Ae 1-x K x Fe 2 As 2 The superconductor adopts KF to replace K as raw material, the KF has the characteristics of stable chemical property and easy storage, and can reduce Ae 1-x K x Fe 2 As 2 The superconductor is exposed in a humid environment to cause explosion danger in the preparation process, so that the preparation safety and practicability are improved, and the superconductor is favorable for batch production.
The invention removes the F element while carrying out solid-phase reaction by controlling the calcining temperature.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
2g of KF was weighed into a vacuum oven, and the vacuum oven was placed in a vacuum atmosphere (degree of vacuum 1X 10) -2 Pa) is carried out, the temperature is raised to 180 ℃, the temperature is kept for 24h, and the moisture in KF is removed;
putting the KF subjected to moisture removal into an argon atmosphere glove box, and mixing Ba blocks, KF powder, fe powder and As blocks according to a molar ratio of 0.6:0.4:2:2, weighing 4.5831g of Ba block, 1.2926g of KF powder, 6.2124g of Fe powder, 8.3346g of As block and putting the Ba block, the KF powder, the As block and the As block into a ball milling tank;
putting the ball milling tank into a planetary ball mill, running for 1h at the speed of 200r/min, then running for 1h at the speed of 500r/min, taking the ball milling tank back into the glove box, opening the ball milling tank, scraping off the blocks attached to the inner wall of the ball milling tank, and re-sealing the ball milling tank;
putting the ball milling tank into a planetary ball mill, operating at the speed of 500r/min for 2h, taking the ball milling tank back into the glove box, opening the ball milling tank, scraping off the blocks attached to the inner wall of the ball milling tank, and sealing the ball milling tank again; repeating the step for three times to obtain a mixture;
putting the mixture into a cylindrical die with the inner diameter of 12mm, applying a pressure of 200MPa to the mixture in the cylindrical die, compressing to obtain a block, putting the block into a crucible with the inner diameter of 13mm and the outer diameter of 16mm, putting the crucible into an iron pipe with the length of 18cm, the outer diameter of 22mm and the inner diameter of 18mm, plugging two ends of the iron pipe by a patch with the diameter of 18mm and the thickness of 3mm, and welding a gap between an iron sheet at two ends and the iron pipe by argon arc welding to finally enable the whole iron pipe to be in a closed state;
and (3) putting the sealed iron pipe into a tubular furnace, calcining in the protection of argon atmosphere, wherein the calcining temperature is 900 ℃, the heating rate of heating from room temperature to the calcining temperature is 10 ℃/min, and the calcining time is 35h. Sawing the iron pipe after the furnace is cooled to room temperature, taking out the bar material therein to obtain Ba 0.6 K 0.4 Fe 2 As 2 (Ba 122) superconductor.
XRD identification is carried out on the product of the example 1 by a Bruker D8 type X-ray diffractometer (XRD), the test range is 10 degrees to 2 degrees and 80 degrees, and the XRD detection result is shown in figure 1. As can be seen from FIG. 1, the product prepared in example 1 had a structure of "122", which is the same as that of the product prepared in the prior art using F as a starting material, but the characteristic peaks marked "#" and "#" in the product prepared in example 1 were the characteristic peaks of FeAs and BaF, respectively 2 The characteristic peak of (A) shows that the product prepared by the example also contains a certain amount of impure phase, but the content is very low, and the influence on the service performance of the superconductor is not great.
FIG. 2 is an Ae prepared in example 1 of the present invention 1-x K x Fe 2 As 2 The M-T diagram of the superconductor can be seen from FIG. 2, where the ZFC curve and the FC curve are separated at 37K, which shows that the product prepared in the example has superconducting property and the transition temperature is 37K, which is similar to that of the product prepared by using F as raw material in the prior artThe transition temperatures are close.
The results shown in fig. 1 and 2 show that the product obtained in example 1 is a Ba122 phase superconductor.
Example 2
2g of KF was weighed into a vacuum oven, and the vacuum oven was placed in a vacuum atmosphere (degree of vacuum 1X 10) -2 Pa) is carried out, the temperature is raised to 180 ℃, and the temperature is kept for 24h, and the moisture in KF is removed;
putting the KF subjected to moisture removal into an argon atmosphere glove box, and mixing Sr blocks, KF powder, fe powder and As blocks according to a molar ratio of 0.6:0.4:2:2, weighing 2.9248g of Sr block, 1.2926g of KF powder, 6.2124g of Fe powder, 8.3346g of As block and placing the Sr block, the KF powder, the As block and the As block into a ball milling tank;
putting the ball milling tank into a planetary ball mill, running for 1h at the speed of 200r/min, then running for 1h at the speed of 500r/min, taking the ball milling tank back into the glove box, opening the ball milling tank, scraping off the blocks attached to the inner wall of the ball milling tank, and re-sealing the ball milling tank;
putting the ball milling tank into a planetary ball mill, operating for 2 hours at the speed of 500r/min, taking the ball milling tank back into the glove box, opening the ball milling tank, scraping off the blocks attached to the inner wall of the ball milling tank, and resealing the ball milling tank; repeating the step for three times to obtain a mixture;
putting the mixture into a cylindrical die with the inner diameter of 12mm, applying a pressure of 200MPa to the mixture in the cylindrical die, compressing to obtain a block, putting the block into a crucible with the inner diameter of 13mm and the outer diameter of 16mm, putting the crucible into an iron pipe with the length of 18cm, the outer diameter of 22mm and the inner diameter of 18mm, plugging two ends of the iron pipe by a patch with the diameter of 18mm and the thickness of 3mm, and welding a gap between an iron sheet at two ends and the iron pipe by argon arc welding to finally enable the whole iron pipe to be in a closed state;
and (3) putting the sealed iron pipe into a tubular furnace, calcining under the protection of argon atmosphere, wherein the calcining temperature is 900 ℃, the heating rate of heating from room temperature to the calcining temperature is 20 ℃/min, and the calcining time is 35h. Sawing the iron pipe after the furnace is cooled to room temperature, taking out the bar material to obtain Sr 0.6 K 0.4 Fe 2 As 2 A superconductor.
The results for the product of example 2 were the same as those for the product of example 1.
Example 3
2g of KF was weighed into a vacuum oven, and the vacuum oven was placed in a vacuum atmosphere (degree of vacuum 1X 10) -2 Pa) is carried out, the temperature is raised to 180 ℃, and the temperature is kept for 24h, and the moisture in KF is removed;
putting the KF subjected to moisture removal into an argon atmosphere glove box, and mixing Ba blocks, KF powder, fe powder and As blocks according to a molar ratio of 0.6:0.4:2:2, weighing 4.5831g of Ba block, 1.2926g of KF powder, 6.2124g of Fe powder, 8.3346g of As block and putting the Ba block, the KF powder, the As block and the As block into a ball milling tank;
putting the ball milling tank into a planetary ball mill, running for 1h at the speed of 200r/min, then running for 1h at the speed of 500r/min, taking the ball milling tank back into the glove box, opening the ball milling tank, scraping off the blocks attached to the inner wall of the ball milling tank, and resealing the ball milling tank;
putting the ball milling tank into a planetary ball mill, operating for 2 hours at the speed of 500r/min, taking the ball milling tank back into the glove box, opening the ball milling tank, scraping off the blocks attached to the inner wall of the ball milling tank, and re-sealing the ball milling tank; repeating the step for three times to obtain a mixture;
putting the mixture into a cylindrical die with the inner diameter of 12mm, applying a pressure of 200MPa to the mixture in the cylindrical die, compressing to obtain a block material, then putting the block material into a crucible with the inner diameter of 13mm and the outer diameter of 16mm, putting the crucible into an iron pipe with the length of 18cm, the outer diameter of 22mm and the inner diameter of 18mm, blocking two ends of the iron pipe by adopting a patch with the diameter of 18mm and the thickness of 3mm, and welding gaps between iron sheets at two ends and the iron pipe by adopting argon arc welding to finally enable the whole iron pipe to be in a closed state;
and (3) putting the sealed iron pipe into a tubular furnace, calcining in the protection of argon atmosphere, wherein the calcining temperature is 900 ℃, the heating rate of heating from room temperature to the calcining temperature is 30 ℃/min, and the calcining time is 90h. Sawing the iron pipe after the furnace is cooled to room temperature, taking out the bar material to obtain Ba 0.6 K 0.4 Fe 2 As 2 A superconductor.
The results for the product of example 3 were the same as those for the product of example 1.
Example 4
2g of KF was weighed into a vacuum oven, and the vacuum oven was placed in a vacuum atmosphere (degree of vacuum 1X 10) -2 Pa) is carried out, the temperature is raised to 180 ℃, and the temperature is kept for 24h, and the moisture in KF is removed;
putting the KF subjected to moisture removal into an argon atmosphere glove box, and mixing Ba blocks, KF powder, fe powder and As blocks according to a molar ratio of 0.6:0.4:2:2, weighing 4.5831g of Ba block, 1.2926g of KF powder, 6.2124g of Fe powder, 8.3346g of As block and putting the Ba block, the KF powder, the As block and the As block into a ball milling tank;
putting the ball milling tank into a planetary ball mill, running for 1h at the speed of 200r/min, then running for 1h at the speed of 500r/min, taking the ball milling tank back into the glove box, opening the ball milling tank, scraping off the blocks attached to the inner wall of the ball milling tank, and re-sealing the ball milling tank;
putting the ball milling tank into a planetary ball mill, operating for 2 hours at the speed of 500r/min, taking the ball milling tank back into the glove box, opening the ball milling tank, scraping off the blocks attached to the inner wall of the ball milling tank, and resealing the ball milling tank; repeating the step for three times to obtain a mixture;
putting the mixture into a cylindrical die with the inner diameter of 12mm, applying a pressure of 200MPa to the mixture in the cylindrical die, compressing to obtain a block, putting the block into a crucible with the inner diameter of 13mm and the outer diameter of 16mm, putting the crucible into an iron pipe with the length of 18cm, the outer diameter of 22mm and the inner diameter of 18mm, plugging two ends of the iron pipe by a patch with the diameter of 18mm and the thickness of 3mm, and welding a gap between an iron sheet at two ends and the iron pipe by argon arc welding to finally enable the whole iron pipe to be in a closed state;
and (3) putting the sealed iron pipe into a tubular furnace, calcining in the protection of argon atmosphere, wherein the calcining temperature is 600 ℃, the heating rate of heating from room temperature to the calcining temperature is 5 ℃/min, and the calcining time is 35h. Sawing the iron pipe after the furnace is cooled to room temperature, taking out the bar material to obtain Ba 0.6 K 0.4 Fe 2 As 2 A superconductor.
The results for the product of example 4 were the same as those for the product of example 1.
Example 5
Weighing 2g of KF, putting the KF into a vacuum oven, heating the vacuum oven to 180 ℃ in a vacuum environment, keeping the temperature for 24h, and removing water in the KF;
putting the KF subjected to moisture removal into an argon atmosphere glove box, and mixing Ba blocks, KF powder, fe powder and As blocks according to a molar ratio of 0.5:0.5:2:2, 3.9265g of Ba block, 1.6611g of KF powder, 6.3869g of Fe powder, 3242 g of As block 8.5687g are weighed and put into a ball milling pot;
putting the ball milling tank into a planetary ball mill, running for 1h at the speed of 200r/min, then running for 1h at the speed of 500r/min, taking the ball milling tank back into the glove box, opening the ball milling tank, scraping off the blocks attached to the inner wall of the ball milling tank, and re-sealing the ball milling tank;
putting the ball milling tank into a planetary ball mill, operating for 2 hours at the speed of 500r/min, taking the ball milling tank back into the glove box, opening the ball milling tank, scraping off the blocks attached to the inner wall of the ball milling tank, and re-sealing the ball milling tank; repeating the step for three times to obtain a mixture;
putting the mixture into a cylindrical die with the inner diameter of 12mm, applying a pressure of 200MPa to the mixture in the cylindrical die, compressing to obtain a block, putting the block into a crucible with the inner diameter of 13mm and the outer diameter of 16mm, putting the crucible into an iron pipe with the length of 18cm, the outer diameter of 22mm and the inner diameter of 18mm, plugging two ends of the iron pipe by a patch with the diameter of 18mm and the thickness of 3mm, and welding a gap between an iron sheet at two ends and the iron pipe by argon arc welding to finally enable the whole iron pipe to be in a closed state;
and (3) putting the sealed iron pipe into a tubular furnace, calcining in the protection of argon atmosphere, wherein the calcining temperature is 900 ℃, the heating rate of heating from room temperature to the calcining temperature is 12 ℃/min, and the calcining time is 35h. Sawing the iron pipe after the furnace is cooled to room temperature, taking out the bar material to obtain Ba 0.6 K 0.4 Fe 2 As 2 A superconductor.
The results for the product of example 5 were the same as those for the product of example 1.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
- KF as a starting Material in the preparation of Ae 1-x K x Fe 2 As 2 Applications in superconductors;said Ae 1-x K x Fe 2 As 2 A method of preparing a superconductor comprising the steps of:in a protective atmosphere, according to the mass ratio of 1-x: x:2:2, mixing and ball-milling the Ae, the KF, the Fe and the As to obtain a mixture;calcining the mixture to obtain the Ae 1-x K x Fe 2 As 2 A superconductor;the calcining temperature is 600-1000 ℃.
- 2. The use according to claim 1, wherein the purity of KF is 99% or more.
- 3. Ae 1-x K x Fe 2 As 2 A method of preparing a superconductor, comprising the steps of:in a protective atmosphere, mixing and ball-milling Ae, KF, fe and As according to the mass ratio of 1-x: x:2:2 to obtain a mixture;calcining the mixture to obtain the Ae 1-x K x Fe 2 As 2 A superconductor;the calcining temperature is 600-1000 ℃.
- 4. The method according to claim 3, wherein Ae is Ba, sr, ca or Eu, and 0 < x < 1.
- 5. The method according to claim 3, wherein the calcination is carried out for a time of 10 to 100 hours.
- 6. The production method according to claim 3, wherein the rate of temperature rise to the calcination temperature is 1 to 50 ℃/min.
- 7. The preparation method of claim 3, wherein the ball milling time is 2-10 h, and the rotation speed of the ball milling is 200-500 r/min.
- 8. The method according to claim 3, wherein the purity of Ae, fe and As is 99% or more.
- 9. The method according to claim 3, wherein the KF is dried before the ball milling;the drying temperature is 150-200 ℃, and the drying time is 10-100 h.
- 10. The preparation method according to claim 3, wherein the mixture is compressed into a block at a pressure of 10 to 200MPa during the calcination.
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| CN202110934020.6A CN113643853B (en) | 2021-08-13 | 2021-08-13 | Application of KF as raw material in preparation of 122-series iron-based superconductor and preparation method of 122-series iron-based superconductor |
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| WO1990011260A1 (en) * | 1989-03-25 | 1990-10-04 | Hoechst Aktiengesellschaft | Dense superconductive bodies with preferred orientation |
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| CN108172334A (en) * | 2017-11-16 | 2018-06-15 | 东南大学 | It is a kind of to prepare Ba1-xKxBiO3The method of superconducting wire |
| CN108878051A (en) * | 2018-05-23 | 2018-11-23 | 中国科学院电工研究所 | A kind of AeAFe4As4Iron-based superconducting wire or band preparation method |
| CN111968788A (en) * | 2020-08-17 | 2020-11-20 | 福建师范大学 | Preparation method of high-performance iron-based superconducting precursor powder and superconducting tape |
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| WO1990011260A1 (en) * | 1989-03-25 | 1990-10-04 | Hoechst Aktiengesellschaft | Dense superconductive bodies with preferred orientation |
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