CN105405531A - Preparation method of novel superconducting material - Google Patents

Preparation method of novel superconducting material Download PDF

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Publication number
CN105405531A
CN105405531A CN201510949659.6A CN201510949659A CN105405531A CN 105405531 A CN105405531 A CN 105405531A CN 201510949659 A CN201510949659 A CN 201510949659A CN 105405531 A CN105405531 A CN 105405531A
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preparation
ball
sinter
atmosphere
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朱正良
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CHANGSHU ORIENT SPECIAL METALLIC MATERIAL FACTORY
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CHANGSHU ORIENT SPECIAL METALLIC MATERIAL FACTORY
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B12/00Superconductive or hyperconductive conductors, cables, or transmission lines
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00Apparatus or processes specially adapted for manufacturing conductors or cables
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E40/00Technologies for an efficient electrical power generation, transmission or distribution
    • Y02E40/60Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Superconductors And Manufacturing Methods Therefor (AREA)

Abstract

The invention discloses a preparation method of a novel superconducting material. The preparation method comprises the following steps: 100) refining: independently weighing and mixing each material according to a ratio, putting the mixture into a wear-proof ball-milling jar, putting the ball-milling jar into a high-temperature energy ball-milling machine, and carrying out ball milling for 0.5-5 hours at the temperature range of 60-150DEG C under the protection of argon protection atmosphere; 200) briquetting: then, under the argon atmosphere, pouring mixed powder subjected to the ball milling into a mould, and pressing the mixed powder into bulks; and 300) sintering: finally, packaging bulk bodies in a quartz tube, vacuumizing, and sintering under the argon protection atmosphere. The preparation method of the superconducting material can improve the phase purity and the crystal connection property of an iron-based superconductor.

Description

A kind of preparation method of new superconduction material
Technical field
The present invention relates to field of material preparation, particularly relate to a kind of preparation method of new superconduction material.
Background technology
Superconduction is one of phenomenon the most marvellous in physical world.General superconducting alloy enters superconducting state reducing to zero close to resistance during absolute zero, and high-temperature superconductor then refers to that material is at certain relatively high critical temperature resistor bust to zero, and it has diverse Physical Mechanism and more wide application prospect.1986, physicist found copper oxide high temperature superconductor, and this works in next year and just obtains Nobel Prize in physics.Since then, scientists just never stopped the exploration of new high temperature superconducting materia, and constantly pursuing more while high-critical temperature, physicists are making great efforts announcement mechanism wherein always.At present, Dou You research institution of nearly all developed country is engaged in the research of high-temperature superconductor aspect in the world.On the one hand, the exploration of high-temperature superconductor mechanism is attract to the concern of numerous physicist; On the other hand, due to the energy and other specific demands, industrial quarters is placed high hopes to superconductor technology, but because the critical temperature of general superconducting alloy is close to absolute zero, the reason of refrigeration causes applying facing lots of obstruction, and high-temperature superconductor is then one of following outlet of expecting of everybody.
Compared with traditional superconductor, iron-based superconductor has higher transition temperature, larger upper critical field, critical current to advantages such as the less dependences of high-intensity magnetic field.Compare with high temperature YBCO coating superconducting material and Bi system superconducting line strips with traditional cryogenic superconductor Nb3Sn, the serviceability temperature that iron-based superconductor tool is higher; Under this temperature range and highfield condition, its superconductivity has has met or exceeded the Conventional cryogenic superconductor now used.Compared with oxide high-temperature superconductor, the crystal structure of iron-based superconductor is simpler, coherence length is large, anisotropy is little, preparation technology is simple, is therefore subject to international extensive concern.
But existing iron-based superconducting material also exists, and critical current density is low, crystal grain connectivity difference and the problem such as phase purity is low, therefore greatly limit its practicalization.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of preparation method of new superconduction material, can improve phase purity and the crystal switching performance of iron-based superconductor.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: the preparation method providing a kind of new superconduction material, comprises the following steps:
100) refinement: weighed in proportion respectively by each raw material and mix, putting into wear-resistant ball grinding jar, then puts into high temperature energy spheroidal graphite machine by ball grinder, under the protection of argon atmosphere, under DEG C scope of temperature 60 C ~ 150, carry out ball milling 0.5 ~ 5 hour;
200) briquetting: then under the atmosphere of argon gas, pours into the mixed-powder after ball milling in mould and is pressed into bulk;
300) sinter: finally block is encapsulated in quartz ampoule and vacuumizes, under argon atmosphere, sinter.
In a preferred embodiment of the present invention, described wear-resistant ball grinding jar is that mould steel is made.
In a preferred embodiment of the present invention, described raw material comprises iron, arsenic, selenium, potassium and rare earth element.
In a preferred embodiment of the present invention, described step 300) in, pressure limit is sinter under 0.01 ~ 0.05MPa, with the heating rate of 8 DEG C/min, after rising to 700 DEG C ~ 950 DEG C, sinters 10 ~ 12 hours.
The invention has the beneficial effects as follows: the preparation method of new superconduction material of the present invention, phase purity and the crystal switching performance of iron-based superconductor can be improved.
Embodiment
Below preferred embodiment of the present invention is described in detail, can be easier to make advantages and features of the invention be readily appreciated by one skilled in the art, thus more explicit defining is made to protection scope of the present invention.
The preparation method of new superconduction material of the present invention, comprises the following steps:
100) refinement: weighed in proportion respectively by each raw material and mix, putting into wear-resistant ball grinding jar, then puts into high temperature energy spheroidal graphite machine by ball grinder, under the protection of argon atmosphere, under DEG C scope of temperature 60 C ~ 150, carry out ball milling 0.5 ~ 5 hour;
200) briquetting: then under the atmosphere of argon gas, pours into the mixed-powder after ball milling in mould and is pressed into bulk;
300) sinter: finally block is encapsulated in quartz ampoule and vacuumizes, under argon atmosphere, sinter.
Embodiment one
By iron powder, arsenic powder, selenium, potassium and rare earth element respectively in proportion 1:1:0.3:0.1:0.05 weigh and mix, put into wear-resistant ball grinding jar, then ball grinder is put into high temperature energy spheroidal graphite machine, under the protection of high purity argon protective atmosphere, at temperature 80 DEG C, carry out ball milling 1 hour; Then, under the atmosphere of argon gas, the mixed-powder after ball milling is poured in mould and is pressed into bulk; Finally be encapsulated in quartz ampoule by block and vacuumize, under argon atmosphere, pressure is sinter under 0.02MPa, with the heating rate of 8 DEG C/min, after rising to 800 DEG C, sinters 10 hours.
Embodiment two
By iron powder, arsenic powder, selenium, potassium and rare earth element respectively in proportion 1:1.2:0.2:0.2:0.03 weigh and mix, put into wear-resistant ball grinding jar, then ball grinder is put into high temperature energy spheroidal graphite machine, under the protection of high purity argon protective atmosphere, at temperature 80 DEG C, carry out ball milling 1 hour; Then, under the atmosphere of argon gas, the mixed-powder after ball milling is poured in mould and is pressed into bulk; Finally be encapsulated in quartz ampoule by block and vacuumize, under argon atmosphere, pressure is sinter under 0.03MPa, with the heating rate of 8 DEG C/min, after rising to 900 DEG C, sinters 10 hours.
Embodiment three
By iron powder, arsenic powder, selenium, potassium and rare earth element respectively in proportion 1:0.8:0.1:0.3:0.02 weigh and mix, put into wear-resistant ball grinding jar, then ball grinder is put into high temperature energy spheroidal graphite machine, under the protection of high purity argon protective atmosphere, at temperature 80 DEG C, carry out ball milling 1 hour; Then, under the atmosphere of argon gas, the mixed-powder after ball milling is poured in mould and is pressed into bulk; Finally be encapsulated in quartz ampoule by block and vacuumize, under argon atmosphere, pressure is sinter under 0.03MPa, with the heating rate of 8 DEG C/min, after rising to 750 DEG C, sinters 12 hours.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.

Claims (4)

1. a preparation method for new superconduction material, is characterized in that, comprises the following steps:
100) refinement: weighed in proportion respectively by each raw material and mix, putting into wear-resistant ball grinding jar, then puts into high temperature energy spheroidal graphite machine by ball grinder, under the protection of argon atmosphere, under DEG C scope of temperature 60 C ~ 150, carry out ball milling 0.5 ~ 5 hour;
200) briquetting: then under the atmosphere of argon gas, pours into the mixed-powder after ball milling in mould and is pressed into bulk;
300) sinter: finally block is encapsulated in quartz ampoule and vacuumizes, under argon atmosphere, sinter.
2. the preparation method of new superconduction material according to claim 1, is characterized in that, described wear-resistant ball grinding jar is that mould steel is made.
3. the preparation method of new superconduction material according to claim 1, is characterized in that, described raw material comprises iron, arsenic, selenium, potassium and rare earth element.
4. the preparation method of new superconduction material according to claim 1, is characterized in that, described step 300) in, pressure limit is sinter under 0.01 ~ 0.05MPa, with the heating rate of 8 DEG C/min, after rising to 700 DEG C ~ 950 DEG C, sinter 10 ~ 12 hours.
CN201510949659.6A 2015-12-18 2015-12-18 Preparation method of novel superconducting material Pending CN105405531A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106521291A (en) * 2016-11-04 2017-03-22 金福兴 Composite superconductive nanometer block material and preparation method thereof
CN108083799A (en) * 2017-12-21 2018-05-29 叶芳 A kind of new energy superconductor and preparation method thereof
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
CN109244229A (en) * 2018-09-13 2019-01-18 安徽建筑大学 A kind of microelectronics superconductor and preparation method thereof
CN110931160A (en) * 2019-10-23 2020-03-27 中国科学院电工研究所 Iron-based superconducting precursor powder, preparation method thereof and iron-based superconducting wire strip

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CN101550009A (en) * 2009-04-30 2009-10-07 中国科学院上海硅酸盐研究所 Preparation method of iron-base high-temperature superconductor
WO2010007929A1 (en) * 2008-07-16 2010-01-21 独立行政法人科学技術振興機構 Layered compound, superconductor and method for producing same
CN102142302A (en) * 2011-04-25 2011-08-03 中国科学院电工研究所 FeSe-based ferrous superconducting material and preparation method thereof
CN102412017A (en) * 2011-10-19 2012-04-11 中国科学院电工研究所 Method for improving upper critical field and critical current density of iron-based superconductor
CN103943280A (en) * 2014-04-30 2014-07-23 中国科学院电工研究所 Manufacturing method of REFeAsO1-xFx iron-based superconducting wire or strip
CN105016730A (en) * 2015-07-09 2015-11-04 成都点石创想科技有限公司 Superconducting material preparation method with simple process and simple operation

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010007929A1 (en) * 2008-07-16 2010-01-21 独立行政法人科学技術振興機構 Layered compound, superconductor and method for producing same
CN101550009A (en) * 2009-04-30 2009-10-07 中国科学院上海硅酸盐研究所 Preparation method of iron-base high-temperature superconductor
CN102142302A (en) * 2011-04-25 2011-08-03 中国科学院电工研究所 FeSe-based ferrous superconducting material and preparation method thereof
CN102412017A (en) * 2011-10-19 2012-04-11 中国科学院电工研究所 Method for improving upper critical field and critical current density of iron-based superconductor
CN103943280A (en) * 2014-04-30 2014-07-23 中国科学院电工研究所 Manufacturing method of REFeAsO1-xFx iron-based superconducting wire or strip
CN105016730A (en) * 2015-07-09 2015-11-04 成都点石创想科技有限公司 Superconducting material preparation method with simple process and simple operation

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106521291A (en) * 2016-11-04 2017-03-22 金福兴 Composite superconductive nanometer block material and preparation method thereof
CN108083799A (en) * 2017-12-21 2018-05-29 叶芳 A kind of new energy superconductor and preparation method thereof
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
CN109244229A (en) * 2018-09-13 2019-01-18 安徽建筑大学 A kind of microelectronics superconductor and preparation method thereof
CN109244229B (en) * 2018-09-13 2022-03-18 安徽建筑大学 Microelectronic superconducting material and preparation method thereof
CN110931160A (en) * 2019-10-23 2020-03-27 中国科学院电工研究所 Iron-based superconducting precursor powder, preparation method thereof and iron-based superconducting wire strip
CN110931160B (en) * 2019-10-23 2021-03-19 中国科学院电工研究所 Iron-based superconducting precursor powder, preparation method thereof and iron-based superconducting wire strip

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Application publication date: 20160316