CN109786025A - A kind of preparation method of modified Bismuth-system superconductor - Google Patents
A kind of preparation method of modified Bismuth-system superconductor Download PDFInfo
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- CN109786025A CN109786025A CN201910078166.8A CN201910078166A CN109786025A CN 109786025 A CN109786025 A CN 109786025A CN 201910078166 A CN201910078166 A CN 201910078166A CN 109786025 A CN109786025 A CN 109786025A
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Abstract
The present invention discloses a kind of preparation method of modified Bismuth-system superconductor, belongs to technical field of functional ceramics, includes the following steps: to take Bi2O3、SrCO3、CaCO3, PbO and BaO, be sufficiently mixed it is levigate after be put into alumina crucible, synthesized 4~7 hours at a temperature of 780~810 DEG C；Synthetic product uniformly forms afterwards with CuO ground and mixed, is put into firing in resistance furnace, takes out, be rapidly cooled to room temperature in air；It is formed under 1.5~2MPa pressure after burned material is ground, is placed again into firing in resistance furnace, 820~850 DEG C of firing temperature, keeps the temperature 2~5 hours, take out, be rapidly cooled to room temperature in air.Compared with original Bi2223 supercondutive powder, Bi2223 superconducting tape performance is obtained by PIT preparation process by the Bi2223 supercondutive powder of doping vario-property, 170A is increased to by original 130A.
Description
Technical field
The present invention relates to technical field of functional ceramics, in particular to a kind of preparation method of modified Bismuth-system superconductor.
Background technique
Superconductor technology is the new and high technology for 21 century having great economy and strategic importance, is had in all fields of national economy
Wide application prospect, superconducting quantum interference device, filter such as in the application of superconduction light current；Electricity in the application of superconduction forceful electric power
Cable, current limiter, motor, energy-storage system, transformer, magnet technology, medical Magnetic resonance imaging, high-energy physics experiment and high speed are handed over
It is logical to transport.
In all kinds of high-temperature oxide superconductors having now been found that, Bi system with its stronger stability, higher face
Boundary's transition temperature, at low cost, raw material are easy to get and pollute the advantages that small and paid much attention to, and becoming in superconductor applications research most has
One of future and the material of development potentiality.
But the less reproducible problem of its generally existing bulk material sintering process in the preparation of Bi series superconducting material.This is
Due to Bi (2223) phase, Bi (2212) mutually with Bi (2201) mutually can mutually convert at different conditions, often occur same composition,
Under identical preparation process condition, the superconductivity between different furnace samples is had differences, this makes the stability of superconductor
At adverse effect.
The part Sunshine et al. first discovery Pb replaces Bi that can promote the formation of Bi-2223 phase and keep it more steady
It is fixed.In fact, can just there is a large amount of Bi-2223 phase to be formed in the case where only adding Pb in the mixture, the name of supercondutive powder
Usually there is highest conversion ratio as 0.2≤x≤0.5 in proportion Bi2-x Pb xSr2Ca2Cu30y.Pb is to a certain extent
To a kind of doping vario-property of Bi-Sr-Ca-Cu-O oxide system.Scholars have put into a large amount of energy in doping member at present
In plain type and content, it is desirably to obtain higher superconductor performance.
Summary of the invention
In view of the above technical problems, the present invention provides a kind of preparation methods of modified Bismuth-system superconductor, in original Bi-
The modified invention that the performance carried out on the basis of Pb-Sr-Ca-Cu-O system improves.
To reach above-mentioned technical purpose, the technical solution of the present invention is as follows:
The present invention provides a kind of preparation method of modified Bismuth-system superconductor, includes the following steps:
A kind of preparation method of modified Bismuth-system superconductor, includes the following steps:
(1) Bi is taken2O3、SrCO3、CaCO3, PbO and BaO, be sufficiently mixed it is levigate after be put into alumina crucible, 780~
It is synthesized 4~7 hours at a temperature of 810 DEG C；
(2) it is formed under 1.5~2MPa pressure after synthetic product and CuO ground and mixed are uniform, is put into firing in resistance furnace,
Firing temperature is 800~820 DEG C, keeps the temperature 4~8 hours, takes out, is rapidly cooled to room temperature in air；
(3) it will be formed under 1.5~2MPa pressure after step (2) the burned material grinding, be placed again into resistance furnace and burn
At 820~850 DEG C of firing temperature, heat preservation 2~5 hours is taken out, is rapidly cooled to room temperature in air.
Wherein it is preferred to the mol ratio of Bi, Sr, Ca, Cu, Pb and Ba element be 1:1:1:2:0.2:0.01~
0.02。
Wherein it is preferred to which the synthesis of the step (1) is carried out in air or oxygen atmosphere.
Wherein it is preferred to which the speed of step (1) heating is 30-60 DEG C per hour.
Wherein it is preferred to which the firing of the step (2) is carried out in air or oxygen atmosphere.
Wherein it is preferred to room temperature to 300 DEG C of heating rates is 3-5 DEG C per minute in step (2) temperature-rise period,
300 DEG C or more heating rates are 5-10 DEG C per minute.
Wherein it is preferred to which the firing of the step (3) is carried out in air or oxygen atmosphere.
Wherein it is preferred to room temperature to 300 DEG C of heating rates is 1-2 DEG C per minute in step (3) temperature-rise period,
300 DEG C or more heating rates are 8-10 DEG C per minute.
Beneficial effects of the present invention:
The present invention first takes Bi for analytically pure2O3、SrCO3、CaCO3, after PbO and BaO mix in proportion, burn Bi- in advance
Sr-Ca-Pb-Ba-O presoma carries out double sintering, and in sintering process after being then mixed the presoma and CuO grinding
Using the temperature program of setting, cooling process and quenching, annealing process, the superconductivity between different furnace samples is stablized.And with
Original Bi2223 supercondutive powder is compared, and is obtained Bi2223 by PIT preparation process by the Bi2223 supercondutive powder of doping vario-property and is surpassed
Conduction band material performance is increased to 170A by original 130A.
Specific embodiment
Below in conjunction with the specific embodiment of the invention, technical solution of the present invention is clearly and completely described, is shown
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
Embodiment 1
The present embodiment provides a kind of preparation methods of modified Bismuth-system superconductor, include the following steps:
(1) Bi is taken2O3、SrCO3、CaCO3, PbO and BaO, be sufficiently mixed it is levigate after be put into alumina crucible, at 800 DEG C
At a temperature of synthesize 5 hours, the speed of heating is 45 DEG C per hour, and synthesis is carried out in air atmosphere；
(2) it forms, is put into resistance furnace in air atmosphere under 2MPa pressure after synthetic product and CuO ground and mixed are uniform
In be burnt into, firing temperature is 810 DEG C, keeps the temperature 6 hours, and room temperature to 300 DEG C of heating rates are per minute 4 in temperature-rise period
DEG C, 300 DEG C or more heating rates are 8 DEG C per minute；It takes out, is rapidly cooled to room temperature in air；
(3) it will be formed under 2MPa pressure after step (2) the burned material grinding, being placed again into resistance furnace is in air
The firing carried out in atmosphere, keeps the temperature 4 hours by 840 DEG C of firing temperature, and in temperature-rise period, room temperature to 300 DEG C of heating rates is every point
1.5 DEG C of clock, 300 DEG C or more heating rates are 9 DEG C per minute, take out, are rapidly cooled to room temperature in air.
Wherein, the mol ratio of Bi, Sr, Ca, Cu, Pb and Ba element is 1:1:1:2:0.2:0.015.
Modified Bismuth-system superconductor critical electric current value made from the present embodiment is 130A.
Embodiment 2
The present embodiment provides a kind of preparation methods of modified Bismuth-system superconductor, include the following steps:
(1) Bi is taken2O3、SrCO3、CaCO3, PbO and BaO, be sufficiently mixed it is levigate after be put into alumina crucible, at 780 DEG C
At a temperature of synthesize 7 hours, the speed of heating is 30 DEG C per hour, and synthesis is carried out in oxygen atmosphere；
(2) it forms, is put into resistance furnace in oxygen atmosphere under 2MPa pressure after synthetic product and CuO ground and mixed are uniform
In be burnt into, firing temperature is 800 DEG C, keeps the temperature 8 hours, and room temperature to 300 DEG C of heating rates are per minute 3 in temperature-rise period
DEG C, 300 DEG C or more heating rates are 10 DEG C per minute；It takes out, is rapidly cooled to room temperature in air；
(3) it will be formed under 1.5MPa pressure after step (2) the burned material grinding, being placed again into resistance furnace is in oxygen
The firing carried out in gas atmosphere, keeps the temperature 2 hours, in temperature-rise period, room temperature to 300 DEG C of heating rates is every by 850 DEG C of firing temperature
2 DEG C of minute, 300 DEG C or more heating rates are 8 DEG C per minute, take out, are rapidly cooled to room temperature in air.
Wherein, the mol ratio of Bi, Sr, Ca, Cu, Pb and Ba element is 1:1:1:2:0.2:0.01.
Modified Bismuth-system superconductor critical electric current value made from the present embodiment is 105A.
Embodiment 3
The present embodiment provides a kind of preparation methods of modified Bismuth-system superconductor, include the following steps:
(1) Bi is taken2O3、SrCO3、CaCO3, PbO and BaO, be sufficiently mixed it is levigate after be put into alumina crucible, at 810 DEG C
At a temperature of synthesize 4 hours, the speed of heating is 60 DEG C per hour, and synthesis is carried out in oxygen atmosphere；
(2) it forms, is put into resistance furnace in oxygen gas under 1.5MPa pressure after synthetic product and CuO ground and mixed are uniform
It is burnt into atmosphere, firing temperature is 820 DEG C, keeps the temperature 4 hours, and room temperature to 300 DEG C of heating rates are per minute 5 in temperature-rise period
DEG C, 300 DEG C or more heating rates are 5 DEG C per minute；It takes out, is rapidly cooled to room temperature in air；
(3) it will be formed under 2MPa pressure after step (2) the burned material grinding, being placed again into resistance furnace is in oxygen
The firing carried out in atmosphere, keeps the temperature 5 hours by 820 DEG C of firing temperature, and in temperature-rise period, room temperature to 300 DEG C of heating rates is every point
1 DEG C of clock, 300 DEG C or more heating rates are 10 DEG C per minute, take out, are rapidly cooled to room temperature in air.
Wherein, the mol ratio of Bi, Sr, Ca, Cu, Pb and Ba element is 1:1:1:2:0.2:0.02.
Modified Bismuth-system superconductor critical electric current value made from the present embodiment is 125A.
Embodiment 4
The present embodiment provides a kind of preparation methods of modified Bismuth-system superconductor, include the following steps:
(1) Bi is taken2O3、SrCO3、CaCO3, PbO and BaO, be sufficiently mixed it is levigate after be put into alumina crucible, at 800 DEG C
At a temperature of synthesize 5 hours, the speed of heating is 50 DEG C per hour, and synthesis is carried out in air atmosphere；
(2) it forms, is put into resistance furnace in oxygen atmosphere under 2MPa pressure after synthetic product and CuO ground and mixed are uniform
In be burnt into, firing temperature is 820 DEG C, keeps the temperature 7 hours, and room temperature to 300 DEG C of heating rates are per minute 4 in temperature-rise period
DEG C, 300 DEG C or more heating rates are 8 DEG C per minute；It takes out, is rapidly cooled to room temperature in air；
(3) it will be formed under 1.8MPa pressure after step (2) the burned material grinding, being placed again into resistance furnace is in sky
The firing carried out in gas atmosphere, keeps the temperature 3 hours, in temperature-rise period, room temperature to 300 DEG C of heating rates is every by 840 DEG C of firing temperature
1.5 DEG C of minute, 300 DEG C or more heating rates are 9 DEG C per minute, take out, are rapidly cooled to room temperature in air.
Wherein, the mol ratio of Bi, Sr, Ca, Cu, Pb and Ba element is 1:1:1:2:0.2:0.012.
Modified Bismuth-system superconductor critical electric current value made from the present embodiment is 121A.
Embodiment 5
The present embodiment provides a kind of preparation methods of modified Bismuth-system superconductor, include the following steps:
(1) Bi is taken2O3、SrCO3、CaCO3, PbO and BaO, be sufficiently mixed it is levigate after be put into alumina crucible, at 790 DEG C
At a temperature of synthesize 6 hours, the speed of heating is 45 DEG C per hour, and synthesis is carried out in air atmosphere；
(2) it forms, is put into resistance furnace in air gas under 1.8MPa pressure after synthetic product and CuO ground and mixed are uniform
It is burnt into atmosphere, firing temperature is 810 DEG C, keeps the temperature 7 hours, and room temperature to 300 DEG C of heating rates are per minute 3 in temperature-rise period
DEG C, 300 DEG C or more heating rates are 10 DEG C per minute；It takes out, is rapidly cooled to room temperature in air；
(3) it will be formed under 2MPa pressure after step (2) the burned material grinding, being placed again into resistance furnace is in air
The firing carried out in atmosphere, keeps the temperature 4 hours by 830 DEG C of firing temperature, and in temperature-rise period, room temperature to 300 DEG C of heating rates is every point
1.5 DEG C of clock, 300 DEG C or more heating rates are 9 DEG C per minute, take out, are rapidly cooled to room temperature in air.
Wherein, the mol ratio of Bi, Sr, Ca, Cu, Pb and Ba element is 1:1:1:2:0.2:0.018.
Modified Bismuth-system superconductor critical electric current value made from the present embodiment is 122A.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of preparation method of modified Bismuth-system superconductor, it is characterised in that include the following steps:
(1) Bi is taken2O3、SrCO3、CaCO3, PbO and BaO, be sufficiently mixed it is levigate after be put into alumina crucible, at 780~810 DEG C
At a temperature of synthesize 4~7 hours；
(2) it is formed under 1.5~2MPa pressure after synthetic product and CuO ground and mixed are uniform, is put into firing in resistance furnace, firing
Temperature is 800~820 DEG C, keeps the temperature 4~8 hours, takes out, is rapidly cooled to room temperature in air；
(3) it will be formed under 1.5~2MPa pressure after step (2) the burned material grinding, be placed again into firing in resistance furnace, burn
At 820~850 DEG C of temperature, 2~5 hours are kept the temperature, takes out, is rapidly cooled to room temperature in air.
2. a kind of preparation method of modified Bismuth-system superconductor according to claim 1, it is characterised in that: the Bi, Sr,
The mol ratio of Ca, Cu, Pb and Ba element is 1:1:1:2:0.2:0.01~0.02.
3. a kind of preparation method of modified Bismuth-system superconductor according to claim 1, it is characterised in that: the step (1)
Synthesis be to be carried out in air or oxygen atmosphere.
4. a kind of preparation method of modified Bismuth-system superconductor according to claim 1, it is characterised in that: the step (1)
The speed of heating is 30-60 DEG C per hour.
5. a kind of preparation method of modified Bismuth-system superconductor according to claim 1, it is characterised in that: the step (2)
Firing be to be carried out in air or oxygen atmosphere.
6. a kind of preparation method of modified Bismuth-system superconductor according to claim 1, it is characterised in that: the step (2)
In temperature-rise period, room temperature to 300 DEG C of heating rates is 3-5 DEG C per minute, and 300 DEG C or more heating rates are 5-10 DEG C per minute.
7. a kind of preparation method of modified Bismuth-system superconductor according to claim 1, it is characterised in that: the step (3)
Firing be to be carried out in air or oxygen atmosphere.
8. a kind of preparation method of modified Bismuth-system superconductor according to claim 1, it is characterised in that: the step (3)
In temperature-rise period, room temperature to 300 DEG C of heating rates is 1-2 DEG C per minute, and 300 DEG C or more heating rates are 8-10 DEG C per minute.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115745595A (en) * | 2021-05-12 | 2023-03-07 | 张建军 | High-temperature electronic superconductor |
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| CN1143061A (en) * | 1996-05-21 | 1997-02-19 | 浙江大学 | Single phase Bi2Sr2Ca2Cu3O10+delt high temperature superconducting phase step synthetic method |
| JPH1036119A (en) * | 1996-07-19 | 1998-02-10 | Kokusai Chodendo Sangyo Gijutsu Kenkyu Center | Production of oxide superconductor film |
| CN102503402A (en) * | 2011-09-19 | 2012-06-20 | 北京英纳超导技术有限公司 | Preparation method of bismuth-system superconductive powder |
| CN102807362A (en) * | 2012-09-14 | 2012-12-05 | 西北有色金属研究院 | Preparation method for Bi-2212-based high-temperature superconducting block material |
| CN103896576A (en) * | 2014-03-06 | 2014-07-02 | 北京英纳超导技术有限公司 | Modified bismuth-system superconductive powder and preparation method thereof |
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- 2019-01-28 CN CN201910078166.8A patent/CN109786025B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1143061A (en) * | 1996-05-21 | 1997-02-19 | 浙江大学 | Single phase Bi2Sr2Ca2Cu3O10+delt high temperature superconducting phase step synthetic method |
| JPH1036119A (en) * | 1996-07-19 | 1998-02-10 | Kokusai Chodendo Sangyo Gijutsu Kenkyu Center | Production of oxide superconductor film |
| CN102503402A (en) * | 2011-09-19 | 2012-06-20 | 北京英纳超导技术有限公司 | Preparation method of bismuth-system superconductive powder |
| CN102807362A (en) * | 2012-09-14 | 2012-12-05 | 西北有色金属研究院 | Preparation method for Bi-2212-based high-temperature superconducting block material |
| CN103896576A (en) * | 2014-03-06 | 2014-07-02 | 北京英纳超导技术有限公司 | Modified bismuth-system superconductive powder and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115745595A (en) * | 2021-05-12 | 2023-03-07 | 张建军 | High-temperature electronic superconductor |
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