CN107564622A - A kind of preparation method of yttrium niobium copper superconductor - Google Patents
A kind of preparation method of yttrium niobium copper superconductor Download PDFInfo
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- CN107564622A CN107564622A CN201710744713.2A CN201710744713A CN107564622A CN 107564622 A CN107564622 A CN 107564622A CN 201710744713 A CN201710744713 A CN 201710744713A CN 107564622 A CN107564622 A CN 107564622A
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Abstract
The invention discloses a kind of preparation method of yttrium niobium copper superconductor, niobium powder is added to nano-sized carbon conductive fiber material solution by the preparation method, a nanometer carbon conductive fibers cladding niobium powder is realized, soilless sticking after heat treatment, closely can uniformly combine niobium powder, not only there is improved electric conductivity, products obtained therefrom critical transition temperature is high, and superconductivity products made thereby technique well of the present invention is simple, regular appearance, surface compact and connectivity is good, superconduction critical temperature are high.
Description
Technical field
The present invention relates to superconductor field, and in particular to a kind of preparation method of yttrium niobium copper superconductor.
Background technology
Superconductor, refer to showed under certain cryogenic conditions resistance equal to zero and repel the magnetic line of force property
The material of matter.Copper oxygen compound high-temperature superconductor is as a kind of present superconductor of critical-temperature highest, domestic and international scientist couple
It expands substantial amounts of research, and this type I superconductors I can realize superconduction in liquid nitrogen temperature at present, have been equipped with the valency of practical application
How value, but improve its every critical parameters, especially improves critical temperature Tc, be still high-temperature superconductor research field one most
Big problem.
The universal component difficulty of technique of high―temperature nuclei yttrium niobium copper superconductor is big, or to equipment requirement height.It is general based on density
The series of computation of letter shows that the activation energy in reaction is greatly decreased in the tiny reactant of particle, reduces synthesis difficulty.This hair
The bright characteristic that gas is absorbed using niobium powder, first by the physics chemical action of hydrogen and niobium powder, produces the niobium powder containing hydrogen
With trace niobium hydrogen compound, reach the purpose of refinement niobium powder, the activation energy in reaction is greatly decreased, reduce synthesis difficulty.Afterwards
Hydrogen and a small amount of hydride can suppress niobium powder and aluminium powder and micro-air hair present in sintering environment in continuous heat treatment process
Raw oxidation reaction, avoid introducing the impurity such as oxide, nitride, it is ensured that product quality.Adding nano-sized carbon conductive fiber material is
Improve superconducting wire antioxygenic property, improve the effective ways of conductance.
The content of the invention
The present invention provides a kind of preparation method of yttrium niobium copper superconductor, and niobium powder is added to nano-sized carbon and led by the preparation method
Electric fibrous material solution, a nanometer carbon conductive fibers cladding niobium powder is realized, soilless sticking after heat treatment, closely can uniformly combine niobium
Powder, not only with improved electric conductivity, products obtained therefrom critical transition temperature is high, and superconductivity is good；Products made thereby work of the present invention
Skill is simple, regular appearance, surface compact and connectivity is good, and superconduction critical temperature is high.
To achieve these goals, the invention provides a kind of preparation method of yttrium niobium copper superconductor, this method to include
Following steps：
（1）Prepare nano-sized carbon conductive fiber material solution
Graphitic pretreatment, sodium fluoride is mixed in Nano graphite powder, and add metallic catalyst, mixed, in inert gas shielding
Under sodium fluoride is fixed in 600-650 DEG C of heating, heat time control on Nano graphite powder surface in 10-15min；
Carbon nano-fiber is pre-processed, and the Nano carbon fibers Wesy concentrated sulfuric acid is carried out with potassium permanganate to mix acid oxidase, violent through ultrasound
After stirring, the carbon nano-fiber of carboxylated is obtained, adds surface conditioning agent, heats 10-15min at 150-200 DEG C, adds
Enter silver, nitrogen and helium it is mixed gas protected under at 400-450 DEG C heat 30-45min, silver is dispersed in nano-sized carbon
In fiber；
The carbon nano-fiber of the graphite of pretreatment and pretreatment is placed in container, is dissolved, added with 150-250 parts isopropanol
Dispersant, polyphenylene sulfide, PPS resin, are blended with forced mixer, then carry out ultrasonic disperse with ultrasonic wave separating apparatus again, are surpassed
Acoustic frequency is 25-30kHz, time 1-2h, forms the nano-sized carbon conductive fiber material solution of homogeneous；
（2）Ball shaped nano niobium powder is added into nano-sized carbon conductive fiber material solution, filter residue is filtrated to get after stirring, by institute
Filter residue vacuum drying is stated, obtains mixed powder；The quality of the ball shaped nano niobium powder is nano-sized carbon conductive fiber material quality
50-80 times；The mixed powder is heat-treated in reducing atmosphere, and the temperature of the heat treatment is 500 DEG C -800 DEG C, is risen
Warm speed is 20 DEG C/min-50 DEG C/min, obtains nano-sized carbon conductive fiber material cladding niobium powder；
（3）Above-mentioned nano-sized carbon conductive fiber material cladding niobium powder, yittrium oxide and cupric oxide are dried, is placed in grinder and grinds
10-12 hours, powder is made, powder is placed in vacuum tube furnace, and heating is heated to 850-900 DEG C, and constant temperature preheating 10-16 is small
When, take out, mixed powder 1 is made；
（4）Calcium carbonate, methylcellulose, Boratex, benzoic acid, calcium nitrate and barium sulfate is taken to be placed in grinder, with distilled water
For grinding aid ball milling 2-6 hours, then add sodium lignin sulfonate and continue ball milling 4 hours, take out, drying, mixed powder is made
2；
（5）It is compressing using mould after above-mentioned mixed powder 1 and mixed powder 2 are mixed, pressing pressure 15-20MPa,
Block piece shape material base is made, is wrapped up with niobium paper tinsel, the block piece shape material base wrapped is fitted into quartz boat, quartz boat is placed on tube furnace
In, in the nitrogen mixture protection of 4-6% hydrogen and 96-94%, furnace temperature is warming up to 1000-1400 DEG C, is incubated 6-8h
Reaction is sintered, is then quickly cooled to room temperature, that is, yttrium niobium copper superconductor is made.
Preferably, the weight of the various raw materials of the yttrium niobium copper superconductor is：Above-mentioned nanometer carbon conductive fibers
Material cladding niobium powder 5.1-5.5, yittrium oxide 5.1-5.3, cupric oxide 4.2-4.3, sodium lignin sulfonate 1.5-1.7, calcium carbonate
2.5-2.6, methylcellulose 1.8-2.0, Boratex 1.7-1.9, benzoic acid 1.5-1.6, calcium nitrate 2.4-2.5, barium sulfate
2.3-2.5。
Embodiment
Embodiment one
Graphitic pretreatment, sodium fluoride is mixed in Nano graphite powder, and add metallic catalyst, mixed, in inert gas shielding
Under sodium fluoride is fixed in 600 DEG C of heating, heat time control on Nano graphite powder surface in 10min.
Carbon nano-fiber pre-processes, and the Nano carbon fibers Wesy concentrated sulfuric acid is carried out with potassium permanganate to mix acid oxidase, through ultrasound
After being stirred vigorously, the carbon nano-fiber of carboxylated is obtained, adds surface conditioning agent, heats 10min at 150 DEG C, adds
Silver, nitrogen and helium it is mixed gas protected under at 400 DEG C heat 30min, silver is dispersed in carbon nano-fiber.
The carbon nano-fiber of the graphite of pretreatment and pretreatment is placed in container, is dissolved, added with 150 parts of isopropanols
Dispersant, polyphenylene sulfide, PPS resin, are blended with forced mixer, then carry out ultrasonic disperse with ultrasonic wave separating apparatus again, are surpassed
Acoustic frequency is 25kHz, time 1h, forms the nano-sized carbon conductive fiber material solution of homogeneous.
Ball shaped nano niobium powder is added into nano-sized carbon conductive fiber material solution, filter residue is filtrated to get after stirring, will
The filter residue vacuum drying, obtains mixed powder；The quality of the ball shaped nano niobium powder is nano-sized carbon conductive fiber material quality
50 times；The mixed powder is heat-treated in reducing atmosphere, and the temperature of the heat treatment is 500 DEG C, programming rate
For 20 DEG C/min, nano-sized carbon conductive fiber material cladding niobium powder is obtained.
Above-mentioned nano-sized carbon conductive fiber material cladding niobium powder, yittrium oxide and cupric oxide are dried, is placed in grinder and grinds
10 hours, powder is made, powder is placed in vacuum tube furnace, and heating is heated to 850 DEG C, and constant temperature preheats 10 hours, takes out, and is made
Mixed powder 1.
Calcium carbonate, methylcellulose, Boratex, benzoic acid, calcium nitrate and barium sulfate is taken to be placed in grinder, with distilled water
For grinding aid ball milling 2 hours, then add sodium lignin sulfonate and continue ball milling 4 hours, take out, drying, mixed powder 2 is made.
It is compressing using mould after above-mentioned mixed powder 1 and mixed powder 2 are mixed, pressing pressure 15MPa, system
Blocking sheet material base, wrapped up with niobium paper tinsel, the block piece shape material base wrapped is fitted into quartz boat, quartz boat is placed on tube furnace
In, in 4% hydrogen and the protection of 96% nitrogen mixture, furnace temperature is warming up to 1000 DEG C, insulation 6h is sintered reaction,
Then room temperature is quickly cooled to, that is, yttrium niobium copper superconductor is made.
The weight of the various raw materials of the yttrium niobium copper superconductor is：Above-mentioned nano-sized carbon conductive fiber material cladding
Niobium powder 5.1, yittrium oxide 5.1, cupric oxide 4.2, sodium lignin sulfonate 1.5, calcium carbonate 2.5, methylcellulose 1.8, Boratex
1.7, benzoic acid 1.5, calcium nitrate 2.4, barium sulfate 2.3.
Embodiment two
Graphitic pretreatment, sodium fluoride is mixed in Nano graphite powder, and add metallic catalyst, mixed, in inert gas shielding
Under sodium fluoride is fixed in 650 DEG C of heating, heat time control on Nano graphite powder surface in 15min.
Carbon nano-fiber pre-processes, and the Nano carbon fibers Wesy concentrated sulfuric acid is carried out with potassium permanganate to mix acid oxidase, through ultrasound
After being stirred vigorously, the carbon nano-fiber of carboxylated is obtained, adds surface conditioning agent, heats 15min at 200 DEG C, adds
Silver, nitrogen and helium it is mixed gas protected under at 450 DEG C heat 45min, silver is dispersed in carbon nano-fiber.
The carbon nano-fiber of the graphite of pretreatment and pretreatment is placed in container, is dissolved, added with 250 parts of isopropanols
Dispersant, polyphenylene sulfide, PPS resin, are blended with forced mixer, then carry out ultrasonic disperse with ultrasonic wave separating apparatus again, are surpassed
Acoustic frequency is 0kHz, time 2h, forms the nano-sized carbon conductive fiber material solution of homogeneous.
Ball shaped nano niobium powder is added into nano-sized carbon conductive fiber material solution, filter residue is filtrated to get after stirring, will
The filter residue vacuum drying, obtains mixed powder；The quality of the ball shaped nano niobium powder is nano-sized carbon conductive fiber material quality
80 times；The mixed powder is heat-treated in reducing atmosphere, and the temperature of the heat treatment is 800 DEG C, programming rate
For 50 DEG C/min, nano-sized carbon conductive fiber material cladding niobium powder is obtained.
Above-mentioned nano-sized carbon conductive fiber material cladding niobium powder, yittrium oxide and cupric oxide are dried, is placed in grinder and grinds
12 hours, powder is made, powder is placed in vacuum tube furnace, and heating is heated to 900 DEG C, and constant temperature preheats 16 hours, takes out, and is made
Mixed powder 1.
Calcium carbonate, methylcellulose, Boratex, benzoic acid, calcium nitrate and barium sulfate is taken to be placed in grinder, with distilled water
For grinding aid ball milling 6 hours, then add sodium lignin sulfonate and continue ball milling 4 hours, take out, drying, mixed powder 2 is made.
It is compressing using mould after above-mentioned mixed powder 1 and mixed powder 2 are mixed, pressing pressure 20MPa, system
Blocking sheet material base, wrapped up with niobium paper tinsel, the block piece shape material base wrapped is fitted into quartz boat, quartz boat is placed on tube furnace
In, in 6% hydrogen and the protection of 94% nitrogen mixture, furnace temperature is warming up to 1400 DEG C, insulation 8h is sintered reaction,
Then room temperature is quickly cooled to, that is, yttrium niobium copper superconductor is made.
The weight of the various raw materials of the yttrium niobium copper superconductor is：Above-mentioned nano-sized carbon conductive fiber material cladding
Niobium powder 5.1, yittrium oxide 5.1, cupric oxide 4.2, sodium lignin sulfonate 1.5, calcium carbonate 2.5, methylcellulose 2.0, Boratex
1.9, benzoic acid 1.6, calcium nitrate 2.5, barium sulfate 2.5.
It is described above, only it is presently preferred embodiments of the present invention, any restrictions is not done to the present invention, it is every according to invention skill
Any simple modification, change and the equivalent structure change that art is substantially made to above example, still fall within the technology of the present invention
In the protection domain of scheme.
Claims (2)
1. a kind of preparation method of yttrium niobium copper superconductor, this method comprise the following steps：
（1）Prepare nano-sized carbon conductive fiber material solution
Graphitic pretreatment, sodium fluoride is mixed in Nano graphite powder, and add metallic catalyst, mixed, in inert gas shielding
Under sodium fluoride is fixed in 600-650 DEG C of heating, heat time control on Nano graphite powder surface in 10-15min；
Carbon nano-fiber is pre-processed, and the Nano carbon fibers Wesy concentrated sulfuric acid is carried out with potassium permanganate to mix acid oxidase, violent through ultrasound
After stirring, the carbon nano-fiber of carboxylated is obtained, adds surface conditioning agent, heats 10-15min at 150-200 DEG C, adds
Enter silver, nitrogen and helium it is mixed gas protected under at 400-450 DEG C heat 30-45min, silver is dispersed in nano-sized carbon
In fiber；
The carbon nano-fiber of the graphite of pretreatment and pretreatment is placed in container, is dissolved, added with 150-250 parts isopropanol
Dispersant, polyphenylene sulfide, PPS resin, are blended with forced mixer, then carry out ultrasonic disperse with ultrasonic wave separating apparatus again, are surpassed
Acoustic frequency is 25-30kHz, time 1-2h, forms the nano-sized carbon conductive fiber material solution of homogeneous；
（2）Ball shaped nano niobium powder is added into nano-sized carbon conductive fiber material solution, filter residue is filtrated to get after stirring, by institute
Filter residue vacuum drying is stated, obtains mixed powder；The quality of the ball shaped nano niobium powder is nano-sized carbon conductive fiber material quality
50-80 times；The mixed powder is heat-treated in reducing atmosphere, and the temperature of the heat treatment is 500 DEG C -800 DEG C, is risen
Warm speed is 20 DEG C/min-50 DEG C/min, obtains nano-sized carbon conductive fiber material cladding niobium powder；
（3）Above-mentioned nano-sized carbon conductive fiber material cladding niobium powder, yittrium oxide and cupric oxide are dried, is placed in grinder and grinds
10-12 hours, powder is made, powder is placed in vacuum tube furnace, and heating is heated to 850-900 DEG C, and constant temperature preheating 10-16 is small
When, take out, mixed powder 1 is made；
（4）Calcium carbonate, methylcellulose, Boratex, benzoic acid, calcium nitrate and barium sulfate is taken to be placed in grinder, with distilled water
For grinding aid ball milling 2-6 hours, then add sodium lignin sulfonate and continue ball milling 4 hours, take out, drying, mixed powder is made
2；
（5）It is compressing using mould after above-mentioned mixed powder 1 and mixed powder 2 are mixed, pressing pressure 15-20MPa,
Block piece shape material base is made, is wrapped up with niobium paper tinsel, the block piece shape material base wrapped is fitted into quartz boat, quartz boat is placed on tube furnace
In, in the nitrogen mixture protection of 4-6% hydrogen and 96-94%, furnace temperature is warming up to 1000-1400 DEG C, is incubated 6-8h
Reaction is sintered, is then quickly cooled to room temperature, that is, yttrium niobium copper superconductor is made.
2. the method as described in claim 1, it is characterised in that the parts by weight of the various raw materials of the yttrium niobium copper superconductor are matched somebody with somebody
Than for：Above-mentioned nano-sized carbon conductive fiber material coats niobium powder 5.1-5.5, yittrium oxide 5.1-5.3, cupric oxide 4.2-4.3, lignin
Sodium sulfonate 1.5-1.7, calcium carbonate 2.5-2.6, methylcellulose 1.8-2.0, Boratex 1.7-1.9, benzoic acid 1.5-1.6, nitre
Sour calcium 2.4-2.5, barium sulfate 2.3-2.5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108687342A (en) * | 2018-06-14 | 2018-10-23 | 浙江中平粉末冶金有限公司 | A kind of nano superconductive composite material and preparation method |
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| CN106956063A (en) * | 2017-05-29 | 2017-07-18 | 苏州南尔材料科技有限公司 | A kind of method of utilization resurfacing welding material tipped drill |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106782897A (en) * | 2017-03-11 | 2017-05-31 | 苏州思创源博电子科技有限公司 | A kind of method that high-temperature sintering process prepares yttrium niobium copper superconductor |
| CN106898432A (en) * | 2017-03-11 | 2017-06-27 | 苏州思创源博电子科技有限公司 | A kind of preparation method of Graphene yttrium niobium copper superconductor |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108687342A (en) * | 2018-06-14 | 2018-10-23 | 浙江中平粉末冶金有限公司 | A kind of nano superconductive composite material and preparation method |
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