CN106876042A - A kind of method that high-temperature sintering process prepares niobium aluminium superconductor - Google Patents
A kind of method that high-temperature sintering process prepares niobium aluminium superconductor Download PDFInfo
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- CN106876042A CN106876042A CN201710143508.0A CN201710143508A CN106876042A CN 106876042 A CN106876042 A CN 106876042A CN 201710143508 A CN201710143508 A CN 201710143508A CN 106876042 A CN106876042 A CN 106876042A
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- H—ELECTRICITY
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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B12/00—Superconductive or hyperconductive conductors, cables, or transmission lines
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- H01B13/0016—Apparatus or processes specially adapted for manufacturing conductors or cables for heat treatment
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Abstract
The invention discloses a kind of method that high-temperature sintering process prepares niobium aluminium superconductor, aluminium powder is added to graphene oxide solution by the preparation method, realize single-layer graphene cladding aluminium powder, Graphene soilless sticking after heat treatment, closely can uniformly combine aluminium powder, the graphene coated aluminium powder of preparation, its interface is Graphene, avoid the oxidation of aluminium powder, the preparation method also absorbs the characteristic of gas using niobium powder, first by hydrogen and the physics chemical action of niobium powder, produce the niobium powder containing hydrogen and trace niobium hydrogen compound, reach the purpose of refinement niobium powder, the activation energy in reaction is greatly decreased, reduce synthesis difficulty.
Description
Technical field
The present invention relates to superconductor field, and in particular to a kind of method that high-temperature sintering process prepares niobium aluminium superconductor.
Background technology
Superconductor, refers to the property for having and resistance being showed under certain cryogenic conditions equal to zero and repels the magnetic line of force
The material of matter.Have now found that 28 kinds of elements and thousands of kinds of alloys and compound can turn into superconductor.High temperature superconducting materia
Production technology development over time is constantly ripe, and price is also decreased, and the market competitiveness is continuously increased, with volume
It is small, it is lightweight, the low and big advantage of transmission capacity is lost, it is the upgraded product of traditional cable.
In practical superconductor, A15 types intermetallic compound is due to critical-temperature higher, critical magnetic field and facing
Boundary's current density, its development and application is the most universal and rapid.As one kind of A15 type intermetallic compounds, Nb3Al superconduction materials
Material allows characteristic with critical magnetic field and critical current density higher and more preferable strain.Its superconducting critical transition temperature is reachable
18.9K, upper critical field is 29.5T (4.2K), has exceeded Nb3Sn superconductors.Additionally, its critical current density is up to
1000A/mm2 (16T, 4.2K), under conditions of stress is no more than 210MPa, critical current density has almost no change.Therefore,
Nb3Al superconductors are to make one of large-scale optimal superconductor of high field magnet.
The universal component difficulty of technique of high―temperature nuclei niobium aluminium superconductor is big, or high to equipment requirement.Based on Density functional
Series of computation show that the tiny reactant of particle is greatly decreased the activation energy in reaction, reduce synthesis difficulty.The present invention
The characteristic of gas is absorbed using niobium powder, first by the physics chemical action of hydrogen and niobium powder, produce the niobium powder containing hydrogen with
Trace niobium hydrogen compound, reaches the purpose of refinement niobium powder, and the activation energy in reaction is greatly decreased, and reduces synthesis difficulty.Subsequently
Heat treatment process in hydrogen and a small amount of hydride can suppress niobium powder and aluminium powder and occur with micro-air present in sintering environment
Oxidation reaction, it is to avoid introduce the impurity such as oxide, nitride, it is ensured that product quality.
The content of the invention
The present invention provides a kind of method that high-temperature sintering process prepares niobium aluminium superconductor, and be added to for aluminium powder by the preparation method
Graphene oxide solution, realizes single-layer graphene cladding aluminium powder, and Graphene soilless sticking after heat treatment closely can be combined uniformly
Aluminium powder, the graphene coated aluminium powder of preparation, its interface is Graphene, it is to avoid the oxidation of aluminium powder, the preparation method also utilizes niobium
Powder absorbs the characteristic of gas, first by hydrogen and the physics chemical action of niobium powder, produces niobium powder and trace niobium containing hydrogen
Hydrogen compound, reaches the purpose of refinement niobium powder, and the activation energy in reaction is greatly decreased, and reduces synthesis difficulty.
To achieve these goals, the invention provides a kind of method that high-temperature sintering process prepares niobium aluminium superconductor, should
Method comprises the following steps：
（1）Prepare the aluminium powder of graphene coated
Graphene oxide is placed in ethanol, ultrasonic disperse obtains graphene oxide solution, the power of the ultrasonic disperse is
1200W-3000W, the time of ultrasonic disperse is 20min-40min；Then to addition ball shaped nano aluminium in graphene oxide solution
Powder, filter residue is filtrated to get after stirring, and by filter residue vacuum drying, obtains mixed powder；The ball shaped nano aluminium powder
Quality is 50-80 times of graphene oxide quality；
The mixed powder is heat-treated in reducing atmosphere, and the temperature of the heat treatment is 500 DEG C -800 DEG C, and heat up speed
It is 20 DEG C/min-50 DEG C/min to spend, and obtains graphene coated aluminium powder；
（2）Pretreatment niobium powder
The Nb powder that purity is 99.999% is uniformly spread and is sprinkled upon in quartz boat, be put into tube furnace, be passed through volume proportion for 10%-
100% hydrogen and the nitrogen mixture of 90%-0, heat in 400-420 DEG C of temperature range, are incubated 3 hours, furnace cooling
After take out, obtain pre-process niobium powder；
（3）Above-mentioned pretreatment Nb powder and above-mentioned graphene coated aluminium powder are taken, is 3 according to the atomic ratio of Nb and Al:1 ratio is mixed
Close, mixed-powder is placed in ball grinder, add ball milling agent, carry out high-energy ball milling processing, ball and mixed powder in the ball grinder
The mass ratio at end is 10:（1-1.5）, nitrogen is filled with ball grinder, rotating speed is 1000-1500r/min, and Ball-milling Time is 6-8h,
Mixed powder is obtained；
（4）Above-mentioned mixed powder is compressing using mould, and pressing pressure is 15-20MPa, is made block piece shape material base, uses niobium
Paper tinsel is wrapped up, and the block piece shape material base that will be wrapped is fitted into quartz boat, quartz boat is placed in tube furnace, 4-6% hydrogen and
In the nitrogen mixture protection of 96-94%, furnace temperature is warming up to 1000-1400 DEG C, insulation 6-8h is sintered reaction, then soon
Speed is cooled to room temperature, that is, niobium aluminium superconductor is obtained.
Preferably, the step（1）In, described reducing atmosphere is nitrogen and the mixed gas of hydrogen, mixed gas
The volumn concentration of middle hydrogen is 10%-15%, and the concentration of the graphene oxide solution is 1mg/mL-3mg/mL.
Specific embodiment
Embodiment one
Graphene oxide is placed in ethanol, ultrasonic disperse obtains graphene oxide solution, the power of the ultrasonic disperse is
1200W, the time of ultrasonic disperse is 20min；Then to addition ball shaped nano aluminium powder in graphene oxide solution, after stirring
Filter residue is filtrated to get, by filter residue vacuum drying, mixed powder is obtained；The quality of the ball shaped nano aluminium powder is graphite oxide
50 times of alkene quality；The concentration of the graphene oxide solution is 1mg/mL.
The mixed powder is heat-treated in reducing atmosphere, and the temperature of the heat treatment is 500 DEG C, programming rate
It is 20 DEG C/min, obtains graphene coated aluminium powder；Described reducing atmosphere is the mixed gas of nitrogen and hydrogen, mixed gas
The volumn concentration of middle hydrogen is 10%.
The Nb powder that purity is 99.999% is uniformly spread and is sprinkled upon in quartz boat, be put into tube furnace, being passed through volume proportion is
10% hydrogen and 90% nitrogen mixture, heat in 400 DEG C of temperature ranges, are incubated 3 hours, are taken out after furnace cooling,
Obtain pre-processing niobium powder.
Above-mentioned pretreatment Nb powder and above-mentioned graphene coated aluminium powder are taken, is 3 according to the atomic ratio of Nb and Al:1 ratio is mixed
Close, mixed-powder is placed in ball grinder, add ball milling agent, carry out high-energy ball milling processing, ball and mixed powder in the ball grinder
The mass ratio at end is 10:1, nitrogen is filled with ball grinder, rotating speed is 1000r/min, and Ball-milling Time is 6h, and mixed powder is obtained.
Above-mentioned mixed powder is compressing using mould, and pressing pressure is 15MPa, is made block piece shape material base, uses niobium paper tinsel
Parcel, the block piece shape material base that will be wrapped is fitted into quartz boat, quartz boat is placed in tube furnace, in 4% hydrogen and 96%
Nitrogen mixture protection in, furnace temperature is warming up to 1000 DEG C, insulation 6h is sintered reaction, is then quickly cooled to room temperature,
Niobium aluminium superconductor is obtained.
Embodiment two
Graphene oxide is placed in ethanol, ultrasonic disperse obtains graphene oxide solution, the power of the ultrasonic disperse is
3000W, the time of ultrasonic disperse is 40min；Then to addition ball shaped nano aluminium powder in graphene oxide solution, after stirring
Filter residue is filtrated to get, by filter residue vacuum drying, mixed powder is obtained；The quality of the ball shaped nano aluminium powder is graphite oxide
80 times of alkene quality；The concentration of the graphene oxide solution is 3mg/mL.
The mixed powder is heat-treated in reducing atmosphere, and the temperature of the heat treatment is 800 DEG C, programming rate
It is 50 DEG C/min, obtains graphene coated aluminium powder；Described reducing atmosphere is the mixed gas of nitrogen and hydrogen, mixed gas
The volumn concentration of middle hydrogen is 15%.
The Nb powder that purity is 99.999% is uniformly spread and is sprinkled upon in quartz boat, be put into tube furnace, being passed through volume proportion is
100% hydrogen, heats in 400-420 DEG C of temperature range, is incubated 3 hours, is taken out after furnace cooling, obtains pre-processing niobium
Powder.
Above-mentioned pretreatment Nb powder and above-mentioned graphene coated aluminium powder are taken, is 3 according to the atomic ratio of Nb and Al:1 ratio is mixed
Close, mixed-powder is placed in ball grinder, add ball milling agent, carry out high-energy ball milling processing, ball and mixed powder in the ball grinder
The mass ratio at end is 10:1.5, nitrogen is filled with ball grinder, rotating speed is 1500r/min, and Ball-milling Time is 8h, and mixed powder is obtained
Body.
Above-mentioned mixed powder is compressing using mould, and pressing pressure is 20MPa, is made block piece shape material base, uses niobium paper tinsel
Parcel, the block piece shape material base that will be wrapped is fitted into quartz boat, quartz boat is placed in tube furnace, in 6% hydrogen and 94%
Nitrogen mixture protection in, furnace temperature is warming up to 1400 DEG C, insulation 8h is sintered reaction, is then quickly cooled to room temperature,
Niobium aluminium superconductor is obtained.
The above, is only presently preferred embodiments of the present invention, and any limitation is not done to the present invention, every according to invention skill
Any simple modification, change and 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 method that high-temperature sintering process prepares niobium aluminium superconductor, the method comprises the following steps：
（1）Prepare the aluminium powder of graphene coated
Graphene oxide is placed in ethanol, ultrasonic disperse obtains graphene oxide solution, the power of the ultrasonic disperse is
1200W-3000W, the time of ultrasonic disperse is 20min-40min；Then to addition ball shaped nano aluminium in graphene oxide solution
Powder, filter residue is filtrated to get after stirring, and by filter residue vacuum drying, obtains mixed powder；The ball shaped nano aluminium powder
Quality is 50-80 times of graphene oxide quality；
The mixed powder is heat-treated in reducing atmosphere, and the temperature of the heat treatment is 500 DEG C -800 DEG C, and heat up speed
It is 20 DEG C/min-50 DEG C/min to spend, and obtains graphene coated aluminium powder；
（2）Pretreatment niobium powder
The Nb powder that purity is 99.999% is uniformly spread and is sprinkled upon in quartz boat, be put into tube furnace, be passed through volume proportion for 10%-
100% hydrogen and the nitrogen mixture of 90%-0, heat in 400-420 DEG C of temperature range, are incubated 3 hours, furnace cooling
After take out, obtain pre-process niobium powder；
（3）Above-mentioned pretreatment Nb powder and above-mentioned graphene coated aluminium powder are taken, is 3 according to the atomic ratio of Nb and Al:1 ratio is mixed
Close, mixed-powder is placed in ball grinder, add ball milling agent, carry out high-energy ball milling processing, ball and mixed powder in the ball grinder
The mass ratio at end is 10:（1-1.5）, nitrogen is filled with ball grinder, rotating speed is 1000-1500r/min, and Ball-milling Time is 6-8h,
Mixed powder is obtained；
（4）Above-mentioned mixed powder is compressing using mould, and pressing pressure is 15-20MPa, is made block piece shape material base, uses niobium
Paper tinsel is wrapped up, and the block piece shape material base that will be wrapped is fitted into quartz boat, quartz boat is placed in tube furnace, 4-6% hydrogen and
In the nitrogen mixture protection of 96-94%, furnace temperature is warming up to 1000-1400 DEG C, insulation 6-8h is sintered reaction, then soon
Speed is cooled to room temperature, that is, niobium aluminium superconductor is obtained.
2. preparation method as claimed in claim 1, it is characterised in that the step（1）In, described reducing atmosphere is nitrogen
The mixed gas of gas and hydrogen, the volumn concentration of hydrogen is 10%-15%, the graphene oxide solution in mixed gas
Concentration be 1mg/mL-3mg/mL.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107464628A (en) * | 2017-08-23 | 2017-12-12 | 苏州南尔材料科技有限公司 | A kind of preparation method of nanometer of carbon conductive fibers yttrium niobium aluminium superconductor |
| CN107527693A (en) * | 2017-08-25 | 2017-12-29 | 苏州南尔材料科技有限公司 | A kind of method that high-temperature sintering process prepares superconductor |
-
2017
- 2017-03-11 CN CN201710143508.0A patent/CN106876042A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107464628A (en) * | 2017-08-23 | 2017-12-12 | 苏州南尔材料科技有限公司 | A kind of preparation method of nanometer of carbon conductive fibers yttrium niobium aluminium superconductor |
| CN107527693A (en) * | 2017-08-25 | 2017-12-29 | 苏州南尔材料科技有限公司 | A kind of method that high-temperature sintering process prepares superconductor |
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