CN108083799A - A kind of new energy superconductor and preparation method thereof - Google Patents
A kind of new energy superconductor and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of new energy superconductor, and Mg powder, lanthana, Se powder are mixed, added in ball grinder, 1 2h of ball milling in argon atmosphere；Powder after ball milling is put into S type plane moulds, then applies the pressure of 2 8MPa, 10 15min of pressurize to mold；Gained sample is put into vacuum sintering furnace to be sintered；Vacuum degree is maintained at below 3.5Pa；Temperature program is：350 450 DEG C of 1 2h of insulation reaction are warming up to 5 10 DEG C/min；650 750 DEG C of 50 80min of insulation reaction are warming up to 10 15 DEG C/min of rate；850 950 DEG C of 1.5 2.5h of insulation reaction are warming up to 15 20 DEG C/min of rate；Room temperature is down to the cooling velocity of 20 30 DEG C/min, it is polished to can obtain the new energy superconductor.
Description
Technical field
The invention belongs to new energy materials field, more particularly to a kind of new energy superconductor and preparation method thereof.
Background technology
When temperature drops to a certain critical-temperature, resistance completely disappears some materials, and this phenomenon is known as superconducting
Property, the material with this phenomenon is known as superconductor.Another of superconductor is characterized in：When resistance disappears, magnetic induction
Line will not pass through superconductor, and this phenomenon is known as diamagnetism.Common metal (such as：Copper) resistivity with the decline of temperature and
It is gradually reduced, when temperature is close to 0K, resistance reaches a certain value.And Holland scientist Ang Neisi in 1919 is cooled down with liquid helium
Mercury when temperature drops to 4.2K (i.e. -269 DEG C), it is found that the resistance of mercury completely disappears.Superconductivity and diamagnetism are super
Two key properties of conductor.The temperature that superconduction bulk resistor is made to be zero is known as critical-temperature (TC).The problem of superconductor research
It is to break through " temperature obstacle ", that is, finds high temperature superconducting materia.
Practical superconductor using NbTi, Nb3Sn as representative has been achieved with commercialization, is imaged in nuclear magnetic resonance human body
(NMRI), the multiple fields such as superconducting magnet and large-scale accelerator magnet obtain application；SQUID is applied as superconductor light current
Model plays important function in terms of weak electromagnetic signal measurement, and sensitivity is that the device of other any non-superconductings can not
Reach.But since the critical-temperature of Conventional cryogenic superconductor is too low, it is necessary in liquid helium (4.2K) system costly
It uses, thus seriously limits the development of low-temperature superconducting application.The appearance of high-temperature oxide superconductor breaches temperature wall
It builds, superconductor applications temperature is increased to liquid nitrogen (77K) warm area from liquid helium (4.2K).But it is influenced while often critical-temperature improves
Superconductor obtains other performances, is unfavorable for the raising of superconductor overall performance.
The content of the invention
The deficiency that superconductor comprehensive performance is short of when reaching higher critical temperatures in for the above-mentioned prior art, the present invention
Purpose be to provide a kind of new energy superconductor and preparation method thereof, make the superconductor comprehensive performance being prepared excellent
It is different.
Purpose technical solution is as follows to realize the present invention：
A kind of preparation method of new energy superconductor, includes the following steps：
S1：By Mg powder, lanthana, Se powder in mass ratio 1:3-5:2-4 is mixed, and is added in ball grinder, in 0.08-
Ball milling 1-2h in 0.16MPa argon atmospheres；
S2：Powder after ball milling in step S1 is put into S type plane moulds, then applies the pressure of 2-8MPa to mold
Power, pressurize 10-15min；
S3：Sample obtained by step S2 is put into vacuum sintering furnace to be sintered；Vacuum degree is maintained at below 3.5Pa；Heating
Program is：350-450 DEG C of insulation reaction 1-2h is warming up to 5-10 DEG C/min；650-750 is warming up to 10-15 DEG C/min of rate
DEG C insulation reaction 50-80min；850-950 DEG C of insulation reaction 1.5-2.5h is warming up to 15-20 DEG C/min of rate；With 20-30
DEG C/cooling velocity of min is down to room temperature, it is polished to can obtain the superconductive composite materials.
Preferably, Mg powder described in step S1, lanthana, the mass ratio of Se powder are 1:4:3；In 0.12MPa argon atmospheres
A diameter of 3-5mm of middle ball milling 1.5h, wherein stainless steel bead.
Preferably, the thickness of S types plane mould described in step S2 is 5-8mm, length 0.5-1cm.
Preferably, the thickness of the S types plane mould is 7mm, length 0.8cm；Apply the pressure of 6.5MPa, pressurize
12min.
Preferably, vacuum degree keeps 2.5-3.2MPa in step S3.
Preferably, temperature program is in step S3：420 DEG C of insulation reaction 1.5h are warming up to 8 DEG C/min；With rate 12
DEG C/min is warming up to 700 DEG C of insulation reaction 75min；880 DEG C of insulation reaction 2h are warming up to 18 DEG C/min of rate；With 25 DEG C/min
Cooling velocity be down to room temperature.
The composite superconductor that above-mentioned any one preparation method is prepared.
Compared with prior art, the present invention its advantage is：
A kind of preparation method of new energy superconductor of the present invention, based on Mg powder, lanthana and Se powder, and
By S type plane grinding tool compression mouldings, composite superconductor is made after being handled by temperature programming formula sintering process；Due to S types
On the one hand the use of mold and the combination of sintering process improve sintering efficiency, on the other hand also form new crystalline structure；
Therefore, the critical transition temperature of the superconductor is up to more than 60K, and critical current density under 10K null fields higher than 0.8 ×
107A/cm2。
Specific embodiment
The present invention is further illustrated with reference to embodiments.
Embodiment 1
S1：By Mg powder, lanthana, Se powder in mass ratio 1:3:2 mixing, add in ball grinder, the diameter of stainless steel bead
For 3mm, the ball milling 2h in 0.08MPa argon atmospheres；
S2：Powder after ball milling in step S1 is put into S type plane moulds, the thickness of S type plane moulds is 5mm, long
It spends for 0.5cm；Then the pressure of 8MPa, pressurize 10min are applied to mold；
S3：Sample obtained by step S2 is put into vacuum sintering furnace to be sintered；Vacuum degree is maintained at 3.5Pa；Temperature program
For：350 DEG C of insulation reaction 1h are warming up to 5 DEG C/min；650 DEG C of insulation reaction 50min are warming up to 15 DEG C/min of rate；With speed
15 DEG C/min of rate is warming up to 850 DEG C of insulation reaction 1.5h；Room temperature is down to the cooling velocity of 20 DEG C/min, it is polished to obtain
To the superconductive composite materials.
Embodiment 2
S1：By Mg powder, lanthana, Se powder in mass ratio 1:5:4 mixing, add in ball grinder, the diameter of stainless steel bead
For 5mm, the ball milling 1h in 0.16MPa argon atmospheres；
S2：Powder after ball milling in step S1 is put into S type plane moulds, the thickness of S type plane moulds is 8mm, long
It spends for 1cm；Then the pressure of 2MPa, pressurize 15min are applied to mold；
S3：Sample obtained by step S2 is put into vacuum sintering furnace to be sintered；Vacuum degree is maintained at 1.5Pa；Temperature program
For：450 DEG C of insulation reaction 2h are warming up to 10 DEG C/min；750 DEG C of insulation reaction 80min are warming up to 10 DEG C/min of rate；With
20 DEG C/min of rate is warming up to 950 DEG C of insulation reaction 2.5h；Room temperature is down to the cooling velocity of 30 DEG C/min, it is polished
Obtain the superconductive composite materials.
Embodiment 3
S1：By Mg powder, lanthana, Se powder in mass ratio 1:3:4 mixing, add in ball grinder, the diameter of stainless steel bead
For 5mm, the ball milling 1.5h in 0.12MPa argon atmospheres；
S2：Powder after ball milling in step S1 is put into S type plane moulds, the thickness of S type plane moulds is 7mm, long
It spends for 0.8cm；Then the pressure of 5MPa, pressurize 12min are applied to mold；
S3：Sample obtained by step S2 is put into vacuum sintering furnace to be sintered；Vacuum degree is maintained at 2.5Pa；Temperature program
For：380 DEG C of insulation reaction 1.5h are warming up to 7 DEG C/min；680 DEG C of insulation reaction 65min are warming up to 12 DEG C/min of rate；With
18 DEG C/min of rate is warming up to 900 DEG C of insulation reaction 2h；Room temperature is down to the cooling velocity of 22 DEG C/min, it is polished to obtain
To the superconductive composite materials.
Embodiment 4
S1：By Mg powder, lanthana, Se powder in mass ratio 1:5:2 mixing, add in ball grinder, the diameter of stainless steel bead
For 3mm, the ball milling 2h in 0.15MPa argon atmospheres；
S2：Powder after ball milling in step S1 is put into S type plane moulds, the thickness of S type plane moulds is 5.5mm,
Length is 0.75cm；Then the pressure of 3MPa, pressurize 15min are applied to mold；
S3：Sample obtained by step S2 is put into vacuum sintering furnace to be sintered；Vacuum degree is maintained at below 3.2Pa；Heating
Program is：420 DEG C of insulation reaction 2h are warming up to 9 DEG C/min；700 DEG C of insulation reaction 75min are warming up to 15 DEG C/min of rate；
860 DEG C of insulation reaction 1.8h are warming up to 16 DEG C/min of rate；Room temperature is down to the cooling velocity of 28 DEG C/min, it is polished to be
It can obtain the superconductive composite materials.
Embodiment 5
S1：By Mg powder, lanthana, Se powder in mass ratio 1:4:3 mixing, add in ball grinder, the diameter of stainless steel bead
For 4mm, the ball milling 1.5h in 0.12MPa argon atmospheres；
S2：Powder after ball milling in step S1 is put into S type plane moulds, the thickness of S type plane moulds is 6.5mm,
Length is 0.8cm；Then the pressure of 6MPa, pressurize 13min are applied to mold；
S3：Sample obtained by step S2 is put into vacuum sintering furnace to be sintered；Vacuum degree is maintained at 2.8Pa；Temperature program
For：420 DEG C of insulation reaction 1.5h are warming up to 8 DEG C/min；700 DEG C of insulation reaction 75min are warming up to 12 DEG C/min of rate；With
18 DEG C/min of rate is warming up to 880 DEG C of insulation reaction 2h；Room temperature is down to the cooling velocity of 25 DEG C/min, it is polished to obtain
To the superconductive composite materials.
Superconductive composite materials performance obtained by above-mentioned each embodiment is as follows：
| Experiment | Critical transition temperature (K) | Critical current density (under 10K null fields) |
| Embodiment 1 | 60 | 0.8×107 |
| Embodiment 2 | 62 | 3.1×107 |
| Embodiment 3 | 63.5 | 5.4×107 |
| Embodiment 4 | 64 | 7.3×107 |
| Embodiment 5 | 67 | 8.7×107 |
The invention is not restricted to embodiment here, those skilled in the art's announcement according to the present invention does not depart from the present invention
The improvement and modification that scope is made all should be within protection scope of the present invention.
Claims (7)
1. a kind of preparation method of new energy superconductor, which is characterized in that include the following steps：
S1：By Mg powder, lanthana, Se powder in mass ratio 1:3-5:2-4 is mixed, and is added in ball grinder, in 0.08-0.16MPa argons
Atmosphere encloses middle ball milling 1-2h；
S2：Powder after ball milling in step S1 is put into S type plane moulds, then applies the pressure of 2-8MPa to mold, is protected
Press 10-15min；
S3：Sample obtained by step S2 is put into vacuum sintering furnace to be sintered；Vacuum degree is maintained at below 3.5Pa；Temperature program
For：
350-450 DEG C of insulation reaction 1-2h is warming up to 5-10 DEG C/min；650-750 DEG C is warming up to 10-15 DEG C/min of rate
Insulation reaction 50-80min；850-950 DEG C of insulation reaction 1.5-2.5h is warming up to 15-20 DEG C/min of rate；With 20-30 DEG C/
The cooling velocity of min is down to room temperature, polished to can obtain the superconducting energy composite material.
A kind of 2. preparation method of new energy superconductor according to claim 1, which is characterized in that institute in step S1
It is 1 to state Mg powder, lanthana, the mass ratio of Se powder:4:3；The ball milling 1.5h in 0.12MPa argon atmospheres, wherein stainless steel bead
A diameter of 3-5mm.
A kind of 3. preparation method of new energy superconductor according to claim 1, which is characterized in that institute in step S2
The thickness for stating S type plane moulds is 5-8mm, length 0.5-1cm.
4. the preparation method of a kind of new energy superconductor according to claim 3, which is characterized in that the S types are put down
The thickness of face mould tool is 7mm, length 0.8cm；Apply the pressure of 6.5MPa, pressurize 12min.
5. the preparation method of a kind of new energy superconductor according to claim 3, which is characterized in that true in step S3
Reciprocal of duty cycle keeps 2.5-3.2MPa.
6. the preparation method of a kind of new energy superconductor according to claim 3, which is characterized in that risen in step S3
Warm program is：420 DEG C of insulation reaction 1.5h are warming up to 8 DEG C/min；700 DEG C of insulation reactions are warming up to 12 DEG C/min of rate
75min；880 DEG C of insulation reaction 2h are warming up to 18 DEG C/min of rate；Room temperature is down to the cooling velocity of 25 DEG C/min.
7. the composite superconductor being prepared according to any one preparation method of claim 1-6.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN88101032A (en) * | 1987-02-27 | 1988-09-21 | 株式会社日立制作所 | Superconductive device |
| US20040058823A1 (en) * | 1999-02-27 | 2004-03-25 | Nexans Superconductors Gmbh. | Method for the heat treatment of a superconductor material having a high remanent induction, a heat treated superconductor material and the use thereof |
| CN102082010A (en) * | 2010-12-28 | 2011-06-01 | 中国科学院电工研究所 | Method for preparing iron-based superconductor |
| 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 |
| CN102503424A (en) * | 2011-11-11 | 2012-06-20 | 天津大学 | Method for increasing sintering efficiency of FeSe superconducting material |
| CN105355357A (en) * | 2015-11-17 | 2016-02-24 | 中国科学院电工研究所 | Iron-based compound superconducting joint and preparation method thereof |
| CN105405531A (en) * | 2015-12-18 | 2016-03-16 | 常熟市东方特种金属材料厂 | Preparation method of novel superconducting material |
| CN107112411A (en) * | 2014-10-27 | 2017-08-29 | 量子设计材料有限公司 | High-temperature superconductor |
-
2017
- 2017-12-21 CN CN201711389987.0A patent/CN108083799A/en not_active Withdrawn
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN88101032A (en) * | 1987-02-27 | 1988-09-21 | 株式会社日立制作所 | Superconductive device |
| US20040058823A1 (en) * | 1999-02-27 | 2004-03-25 | Nexans Superconductors Gmbh. | Method for the heat treatment of a superconductor material having a high remanent induction, a heat treated superconductor material and the use thereof |
| CN102082010A (en) * | 2010-12-28 | 2011-06-01 | 中国科学院电工研究所 | Method for preparing iron-based superconductor |
| 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 |
| CN102503424A (en) * | 2011-11-11 | 2012-06-20 | 天津大学 | Method for increasing sintering efficiency of FeSe superconducting material |
| CN107112411A (en) * | 2014-10-27 | 2017-08-29 | 量子设计材料有限公司 | High-temperature superconductor |
| CN105355357A (en) * | 2015-11-17 | 2016-02-24 | 中国科学院电工研究所 | Iron-based compound superconducting joint and preparation method thereof |
| CN105405531A (en) * | 2015-12-18 | 2016-03-16 | 常熟市东方特种金属材料厂 | Preparation method of novel superconducting material |
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