CN103567407B - Preparation method of Nb3Al superconducting material - Google Patents
Preparation method of Nb3Al superconducting material Download PDFInfo
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- CN103567407B CN103567407B CN201310512002.4A CN201310512002A CN103567407B CN 103567407 B CN103567407 B CN 103567407B CN 201310512002 A CN201310512002 A CN 201310512002A CN 103567407 B CN103567407 B CN 103567407B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000463 material Substances 0.000 title abstract description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 29
- 239000006104 solid solution Substances 0.000 claims abstract description 22
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052802 copper Inorganic materials 0.000 claims abstract description 19
- 239000010949 copper Substances 0.000 claims abstract description 19
- 229910052786 argon Inorganic materials 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000005266 casting Methods 0.000 claims abstract description 8
- 230000006698 induction Effects 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 239000002887 superconductor Substances 0.000 claims description 23
- 239000007791 liquid phase Substances 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 9
- 238000005516 engineering process Methods 0.000 claims description 8
- 229910052582 BN Inorganic materials 0.000 claims description 7
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 7
- 230000014759 maintenance of location Effects 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 230000007704 transition Effects 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 3
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 238000005096 rolling process Methods 0.000 abstract 1
- 238000009792 diffusion process Methods 0.000 description 3
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
Classifications
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E40/00—Technologies for an efficient electrical power generation, transmission or distribution
- Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment
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- Superconductors And Manufacturing Methods Therefor (AREA)
Abstract
The invention relates to a preparation method of an Nb3Al superconducting material. The preparation method comprises the following steps: heating Nb powder and Al powder by using a belt throwing machine and through an induction coil; after completely melting, cooling to form a solid-liquid coexistence body; introducing high-purity argon and jetting melt in a water-cooling copper casting mould or a rolling wheel which rotates at high speed to form a supersaturated solid solution; performing low-temperature heat treatment to obtain the Nb3Al superconducting material. According to the preparation method of the Nb3Al superconducting material, the problems that the Al content is slightly low in the process of preparing the Nb3Al superconducting material and crystal grains grow in the high-temperature heat treatment process in the prior art are overcome; the Al content of the obtained Nb3Al superconducting material is close to 25%, the crystal grains are small, and the superconducting transition temperature and the critical current density can reach ideal values.
Description
Technical field
The invention belongs to superconductor preparation method technical field, relate to a kind of Nb
3the preparation method of Al superconductor.
Background technology
Compared to NbTi and Nb
3sn superconductor, the intermetallic compound Nb of A15 type structure
3al has higher critical magnetic field and critical current density, Nb under High-Field
3the stress and strain relation research of Al shows, this material has extraordinary anti-adaptability to changes, has good radiation sensitivity simultaneously, is the ideal material of the High-Field application such as following large-scale fusion reactor, high-energy particle accelerator, NMR.
Because Nb/Al diffusion length is very little, the Nb prepared by low temperature diffusion method
3al content in Al superconductor is on the low side in 25%, make superconducting transition temperature lower than ideal value, and high-temperature processing method easily causes grain growth, reduces the critical current density of material, seriously constrains the application of this material.
Summary of the invention
The object of the present invention is to provide a kind of Nb
3the preparation method of Al superconductor, solves the Nb that prior art exists
3the problem of on the low side, the grain growth of Al content in Al superconductor.
Technical scheme of the present invention is, Nb
3the preparation method of Al superconductor, first utilization is got rid of band machine and Nb powder and Al powder is heated by induction coil, after fusing, cooling forms solid-liquid body completely, then pass into high-purity argon gas melt jet is intake in cold Copper casting mould or High Rotation Speed running roller on, form supersaturated solid solution, after Low Temperature Heat Treatment, obtain Nb
3al superconductor.
Feature of the present invention is also, specifically comprises the steps:
The first step, gets Nb powder and the mixing of Al powder, is placed in boron nitride crucible, installs a water-cooled copper mold at crucible bottom, then will get rid of band machine vacuum chamber and vacuumize, then be filled with argon gas to normal pressure to cavity;
Second step, switch on power, heat induced coil, Nb and Al is made to form liquid phase, then lower the temperature, form solid-liquid phase, be then rapidly to crucible cavity and be filled with high-purity argon, utilize pressure to be sprayed in the cold Copper casting mould of water inlet by crucible bottom nozzle by melt, obtain supersaturated solid solution Nb (Al) ss;
3rd step, is pressed into bulk with mould after being pulverized by supersaturated solid solution Nb (Al) ss that second step obtains, is heat-treated by described bulk.
In the above-mentioned first step, the purity of Nb powder and Al powder is 99.99%; According to the ratio mixing that Nb and Al atomic ratio is 3:1; Get rid of band machine vacuum chamber and be evacuated down to 10
-3~ 10
-5pa.
Further, in the above-mentioned first step, water-cooled copper mold also can be running roller, and roller diameter is 200 ~ 250mm, roller surface wire rate is 30 ~ 50m/s, by melt jet is formed supersaturated solid solution Nb (Al) ss band to the roller surface of High Rotation Speed with the form of getting rid of band;
In above-mentioned second step, induction coil heating-up temperature is 2450 DEG C, keeps 20min to make Nb and Al form liquid phase, is then cooled to 1900 DEG C ~ 2040 DEG C with the speed of 50 DEG C/h, and keep 30min to form solid-liquid phase.
In above-mentioned 3rd step, Technology for Heating Processing is: sintering temperature is 800 ~ 850 DEG C, and temperature retention time 2-10h sinters and carries out under vacuum or ar gas environment, obtains Nb
3al superconductor.
The present invention has following beneficial effect:
1, the present invention be by Nb and Al of liquid state lower the temperature formed solid-liquid mutually after, supersaturated solid solution Nb (Al) ss can be formed by rapid quenching, in follow-up low temperature heat treatment by Al separate out directly formation needed for Nb
3al superconducting phase, avoids in the problem of growing up of crystal grain in conventional high temperature heat treatment process and low temperature diffusion method preparation process and reacts insufficient problem causing Al content on the low side.Gained Nb
3al superconductor Al content is close to 25%, and crystal grain is little, and superconducting transition temperature and critical current density all can reach ideal value.
2, preparation method of the present invention is simple, is easy to realize, and cost is low.
Accompanying drawing explanation
Fig. 1 is that embodiment of the present invention 1-3 prepares vacuum involved by supersaturated solid solution Nb (Al) ss bulk and gets rid of the structural representation of band machine;
Fig. 2 is that embodiment of the present invention 4-5 prepares vacuum involved by supersaturated solid solution Nb (Al) ss band and gets rid of the structural representation of band machine.
In figure: 1. vacuum chamber, 2. crucible, 3. power supply, 4. water-cooled copper mold, 4-1 running roller, 5. air inlet pipe, 6. blast pipe, 7. bipass, 8. molecular pump, 9. mechanical pump.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in detail.
The band machine that gets rid of holonomic system involved in the present invention is made up of small size vacuum chamber (comprising crucible, induction coil, running roller or mold), frame, sufficiently high vacuum-pumping system and radio-frequency signal generator.Operation principle is: after being melted by eddy-current heating by material in crucible, passes into inert gas and utilizes pressure melt to be sprayed the roller surface of the cold Copper casting mould of water inlet or High Rotation Speed by crucible bottom nozzle, realize rapid quenching.
Embodiment 1
The first step, get purity be 99.99% Nb powder and purity be 99.99% Al powder, according to Nb and Al atomic ratio be 3:1 ratio mixing, take the powder 5g mixed and be placed in boron nitride crucible, at crucible bottom, a water-cooled copper mold is installed, then will gets rid of band machine vacuum chamber and be evacuated down to 10
-3pa, then be filled with argon gas to normal pressure to cavity.Get rid of band machine see Fig. 1, comprise vacuum chamber 1, have crucible 2 and water-cooled copper mold 4 in vacuum chamber 1, crucible 2 is with power supply 3, and vacuum chamber 1 is connected with air inlet pipe 5, blast pipe 6, bipass 7, and bipass 7 is connected with molecular pump 8, mechanical pump 9.
Second step, switch on power, Perceived control answers coil heats temperature to be 2450 DEG C, 20min is kept to make Nb and Al form liquid phase, then be cooled to 1900 DEG C with the speed of 50 DEG C/h, and keep 30min to form solid-liquid phase, be then rapidly to crucible cavity and be filled with high-purity argon, utilize pressure to be sprayed in the cold Copper casting mould of water inlet by crucible bottom nozzle by melt, obtain supersaturated solid solution Nb (Al) ss;
3rd step, is pressed into bulk with mould after being pulverized by supersaturated solid solution Nb (Al) ss that second step obtains, is heat-treated by described bulk, Technology for Heating Processing is: sintering temperature is 830 DEG C, temperature retention time 10h, sinters and carries out under ar gas environment, obtains Nb
3al superconductor.
The sample got in the present embodiment is measured, and superconducting transition temperature reaches 17.8K, and critical current density reaches 700A/mm
2(16T, 4.2K).
Embodiment 2
The first step, get purity be 99.99% Nb powder and purity be 99.99% Al powder, according to Nb and Al atomic ratio be 3:1 ratio mixing, take the powder 2g mixed and be placed in boron nitride crucible, at crucible bottom, a water-cooled copper mold is installed, then will gets rid of band machine vacuum chamber and be evacuated down to 10
-4pa, then be filled with argon gas to normal pressure to cavity, get rid of band machine see Fig. 1;
Second step, switch on power, Perceived control answers coil heats temperature to be 2450 DEG C, 20min is kept to make Nb and Al form liquid phase, then be cooled to 1950 DEG C with the speed of 50 DEG C/h, and keep 30min to form solid-liquid phase, be then rapidly to crucible cavity and be filled with high-purity argon, utilize pressure to spray in mold by melt by crucible bottom nozzle, obtain supersaturated solid solution Nb (Al) ss;
3rd step, is pressed into bulk with mould after being pulverized by supersaturated solid solution Nb (Al) ss of above-mentioned acquisition, is heat-treated by described bulk, Technology for Heating Processing is: sintering temperature is 850 DEG C, temperature retention time 6h, sintering carries out under vacuum conditions, obtains Nb
3al superconductor.
The sample got in the present embodiment is measured, and superconducting transition temperature reaches 18.1K, and critical current density reaches 730A/mm
2(16T, 4.2K).
Embodiment 3
The first step, get purity be 99.99% Nb powder and purity be 99.99% Al powder, according to Nb and Al atomic ratio be 3:1 ratio mixing, take the powder 8g mixed and be placed in boron nitride crucible, at crucible bottom, a water-cooled copper mold is installed, then will gets rid of band machine vacuum chamber and be evacuated down to 10
-5pa, then be filled with argon gas to normal pressure to cavity, get rid of band machine see Fig. 1;
Second step, switch on power, Perceived control answers coil heats temperature to be 2450 DEG C, 20min is kept to make Nb and Al form liquid phase, then be cooled to 2040 DEG C with the speed of 50 DEG C/h, and keep 30min to form solid-liquid phase, be then rapidly to crucible cavity and be filled with high-purity argon, utilize pressure to be sprayed in the cold Copper casting mould of water inlet by crucible bottom nozzle by melt, obtain supersaturated solid solution Nb (Al) ss;
3rd step, is pressed into bulk with mould after being pulverized by supersaturated solid solution Nb (Al) ss of above-mentioned acquisition, is heat-treated by described bulk, Technology for Heating Processing is: sintering temperature is 820 DEG C, temperature retention time 2h, sinters and carries out under ar gas environment, obtains Nb3Al superconductor.
The sample got in the present embodiment is measured, and superconducting transition temperature reaches 17.6K, and critical current density reaches 680A/mm
2(16T, 4.2K).
Embodiment 4
The first step, get purity be 99.99% Nb powder and purity be 99.99% Al powder, according to the ratio mixing that Nb and Al atomic ratio is 3:1, take the powder 8g mixed and be placed in boron nitride crucible, the copper running roller of a diameter 230mm is installed at crucible bottom, then will gets rid of band machine vacuum chamber and be evacuated down to 10
-5pa, then be filled with argon gas to normal pressure to cavity, get rid of band machine see Fig. 2, comprise vacuum chamber 1, have crucible 2 and running roller 4-1 in vacuum chamber 1, crucible 2 is with power supply 3, vacuum chamber 1 is connected with air inlet pipe 5, blast pipe 6, bipass 7, and bipass 7 is connected with molecular pump 8, mechanical pump 9.
Second step, switch on power, Perceived control answers coil heats temperature to be 2450 DEG C, 20min is kept to make Nb and Al form liquid phase, then be cooled to 2040 DEG C with the speed of 50 DEG C/h, and keep 30min to form solid-liquid phase, be then rapidly to crucible cavity and be filled with high-purity argon, utilize pressure to be ejected into the roller surface of the wire rate High Rotation Speed of 30 meter per seconds by melt by crucible bottom nozzle, obtain supersaturated solid solution Nb (Al) ss band;
3rd step, heat-treated by supersaturated solid solution Nb (Al) the ss band of above-mentioned acquisition, Technology for Heating Processing is: sintering temperature is 800 DEG C, and temperature retention time 2h sinters and carries out under ar gas environment, obtains Nb
3al superconductor.
The sample got in the present embodiment is measured, and superconducting transition temperature reaches 17.3K, and critical current density reaches 650A/mm
2(16T, 4.2K).
Embodiment 5
The first step, get purity be 99.99% Nb powder and purity be 99.99% Al powder, according to the ratio mixing that Nb and Al atomic ratio is 3:1, take the powder 10g mixed and be placed in boron nitride crucible, the copper running roller of a diameter 250mm is installed at crucible bottom, then will gets rid of band machine vacuum chamber and be evacuated down to 10
-4pa, then be filled with argon gas to normal pressure to cavity, get rid of band machine see Fig. 2;
Second step, switch on power, Perceived control answers coil heats temperature to be 2450 DEG C, 20min is kept to make Nb and Al form liquid phase, then be cooled to 1950 DEG C with the speed of 50 DEG C/h, and keep 30min to form solid-liquid phase, be then rapidly to crucible cavity and be filled with high-purity argon, utilize pressure to be ejected into the roller surface of the wire rate High Rotation Speed of 50 meter per seconds by melt by crucible bottom nozzle, obtain supersaturated solid solution Nb (Al) ss band;
3rd step, heat-treated by supersaturated solid solution Nb (Al) the ss band of above-mentioned acquisition, Technology for Heating Processing is: sintering temperature is 850 DEG C, temperature retention time 6h, and sintering carries out under vacuum conditions, obtains Nb3Al superconductor.
The sample got in the present embodiment is measured, and superconducting transition temperature reaches 17.9K, and critical current density reaches 720A/mm
2(16T, 4.2K).
Claims (5)
1.Nb
3the preparation method of Al superconductor, it is characterized in that: first utilization is got rid of band machine and Nb powder and Al powder heated by induction coil, after fusing, cooling forms solid-liquid body completely, then pass into high-purity argon gas melt jet is intake in cold Copper casting mould or High Rotation Speed running roller on, form supersaturated solid solution, after Low Temperature Heat Treatment, obtain Nb
3al superconductor, is specially:
The first step, gets Nb powder and the mixing of Al powder, is placed in boron nitride crucible, installs a water-cooled copper mold at crucible bottom, then will get rid of band machine vacuum chamber and vacuumize, then be filled with argon gas to normal pressure to cavity;
Second step, switch on power, heat induced coil, Nb and Al is made to form liquid phase, then lower the temperature, form solid-liquid phase, be then rapidly to crucible cavity and be filled with high-purity argon, utilize pressure to be sprayed in the cold Copper casting mould of water inlet by crucible bottom nozzle by melt, obtain supersaturated solid solution Nb (Al) ss;
3rd step, is pressed into bulk with mould after being pulverized by supersaturated solid solution Nb (Al) ss that second step obtains, is heat-treated by described bulk.
2. Nb as claimed in claim 1
3the preparation method of Al superconductor, is characterized in that: in the described first step, and the purity of Nb powder and Al powder is 99.99%; According to the ratio mixing that Nb and Al atomic ratio is 3:1; Get rid of band machine vacuum chamber and be evacuated down to 10
-3~ 10
-5pa.
3. Nb as claimed in claim 1 or 2
3the preparation method of Al superconductor, it is characterized in that: in the described first step, water-cooled copper mold replaces with running roller, roller diameter is 200 ~ 250mm, roller surface wire rate is 30 ~ 50m/s, by melt jet is formed supersaturated solid solution Nb (Al) ss band to the roller surface of High Rotation Speed with the form of getting rid of band.
4. Nb as claimed in claim 1
3the preparation method of Al superconductor, it is characterized in that: in described second step, induction coil heating-up temperature is 2450 DEG C, keeps 20min to make Nb and Al form liquid phase, then be cooled to 1900 DEG C ~ 2040 DEG C with the speed of 50 DEG C/h, and keep 30min to form solid-liquid phase.
5. Nb as claimed in claim 1
3the preparation method of Al superconductor, is characterized in that: in described 3rd step, Technology for Heating Processing is: sintering temperature is 800 DEG C ~ 850 DEG C, and temperature retention time 2-10h, sinters and carry out under vacuum or ar gas environment, obtains Nb
3al superconductor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310512002.4A CN103567407B (en) | 2013-10-25 | 2013-10-25 | Preparation method of Nb3Al superconducting material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310512002.4A CN103567407B (en) | 2013-10-25 | 2013-10-25 | Preparation method of Nb3Al superconducting material |
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| Publication Number | Publication Date |
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| CN103567407A CN103567407A (en) | 2014-02-12 |
| CN103567407B true CN103567407B (en) | 2015-05-20 |
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Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004045794A1 (en) * | 2002-11-18 | 2004-06-03 | Cbmm Asia Co.,Ltd. | Nb-Al ALLOY POWDER AND METHOD FOR ELECTROLYTIC CAPACITOR AND METHOD FOR PREPARATION THEREOF, AND ELECTROLYTIC CAPACITOR |
| CN101967591B (en) * | 2010-11-09 | 2012-08-08 | 上海大学 | Method for preparing Nb3Al superconducting material by mechanical alloying |
| CN103093898B (en) * | 2013-02-25 | 2015-10-28 | 西部超导材料科技股份有限公司 | High-energy ball milling method is adopted to prepare Nb 3the method of Al superconducting wire |
| CN103337333B (en) * | 2013-05-27 | 2015-10-28 | 西部超导材料科技股份有限公司 | Nb 3al superconducting joint and preparation method thereof |
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