CN101386529B - Method for preparing Fe-base compound superconductor - Google Patents
Method for preparing Fe-base compound superconductor Download PDFInfo
- Publication number
- CN101386529B CN101386529B CN200810224178.9A CN200810224178A CN101386529B CN 101386529 B CN101386529 B CN 101386529B CN 200810224178 A CN200810224178 A CN 200810224178A CN 101386529 B CN101386529 B CN 101386529B
- Authority
- CN
- China
- Prior art keywords
- powder
- pipe
- room temperature
- make
- metal tube
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
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
Abstract
The invention provides a method for preparing an iron-based compound superconductor, which comprises the following steps: (1) evenly mixing raw material powder which is prepared according to a chemical formula of ReMPnO1-xFx, ReM1-xTmxPnO or Ae1-xAxM2Pn2, and filling the raw material powder into a metal tube, tamping the powder completely, and closing two ends of the metal tube; (2) swaging, drawing and rolling the metal tube according to the pass deformation of between 5 and 20 percent; and (3) placing the metal tube which is processed through step 2 in a high-temperature heating furnace, vacuumizing until the pressure is between 10<-2> and 10<-5> Pa at room temperature, introducing argon into the metal tube, insulating the metal tube for 5 to 100 hours at a temperature of between 700 and 1,500 DEG C, and peeling the metal sleeve to obtain the iron-based compound novel superconductor after the high-temperature furnace is cooled to room temperature. Compared with the prior method for preparing quartz glass in two steps, the method has the advantages of effective bursting prevention, safety and reliability, one-step completion for sintering process, simple process and high production efficiency; and the prepared iron-based compound has high density and excellent superconductive performance.
Description
Technical field
The present invention relates to a kind of preparation method of Fe-base compound superconductor.
Background technology
Fe-base compound superconductor is a kind of compound superconductive of recently finding.That Japanese Kamihara Y.et al. report has been found new high-temperature superconductor LaO at first
1-xf
xfeAs (x=0.05-0.12), its transition temperature is 26K[Iron-based layered superconductor LaO
1-xf
xfeAs (x=0.05-0.12) with T
c=26K.J.Am.Chem.Sco.130,3296-3297 (2008)], use subsequently other rare earth elements (Ce, Pr, Nd, Sm, Gd) to replace La, its the highest superconducting transition temperature has reached 55K, this is the novel high temperature superconducting materia that copper removal oxygen compound high temperature superconducting materia the first critical transition temperature in addition surpasses 40K, and this performance for researching high-temperature superconductor and Superconducting Mechanism provide more chance.In addition, theoretical calculate show the upper critical field of Fe-base compound superconductor and irreversible all very high, and there is larger coherence length, these fully show that Fe-base compound superconductor has good application prospect, so the preparation of Fe-base compound superconductor is subject to international extensive concern.Preparation about Fe-base compound superconductor is mainly that legal system is standby in two steps for quartz glass at present, process complexity and cost are higher, what is more important is owing to containing poisonous element, and quartz ampoule easily explosion in the process of heating, these all exist serious potential safety hazard.
Summary of the invention
The object of the invention is to overcome the shortcoming of prior art adopting quartz glass pipe, propose a kind of preparation method of new Fe-base compound high-temperature superconductor.
The present invention selects metal tube, comprises simple metal pipe, composite metal pipe or compo pipe.Making material chosen from Fe, copper, mild steel, stainless steel, chromium, vanadium, manganese, titanium, zirconium, molybdenum, nickel, niobium, tungsten, hafnium or the tantalum of metal tube, composite metal pipe or compo pipe.
Concrete preparation process of the present invention is:
(1) will be according to ReMPnO
1-xf
xor ReM
1-xtm
xpnO or Ae
1-xa
xm
2pn
2in the material powder of a kind of chemical formula preparation mix after, pack metal tube into, fully compacting, the then two ends of closed metal pipe; Wherein said chemical formula ReMPnO
1-xf
x, ReM
1-xtm
xpnO or Ae
1-xa
xm
2pn
2: Re is one or more elements that are selected from La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y; M is a kind of element being selected from Fe, Co, Ni, Ru; Tm is a kind of element in Co, Ni, Mn, Zn; Pn is a kind of element in As, P, Sb; Ae is a kind of element in Ca, Sr, Ba, Eu; A is a kind of element in Li, Na, K, Rb, Cs; X=0-0.50;
(2) by metal tube according to certain pass deformation (5%-20%) swage, the operation processing such as drawing, rolling;
(3) metal tube obtaining through step 2 machining is placed in to high-temperature heater, under room temperature, is evacuated to 10
-2-10
-5handkerchief, is filled with argon gas afterwards, then at the temperature of 700-1500 ℃, is incubated 5-100 hour, finally treats that high temperature furnace is cooled to room temperature, and strip off metal jacket obtains Fe-base compound new superconductive body.
Preparing Fe-base compound new superconductive body with the quartz glass method of fractional steps conventionally adopting now compares, advantage of the present invention is, first adopt metal tube to prepare superconductor, the fusing point of metal is higher, can at higher temperature, carry out solid phase reaction, thus the softening problem while avoiding the long-time high-temperature heating of quartz glass tube.Secondly, metal tube mostly has good processing characteristics, is conducive to initial raw meal is fully broken, compacting in the course of processing, makes the final Fe-base compound grain refinement forming, the crystal grain connectivity of efficient hardening Fe-base compound, thus the density of superconductor improved.Again, novel Fe-base compound superconductor comprises poisonous phosphorus family element, and the general evaporation point of phosphorus family element is very low, if adopting quartz glass control for time when the high temperature sintering because vapour pressure in pipe is very high, easily there is glass tube Decrepitation Phenomena, cause and wound and the consequence such as toxic gas leakage.And adopt metal tube can avoid above problem completely, safe and reliable.In addition, the present invention can realize the disposable Fast Sintering of Fe-base compound superconductor, convenient and simple and effective, has avoided the problems such as the preparation time that generally the step sintering method of employing is brought is at present long, and cost is higher.
Embodiment:
The concrete preparation process of the present invention is:
(1) will be according to ReMPnO
1-xf
xor ReM
1-xtm
xpnO or Ae
1-xa
xm
2pn
2in the material powder of a kind of chemical formula preparation mix after, pack metal tube into, fully compacting, the then two ends of closed metal pipe; Wherein said chemical formula ReMPnO
1-xf
x, ReM
1-xtm
xpnO or Ae
1-xa
xm
2pn
2: Re is one or more elements that are selected from La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y; M is a kind of element being selected from Fe, Co, Ni, Ru; Tm is a kind of element in Co, Ni, Mn, Zn; Pn is a kind of element in As, P, Sb; Ae is a kind of element in Ca, Sr, Ba, Eu; A is a kind of element in Li, Na, K, Rb, Cs; X=0-0.50;
(2) by metal tube according to certain pass deformation (5%-20%) swage, the operation processing such as drawing, rolling;
(3) metal tube obtaining through step 2 machining is placed in to high-temperature heater, under room temperature, is evacuated to 10
-2-10
-5handkerchief, is filled with argon gas afterwards, then at the temperature of 700-1500 ℃, is incubated 5-100 hour, finally treats that high temperature furnace is cooled to room temperature, and strip off metal jacket obtains Fe-base compound new superconductive body.
Embodiment 1
First according to chemical formula LaO
0.9f
0.1shown in FeAs, weigh La powder 2.35g, Fe powder 0.39g, Fe
2o
3powder 0.84g, LaF
3powder 0.11g, As powder 1.31g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long iron pipe of 10cm into iron pipe internal diameter 5mm, external diameter 8mm, makes powder in iron pipe, reach substantial, tight, then seals iron pipe two ends.Then the iron pipe that this is equipped with to mixed-powder is swaged to 4mm by 8% pass deformation.Iron pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, wait to reach 10
-2after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1200 ℃ of insulations 40 hours, finally with annealing furnace, be cooled to room temperature, just make the LaO that superconducting transition temperature is 26K
0.9f
0.1feAs superconductor.
Embodiment 2
First according to chemical formula Eu
0.7na
0.3fe
2as
2shown in weigh Eu powder 0.71g, Fe powder 0.74g, As powder 1.00g and Na fritter 0.05g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long niobium pipe of 5cm, bore 10mm, external diameter 12mm, makes powder in niobium pipe, reach substantial, tight, then seals niobium pipe two ends.Then the niobium pipe that this is equipped with to mixed-powder is drawn to 6mm by 8% pass deformation, and the niobium pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then slowly warming up to 850 ℃ of insulations 35 hours, finally with stove, be cooled to room temperature, just make the Eu that transition temperature is 35K
0.7na
0.3fe
2as
2superconductor.
Embodiment 3
First according to weighing Ce powder 2.77g shown in chemical formula CeOFeAs, Fe powder 0.51g, Fe
2o
3powder 0.93g, As powder 1.56g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long stainless steel tube of 6cm into bore 8mm, external diameter 12mm, make powder in stainless steel tube, reach substantial, tight, then seal stainless steel tube two ends.Then the stainless steel tube that this is equipped with to mixed-powder is swaged to 3mm by 5% pass deformation, and the stainless steel tube after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-4after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1150 ℃ of insulations 50 hours, finally with stove, be cooled to room temperature, just make CeOFeAs superconductor.
Embodiment 4
First according to chemical formula Ba
0.5k
0.5fe
2as
2shown in weigh Ba powder 1.28g, Fe powder 2.08g, As powder 2.78g and K fritter 0.36g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long zirconium pipe of 5cm, bore 10mm, external diameter 12mm, makes powder in zirconium pipe, reach substantial, tight, then seals zirconium pipe two ends.Then the zirconium pipe that this is equipped with to mixed-powder is swaged to 6mm by 10% pass deformation, and the zirconium pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-5after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then slowly warming up to 850 ℃ of insulations 35 hours, finally with stove, be cooled to room temperature, just make the Ba that transition temperature is 38K
0.5k
0.5fe
2as
2superconductor.
Embodiment 5
First according to chemical formula SmO
0.7f
0.3shown in FeAs, weigh Sm powder 5.45g, Fe powder 1.20g, Fe
2o
3powder 1.50g, SmF
3powder 0.83g, As powder 3.02g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long nickel pipe of 8cm into bore 16mm, external diameter 20mm, makes powder in nickel pipe, reach substantial, tight, then Nickel Sealing pipe two ends.Then the nickel pipe that this is equipped with to mixed-powder is swaged to 5mm by 20% pass deformation, and the nickel pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1160 ℃ of insulations 40 hours, finally with stove, be cooled to room temperature, just make SmO
0.7f
0.3feAs superconductor, superconducting transition temperature is not less than 50K after measured, and upper critical field is up to 120T (T=0K).
Embodiment 6
First according to chemical formula NdO
0.89f
0.11shown in NiAs, weigh Nd powder 1.91g, Ni powder 0.31g, NiO powder 0.65g, NdF
3powder 0.10g, As powder 1.03g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long niobium zirconium alloy pipe of 10cm into bore 3mm, external diameter 5mm, make powder in nb-zr tube compo pipe, reach substantial, tight, then seal nb-zr tube two ends.Then the nb-zr tube compo pipe that this is equipped with to mixed-powder is swaged to 4mm by 5% pass deformation, and the nb-zr tube compo pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1300 ℃ of insulations 60 hours, finally with stove, be cooled to room temperature, just make NdO
0.89f
0.11niAs superconductor.
Embodiment 7
First according to chemical formula CaFe
2as
2shown in weigh Ca powder 0.34g, Fe powder 1.91g, As powder 2.56g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long hafnium pipe of 5cm, bore 10mm, external diameter 12mm, makes powder in pipe, reach substantial, tight, then seals two ends.Then the hafnium pipe that this is equipped with to mixed-powder is swaged by 12% pass deformation and is drawn to 6mm, and the hafnium pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then slowly warming up to 850 ℃ of insulations 35 hours, finally with stove, be cooled to room temperature, just make CaFe
2as
2superconductor.
Embodiment 8
First according to chemical formula PrO
0.89f
0.11shown in CoAs, weigh Pr powder 4.89g, Co powder 0.72g, Co
2o
3powder 1.64g, FeF
3powder 0.14g, As powder 2.60g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long vanadium pipe of 10cm into bore 10mm, external diameter 13mm, makes powder in vanadium pipe, reach substantial, tight, then seals vanadium pipe two ends.Then the vanadium pipe that this is equipped with to mixed-powder proceeds to 8mm by 15% pass deformation, then 8% the thick metal tape of pass deformation rolling 4mm.Metal tape after processing is placed in to high-temperature heater, under room temperature, vacuumizes, wait to reach 10
-4after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1200 ℃ of insulations 40 hours, finally with stove, be cooled to room temperature, just make the PrO that superconducting transition temperature is not less than 45K
0.89f
0.11coAs superconductor.
Embodiment 9
First according to chemical formula GdO
0.83f
0.17shown in FeAs, weigh Gd powder 3.90g, Fe powder 0.66g, Fe
2o
3powder 1.16g, GdF
3powder 0.32g, As powder 1.97g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long molybdenum pipe of 15cm into bore 6mm, external diameter 9mm, makes powder in molybdenum pipe, reach substantial, tight, then seals molybdenum pipe two ends.Then the molybdenum pipe that this is equipped with to mixed-powder is drawn to 4mm by 8% pass deformation, and the molybdenum pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-2after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1200 ℃ of insulations 50 hours, finally with stove, be cooled to room temperature, just make GdO
0.83f
0.17feAs new superconductive body.
Embodiment 10
First according to chemical formula TbO
0.95f
0.05shown in RuAs, weigh Tb powder 3.12g, Ru powder 0.38g, RuO
2powder 0.99g, TbF
3powder 0.04g, As powder 1.47g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long tungsten pipe of 10cm into bore 4mm, external diameter 7mm, makes powder in tungsten pipe, reach substantial, tight, then seals tungsten pipe two ends.Then the tungsten pipe that this is equipped with to mixed-powder is swaged to 4mm by 5% pass deformation, and the tungsten pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-5after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1500 ℃ of insulations 80 hours, finally with stove, be cooled to room temperature, just make TbO
0.95f
0.05ruAs new superconductive body.
Embodiment 11
First according to chemical formula SmFe
0.85co
0.15shown in AsO, weigh Sm powder 6.06g, Fe powder 0.75g, Co
2o
3powder 0.50g, Fe
2o
3powder 1.66g, As powder 3.02g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long tantalum pipe of 8cm into bore 12mm, external diameter 15mm, makes powder in tantalum pipe, reach substantial, tight, then seals two ends.Then the tantalum pipe that this is equipped with to mixed-powder is drawn to 10mm by 5% pass deformation, by 5% pass deformation rolling, is then the metal tape after 5mm.Metal tape after processing is placed in to high-temperature heater, under room temperature, vacuumizes, wait to reach 10
-3after the vacuum degree of handkerchief, be filled with argon gas, be then warming up to 1160 ℃ of insulations 40 hours, finally with stove, be cooled to room temperature, just make SmFe
0.85co
0.15asO superconductor, superconducting transition temperature is 15K after measured.
Embodiment 12
First according to chemical formula D yFe
0.95ni
0.05shown in AsO, weigh Dy powder 4.72g, Fe powder 0.96g, Fe
2o
3powder 1.20g, Ni powder 0.91g, As powder 2.42g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long titanium pipe of 12cm, bore 8mm, external diameter 11mm, makes powder in titanium pipe, reach substantial, tight, then seals titanium pipe two ends.Then the titanium pipe that this is equipped with to mixed-powder is swaged to 4mm by 12% pass deformation, and the titanium pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1300 ℃ of insulations 60 hours, finally with stove, be cooled to room temperature, just make DyFe
0.95ni
0.05asO superconductor.
Embodiment 13
First according to chemical formula HoO
0.5f
0.5shown in FeAs, weigh Ho powder 3.01g, Fe powder 0.46g, Fe
2o
3powder 0.67g, HoF
3powder 0.31g, As powder 1.44g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long low carbon steel pipe of 9cm into bore 6mm, external diameter 8mm, make powder in low carbon steel pipe, reach substantial, tight, then seal low carbon steel pipe two ends.And pack low carbon steel pipe into copper pipe, and copper pipe internal diameter is 8.2mm, external diameter is 10mm, then the copper pipe that this is equipped with to mixed-powder is swaged to 4mm by 8% pass deformation, metal tube after processing is placed in to high-temperature heater, under room temperature, vacuumizes, wait to reach 10
-5after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1050 ℃ of insulations 55 hours, finally with stove, be cooled to room temperature, just make HoO
0.5f
0.5feAs new superconductive body.
Embodiment 14
First according to chemical formula Sr
0.5rb
0.5fe
2as
2shown in weigh Sr powder 0.67g, Fe powder 1.72g, the fritter 0.30g of As powder 2.31g and Rb, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long copper pipe of 6cm, bore 6mm, external diameter 8mm, makes powder in copper pipe, reach substantial, tight, then seals copper pipe two ends.Then the copper pipe that this is equipped with to mixed-powder is swaged to 5mm by 5% pass deformation, and the copper pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 700 ℃ of insulations 55 hours, finally with stove, be cooled to room temperature, just make Sr
0.5rb
0.5fe
2as
2new superconductive body.
Embodiment 15
First according to chemical formula YbFe
0.5zn
0.5shown in AsO, weigh Yb powder 2.57g, Fe powder 0.28g, Fe
2o
3powder 0.71g, Zn powder 0.28g, As powder 1.17g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long chromium pipe of 5cm, bore 6mm, external diameter 8mm, makes powder in chromium pipe, reach substantial, tight, then seals chromium pipe two ends.Then the chromium pipe that this is equipped with to mixed-powder is swaged to 4mm by 10% pass deformation, and the metal tube after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1200 ℃ of insulations 55 hours, finally with stove, be cooled to room temperature, just make YbFe
0.5zn
0.5asO new superconductive body.
Embodiment 16
First according to chemical formula La
0.5sm
0.5o
0.85f
0.15shown in FeAs, weigh Sm powder 1.85g, La powder 1.90g, Fe powder 0.66g, Fe
2o
3powder 1.24g, SmF
3powder 0.28g, As powder 2.05g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long manganese pipe of 10cm into bore 6mm, external diameter 8mm, makes powder in manganese pipe, reach substantial, tight, then seals manganese pipe two ends.Then the manganese pipe that this is equipped with to mixed-powder is drawn to 4mm by 15% pass deformation, and the manganese pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1150 ℃ of insulations 100 hours, finally with stove, be cooled to room temperature, just make La
0.5sm
0.5o
0.85f
0.15feAs new superconductive body.
Embodiment 17
First according to chemical formula ErO
0.5f
0.5shown in FeP, weigh Er powder 2.36g, Fe powder 0.39g, Fe
2o
3powder 0.84g, ErF
3powder 0.12g, P powder 1.31g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long ferrochrome pipe of 10cm into bore 5mm, external diameter 8mm, make powder in siderochrome pipe, reach substantial, tight, then seal compo pipe two ends.Then the ferrochrome pipe that this is equipped with to mixed-powder is swaged to 4mm by 8% pass deformation.Compo pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, wait to reach 10
-2after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1200 ℃ of insulations 40 hours, finally with annealing furnace, be cooled to room temperature, just make ErO
0.5f
0.5feP superconductor.
Embodiment 18
First according to chemical formula Eu
0.6na
0.4fe
2as
2shown in weigh Eu powder 0.60g, Fe powder 0.74g, As powder 1.00g and Na fritter 0.06g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long ferromolybdenum pipe of 5cm, bore 10mm, external diameter 12mm, makes powder in pipe, reach substantial, tight, then seals iron molybdenum pipe two ends.Then the iron molybdenum pipe that this is equipped with to mixed-powder is drawn to 6mm by 8% pass deformation, and the iron molybdenum pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then slowly warming up to 850 ℃ of insulations 35 hours, finally with stove, be cooled to room temperature, just make the Eu that transition temperature is 35K
0.6na
0.4fe
2as
2superconductor.
Embodiment 19
First according to chemical formula TmFe
0.8mn
0.2shown in AsO, weigh Tm powder 2.77g, Fe powder 0.51g, Fe
2o
3powder 0.93g, Mn powder 0.22g, As powder 1.56g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long ferrotungsten pipe of 6cm, bore 8mm, external diameter 12mm, makes powder in ferrotungsten pipe, reach substantial, tight, then seals ferrotungsten pipe two ends.Then the ferrotungsten pipe that this is equipped with to mixed-powder is swaged to 3mm by 5% pass deformation, and the ferrotungsten pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-4after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1150 ℃ of insulations 50 hours, finally with stove, be cooled to room temperature, just make TmFe
0.8mn
0.2asO superconductor.
Embodiment 20
First according to chemical formula Ba
0.9k
0.1fe
2as
2shown in weigh Ba powder 1.28g, Fe powder 2.08g, As powder 2.78g and K fritter 0.36g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long iron-nickel alloy pipe of 5cm, bore 10mm, external diameter 12mm, makes powder in iron-nickel alloy pipe, reach substantial, tight, then seals iron-nickel alloy pipe two ends.Then the iron-nickel alloy pipe that this is equipped with to mixed-powder is swaged to 6mm by 10% pass deformation, and the iron-nickel alloy pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-5after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then slowly warming up to 850 ℃ of insulations 35 hours, finally with stove, be cooled to room temperature, just make Ba
0.9k
0.1fe
2as
2superconductor.
Embodiment 21
First according to chemical formula LuO
0.7f
0.3shown in FeSb, weigh Lu powder 5.45g, Fe powder 1.20g, Fe
2o
3powder 1.50g, LuF
3powder 0.83g, Sb powder 3.02g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long ferrovanadium pipe of 8cm into bore 16mm, external diameter 20mm, make powder in ferrovanadium pipe, reach substantial, tight, then seal ferrovanadium pipe two ends.Then the ferrovanadium pipe that this is equipped with to mixed-powder is swaged to 5mm by 20% pass deformation, and the ferrovanadium pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1160 ℃ of insulations 40 hours, finally with stove, be cooled to room temperature, just make LuO
0.7f
0.3feSb superconductor.
Embodiment 22
First according to chemical formula YO
0.5f
0.5shown in FeAs, weigh Nd powder 1.91g, Fe powder 0.31g, Fe
2o
3powder 0.65g, YF
3powder 0.30g, As powder 1.03g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long ferroniobium pipe of 10cm into bore 3mm, external diameter 5mm, make powder in ferroniobium pipe, reach substantial, tight, then seal ferroniobium pipe two ends.Then the ferroniobium pipe that this is equipped with to mixed-powder is swaged to 4mm by 5% pass deformation, and the ferroniobium pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1300 ℃ of insulations 60 hours, finally with stove, be cooled to room temperature, just make YO
0.5f
0.5feAs superconductor.
Embodiment 23
First according to chemical formula Ca
0.5li
0.5fe
2as
2shown in weigh Ca powder 0.34g, Fe powder 1.91g, As powder 2.56g and Li fritter 0.20g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long ferromanganese pipe of 5cm, bore 10mm, external diameter 12mm, makes powder in ferromanganese pipe, reach substantial, tight, then seals ferromanganese pipe two ends.Then the ferromanganese pipe that this is equipped with to mixed-powder is swaged by 12% pass deformation and is drawn to 6mm, and the ferromanganese pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then slowly warming up to 850 ℃ of insulations 35 hours, finally with stove, be cooled to room temperature, just make the Ca that transition temperature is 20K
0.5li
0.5fe
2as
2superconductor.
Embodiment 24
First according to chemical formula La
0.5pr
0.5o
0.89f
0.11shown in FeAs, weigh La powder 2.44g, Pr powder 2.45g, Fe powder 0.72g, Fe
2o
3powder 1.64g, FeF
3powder 0.14g, As powder 2.60g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long ferrotianium pipe of 10cm into bore 10mm, external diameter 13mm, make powder in ferrotianium pipe, reach substantial, tight, then seal ferrotianium pipe two ends.Then the ferrotianium pipe that this is equipped with to mixed-powder proceeds to 8mm by 15% pass deformation, then 8% the thick metal tape of pass deformation rolling 4mm.Metal tape after processing is placed in to high-temperature heater, under room temperature, vacuumizes, wait to reach 10
-4after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1200 ℃ of insulations 40 hours, finally with stove, be cooled to room temperature, just make the La that superconducting transition temperature is not less than 45K
0.5pr
0.5o
0.89f
0.11feAs superconductor.
Embodiment 25
First according to chemical formula La
0.5gd
0.5o
0.83f
0.17shown in FeAs, weigh La powder 2.10g, Gd powder 1.80g, Fe powder 0.66g, Fe
2o
3powder 1.16g, GdF
3powder 0.32g, As powder 1.97g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long ferrozirconium pipe of 15cm into bore 6mm, external diameter 9mm, make powder in ferrozirconium pipe, reach substantial, tight, then seal ferrozirconium pipe two ends.Then the ferrozirconium pipe that this is equipped with to mixed-powder is drawn to 4mm by 8% pass deformation, and the ferrozirconium pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-2after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1200 ℃ of insulations 50 hours, finally with stove, be cooled to room temperature, just make La
0.5gd
0.5o
0.83f
0.17feAs new superconductive body.
Embodiment 26
First according to chemical formula La
0.5tb
0.5o
0.95f
0.05shown in FeAs, weigh La powder 1.52g, Tb powder 1.60g, Fe powder 0.38g, Fe
2o
3powder 0.99g, FeF
3powder 0.04g, As powder 1.47g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long iron tantalum alloy pipe of 10cm into bore 4mm, external diameter 7mm, make powder reach substantial, tight in iron tantalum alloy pipe, then seal iron tantalum alloy pipe two ends.Then the iron tantalum alloy pipe that this is equipped with to mixed-powder is swaged to 4mm by 5% pass deformation, and the iron tantalum alloy pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-5after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1500 ℃ of insulations 80 hours, finally with stove, be cooled to room temperature, just make La
0.5tb
0.5o
0.95f
0.05feAs new superconductive body.
Embodiment 27
First according to chemical formula SmFe
0.8zn
0.2shown in AsO, weigh Sm powder 6.06g, Fe powder 0.75g, ZnO powder 0.58g, Fe
2o
3powder 1.62g, As powder 3.02g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long iron hafnium alloy pipe of 8cm into bore 12mm, external diameter 15mm, make powder reach substantial, tight in iron hafnium alloy pipe, then seal iron hafnium alloy pipe two ends.Then the iron hafnium alloy pipe that this is equipped with to mixed-powder is drawn to 10mm by 5% pass deformation, by 5% pass deformation rolling, is then the metal tape after 5mm.Metal tape after processing is placed in to high-temperature heater, under room temperature, vacuumizes, wait to reach 10
-3after the vacuum degree of handkerchief, be filled with argon gas, be then warming up to 1160 ℃ of insulations 40 hours, finally with stove, be cooled to room temperature, just make SmFe
0.8zn
0.2asO superconductor.
Embodiment 28
First according to chemical formula La
0.5dy
0.5o
0.7f
0.3shown in FeAs, weigh La powder 2.30g, Dy powder 2.32g, Fe powder 0.96g, Fe
2o
3powder 1.20g, DyF
3powder 0.71g, As powder 2.42g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long nickel tungsten pipe of 12cm into bore 8mm, external diameter 11mm, make powder in nickel tungsten pipe, reach substantial, tight, then Nickel Sealing tungsten alloy pipe two ends.Then the nickel tungsten pipe that this is equipped with to mixed-powder is swaged to 4mm by 12% pass deformation, and the nickel tungsten pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1300 ℃ of insulations 60 hours, finally with stove, be cooled to room temperature, just make La
0.5dy
0.5o
0.7f
0.3feAs superconductor.
Embodiment 29
First according to chemical formula La
0.7ho
0.3o
0.85f
0.15shown in FeAs, weigh La powder 1.81g, Ho powder 1.21g, Fe powder 0.46g, Fe
2o
3powder 0.87g, HoF
3powder 0.21g, As powder 1.44g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long nickel-molybdenum alloy pipe of 9cm into bore 6mm, external diameter 8mm, make powder in nickel-molybdenum alloy pipe, reach substantial, tight, then Nickel Sealing molybdenum alloy pipe two ends.And pack nickel-molybdenum alloy pipe into niobium pipe, and niobium bore is 8.2mm, external diameter is 10mm, then the niobium pipe that this is equipped with to mixed-powder is swaged to 4mm by 8% pass deformation, metal tube after processing is placed in to high-temperature heater, under room temperature, vacuumizes, wait to reach 10
-5after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1050 ℃ of insulations 55 hours, finally with stove, be cooled to room temperature, just make La
0.7ho
0.3o
0.85f
0.15feAs new superconductive body.
Embodiment 30
First according to chemical formula Sr
0.6cs
0.4fe
2as
2shown in weigh Sr powder 0.67g, Fe powder 1.72g, the fritter 0.28g of As powder 2.31g and Cs, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long nickel hafnium alloy pipe of 6cm, bore 6mm, external diameter 8mm, makes powder reach substantial, tight in nickel hafnium alloy pipe, then Nickel Sealing hafnium alloy pipe two ends.Then the nickel hafnium alloy pipe that this is equipped with to mixed-powder is swaged to 5mm by 5% pass deformation, and the nickel hafnium alloy pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 700 ℃ of insulations 55 hours, finally with stove, be cooled to room temperature, just make Sr
0.6cs
0.4fe
2as
2new superconductive body.
Embodiment 31
First according to chemical formula La
0.8yb
0.2shown in OFeAs, weigh La powder 1.85g, Yb powder 0.82g, Fe powder 0.38g, Fe
2o
3powder 0.71g, As powder 1.17g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long Nitinol pipe of 5cm into bore 6mm, external diameter 8mm, makes powder in pipe, reach substantial, tight, then sealed tube two ends.Then the Nitinol pipe that this is equipped with to mixed-powder is swaged to 4mm by 10% pass deformation, and the Nitinol pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1200 ℃ of insulations 55 hours, finally with stove, be cooled to room temperature, just make La
0.8yb
0.2oFeAs new superconductive body.
Embodiment 32
First according to chemical formula La
0.5ce
0.5o
0.85f
0.15shown in FeAs, weigh Ce powder 1.85g, La powder 1.90g, Fe powder 0.66g, Fe
2o
3powder 1.24g, LaF
3powder 0.28g, As powder 2.05g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long ickel-niobium alloy pipe of 10cm into bore 6mm, external diameter 8mm, make powder in ickel-niobium alloy pipe, reach substantial, tight, then sealed tube two ends.Then the ickel-niobium alloy pipe that this is equipped with to mixed-powder is drawn to 4mm by 15% pass deformation, and the ickel-niobium alloy pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1150 ℃ of insulations 100 hours, finally with stove, be cooled to room temperature, just make La
0.5ce
0.5o
0.85f
0.15feAs new superconductive body.
Embodiment 33
First according to chemical formula Sm
0.5ce
0.5o
0.9f
0.1shown in FeAs, weigh Sm powder 1.15g, Ce powder 1.20g, Fe powder 0.39g, Fe
2o
3powder 0.84g, SmF
3powder 0.11g, As powder 1.31g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long nickel tantalum alloy pipe of 10cm into bore 5mm, external diameter 8mm, make powder in nickel tantalum alloy pipe, reach substantial, tight, then Nickel Sealing tantalum alloy pipe two ends.Then the nickel tantalum alloy pipe that this is equipped with to mixed-powder is swaged to 4mm by 8% pass deformation.Nickel tantalum alloy pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, wait to reach 10
-2after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1200 ℃ of insulations 40 hours, finally with annealing furnace, be cooled to room temperature, just make the Sm that superconducting transition temperature is 26K
0.5ce
0.5o
0.9f
0.1feAs superconductor.
Embodiment 34
First according to chemical formula Eu
0.7k
0.3fe
2as
2shown in weigh Eu powder 0.71g, Fe powder 0.74g, As powder 1.00g and K fritter 0.05g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long nickel-vanadium alloy pipe of 5cm, bore 10mm, external diameter 12mm, makes powder in nickel-vanadium alloy pipe, reach substantial, tight, then Nickel Sealing vanadium alloy pipe two ends.Then the nickel-vanadium alloy pipe that this is equipped with to mixed-powder is drawn to 6mm by 8% pass deformation, and the nickel-vanadium alloy pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then slowly warming up to 850 ℃ of insulations 35 hours, finally with stove, be cooled to room temperature, just make the Eu that transition temperature is 35K
0.7k
0.3fe
2as
2superconductor.
Embodiment 35
First according to chemical formula Pr
0.5ce
0.5o
0.84f
0.16shown in FeAs, weigh Ce powder 1.41g, Pr powder 1.38g, Fe powder 0.51g, Fe
2o
3powder 0.93g, CeF
3powder 0.22g, As powder 1.56g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long Zirconium-nickel alloy pipe of 6cm into bore 8mm, external diameter 12mm, make powder in Zirconium-nickel alloy pipe, reach substantial, tight, then seal Zirconium-nickel alloy pipe two ends.Then the Zirconium-nickel alloy pipe that this is equipped with to mixed-powder is swaged to 3mm by 5% pass deformation, and the Zirconium-nickel alloy pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-4after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1150 ℃ of insulations 50 hours, finally with stove, be cooled to room temperature, just make Pr
0.5ce
0.5o
84f
0.16feAs superconductor.
Embodiment 36
First according to chemical formula Ba
0.7k
0.3fe
2as
2shown in weigh Ba powder 1.38g, Fe powder 2.08g, As powder 2.78g and K fritter 0.26g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long nickel-manganese pipe of 5cm, bore 10mm, external diameter 12mm, makes powder in nickel-manganese pipe, reach substantial, tight, then Nickel Sealing manganese alloy pipe two ends.Then the nickel-manganese pipe that this is equipped with to mixed-powder is swaged to 6mm by 10% pass deformation, and the nickel-manganese pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-5after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then slowly warming up to 850 ℃ of insulations 35 hours, finally with stove, be cooled to room temperature, just make the Ba that transition temperature is 38K
0.7k
0.3f
e2as
2superconductor.
Embodiment 37
First according to chemical formula Sm
0.5pr
0.5o
0.7f
0.3shown in FeAs, weigh Sm powder 2.82g, Pr powder 2.65g, Fe powder 1.20g, Fe
2o
3powder 1.50g, SmF
3powder 0.83g, As powder 3.02g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long nichrome pipe of 8cm into bore 16mm, external diameter 20mm, make powder in pipe, reach substantial, tight, then Nickel Sealing evanohm pipe two ends.Then the nichrome pipe that this is equipped with to mixed-powder is swaged to 5mm by 20% pass deformation, and the nichrome pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1160 ℃ of insulations 40 hours, finally with stove, be cooled to room temperature, just make Sm
0.5pr
0.5o
0.7f
0.3feAs superconductor.
Embodiment 38
First according to chemical formula Sm
0.2nd
0.8o
0.89f
0.11shown in FeAs, weigh Sm powder 0.52g, Nd powder 1.46g, Fe powder 0.31g, Fe
2o
3powder 0.65g, NdF
3powder 0.10g, As powder 1.03g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long titanium-zirconium alloy pipe of 10cm into bore 3mm, external diameter 5mm, make powder reach substantial, tight in titanium zirconium pipe compo pipe, then seal titanium zirconium pipe two ends.Then the titanium zirconium pipe compo pipe that this is equipped with to mixed-powder is swaged to 4mm by 5% pass deformation, and the titanium zirconium pipe compo pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1300 ℃ of insulations 60 hours, finally with stove, be cooled to room temperature, just make Sm
0.2nd
0.8o
0.89f
0.11feAs superconductor.
Embodiment 39
First according to chemical formula Ca
0.6na
0.4fe
2as
2shown in weigh Ca powder 0.34g, Fe powder 1.91g, As powder 2.56g and Na fritter 0.18g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long titanium vanadium alloy pipe of 5cm, bore 10mm, external diameter 12mm, makes powder in titanium vanadium alloy pipe, reach substantial, tight, then seals titanium vanadium alloy pipe two ends.Then the titanium vanadium alloy pipe that this is equipped with to mixed-powder is swaged by 12% pass deformation and is drawn to 6mm, and the titanium vanadium alloy pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then slowly warming up to 850 ℃ of insulations 35 hours, finally with stove, be cooled to room temperature, just make the Ca that transition temperature is 20K
0.6na
0.4fe
2as
2superconductor.
Embodiment 40
First according to chemical formula Pr
0.7ho
0.3o
0.89f
0.11shown in FeAs, weigh Pr powder 3.60g, Ho powder 1.29g, Fe powder 0.72g, Fe
2o
3powder 1.64g, FeF
3powder 0.14g, As powder 2.60g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long titanium maxter alloy pipe of 10cm into bore 10mm, external diameter 13mm, make powder in pipe, reach substantial, tight, then seal titanium maxter alloy pipe two ends.Then the titanium maxter alloy pipe that this is equipped with to mixed-powder proceeds to 8mm by 15% pass deformation, then 8% the thick metal tape of pass deformation rolling 4mm.Metal tape after processing is placed in to high-temperature heater, under room temperature, vacuumizes, wait to reach 10
-4after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1200 ℃ of insulations 40 hours, finally with stove, be cooled to room temperature, just make Pr
0.7ho
0.3o
0.89f
0.11feAs superconductor.
Embodiment 41
First according to chemical formula Sm
0.6gd
0.4o
0.83f
0.17shown in FeAs, weigh Sm powder 2.30g, Gd powder 1.60g, Fe powder 0.66g, Fe
2o
3powder 1.16g, GdF
3powder 0.32g, As powder 1.97g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long titanium manganese alloy pipe of 15cm into bore 6mm, external diameter 9mm, make powder reach substantial, tight in titanium manganese alloy pipe, then seal titanium manganese alloy pipe two ends.Then the titanium manganese alloy pipe that this is equipped with to mixed-powder is drawn to 4mm by 8% pass deformation, and the titanium manganese alloy pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-2after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1200 ℃ of insulations 50 hours, finally with stove, be cooled to room temperature, just make Sm
0.6gd
0.4o
0.83f
0.17feAs new superconductive body.
Embodiment 42
First according to chemical formula Sm
0.5tb
0.5o
0.95f
0.05shown in FeAs, weigh Sm powder 1.60g, Tb powder 1.52g, Fe powder 0.38g, Fe
2o
3powder 0.99g, FeF
3powder 0.04g, As powder 1.47g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long titanium chrome alloy pipe of 10cm into bore 4mm, external diameter 7mm, make powder in pipe, reach substantial, tight, then seal titanium chrome alloy pipe two ends.Then the titanium chrome alloy pipe that this is equipped with to mixed-powder is swaged to 4mm by 5% pass deformation, and the titanium chrome alloy pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-5after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1500 ℃ of insulations 80 hours, finally with stove, be cooled to room temperature, just make Sm
0.5tb
0.5o
0.95f
0.05feAs new superconductive body.
Embodiment 43
First according to chemical formula SmFe
0.9co
0.1shown in AsO, weigh Sm powder 6.06g, Fe powder 0.75g, Co
2o
3powder 0.45g, Fe
2o
3powder 1.66g, As powder 3.02g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long titanium-tungsten pipe of 8cm into bore 12mm, external diameter 15mm, make powder in pipe, reach substantial, tight, then seal titanium-tungsten pipe two ends.Then the titanium-tungsten pipe that this is equipped with to mixed-powder is drawn to 10mm by 5% pass deformation, by 5% pass deformation rolling, is then the metal tape after 5mm.Metal tape after processing is placed in to high-temperature heater, under room temperature, vacuumizes, wait to reach 10
-3after the vacuum degree of handkerchief, be filled with argon gas, be then warming up to 1160 ℃ of insulations 40 hours, finally with stove, be cooled to room temperature, just make SmFe
0.9co
0.1asO superconductor, superconducting transition temperature is 15K after measured.
Embodiment 44
First according to chemical formula Sm
0.5dy
0.5o
0.7f
0.3shown in FeAs, weigh Sm powder 2.32g, Dy powder 2.40g, Fe powder 0.96g, Fe
2o
3powder 1.20g, DyF
3powder 0.71g, As powder 2.42g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long titanium niobium alloy pipe of 12cm into bore 8mm, external diameter 11mm, make powder in pipe, reach substantial, tight, then seal titanium niobium alloy pipe two ends.Then the titanium niobium alloy pipe that this is equipped with to mixed-powder is swaged to 4mm by 12% pass deformation, and the titanium niobium alloy pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1300 ℃ of insulations 60 hours, finally with stove, be cooled to room temperature, just make Sm
0.5dy
0.5o
0.7f
0.3feAs superconductor.
Embodiment 45
First according to chemical formula Er
0.5ho
0.5o
0.85f
0.15shown in FeAs, weigh Er powder 1.50g, Ho powder 1.51g, Fe powder 0.46g, Fe
2o
3powder 0.87g, HoF
3powder 0.21g, As powder 1.44g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long niobium tungsten alloy pipe of 9cm into bore 6mm, external diameter 8mm, make powder in pipe, reach substantial, tight, then seal niobium tungsten alloy pipe two ends.And pack niobium tungsten alloy pipe into titanium pipe, and titanium bore is 8.2mm, external diameter is 10mm, then the titanium pipe that this is equipped with to mixed-powder is swaged to 4mm by 8% pass deformation, metal tube after processing is placed in to high-temperature heater, under room temperature, vacuumizes, wait to reach 10
-5after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1050 ℃ of insulations 55 hours, finally with stove, be cooled to room temperature, just make Er
0.5ho
0.5o
0.85f
0.15feAs new superconductive body.
Embodiment 46
First according to chemical formula Sr
0.5na
0.5fe
2as
2shown in weigh Sr powder 0.67g, Fe powder 1.72g, the fritter 0.30g of As powder 2.31g and Na, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long niobium molybdenum alloy pipe of 6cm, bore 6mm, external diameter 8mm, makes powder in pipe, reach substantial, tight, then seals niobium molybdenum alloy pipe two ends.Then the niobium molybdenum alloy pipe that this is equipped with to mixed-powder is swaged to 5mm by 5% pass deformation, and the niobium molybdenum alloy pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 700 ℃ of insulations 55 hours, finally with stove, be cooled to room temperature, just make Sr
0.5na
0.5fe
2as
2new superconductive body.
Embodiment 47
First according to chemical formula Sm
0.5yb
0.5o
0.85f
0.15shown in FeAs, weigh Sm powder 1.25g, Yb powder 1.37g, Fe powder 0.38g, Fe
2o
3powder 0.71g, YbF
3powder 0.18g, As powder 1.17g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long zirconium molybdenum alloy pipe of 5cm into bore 6mm, external diameter 8mm, make powder in pipe, reach substantial, tight, then seal zirconium molybdenum alloy pipe two ends.Then the zirconium molybdenum alloy pipe that this is equipped with to mixed-powder is swaged to 4mm by 10% pass deformation, and the metal tube after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1200 ℃ of insulations 55 hours, finally with stove, be cooled to room temperature, just make Sm
0.5yb
0.5o
0.85f
0.15feAs new superconductive body.
Embodiment 48
First according to chemical formula La
0.5sm
0.4ce
0.1o
0.85f
0.15shown in FeAs, weigh Sm powder 1.85g, La powder 1.90g, Ce powder 0.04g, Fe powder 0.66g, Fe
2o
3powder 1.24g, SmF
3powder 0.28g, As powder 2.05g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long zirconium tungsten alloy pipe of 10cm into bore 6mm, external diameter 8mm, make powder in pipe, reach substantial, tight, then seal zirconium tungsten alloy pipe two ends.Then the zirconium tungsten alloy pipe that this is equipped with to mixed-powder is drawn to 4mm by 15% pass deformation, and the zirconium tungsten alloy pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1150 ℃ of insulations 100 hours, finally with stove, be cooled to room temperature, just make La
0.5sm
0.4ce
0.1o
0.85f
0.15feAs new superconductive body.
Embodiment 49
First according to chemical formula La
0.6sm
0.2gd
0.2o
0.9f
0.1shown in FeAs, weigh La powder 1.35g, Sm powder 0.45g, Gd powder 0.55g, Fe powder 0.39g, Fe
2o
3powder 0.84g, LaF
3powder 0.11g, As powder 1.31g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, powder after mixing is packed in the long hafnium tantalum alloy pipe of 10cm into bore 5mm, external diameter 8mm, make powder reach substantial, tight in hafnium tantalum alloy pipe, then seal hafnium tantalum alloy pipe two ends.Then the hafnium tantalum alloy pipe that this is equipped with to mixed-powder is swaged to 4mm by 8% pass deformation.Hafnium tantalum alloy pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, wait to reach 10
-2after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then warming up to 1200 ℃ of insulations 40 hours, finally with annealing furnace, be cooled to room temperature, just make La
0.6sm
0.2gd
0.2o
0.9f
0.1feAs superconductor.
Embodiment 50
First according to chemical formula Eu
0.8na
0.2fe
2as
2shown in weigh Eu powder 0.71g, Fe powder 0.74g, As powder 1.00g and Na fritter 0.03g, and this powder is placed in to argon atmospher glove box grinds, make its full and uniform mixing, the powder after mixing is packed in the long chromansil pipe of 5cm, bore 10mm, external diameter 12mm, makes powder in pipe, reach substantial, tight, then seals chromansil pipe two ends.Then the chromansil pipe that this is equipped with to mixed-powder is drawn to 6mm by 8% pass deformation, and the chromansil pipe after processing is placed in to high-temperature heater, under room temperature, vacuumizes, and waits to reach 10
-3after the vacuum degree of handkerchief, be filled with high-purity argon gas, be then slowly warming up to 850 ℃ of insulations 35 hours, finally with stove, be cooled to room temperature, just make Eu
0.8na
0.2fe
2as
2superconductor.
This technology of above embodiment application can the good superconductor of processability, for mechanism research and the practical application of Fe-base compound superconductor provides material foundation.
Claims (2)
1. a preparation method for Fe-base compound superconductor, is characterized in that this preparation method comprises the following steps:
(1) will be according to ReMPnO
1-xf
xor ReM
1-xtm
xpnO or Ae
1-xa
xm
2pn
2in the material powder of a kind of chemical formula preparation mix after, pack metal tube into, fully compacting, the then two ends of closed metal pipe; Wherein Re is one or more elements that are selected from La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y; M is a kind of element being selected from Fe, Co, Ni, Ru; Tm is a kind of element in Co, Ni, Mn, Zn; Pn is a kind of element in As, P, Sb; Ae is a kind of element in Ca, Sr, Ba, Eu; A is a kind of element in Li, Na, K, Rb, Cs; X=0-0.50;
(2) by metal tube according to the pass deformation of 5%-20% swage, drawing, rolling processing;
(3) metal tube obtaining through step 2 machining is placed in to high-temperature heater, under room temperature, is evacuated to 10
-2-10
-5handkerchief, is filled with argon gas afterwards, then at the temperature of 700-1500 ℃, is incubated 5-100 hour, finally treats that high temperature furnace is cooled to room temperature, and strip off metal jacket obtains Fe-base compound superconductor.
2. the preparation method of a kind of Fe-base compound superconductor according to claim 1, it is characterized in that: described metal tube is simple metal pipe or composite metal pipe or compo pipe making material chosen from Fe, copper, mild steel, stainless steel, chromium, vanadium, manganese, titanium, zirconium, molybdenum, nickel, niobium, tungsten, hafnium or the tantalum of described metal tube or composite metal pipe or compo pipe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810224178.9A CN101386529B (en) | 2008-10-24 | 2008-10-24 | Method for preparing Fe-base compound superconductor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810224178.9A CN101386529B (en) | 2008-10-24 | 2008-10-24 | Method for preparing Fe-base compound superconductor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101386529A CN101386529A (en) | 2009-03-18 |
| CN101386529B true CN101386529B (en) | 2014-03-19 |
Family
ID=40476232
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200810224178.9A Active CN101386529B (en) | 2008-10-24 | 2008-10-24 | Method for preparing Fe-base compound superconductor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101386529B (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550009B (en) * | 2009-04-30 | 2013-10-16 | 中国科学院上海硅酸盐研究所 | Preparation method of iron-base high-temperature superconductor |
| CN101707083B (en) * | 2009-12-15 | 2012-01-25 | 中国科学院电工研究所 | Iron-based compound superconducting wire or tape prepared from silver sheath |
| CN101814344A (en) * | 2010-03-10 | 2010-08-25 | 中国科学院电工研究所 | Method for preparing iron-based superconductor |
| CN102074311B (en) * | 2010-12-08 | 2012-07-04 | 中国科学院电工研究所 | Method for preparing high-density iron-based compound superconducting tape |
| CN102082010B (en) * | 2010-12-28 | 2012-11-14 | 中国科学院电工研究所 | Method for preparing iron-based superconductor |
| CN102412017B (en) * | 2011-10-19 | 2014-06-04 | 中国科学院电工研究所 | Method for improving upper critical field and critical current density of iron-based superconductor |
| CN102522154B (en) * | 2011-11-23 | 2013-07-31 | 北京工业大学 | Preparation method for iron-based super conductor |
| CN103354130B (en) * | 2013-05-15 | 2016-01-20 | 中国科学院电工研究所 | A kind of preparation method of iron-based superconductivity wire |
| 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 |
| CN108728678A (en) * | 2018-05-03 | 2018-11-02 | 北京科技大学 | A kind of iron-based superconductor preparation method based on isostatic cool pressing and directional solidification technique |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1945757A (en) * | 2006-11-08 | 2007-04-11 | 中国科学院电工研究所 | MgB2 composite superconductive wire (band) material and its preparing method |
| CN1986407A (en) * | 2005-12-23 | 2007-06-27 | 中国科学院电工研究所 | Corbon-containing superconductive MgB2 material and its preparing process |
| CN101150004A (en) * | 2007-08-30 | 2008-03-26 | 中国科学院电工研究所 | High performance Fe/Cu wrapping structure magnesium diboride multiple core superconductive wire preparation method |
| CN101168441A (en) * | 2007-09-25 | 2008-04-30 | 中国科学院电工研究所 | Method for preparing MgB2 superconducting material |
| CN101271747A (en) * | 2008-05-07 | 2008-09-24 | 中国科学院电工研究所 | Iron based compounds superconducting wire, belt material and method for producing the same |
-
2008
- 2008-10-24 CN CN200810224178.9A patent/CN101386529B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1986407A (en) * | 2005-12-23 | 2007-06-27 | 中国科学院电工研究所 | Corbon-containing superconductive MgB2 material and its preparing process |
| CN1945757A (en) * | 2006-11-08 | 2007-04-11 | 中国科学院电工研究所 | MgB2 composite superconductive wire (band) material and its preparing method |
| CN101150004A (en) * | 2007-08-30 | 2008-03-26 | 中国科学院电工研究所 | High performance Fe/Cu wrapping structure magnesium diboride multiple core superconductive wire preparation method |
| CN101168441A (en) * | 2007-09-25 | 2008-04-30 | 中国科学院电工研究所 | Method for preparing MgB2 superconducting material |
| CN101271747A (en) * | 2008-05-07 | 2008-09-24 | 中国科学院电工研究所 | Iron based compounds superconducting wire, belt material and method for producing the same |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101386529A (en) | 2009-03-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101386529B (en) | Method for preparing Fe-base compound superconductor | |
| CN101271747B (en) | Iron based compounds superconducting wire, belt material and method for producing the same | |
| CN101383204B (en) | Preparation method for europium iron arsenic super conductor wire and strip material | |
| CN104195372B (en) | One uses for nickel-hydrogen battery many phase hydrogen storage alloys of RE-Mg-Ni system and preparation method thereof | |
| CN101707089B (en) | Method for improving upper critical field and critical current density of iron-based superconductor | |
| CN106601366B (en) | A kind of preparation method of 122 type iron-based compound superconducting wire or band | |
| CN110317974B (en) | Yttrium-nickel rare earth hydrogen storage alloy | |
| CN101597711A (en) | A kind of rare-earth and Mg-transition metal base hydrogen storage metal and preparation method thereof | |
| CN102522154B (en) | Preparation method for iron-based super conductor | |
| CN105695775B (en) | A kind of yttrium iron base alloy material, preparation method and application | |
| JPH07118076A (en) | Porous sintered compact and solid electrolyte type fuel cell | |
| CN108517470A (en) | A kind of yttrium-zirconium-iron alloy material storing hydrogen and preparation method thereof | |
| CN101487106B (en) | High magnetic striction iron based metallic glass magnetic material and preparation thereof | |
| CN101552337A (en) | Superlattice hydrogen storage alloy and preparation method thereof | |
| CN102453466A (en) | Rare earth-copper-aluminum material for magnetic refrigeration and preparation method thereof | |
| CN101613818A (en) | A kind of low-cost hydrogen storage alloy and its production and application | |
| CN104404280A (en) | Preparation method for superlattice RE-Mg-Ni hydrogen storage alloy | |
| CN101899591B (en) | Superlattice hydrogen storage alloy material for nickel hydrogen battery and preparation method thereof | |
| CN103556071B (en) | High temperature radiation resistant magnetostriction alloy | |
| CN108172817A (en) | A kind of single-phase Gd2Co7Type rare earth magnesium nickel system hydrogen storage alloy, preparation method and applications | |
| CN104294087B (en) | The preparation method of superlattice hydrogen storage alloy | |
| WO2016029861A1 (en) | Rare-earth based hydrogen storage alloy and application thereof | |
| CN101608340B (en) | Iron-based high-temperature superconductive crystal and preparation method thereof | |
| CN101463445B (en) | NiMnGaCu high temperature shape-memory alloy and manufacturing method thereof | |
| CN1786239A (en) | Preparation method of high capacity rare earth magnesium base hydrogen storage alloy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |