CN104774013B - Y2O3:Eu3+ illuminant doped MgB2 superconductor with high critical transition temperature - Google Patents
Y2O3:Eu3+ illuminant doped MgB2 superconductor with high critical transition temperature Download PDFInfo
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- CN104774013B CN104774013B CN201510121032.1A CN201510121032A CN104774013B CN 104774013 B CN104774013 B CN 104774013B CN 201510121032 A CN201510121032 A CN 201510121032A CN 104774013 B CN104774013 B CN 104774013B
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Abstract
The invention relates to an Y2O3:Eu3+ illuminant doped MgB2 superconductor with a high critical transition temperature. The Y2O3:Eu3+ illuminant is used to change the MgB2 superconductor transition temperature. The hydrothermal method is adopted to prepare an Y2O3:Eu3+ nano rod, and a solid doping method is utilized to prepare the Y2O3:Eu3+ illuminant doped MgB2 superconductor. In the hydrothermal method, the mole ratio of Y to Eu is 0.95:0.05; in the prepared Y2O3:Eu3+ illuminant doped MgB2 superconductor, the atomic ratio of Mg and B is 1.2:2, and the Y2O3:Eu3+ illuminant accounts for 4 to 8% of the total weight of the MgB2 superconductor. In the absence of an external magnetic field, when the Y2O3:Eu3+ illuminant accounts for 8% of the total weight of the MgB2 superconductor, the Tc (37.4 K) of the doped MgB2 superconductor is higher than that (Tc=37 K) of the pure MgB2.
Description
Technical field
The present invention relates to a kind of improve MgB2The method of superconductor transition temperature, make use of Y2O3：Eu3+Illuminator is to MgB2
The impact of superconductor transition temperature.
Background technology
Intermetallic compound Mg B is found that in calendar year 2001, Akimitsu of Japan et al.2With superconducting characteristic, pass through
The high-pressure sinter of 196MPa obtains its critical-temperature for 39K.Binary metal boride MgB2The discovery of superconducting characteristic, causes this
Very big concern of the researcher in field to fundamental research and the application of superconductor.MgB2With of a relatively high stagnation temperature
Degree (the close 40K of its transition temperature), larger superconduction correlation length, high critical current density and wider energy gap etc. are excellent
Point, therefore it has huge application potential in terms of superconductive device.MgB2Simple structure, it is easy to make and process, it has
Far above the critical-temperature of cryogenic superconductor, and not there are problems that the Weak link for being difficult to overcome in high-temperature superconductor, therefore, MgB2
Development and application to superconductor technology brings new opportunity.Additionally, MgB2Itself belongs to type, with dual intensity
Gap, superconducting mechanism is unique, for the basic research of superconductivity theory has very big impetus.Therefore, MgB2Superconductor without
It is of great significance by all having to basic research or application study.
Y2O3：Eu3+Illuminator has good luminescent properties, in atmosphere with preferable stability, will not be as sulfuration
Thing dangerous property like that.MgB2Belong to the typical material of BCS theory category, be the type of standard, simple structure is made
Valency is cheap, it is easy to synthesize.But MgB2Superconducting critical transition temperature it is not high limit its application, it is desirable to by adulterate come
Improve its superconducting transition temperature.But substantial amounts of result of study shows, many chemical dopings all cause MgB2The T of superconductorcDrop
It is low.Because MgB2The impurity of material is not easily accomplished very much, and most atoms cannot adulterate and enter MgB2Lattice in.Separately
On the one hand, chemical doping can affect the physical propertys such as carrier concentration, lattice paprmeter and crystallization degree.For example, Al and C mixes
Miscellaneous, they instead of respectively MgB2In Mg and B atoms, significantly reduce MgB2Tc.The present invention is from luminous to suiperconducting transition
The impact of temperature is started with, and has prepared a kind of Y2O3：Eu3+The MgB of illuminator doping2Superconductor, by the doping reality of different proportion
The contrast tested, draws a kind of Y with high critical transition temperature2O3：Eu3+Illuminator doping MgB2Superconductor.
The content of the invention
In view of the above circumstances, it is an object of the invention to prepare a kind of Y2O3：Eu3+The MgB of illuminator doping2Superconductor,
The superconductor has high critical transition temperature, and makes easy.
The present invention prepares Y using hydro-thermal method2O3：Eu3+Nanometer rods, solid phase doping methods prepare Y2O3：Eu3+Illuminator doping
MgB2Superconductor.As described below：
(1) a kind of Y with high critical transition temperature2O3：Eu3+The MgB of illuminator doping2Superconductor, wherein Y2O3：Eu3+
Illuminator nanometer rods are distributed in MgB2In superconductor sintered body；Y2O3：Eu3+Illuminator nanometer rods are distributed in MgB2Superconductor crystal grain
Boundary；
(2) according to the MgB of the high critical transition temperature of above-mentioned (1)2Superconductor, wherein, hydro-thermal method prepares Y2O3：Eu3+Nanometer
During rod, the mol ratio of Y and Eu is 0.95: 0.05；When in Y2O3：Eu3+The MgB of illuminator doping2Contain in superconductor sintered body
The atomic ratio of Mg and B is 1.2: 2, wherein Y2O3：Eu3+Mass fraction shared by illuminator is 4%～8%；
(3) according to above-mentioned (1) or the MgB of the high critical transition temperature of (2)2Superconductor, works as Y2O3：Eu3+Shared by illuminator
MgB2When superconductor mass fraction is 8%, under conditions of without external magnetic field, pure MgB2Tc=37K, Y2O3：Eu3+Illuminator
The MgB of doping2The T of superconductorc=37.4K.
Description of the drawings
Fig. 1 .a hydro-thermal methods prepare Y2O3The flow chart of nanometer rods
Fig. 1 .b hydro-thermal methods prepare Y2O3：Eu3+The flow chart of nanometer rods
Fig. 2 Y2O3：Eu3+The SEM figures of illuminator
Fig. 3 Y2O3：Eu3+The MgB of illuminator doping2The SEM figures of superconductor
The Y of Fig. 4 .a embodiments one2O3And Y2O3：Eu3+The MgB of illuminator doping2Superconductor XRD
The Y of Fig. 4 .b embodiments one2O3And Y2O3：Eu3+The MgB of illuminator doping2Superconductor low-temperature resistance figure
The Y of Fig. 5 .a embodiments two2O3And Y2O3：Eu3+The MgB of illuminator doping2Superconductor XRD
The Y of Fig. 5 .b embodiments two2O3And Y2O3：Eu3+The MgB of illuminator doping2Superconductor low-temperature resistance figure
The Y of Fig. 6 .a embodiments three2O3And Y2O3：Eu3+The MgB of illuminator doping2Superconductor XRD
The Y of Fig. 6 .b embodiments three2O3And Y2O3：Eu3+The MgB of illuminator doping2Superconductor low-temperature resistance figure
Specific embodiment
The present invention prepares Y using hydro-thermal method2O3：Eu3+Nanometer rods, solid phase doping methods prepare Y2O3：Eu3+Illuminator doping
MgB2Superconductor.Concrete preparation process is as follows：
(1) Y of 0.306g is weighed2O3With the Eu of 0.025g2O3, the mol ratio of Y and Eu is dissolving at 0.95: 0.05,50 DEG C
In excess nitric acid, Y (NO are obtained3)3With Eu (NO3)3Mixed solution, mixed solution is heated to into 80 DEG C, be evaporated, removed
Amount nitric acid, obtains white crystal, deionized water dissolving.The NaOH solution of addition 1M is in above-mentioned solution.Obtain PH=13.5
Precipitated liquid, move to reactor, 2h is incubated at 180 DEG C, room temperature is naturally cooled to afterwards.The solution in reactor is taken out, is washed,
Alcohol is washed, and each three times, is precipitated liquid A, and A is dried into a few hours acquisition Y at 90 DEG C2O3：Eu3+Rod precursor B.By B at 800 DEG C
Calcining obtains Y in 2 hours2O3：Eu3+Nanometer rods.If being added without Eu in above-mentioned preparation process2O3, can finally prepare Y2O3Receive
Rice rod.Preparation flow figure is as shown in Figure 1.
(2) in glove box, in molar ratio magnesium powder and boron powder are weighed at 1.2: 2, is fully ground after mixing, place into compressing tablet
Compressing tablet is carried out in mould.During tube type vacuum stove is put into after compression molding, under flowing Ar atmosphere, 5 DEG C/min of heating rate exists respectively
640 DEG C and 800 DEG C are incubated 1 hour, so as to obtain MgB2Sample.Weigh magnesium powder 0.22g, boron powder 0.18g, respectively with respective quality
The Y of fraction2O3、Y2O3：Eu3+Mixed grinding, compressing tablet prepare corresponding doped samples according to above-mentioned sintering process.
The present invention's realizes process and material property by embodiment and description of the drawings：
Embodiment one：
(1) hydro-thermal method prepares Y2O3And Y2O3：Eu3+Nanometer rods：Preparation flow figure is as shown in Figure 1.
(2) solid phase doping methods prepare pure MgB2、Y2O3And Y2O3：Eu3+The MgB of illuminator doping2(mass fraction is superconductor
4%).
(3) material phase analysis are carried out to sample using Dutch PANalytical company X ' Pert MPD PRO types X-ray diffractometers；Profit
With the liquid helium cryogenic system of Advanced Research Systems companies of the U.S., sample resistance is measured using four probe method
The curve for varying with temperature：As shown in Figure 4.Can see from Fig. 4 .a, Y2O3And Y2O3：Eu3+The MgB of illuminator doping2It is super
The principal phase of conductor sample is MgB2, also have the Y that some are remained in addition2O3Phase, the source of impurities phase MgO is probably 1. gloves
2. tableting processes or sample are shifted from glove box to vacuum tube furnace for the trace oxygen in high-purity argon in case process of lapping
During to have touched the vacuum of a small amount of oxygen 3. vacuum tube furnace be not to contain micro oxygen in very high 4. Ar gas.From figure
Can see in 4.b, doping causes the T of samplecReduce, and Y2O3：Eu3+The T of nanometer rods doped samplescThan Y2O3Receive
The T of rice rod doped samplescIt is low.
Embodiment two：
(1) hydro-thermal method prepares Y2O3And Y2O3：Eu3+Nanometer rods：Preparation flow figure is as shown in Figure 1.
(2) solid phase doping methods prepare pure MgB2、Y2O3And Y2O3：Eu3+The MgB of illuminator doping2(mass fraction is superconductor
6%).
(3) material phase analysis are carried out to sample using Dutch PANalytical company X ' Pert MPD PRO types X-ray diffractometers；Profit
With the liquid helium cryogenic system of Advanced Research Systems companies of the U.S., sample resistance is measured using four probe method
The curve for varying with temperature：As shown in Figure 5.Can see from Fig. 5 .a, Y2O3And Y2O3：Eu3+The MgB of illuminator doping2Superconduction
The principal phase of body sample is MgB2, also have the Y that some are remained in addition2O3Phase, institute in the source such as embodiment one of impurities phase MgO
State.Can see from Fig. 5 .b, doping causes the T of samplecReduce, and Y2O3：Eu3+The T of nanometer rods doped samplescWill
Compare Y2O3The T of nanometer rods doped samplescIt is low, and comparison diagram 4.b it is found that doping amount it is more, the T of samplecIt is lower.
Embodiment three：
(1) hydro-thermal method prepares Y2O3And Y2O3：Eu3+Nanometer rods：Preparation flow figure is as shown in Figure 1.
(2) solid phase doping methods prepare pure MgB2、Y2O3And Y2O3：Eu3+The MgB of illuminator doping2Superconductor (mass fraction
For 8%).
(3) material phase analysis are carried out to sample using Dutch PANalytical company X ' Pert MPD PRO types X-ray diffractometers；Profit
With the liquid helium cryogenic system of Advanced Research Systems companies of the U.S., sample resistance is measured using four probe method
The curve for varying with temperature：As shown in Figure 6.Can see from Fig. 6 .a, Y2O3And Y2O3：Eu3+The MgB of illuminator doping2Superconduction
The principal phase of body sample is MgB2, also have the Y that some are remained in addition2O3Phase, institute in the source such as embodiment one of impurities phase MgO
State.Can see from Fig. 6 .b, Y2O3The T of nanometer rods doped samplescThan pure MgB2TcIt is low, but Y2O3：Eu3+Illuminator is mixed
Miscellaneous MgB2The T of superconductor samplecPure MgB is exceeded2Tc, this just prepares a kind of Y with high critical transition temperature2O3：Eu3+
Illuminator doping MgB2Superconductor.
The preferred embodiments of the present invention are the foregoing is only, when the scope that the present invention is implemented can not be limited with this, i.e.,
Generally the simple equivalence changes made according to the claims in the present invention and description of the invention content and modification, all should still belong to the present invention
In the range of patent is covered.
Claims (3)
1. a kind of Y with high critical transition temperature2O3：Eu3+Illuminator doping MgB2Superconductor, is primarily characterized in that hydro-thermal
Method prepares Y2O3：Eu3+The mol ratio of nanometer rods, wherein Y and Eu is 0.95: 0.05；Solid phase doping methods prepare Y2O3：Eu3+Illuminator
Doping MgB2Superconductor, wherein raw material Mg and B atomic ratios are 1.2: 2, Y2O3：Eu3+Superconductor mass fraction is shared by illuminator
4%～8%.
2. the as described in claim 1 MgB of high critical transition temperature2Superconductor, it is characterised in that Y2O3：Eu3+Illuminator is received
Rice rod is distributed in MgB2At superconductor grain boundary.
3. the as described in claim 1 MgB of high critical transition temperature2Superconductor, it is characterised in that preparation technology includes following
Step：
(1) Y of 0.306g is weighed2O3With the Eu of 0.025g2O3, it is dissolved at 50 DEG C in excess nitric acid, mixed solution is heated to
80 DEG C, it is evaporated, removes excess nitric acid, obtain white crystal, deionized water dissolving adds the NaOH solution of 1M to above-mentioned solution
In；The precipitated liquid of PH=13.5 is obtained, reactor is moved to, 2h is incubated at 180 DEG C, room temperature is naturally cooled to afterwards；Take out reaction
Solution in kettle, washing, alcohol is washed, and each three times, is precipitated liquid A, and A is dried into a few hours acquisition Y at 90 DEG C2O3：Eu3+Before rod
Drive body B；B is obtained into Y in 2 hours in 800 DEG C of calcinings2O3：Eu3+Nanometer rods；
(2) in glove box, in molar ratio magnesium powder 0.22g, boron powder 0.18g, Y with respective quality fraction are weighed at 1.2: 22O3：
Eu3+It is fully ground after mixing, places into and carry out in compression mold compressing tablet；During tube type vacuum stove is put into after compression molding, flow Ar
Under atmosphere, 5 DEG C/min of heating rate is incubated 1 hour, so as to obtain Y at 640 DEG C and 800 DEG C respectively2O3：Eu3+Illuminator adulterates
MgB2Superconductor sample.
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| CN105788752B (en) * | 2016-04-05 | 2018-04-13 | 西北工业大学 | The MgB that electroluminescent excitation critical transition temperature improves2Base super conductor and preparation method thereof |
| CN108383531B (en) * | 2018-05-15 | 2021-02-19 | 西北工业大学 | MgB doped with topological luminophores in heterogeneous phase2Base superconductor and method for producing same |
| CN109942290A (en) * | 2019-03-12 | 2019-06-28 | 西北工业大学 | Bi (the Pb)-Sr-Ca-Cu-O of the topological heterogeneous phase doping of illuminator is super structure superconductor and preparation method thereof |
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