CN109942290A - Bi (the Pb)-Sr-Ca-Cu-O of the topological heterogeneous phase doping of illuminator is super structure superconductor and preparation method thereof - Google Patents
Bi (the Pb)-Sr-Ca-Cu-O of the topological heterogeneous phase doping of illuminator is super structure superconductor and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of super structure superconductors of Bi (Pb)-Sr-Ca-Cu-O system intelligence and preparation method thereof of topological heterogeneous phase doping of illuminator, and the superconducting transition temperature for improving Bi (Pb)-Sr-Ca-Cu-O series superconducting material is adulterated using topological illuminator.The present invention prepares Y using hydro-thermal method2O3:Eu3+/ Ag (mass fraction of Ag is 1%) topological illuminator, solid sintering technology prepare Bi (Pb)-Sr-Ca-Cu-O series superconducting material of the heterogeneous phase doping of topological illuminator.Y is motivated under DC Electric Field2O3:Eu3+/ Ag topology shines heterogeneous phase electroluminescent, and passing through electroluminescent influences the superconducting transition temperature of Bi (Pb)-Sr-Ca-Cu-O series superconducting material.By changing the mass fraction of dopant, the variation of the superconducting transition temperature of doped samples is studied.Find that the superconducting transition temperature of doped samples is above pure sample in experiment.
Description
Technical field
The present invention relates to a kind of super structure superconductors of Bi (Pb)-Sr-Ca-Cu-O system intelligence of topological heterogeneous phase doping of illuminator
And preparation method thereof, the super structure superconductor of the intelligence can improve the transition temperature of Bi (Pb)-Sr-Ca-Cu-O series superconducting material.
Background technique
Michel in 1987 has found Bi series superconducting material (Bi-Sr-Cu-O superconductor, critical-temperature are 7-22K), though
Its right critical-temperature is not high, but has pulled open prelude for the research that critical-temperature is more than the Bi series superconducting material of 100K.1988,
Maeda etc. has found that transition temperature is more than the Bi-Sr-Ca-Cu-O series superconducting material of 100K, so that it is super to Bi system to have started researcher
The research boom of conductor.Although Bi-Sr-Ca-Cu-O series superconducting material referred to as high-temperature superconductor, its every critical parameters is (special
It is not superconducting transition temperature TC) also there is a big difference with extensive functionization, it is therefore desirable to it is modified.But arrive mesh
Before until, people find an effective method not yet to improve the superconducting transition temperature of Bi-Sr-Ca-Cu-O series superconducting material.
Y2O3:Eu3+Illuminator is a kind of excellent rare earth luminescent material, and preparation process is simple, pattern is relatively easily controlled
System has preferable stability, and it has many advantages, such as luminous intensity is high, monochromaticjty is good, quantum efficiency is high.And by oxygen
Change yttrium and be prepared into a kind of topological illuminator and can be further improved Y2O3:Eu3+Electroluminescent properties.
Infrared intense laser pulse induces La in A.Cavalleri in 2011 et al. utilization1.675Eu0.2Sr0.125CuO4, so that
La1.675Eu0.2Sr0.125CuO4It is changed into the superconducting phase of a transient state from a nonsuperconducting phase.Then, which utilizes identical
Experimental method in La1.84Sr0.16CuO4, YBa2Cu3O6.5And K3C60In observed similar transient state superconductivity, author recognizes
For this is because laser pumping lattice inducing substance has suiperconducting transition to produce transient state superconductivity, so that people gradually realize
Change the superconductivity of material to can use light.
Recent is some studies have shown that Y2O3:Eu3+/ Ag (mass fraction of Ag be 1%) topology shines heterogeneous phase doping
Bi (Pb)-Sr-Ca-Cu-O constitutes Meta Materials superconduction, is expected to improve the superconducting transition temperature of superconductor by the excitation of additional light field.
Summary of the invention
In view of the above circumstances, the present invention opens a kind of new method, using the thinking of Meta Materials, by chemical doping and light field
Excitation is combined together, Y2O3:Eu3+/ Ag topology heterogeneous the phase that shines is doped into Bi (Pb)-Sr-Ca-Cu-O series superconducting material matrix
In, Y is motivated under DC Electric Field2O3:Eu3+/ Ag topology shines heterogeneous phase electroluminescent, so that passing through electroluminescent influences
The superconducting transition temperature of Bi (Pb)-Sr-Ca-Cu-O series superconducting material.A kind of Y is prepared2O3:Eu3+/ Ag topology shines heterogeneous phase
The super structure superconductor of Bi (Pb)-Sr-Ca-Cu-O system intelligence of doping, has studied doping Y2O3:Eu3+/ Ag topology illuminator is to Bi
(Pb) influence of-Sr-Ca-Cu-O series superconducting material superconducting transition temperature.By changing the content of dopant, so that Y2O3:Eu3+/
The shine superconducting transition temperature of Bi (Pb)-Sr-Ca-Cu-O series superconducting material of heterogeneous phase doping of Ag topology is obviously improved.
The present invention prepares Y using hydro-thermal method2O3:Eu3+/ Ag (mass fraction of Ag is 1%) topological illuminator, solid-phase sintering
Method prepares Y2O3:Eu3+/ Ag topology shines Bi (Pb)-Sr-Ca-Cu-O series superconducting material of heterogeneous phase doping.It is as described below:
(1) Bi (Pb)-Sr-Ca-Cu-O series superconducting material and preparation method thereof of the topological heterogeneous phase doping that shines, feature exists
Y is prepared in hydro-thermal method2O3:Eu3+/ Ag topology illuminator；The topological illuminator of solid sintering technology preparation different quality containing
Bi (Pb)-Sr-Ca-Cu-O series superconducting material of heterogeneous phase doping；
(2) Bi (Pb)-Sr-Ca-Cu-O series superconducting material that the topological heterogeneous phase of illuminator is adulterated as described in claim 1
And preparation method thereof, it is characterised in that the topological heterogeneous phase of illuminator is evenly distributed on Bi (Pb)-Sr-Ca-Cu-O series superconducting material
Around grain, the mass fraction for changing the heterogeneous phase of topological illuminator can prepare Bi (Pb)-Sr-Ca- of different superconductivity
Cu-O series superconducting material；
(3) dopant is opened up in Bi (Pb)-Sr-Ca-Cu-O series superconducting material of the heterogeneous phase doping of the topological illuminator of above-mentioned (1)
Flutter illuminator Y2O3:Eu3+/ Ag (mass fraction of Ag be 1%) the preparation method is as follows: weighing 0.153g Y2O3And 0.012g
Eu2O3It is placed in a beaker, excessive concentrated hydrochloric acid is taken to be added dropwise in beaker, 70 DEG C of heating in draught cupboard are until be precipitated white clear crystalline substance
Body, dry 2h obtain presoma；Presoma is dissolved in 4mL water, is slowly dropped into ammonium oxalate solution, 2 DEG C of water-baths are vigorously stirred
30min, solution are precipitated by transparent and homogeneous to white colloidal is generated, and add a certain amount of AgNO3, stir 30min；Use NaOH
Solution adjusts pH to 9~10, and stirring 30min obtains final mixed solution；Mixed solution is transferred to 160 DEG C of water in reaction kettle
Thermal response 2h, product are put in 800 DEG C of high-temperature calcination 2h in tube furnace after centrifugation, washing, drying, obtain Y2O3:Eu3+/
AgCl obtains dopant Y after illumination2O3:Eu3+/Ag；
(4) preparation method of Bi (Pb)-Sr-Ca-Cu-O series superconducting material of the heterogeneous phase doping of the topological illuminator of above-mentioned (1)
It is as follows: 1. Bi in molar ratio2O3:PbO:SrCO3:CaCO3: CuO=0.92:0.34:2.00:2.00:3.00 weighs a certain amount of
Raw material is placed in agate pot, and using ethyl alcohol as grinding aid ball milling 20h, drum's speed of rotation is set as 500r/min.It is after drying
BSCCO raw material；2. raw material are placed in tube furnace, 830 DEG C of heat preservation 10h are ground after being cooled to room temperature, in the agate mortar wait grind
Mill is sufficiently rear to repeat sintering twice by above-mentioned technique, obtains BSCCO pre-burning powder；3. the BSCCO pre-burning powder for weighing certain mass fills
Dividing tabletting, pressure and dwell time after grinding is 10Mpa, 10min, and the piece pressed is placed in 830 DEG C of heat preservation 10h in tube furnace and is obtained
To pure BSCCO sample.4. weighing the heterogeneous phase of topological illuminator and BSCCO pre-burning powder of corresponding different quality containing, set respectively
In two beakers, suitable alcohols ultrasonic disperse 20min is added, uses magnetic stirrer later, while by dopant solution
It is added dropwise in BSCCO pre-burning powder solution；Mixed solution is continued into stirring 10 minutes, ultrasonic 20min is subsequently transferred to train
It supports in ware, 60 DEG C in vacuum oven, dry 4h obtains black powder, when powder is fully ground rear tabletting, pressure and pressure maintaining
Between be 10Mpa, 10min, the piece pressed is finally placed in 830 DEG C of heat preservation 10h in tube furnace and obtains corresponding doped samples.
The present invention is beneficial in that, the thinking based on Meta Materials, by chemical doping by the heterogeneous coupling of topological illuminator
Enter in Bi (Pb)-Sr-Ca-Cu-O series superconducting material, using the excellent electroluminescent properties of topological illuminator, motivates Bi (Pb)-
It is super to open a kind of new raising Bi (Pb)-Sr-Ca-Cu-O system so as to improve the superconducting transition temperature of material by Sr-Ca-Cu-O
It is different experimentally to have prepared a kind of topological illuminator with higher critical transition temperature for the method for conductor superconducting transition temperature
The super structure superconductor of Bi (Pb)-Sr-Ca-Cu-O system intelligence that matter is mutually adulterated, this method is expected to super applied to other high temperature are improved
The superconductivity of conductor.
Detailed description of the invention
Fig. 1 hydro-thermal method prepares Y2O3:Eu3+The flow chart of/Ag topology illuminator
Fig. 2 .a dopant Y2O3:Eu3+The XRD diagram of/Ag topology illuminator
Fig. 2 .b dopant Y2O3:Eu3+The SEM of/Ag topology illuminator schemes
Fig. 2 .c-d dopant Y2O3:Eu3+The AFM of/Ag topology illuminator schemes
Fig. 3 pure BSCCO and different quality containing Y2O3:Eu3+The XRD diagram of/Ag doping BSCCO superconductor
The pure BSCCO (a) of Fig. 4 and 0.2%Y2O3:Eu3+/ Ag adulterates the SEM figure of BSCCO superconductor (b)
The pure BSCCO of Fig. 5 embodiment one and different quality containing Y2O3:Eu3+/ Ag adulterates the resistance and temperature of BSCCO superconductor
Spend relational graph
Specific embodiment
The present invention prepares Y using hydro-thermal method2O3:Eu3+/ Ag topology illuminator dopant, is prepared using solid sintering technology
Bi (Pb)-Sr-Ca-Cu-O series superconducting material of the topological heterogeneous phase doping of illuminator.Specific preparation process is as follows:
(1) dopant Y2O3:Eu3+The preparation of/Ag topology illuminator: 0.153g Y is weighed2O3With 0.012g Eu2O3It is placed in
In beaker, excessive concentrated hydrochloric acid is taken to be added dropwise in beaker, 70 DEG C of heating in draught cupboard are until precipitation white clear crystal, dry 2h
Obtain presoma；Presoma is dissolved in 4mL water, is slowly dropped into ammonium oxalate solution, 2 DEG C of water-baths are vigorously stirred 30min, solution
By transparent and homogeneous to white colloidal precipitating is generated, a certain amount of AgNO is added3, stir 30min；PH is adjusted using NaOH solution
To 9~10, stirring 30min obtains final mixed solution；Mixed solution is transferred to 160 DEG C of hydro-thermal reaction 2h in reaction kettle, it is raw
800 DEG C of high-temperature calcination 2h in tube furnace are put in after centrifugation, washing, drying at object, obtain Y2O3:Eu3+/ AgCl, illumination it
Dopant Y is obtained afterwards2O3:Eu3+/Ag；
(2) Bi in molar ratio2O3:PbO:SrCO3:CaCO3: CuO=0.92:0.34:2.00:2.00:3.00 is weighed centainly
The raw material of amount, is placed in agate pot, and using ethyl alcohol as grinding aid ball milling 20h, drum's speed of rotation is set as 500r/min.After drying i.e.
For BSCCO raw material；Raw material are placed in tube furnace, 830 DEG C of heat preservation 10h are ground after being cooled to room temperature, in the agate mortar wait grind
Mill is sufficiently rear to repeat sintering twice by above-mentioned technique, obtains BSCCO pre-burning powder；
(3) the BSCCO pre-burning powder for weighing certain mass is fully ground rear tabletting, pressure and dwell time be 10Mpa,
The piece pressed is placed in 830 DEG C of heat preservation 10h in tube furnace and obtains pure BSCCO sample by 10min；
(4) the heterogeneous phase of topological illuminator and BSCCO pre-burning powder for weighing corresponding different quality containing, are respectively placed in two
In beaker, suitable alcohols ultrasonic disperse 20min is added, then uses magnetic stirrer, while dopant solution being added dropwise
Enter into BSCCO pre-burning powder solution；Mixed solution is continued into stirring 10 minutes, ultrasonic 20min is finally transferred in culture dish,
60 DEG C in a vacuum drying oven, dry 4h obtains black powder, and powder is fully ground rear tabletting, and pressure and dwell time be
The piece pressed is finally placed in 830 DEG C of heat preservation 10h in tube furnace and obtains corresponding doped samples by 10Mpa, 10min；
(5) topological illuminator dopant electricity is excited using the local electric field that added electric current during measurement transition temperature generates
Photoluminescence measures sample resistance variation with temperature using four probe method to determine the superconducting transition temperature of sample.
Realization process and material property of the invention is by following implementation steps and Detailed description of the invention:
(1) hydro-thermal method prepares Y2O3:Eu3+/ Ag (mass fraction of Ag is 1%) topological illuminator, preparation flow such as Fig. 1 institute
Show.Dopant Y2O3:Eu3+The XRD and SEM of/Ag schemes as shown in Fig. 2 a-b.Dopant Y2O3:Eu3+The thickness of/Ag can pass through
AFM characterization, as shown in Fig. 2 c-d.
(2) solid sintering technology prepares pure BSCCO sample and 0.1%Y2O3:Eu3+/ Ag, 0.2%Y2O3:Eu3+/ Ag and 0.5%
Y2O3:Eu3+The BSCCO superconductor of/Ag doping.
(3) material phase analysis, knot are carried out to sample using Dutch Panaco company's X ' Pert MPD PRO type X-ray diffractometer
Fruit is as shown in Figure 3.Test result shows, pure BSCCO and Y2O3:Eu3+The BSCCO sample of/Ag doping all contains high-temperature-phase Bi-
2223 phases and low-temperature phase Bi-2212 phase, the specific volume fraction of two-phase are provided by table 1, as seen from the table low-temperature phase Bi-2212 compared with
Mostly this is mainly due to sintering time too short reactions to be not enough；Since topological illuminator doping content is lower in doped samples
Y is not found in XRD spectrum2O3Peak.The pattern of the sample of preparation is characterized by SEM, as shown in Figure 4.It can from figure
Out, the BSCCO sample of preparation is irregular layer structure, and the doping of topological illuminator does not change BSCCO sample significantly
Microscopic appearance.Using the liquid helium cryogenic system of Advanced Research Systems company, measured using four probe method
Sample resistance varies with temperature curve, as shown in Figure 5.The specific value of superconducting transition temperature such as table 1.It can from figure
Out, the superconducting transition temperature of doped samples is increased compared to pure BSCCO, and with the increase of doping content, transition temperature
Elevation amplitude reduced.
Table 1
The foregoing is merely preferred implementation implementation steps of the invention, when cannot be limited the scope of implementation of the present invention with this,
It should still belong to this hair according to simple equivalent changes and modifications made by the claims in the present invention and description of the invention content generally
In the range of bright patent covering.
Claims (3)
1. Bi (Pb)-Sr-Ca-Cu-O series superconducting material and preparation method thereof of the topological heterogeneous phase doping of illuminator, it is characterised in that
Y is prepared in hydro-thermal method2O3:Eu3+/ Ag (mass fraction of Ag is 1%) topological illuminator dopant；Solid sintering technology is prepared not
Bi (Pb)-Sr-Ca-Cu-O series superconducting material of the heterogeneous phase doping of homogenous quantities score topology illuminator.
2. as described in claim 1 Bi (the Pb)-Sr-Ca-Cu-O series superconducting material of topology illuminator heterogeneous phase doping and its
Preparation method, it is characterised in that topological illuminator dopant is evenly distributed in Bi (Pb)-Sr-Ca-Cu-O series superconducting material particle
Around, the mass fraction for changing topological illuminator dopant can prepare Bi (Pb)-Sr-Ca-Cu-O of different superconductivity
Series superconducting material.
3. the system of Bi (Pb)-Sr-Ca-Cu-O series superconducting material of the heterogeneous phase doping of topology illuminator as described in claim 1
Preparation Method the following steps are included:
(1) 0.153g Y is weighed2O3With 0.012g Eu2O3It is placed in a beaker, takes excessive concentrated hydrochloric acid to be added dropwise in beaker, Yu Tongfeng
Until white clear crystal is precipitated, dry 2h obtains presoma for 70 DEG C of heating in cupboard；Presoma is dissolved in 4mL water, is slowly dripped
Enter in ammonium oxalate solution, 2 DEG C of water-baths are vigorously stirred 30min, and solution is precipitated by transparent and homogeneous to white colloidal is generated, and add one
Quantitative AgNO3, stir 30min；PH to 9~10 is adjusted using NaOH solution, stirring 30min obtains final mixed solution；It will
Mixed solution is transferred to 160 DEG C of hydro-thermal reaction 2h in reaction kettle, and product is put in tube furnace after centrifugation, washing, drying
800 DEG C of high-temperature calcination 2h, obtain Y2O3:Eu3+/ AgCl obtains dopant Y after illumination2O3:Eu3+/Ag。
(2) Bi in molar ratio2O3:PbO:SrCO3:CaCO3: CuO=0.92:0.34:2.00:2.00:3.00 weighs a certain amount of
Raw material is placed in agate pot, and using ethyl alcohol as grinding aid ball milling 20h, drum's speed of rotation is set as 500r/min.It is after drying
BSCCO raw material；Raw material are placed in tube furnace, 830 DEG C of heat preservation 10h are ground in the agate mortar after being cooled to room temperature, to be ground
Sintering is repeated twice by above-mentioned technique after sufficiently, obtains BSCCO pre-burning powder.
(3) the BSCCO pre-burning powder for weighing certain mass is fully ground rear tabletting, and pressure and dwell time are 10Mpa, 10min, incites somebody to action
The piece pressed is placed in 830 DEG C of heat preservation 10h in tube furnace and obtains pure BSCCO sample.
(4) the heterogeneous phase of topological illuminator and BSCCO pre-burning powder for weighing corresponding different quality containing, are respectively placed in two beakers
In, ultrasound 20min after suitable alcohols is added, then uses magnetic stirrer, while dopant solution being added dropwise to
In BSCCO pre-burning powder solution；Mixed solution is continued to stir 10min, ultrasonic 20min is finally transferred in culture dish, in vacuum
60 DEG C in drying box, dry 4h obtains black powder, and powder is fully ground rear tabletting, pressure and dwell time be 10Mpa,
The piece pressed is finally placed in 830 DEG C of heat preservation 10h in tube furnace and obtains corresponding doped samples by 10min.
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| JPH07141940A (en) * | 1993-11-16 | 1995-06-02 | Takeshi Masumoto | Manufacture of superconductive wire of bismuth oxide |
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