CN102534787B - The preparation method of single domain yttrium barium copper oxide superconductor - Google Patents
The preparation method of single domain yttrium barium copper oxide superconductor Download PDFInfo
- Publication number
- CN102534787B CN102534787B CN201210048104.0A CN201210048104A CN102534787B CN 102534787 B CN102534787 B CN 102534787B CN 201210048104 A CN201210048104 A CN 201210048104A CN 102534787 B CN102534787 B CN 102534787B
- Authority
- CN
- China
- Prior art keywords
- powder
- block
- bacuo
- single domain
- liquid phase
- 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
Abstract
A preparation method for single domain yttrium barium copper oxide superconductor, by preparation Y
2baCuO
5precursor powder, preparation liquid phase source powder, compacting Y
2baCuO
5pioneer's block and liquid phase block, suppress back-up block, prepare base substrate, infiltration growth single domain yttrium, barium, copper and oxygen block, ooze oxygen treatment step composition.The present invention adopts top seed crystal infiltration growth method, by adding metal oxide (Bi
2o
3powder and WO
3powder) adulterating successfully introduces second-phase nanoparticle Y
2ba
4cuBiO
x/ Y
2ba
4cuMO
x(M is Bi, W) forms magnetic flux pinning center, simplifies technique prepared by powder, the flux pinning ability shortening experimental period, reduce experimental cost, improve superconductive block.Have employed Y
2o
3prepare back-up block, in the slow cooling process of growth of yttrium, barium, copper and oxygen block, stably support two briquets above, stop the loss of liquid phase.The present invention can be used for preparing preparing YBCO superconducting blocks, also can be used for the high-temperature superconducting block preparing other series such as Gd, Sm, Nd, Eu.
Description
Technical field
The invention belongs to high temperature cuprate superconductor field of material technology, be specifically related to top seed crystal infiltration growth technique and prepare oxide-doped preparing YBCO superconducting blocks.
Background technology
Single domain copper oxide high temperature superconductive block (RE-Ba-Cu-O, wherein RE is rare earth element, as Y, Gd, Nd etc.) has higher critical temperature and critical current density, and under high-intensity magnetic field, have stronger flux pinning ability.This advantage is that the application of such material in magnetic levitation technology is laid a good foundation, and particularly has a good application prospect in super-conductive magnetic suspension bearing, accumulated energy flywheel and the development such as superconduction electricmachine and generator.In the process of preparation single domain cuprate superconductor bulk, apply more technique and mainly contain two kinds, a kind of is traditional top seed crystal Melt-Textured Growth Process, and another kind is the top seed crystal infiltration growth technique grown up recent years.
Since top seed crystal infiltration growth technique is invented, receive the attention of more and more investigator, because it can solve Problems existing in conventional melt melt texture growth technology effectively, there is a large amount of pore and macrocrack, liquid phase and to run off serious, Y in the contraction of such as sample, distortion, inside
2baCuO
5spot segregation of particle etc.But there is intrinsic lattice defect in the superconductive block prepared by infiltration growth technique, e.g., the Weak link between crystal boundary, weak flux pinning ability etc., these all govern the further raising of superconductive block performance; In addition, Y in the superconductive block prepared due to top seed crystal infiltration process
2baCuO
5the particle of particle has reached 1 μm, namely reaches its minimum grain size, therefore, will improve critical current density J further
cjust must introduce effective magnetic flux pinning center in YBCO superconductive block.Theoretically, only have when the size of the second phase particles introduced in superconductive block and the coherence length of YBCO close to time, just can play flux pinning effect effectively, and the coherence length of YBCO superconductor is nanometer scale, so only have the non-superconducting particle introducing nanometer scale as magnetic flux pinning center, effectively can control the oriented growth of superconductive block sheet tissue and Weak link phenomenon can be eliminated to greatest extent.Facts have proved, effectively improving in the method that material internal component and configuration aspects take, doping is one of the most practical method introducing useful effect pinning center, wherein, the Y with structure of double perovskite
2ba
4cuMO
x(M is Nb, Zr, W, Ag, Mo, Bi etc.) nanoparticle is introduced in YBCO superconductor as second phase particles, effectively can improve magnetic suspension force and the critical current density J of YBCO superconductor
c.But at introducing nanometer Y
2ba
4cuMO
xbefore particle, the method that we must pass through repeatedly sintering and ball milling first prepares nanometer Y
2ba
4cuMO
xpowder, so just substantially increases and introduces nanometer Y at YBCO superconductor
2ba
4cuMO
xthe cost of particle, the present invention then efficiently solves this technical barrier.
Summary of the invention
Technical problem to be solved by this invention is to provide the preparation method of the single domain yttrium barium copper oxide superconductor that a kind of levitation force is high, flux pinning ability is high.
Solve the problems of the technologies described above adopted technical scheme to be made up of following step:
1, solid phase precursor powder is prepared
By Y
2o
3with BaCO
3, CuO powder be in molar ratio 1: 1: 1 ratio mixing, make Y with solid state reaction
2baCuO
5powder, gets Y
2baCuO
5powder joins ball mill, adds Y
2baCuO
5the Bi of opaque amount 0.1% ~ 2%
2o
3powder or 0.1% ~ 3% WO
3powder, mixes, and is prepared into (1-x) Y
2baCuO
5+ xBi
2o
3or (1-y) Y
2baCuO
5+ yWO
3solid phase precursor powder.
0.001≤x≤0.02 in above formula, 0.001≤y≤0.03.
2, liquid phase source powder is prepared
By Y
2o
3with BaCO
3, CuO be in molar ratio 1: 4: 6 mixing, sinter YBa into solid state reaction
2cu
3o
7-δpowder, BaCO
3be 1: 1 in molar ratio with CuO, sinter BaCuO into solid state reaction
2powder, by YBa
2cu
3o
7-δpowder and CuO powder, BaCuO
2powder is to mix, as liquid phase source powder at 1: 2: 3 in molar ratio.
0≤δ≤1 in above formula.
3, solid phase pioneer's block and liquid phase block is suppressed
Get (1-x) Y
2baCuO
5+ xBi
2o
3solid phase precursor powder and liquid phase source powder, be pressed into (1-x) Y that shape same thickness is different respectively
2baCuO
5+ xBi
2o
3solid phase pioneer block and liquid phase block; The mass ratio of solid phase precursor powder and liquid phase source powder is 1: 1.2 ~ 1.56.
Get (1-y) Y
2baCuO
5+ yWO
3solid phase precursor powder and liquid phase source powder, be pressed into (1-y) Y that shape same thickness is different respectively
2baCuO
5+ yWO
3solid phase pioneer block and liquid phase block; The mass ratio of solid phase precursor powder and liquid phase source powder is 1: 1.2 ~ 1.56.
4, back-up block is suppressed
By Y
2o
3powder is pressed into and Y
2baCuO
5pioneer's block identical briquet block-shaped with liquid phase, as back-up block.
5, Nd-Ba-Cu oxygen seed crystal blocks is prepared
Get 54.8586gNd
2o
3, 32.1727gBaCO
3, 12.9687gCuO powder mixing, Nd
2o
3with BaCO
3, CuO powder mol ratio be 1: 1: 1, make Nd with solid state reaction
2baCuO
5powder.Get 20.9895g Y
2o
3, 49.2386gBaCO
3, 29.7719g CuO powder mixing, Nd
2o
3with BaCO
3, CuO powder mol ratio be 1: 4: 6, make NdBa with solid state reaction
2cu
3o
7-δpowder.By Nd
2baCuO
5powder and NdBa
2cu
3o
7-δpowder is to mix at 1: 3 according to mass ratio, as pioneer's block, sinters in a furnace, get naturally cleaved dice as Nd-Ba-Cu oxygen seed crystal blocks by top seed crystal melting texture method.
0≤δ≤1 in above formula.
6, base substrate assembling and laying method
At Al
2o
3pad upper surface to lower and on place MgO single-chip, back-up block, liquid phase block, (1-x) Y successively
2baCuO
5+ xBi
2o
3solid phase pioneer block or (1-y) Y
2baCuO
5+ yWO
3solid phase pioneer block, Nd-Ba-Cu oxygen seed crystal blocks.
7, infiltration growth single domain yttrium, barium, copper and oxygen block
The base substrate assembled is put into tube furnace, is warming up to 900 DEG C with the temperature rise rate of 80 ~ 120 DEG C per hour, then be warming up to 1040 ~ 1045 DEG C with the temperature rise rate of 40 ~ 60 DEG C per hour, be incubated 1 ~ 2.5 hour; Be cooled to 1015 ~ 1025 DEG C with the rate of temperature fall of 60 DEG C per hour, with rate of temperature fall slow cooling to 980 ~ 990 DEG C of 0.1 ~ 0.5 DEG C per hour, naturally cool to room temperature with stove, obtain single domain yttrium, barium, copper and oxygen block.
8, oxygen process is oozed
Inserted by single domain yttrium, barium, copper and oxygen block in quartz tube furnace, in circulation oxygen atmosphere, in the warm area of 440 ~ 410 DEG C, slow cooling 200 hours, obtains single domain yttrium barium copper oxide superconductor.
In preparation solid phase precursor powder step 1 of the present invention, get Y
2baCuO
5powder joins ball mill, adds Y
2baCuO
5the Bi of opaque amount 0.7%
2o
3powder, mixes, and is prepared into (1-x) Y
2baCuO
5+ xBi
2o
3solid phase precursor powder.At compacting (1-x) Y
2baCuO
5+ xBi
2o
3gu in pioneer's block and liquid phase block step 3, the optimum quality ratio of solid phase precursor powder and liquid phase source powder is 1: 1.44.In infiltration growth single domain yttrium, barium, copper and oxygen block step 6, the pioneer's block assembled is put into tube furnace, and the best is warming up to 900 DEG C with the temperature rise rate of 100 DEG C per hour, then is warming up to 1045 DEG C with the temperature rise rate of 50 DEG C per hour, is incubated 2 hours; The best is cooled to 1020 DEG C with the rate of temperature fall of 60 DEG C per hour, then with the rate of temperature fall slow cooling to 990 DEG C of 0.3 DEG C per hour, naturally cools to room temperature, obtain single domain yttrium barium copper oxide superconductor with stove.
In preparation solid phase precursor powder step 1 of the present invention, get Y
2baCuO
5powder joins ball mill, adds Y
2baCuO
5the WO of opaque amount 1.5%
3powder, mixes, and is prepared into (1-y) Y
2baCuO
5+ yWO
3solid phase precursor powder.At compacting (1-y) Y
2baCuO
5+ yWO
3in solid phase pioneer block and liquid phase block step 3, the optimum quality ratio of solid phase precursor powder and liquid phase source powder is 1: 1.44.In infiltration growth single domain yttrium, barium, copper and oxygen block step 6, the pioneer's block assembled is put into tube furnace, and the best is warming up to 900 DEG C with the temperature rise rate of 100 DEG C per hour, then is warming up to 1045 DEG C with the temperature rise rate of 50 DEG C per hour, is incubated 2 hours; The best is cooled to 1020 DEG C with the rate of temperature fall of 60 DEG C per hour, then with the rate of temperature fall slow cooling to 990 DEG C of 0.3 DEG C per hour, naturally cools to room temperature, obtain single domain yttrium barium copper oxide superconductor with stove.
Prepare in base substrate 5 of the present invention, MgO single-chip has contour 3 ~ 5.
Prepare in base substrate 5 in the present invention, back-up block of the present invention, liquid phase block, solid phase pioneer block are the right cylinder that external diameter is identical.
The present invention adopts top seed crystal infiltration growth method, by adding Bi
2o
3powder and other doped metallic oxide successfully introduce second-phase nanoparticle Y
2ba
4cuBiO
x/ Y
2ba
4cuMO
x(M is Bi, W) forms magnetic flux pinning center, invention not only simplifies technique prepared by powder, shortens experimental period, reduces experimental cost, and further increase the flux pinning ability of superconductive block.In the present invention, have employed Y
2o
3prepare back-up block, in the slow cooling process of growth of yttrium, barium, copper and oxygen block, stably support two briquets above, stop the loss of liquid phase.The present invention can be used for preparing preparing YBCO superconducting blocks, also can be used for the high-temperature superconducting block preparing other series such as Y, Sm, Nd, Eu.
Accompanying drawing explanation
Fig. 1 is the structural representation that in embodiment 1, in stove, sample is placed.
Fig. 2 is the surface topography map of single domain yttrium barium copper oxide superconductor prepared by embodiment 1.
Fig. 3 is the magnetic suspension force graphic representation of single domain yttrium barium copper oxide superconductor prepared by embodiment 1.
Fig. 4 is the magnetic suspension force graphic representation of single domain yttrium barium copper oxide superconductor prepared by embodiment 4.
Fig. 5 is the environmental scanning electronic microscope figure of the single domain yttrium barium copper oxide superconductor of embodiment 1
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in more detail, but the invention is not restricted to these embodiments.
Embodiment 1
With doped raw material Bi used
2o
3powder is that example prepares single domain yttrium barium copper oxide superconductor, and its preparation method is as follows:
1, preparation doping Bi
2o
3the Y of powder
2aCuO
5precursor powder
Get 67.3803g Y
2o
3, 58.88387g BaCO
3, 23.7359g CuO powder mixes, Y
2o
3with BaCO
3, CuO powder mol ratio be 1: 1: 1, make Y with solid state reaction
2baCuO
5powder.Get 100g Y
2baCuO
5powder joins ball mill, adds Y
2baCuO
5the Bi of opaque amount 0.7%
2o
3powder, mixes, and is prepared into Y
2baCuO
5precursor powder.
2, liquid phase source powder is prepared
Get 106.9064g BaCO
3, 43.0936g CuO mixes, BaCO
3be 1: 1 with the mol ratio of CuO powder, make BaCuO with solid state reaction
2powder.Get 22.6956g Y
2o
3, 79.3350g BaCO
3, 47.9695g CuO powder mixing, Y
2o
3with BaCO
3, CuO powder mol ratio be 1: 4: 6, make YBa with solid state reaction
2cu
3o
7-δpowder.By 81.4516gBaCuO
2powder, 18.5484gCuO powder, 76.7389g YBa
2cu
3o
7-δpowder mixes at ball mill, YBa
2cu
3o
7-δpowder and CuO, BaCuO
2the mol ratio of powder is 1: 2: 3, as liquid phase source powder.
0≤δ≤1 in above formula.
3, compacting doping Bi
2o
3the Y of powder
2baCuO
5pioneer's block and liquid phase block
Get 9g doping Bi
2o
3the Y of powder
2baCuO
5precursor powder, 13g liquid phase source powder, Y
2baCuO
5the mass ratio of precursor powder and liquid phase source powder is 1: 1.44, is pressed into liquid phase body and Y respectively
2baCuO
5precursor, liquid phase body and Y
2baCuO
5precursor is diameter is the right cylinder that 20mm, thickness are not identical.
4, back-up block is suppressed
Get 2.5gY
2o
3powder is pressed into the back-up block that diameter is 20mm.
5, Nd-Ba-Cu oxygen seed crystal blocks is prepared
Get 54.8586g Nd
2o
3, 32.1727g BaCO
3, 12.9687g CuO powder mixing, Nd
2o
3with BCO
3, CuO powder mol ratio be 1: 1: 1, become Nd with solid state reaction
2baCuO
5powder.Get 20.9895g Y
2o
3, 49.2386gBaCO
3, 29.7719g CuO powder mixing, Nd
2o
3with BaCO
3, CuO powder mol ratio be 1: 4: 6, make NdBa with solid state reaction
2cu
3o
7-δpowder.By Nd
2baCuO
5powder and NdBa
2cu
3o
7-δpowder is to mix at 1: 3 according to mass ratio, as pioneer's block, sinters in a furnace, get naturally cleaved dice as Nd-Ba-Cu oxygen seed crystal blocks by top seed crystal melting texture method.
0≤δ≤1 in above formula.
6, base substrate assembling and laying method
As shown in Figure 1, at Al
2o
3pad 6 upper surface to lower and on place successively 4 MgO single-chips 5, back-up block 4, liquid phase block 3, doping Bi
2o
3the Y of powder
2baCuO
5the height of pioneer's block 2, Nd-Ba-Cu oxygen seed crystal blocks Isosorbide-5-Nitrae sheet MgO single-chip 5 is identical, and Nd-Ba-Cu oxygen seed crystal blocks 1 is positioned at doping Bi
2o
3the Y of powder
2baCuO
5the central position of pioneer's block 2 upper surface.
7, infiltration growth single domain yttrium, barium, copper and oxygen block
The base substrate assembled is put into tube furnace, is warming up to 900 DEG C with the temperature rise rate of 100 DEG C per hour, then be warming up to 1045 DEG C with the temperature rise rate of 50 DEG C per hour, be incubated 2 hours; Be cooled to 1020 DEG C with the rate of temperature fall of 60 DEG C per hour, with the rate of temperature fall slow cooling to 990 DEG C of 0.3 DEG C per hour, naturally cool to room temperature with stove, obtain single domain yttrium, barium, copper and oxygen block.
8, oxygen process is oozed
Inserted by single domain yttrium, barium, copper and oxygen block in quartz tube furnace, in circulation oxygen atmosphere, in the warm area of 410 ~ 440 DEG C, slow cooling 200 hours, is prepared into single domain yttrium barium copper oxide superconductor.
Prepared single domain yttrium barium copper oxide superconductor, take surface topography with photographic camera, Fig. 2 is shown in by surface topography photo.The Bi adulterated in a, b, c, d, e, f in figure
2o
3particle content is followed successively by 0.1wt%, 0.3wt%, 0.5wt%, 0.7wt%, 0.9wt%, 2wt%, and as seen from Figure 2, its surface all generates four symmetrical sectors of position centered by seed crystal, and has obvious cross decorative pattern.Along with Bi
2o
3the continuation of particle doping increases, and the pattern of sample there occurs trickle change, and the growth district of yttrium barium copper oxide crystal presents the trend of reduction.
To prepared single domain yttrium barium copper oxide superconductor, three-dimensional magnetic field and magnetic force test set is adopted to measure its magnetic suspension force, test result is shown in graphic representation 3, the ratio of magnetic suspension force and single domain yttrium, barium, copper and oxygen superconducting block top surface area (upper surface diameter is 20mm) is magnetic suspension force density, as seen from Figure 3, Bi
2o
3the magnetic suspension force of the preparing YBCO superconducting blocks prepared when being 0.7wt% of doping be 24.48N to the maximum, corresponding magnetic suspension force density is 7.80N/cm
2.
Embodiment 2
With doped raw material Bi used
2o
3powder is that example prepares single domain yttrium barium copper oxide superconductor, and its preparation method is as follows:
At preparation doping Bi
2o
3the Y of powder
2baCuO
5in precursor powder step 1, preparation Y
2baCuO
5the raw material that powder is used and preparation method identical with embodiment 1, get 100g Y
2baCuO
5powder joins ball mill and mixes, and adds Y
2baCuO
5the Bi of opaque amount 0.1%
2o
3, mix, be prepared into doping Bi
2o
3the Y of powder
2baCuO
5precursor powder; At compacting doping Bi
2o
3the Y of powder
2baCuO
5in pioneer's block and liquid phase block step 3, get 9g and to adulterate Bi
2o
3the Y of powder
2baCuO
5precursor powder, 10.8g liquid phase source powder, doping Bi
2o
3the Y of powder
2baCuO
5the mass ratio of precursor powder and liquid phase source powder is 1: 1.2, is pressed into the doping Bi that shape same thickness is different respectively
2o
3the Y of powder
2baCuO
5precursor, liquid phase body; In infiltration growth single domain yttrium, barium, copper and oxygen block step 7, the base substrate assembled is put into tube furnace, 900 DEG C are warming up to the temperature rise rate of 80 DEG C per hour, 1045 DEG C are warming up to again with the temperature rise rate of 40 DEG C per hour, be incubated 1 hour, be cooled to 1015 DEG C with the rate of temperature fall of 60 DEG C per hour, with the rate of temperature fall slow cooling to 990 DEG C of 0.1 DEG C per hour, naturally cool to room temperature with stove, obtain single domain yttrium, barium, copper and oxygen block.Other steps are identical with embodiment 1, are prepared into single domain yttrium barium copper oxide superconductor.
Embodiment 3
With doped raw material Bi used
2o
3powder is that example prepares single domain yttrium barium copper oxide superconductor, and its preparation method is as follows:
At preparation doping Bi
2o
3the Y of powder
2baCuO
5in precursor powder step 1, preparation Y
2baCuO
5the raw material that powder is used and preparation method identical with embodiment 1, get 100gY
2baCuO
5powder joins ball mill and mixes, and adds Y
2baCuO
5the Bi of opaque amount 2%
2o
3, mix, be prepared into doping Bi
2o
3the Y of powder
2baCuO
5precursor powder; At compacting doping Bi
2o
3the Y of powder
2baCuO
5in pioneer's block and liquid phase block step 3, get 9g and to adulterate Bi
2o
3the Y of powder
2baCuO
5precursor powder, 14.04g liquid phase source powder, doping Bi
2o
3the Y of powder
2baCuO
5the mass ratio of precursor powder and liquid phase source powder is 1: 1.56, is pressed into the doping Bi that shape same thickness is different respectively
2o
3the Y of powder
2baCuO
5precursor, liquid phase body; In infiltration growth single domain yttrium, barium, copper and oxygen block step 7, the base substrate assembled is put into tube furnace, 900 DEG C are warming up to the temperature rise rate of 120 DEG C per hour, 1040 DEG C are warming up to again with the temperature rise rate of 60 DEG C per hour, be incubated 2.5 hours, be cooled to 1025 DEG C with the rate of temperature fall of 60 DEG C per hour, with the rate of temperature fall slow cooling to 980 DEG C of 0.5 DEG C per hour, naturally cool to room temperature with stove, obtain single domain yttrium, barium, copper and oxygen block.Other steps are identical with embodiment 1, are prepared into single domain yttrium barium copper oxide superconductor.
Embodiment 4
With doped raw material WO used
3powder is that example prepares single domain yttrium barium copper oxide superconductor, and its preparation method is as follows:
At the preparation Y of above embodiment 1 ~ 3
2baCuO
5in the step 1 of precursor powder, preparation Y
2baCuO
5the raw material that powder is used and preparation method identical with embodiment 1.Get 100g Y
2baCuO
5powder joins ball mill, the Bi of interpolation
2o
3powder Y
2baCuO
5the WO of opaque amount 1.5%
3powder is replaced, and mixes, is prepared into Y
2baCuO
5precursor powder.Other steps are identical with corresponding embodiment, are prepared into single domain yttrium barium copper oxide superconductor.
Prepared single domain yttrium barium copper oxide superconductor adopts three-dimensional magnetic field and magnetic force test set to test magnetic suspension force, test result is shown in graphic representation 4, the ratio of magnetic suspension force and single domain yttrium, barium, copper and oxygen superconducting block top surface area (upper surface diameter is 20mm) is magnetic suspension force density, as seen from Figure 4, WO
3the magnetic suspension force of the preparing YBCO superconducting blocks prepared when being 1.5wt% of doping be 25.76N to the maximum, corresponding magnetic suspension force density is 8.20N/cm
2.
Embodiment 5
With doped raw material WO used
3powder is that example prepares single domain yttrium barium copper oxide superconductor, and its preparation method is as follows:
At the preparation Y of above embodiment 1 ~ 3
2baCuO
5in the step 1 of pioneer's powder, preparation Y
2baCuO
5the raw material that powder is used and preparation method identical with embodiment 1.Get 100g Y
2baCuO
5powder joins ball mill, the Bi of interpolation
2o
3powder Y
2baCuO
5the WO of powder quality 0.1%
3powder is replaced, and mixes, is prepared into Y
2baCuO
5precursor powder.Other steps are identical with corresponding embodiment, are prepared into single domain yttrium barium copper oxide superconductor, and prepared single domain yttrium barium copper oxide superconductor adopts three-dimensional magnetic field and magnetic force test set to test magnetic suspension force, and test result is shown in graphic representation 4.
Embodiment 6
With doped raw material WO used
3powder is that example prepares single domain yttrium barium copper oxide superconductor, and its preparation method is as follows:
At the preparation Y of above embodiment 1 ~ 3
2baCuO
5in the step 1 of precursor powder, preparation Y
2baCuO
5the raw material that powder is used and preparation method identical with embodiment 1.Get 100g Y
2baCuO
5powder joins ball mill, the Bi of interpolation
2o
3powder Y
2baCuO
5the WO of opaque amount 3%
3powder is replaced, and mixes, is prepared into Y
2baCuO
5precursor powder.Other steps are identical with corresponding embodiment, are prepared into single domain yttrium barium copper oxide superconductor, and prepared single domain yttrium barium copper oxide superconductor adopts three-dimensional magnetic field and magnetic force test set to test magnetic suspension force, and test result is shown in graphic representation 4.
In order to determine optimum material proportion of the present invention, inventors performed a large amount of laboratory study tests, various experimental conditions is as follows:
1, different oxide compounds is on the impact of single domain yttrium barium copper oxide superconductor pattern and magnetic suspension force
The preparation method of embodiment 1 is adopted to prepare single domain yttrium barium copper oxide superconductor.At preparation Y
2baCuO
5in precursor powder step 1, by analytically pure Y
2o
3(>=99.9%), BaCO
3(>=99.9%) and CuO (>=99.9%) massage that, than the ratio mixing being 1: 1: 1, makes Y with solid state reaction
2baCuO
5powder.Get Y
2baCuO
5powder joins ball mill, and add metal oxide, oxide compound selects Bi
2o
3powder, WO
3any one in powder, mixes, is prepared into Y
2baCuO
5precursor powder, Bi
2o
3powder, WO
3the consumption of powder is as follows:
(1) Y is added
2baCuO
5the Bi of opaque amount 0.1%, 0.3%, 0.5%, 0.7%, 0.9%, 2%
2o
3powder, mixes, and is prepared into Y
2baCuO
5precursor powder.Other steps are identical with embodiment 1, and being prepared into diameter is 20mm single domain yttrium barium copper oxide superconductor, adopt three-dimensional magnetic field and magnetic force test set to test magnetic suspension force respectively to prepared single domain yttrium barium copper oxide superconductor.Test result is in table 1 and Fig. 3, and in figure 3, curve a is 0.1wt%Bi
2o
3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping, curve b is 0.3wt%Bi
2o
3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping, curve c is 0.5wt%Bi
2o
3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping, curve d is 0.7wt%Bi
2o
3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping, curve e is 0.9wt%Bi
2o
3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping, curve f is 2.0wt%Bi
2o
3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping.Fig. 2 is seen, the Bi adulterated in a, b, c, d, e, f in figure with the take pictures surface topography map of single domain yttrium barium copper oxide superconductor of photographic camera
2o
3particle content is followed successively by 0.1wt%, 0.3wt%, 0.5wt%, 0.7wt%, 0.9wt%, 2wt%.Analyze by the structure of environmental scanning electronic microscope to single domain yttrium barium copper oxide superconductor, stereoscan photograph is shown in Fig. 5, the Bi adulterated in a, b, c, d, e, f in Fig. 5
2o
3particle content is followed successively by 0.1wt%, 0.3wt%, 0.5wt%, 0.7wt%, 0.9wt%, 2wt%.
The magnetic suspension force test data of single domain yttrium barium copper oxide superconductor prepared by table 1 embodiment 1
As seen from Figure 2, the surface of preparing YBCO superconducting blocks has all grown up to four symmetrical sectors of position centered by Nd-Ba-Cu oxygen seed crystal, and has obvious cross decorative pattern.Along with Bi
2o
3the increase of doping, the surface topography of preparing YBCO superconducting blocks there occurs trickle change, and the growth district of preparing YBCO superconducting blocks presents the trend of reduction.From table 1 and Fig. 3, Bi
2o
3the magnetic suspension force that particle doping is followed successively by the preparing YBCO superconducting blocks of 0.1wt%, 0.3wt%, 0.5wt%, 0.7wt%, 0.9wt%, 2wt% be respectively 6.84N, 18.48,21.72N, 24.48N, 12.42N, 5.76N, as can be seen here, work as Bi
2o
3when particle doping is 0.7wt%, the magnetic suspension force of preparing YBCO superconducting blocks is up to 24.48N.As seen from Figure 5, be distributed with two kinds of particles in yttrium barium copper oxide superconduction matrix, wherein larger canescence particle is Y
2baCuO
5phase, it is evenly distributed in the middle of yttrium barium copper oxide superconduction matrix, and the size of particle is 1.0 μm ~ 5.0 μm; The particle of another less point-like is by Bi
2o
3particle reacts the nanometer Y of generation under semi-melting state
2ba
4cuMO
xparticle, the size of particle, between 80nm ~ 160nm, compares Y
2baCuO
5particle is little one to two orders of magnitude, relative to Y
2baCuO
5particle, Y
2ba
4cuBiO
xbe on good terms and play flux pinning effect better, thus effectively can improve flux pinning ability and the magnetic suspension force of superconductive block.
(2) Y is added
2baCuO
5opaque amount 0.1%, 0.5%, 0.8%, 1.5%, 2.0%, the WO of 3.0wt%
3powder, mixes, and is prepared into Y
2baCuO
5precursor powder.Other steps are identical with embodiment 1, are prepared into single domain yttrium barium copper oxide superconductor.Being prepared into diameter is 20mm preparing YBCO superconducting blocks, and adopts three-dimensional magnetic field and magnetic force test set to test magnetic suspension force to prepared single domain yttrium barium copper oxide superconductor respectively, and test result is in table 2 and Fig. 4.In the diagram, curve a is 0.1wt%WO
3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping, curve b is 0.5wt%WO
3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping, curve c is 0.8wt%WO
3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping, curve d is 1.5wt%WO
3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping, curve e is 2.0wt%WO
3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping, curve f is 3.0wt%WO
3the magnetic suspension force curve of the single domain yttrium barium copper oxide superconductor of particle doping.
The magnetic suspension force test data of single domain yttrium barium copper oxide superconductor prepared by table 2 embodiment 4
From table 2 and Fig. 4, WO
3particle doping is followed successively by 0.1%, 0.5%, 0.8%, 1.5%, 2.0%, the magnetic suspension force of the preparing YBCO superconducting blocks of 3.0wt% is respectively 11.62N, 14.16N, 23.68N, 25.76N, 21.74N, 5.22N, as can be seen here, works as WO
3when particle doping is 1.5wt%, the magnetic suspension force of preparing YBCO superconducting blocks is up to 25.76N.
Claims (1)
1. a preparation method for single domain yttrium barium copper oxide superconductor, is characterized in that it is made up of following step:
(1) solid phase precursor powder is prepared
By Y
2o
3with BaCO
3, CuO powder be in molar ratio 1:1:1 ratio mixing, make Y with solid state reaction
2baCuO
5powder, gets Y
2baCuO
5powder joins ball mill, adds Y
2baCuO
5the WO of opaque amount 1.5%
3powder, mixes, and is prepared into solid phase precursor powder;
(2) liquid phase source powder is prepared
By Y
2o
3with BaCO
3, CuO be in molar ratio 1:4:6 mixing, sinter YBa into solid state reaction
2cu
3o
7-δpowder, BaCO
3be 1:1 in molar ratio with CuO, sinter BaCuO into solid state reaction
2powder, by YBa
2cu
3o
7-δpowder and CuO powder, BaCuO
2powder mixes for 1:2:3 in molar ratio, as liquid phase source powder;
0≤δ≤1 in above formula;
(3) solid phase pioneer's block and liquid phase block is suppressed
Get solid phase precursor powder and liquid phase source powder, being pressed into diameter is respectively the different solid phase pioneer block of 20mm thickness and liquid phase block; The mass ratio of solid phase precursor powder and liquid phase source powder is 1:1.44%;
(4) back-up block is suppressed
By Y
2o
3powder is pressed into the briquet that diameter is 20mm, as back-up block;
(5) Nd-Ba-Cu oxygen seed crystal blocks is prepared
Get 54.8586g Nd
2o
3, 32.1727g BaCO
3, 12.9687g CuO powder mixing, Nd
2o
3with BaCO
3, CuO powder mol ratio be 1:1:1, make Nd with solid state reaction
2baCuO
5powder; Get 20.9895g Y
2o
3, 49.2386gBaCO
3, 29.7719g CuO powder mixing, Nd
2o
3with BaCO
3, CuO powder mol ratio be 1:4:6, make NdBa with solid state reaction
2cu
3o
7-δpowder; By Nd
2baCuO
5powder and NdBa
2cu
3o
7-δpowder is that 1:3 mixes according to mass ratio, as pioneer's block, sinters in a furnace, get naturally cleaved dice as Nd-Ba-Cu oxygen seed crystal blocks by top seed crystal melting texture method;
0≤δ≤1 in above formula;
(6) base substrate assembling and laying method
At Al
2o
3pad (6) upper surface to lower and on place MgO single-chip (5), back-up block (4), liquid phase block (3), solid phase pioneer block, Nd-Ba-Cu oxygen seed crystal blocks (1) successively;
(7) infiltration growth single domain yttrium, barium, copper and oxygen block
The base substrate assembled is put into tube furnace, is warming up to 900 DEG C with the temperature rise rate of 100 DEG C per hour, then be warming up to 1045 DEG C with the temperature rise rate of 50 DEG C per hour, be incubated 2 hours; Be cooled to 1020 DEG C with the rate of temperature fall of 60 DEG C per hour, with the rate of temperature fall slow cooling to 990 DEG C of 0.3 DEG C per hour, naturally cool to room temperature with stove, obtain single domain yttrium, barium, copper and oxygen block;
(8) oxygen process is oozed
Inserted by single domain yttrium, barium, copper and oxygen block in quartz tube furnace, in circulation oxygen atmosphere, in the warm area of 440 ~ 410 DEG C, slow cooling 200 hours, obtains single domain yttrium barium copper oxide superconductor.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201210048104.0A CN102534787B (en) | 2012-02-28 | 2012-02-28 | The preparation method of single domain yttrium barium copper oxide superconductor |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201210048104.0A CN102534787B (en) | 2012-02-28 | 2012-02-28 | The preparation method of single domain yttrium barium copper oxide superconductor |
Publications (2)
Publication Number | Publication Date |
---|---|
CN102534787A CN102534787A (en) | 2012-07-04 |
CN102534787B true CN102534787B (en) | 2015-08-19 |
Family
ID=46342767
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201210048104.0A Active CN102534787B (en) | 2012-02-28 | 2012-02-28 | The preparation method of single domain yttrium barium copper oxide superconductor |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN102534787B (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US11858853B2 (en) | 2018-09-24 | 2024-01-02 | Imam Abdulrahman Bin Faisal University | Method for making a superconducting YBCO wire or tape |
Families Citing this family (17)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102942359B (en) * | 2012-11-29 | 2014-07-02 | 陕西师范大学 | Preparation method of single domain GdBaCuO superconductor block |
CN102924075B (en) * | 2012-11-29 | 2014-12-24 | 陕西师范大学 | Method for producing single domain yttrium barium copper oxide superconduction block |
CN102925954B (en) * | 2012-11-29 | 2015-05-13 | 陕西师范大学 | Method for preparing single domain yttrium barium copper oxide superconduction block by top seed infiltration process |
CN103361710B (en) * | 2013-07-18 | 2016-02-17 | 陕西师范大学 | Improve the method for single domain yttrium barium copper oxide superconductor preparation efficiency |
CN103979951B (en) * | 2014-05-22 | 2015-04-15 | 天津师范大学 | Method for preparing single-domain yttrium barium copper oxide bulk superconductor by taking Y2BaCuO5 as base material |
CN103951434B (en) * | 2014-05-22 | 2015-07-15 | 天津师范大学 | Method for preparing single-domain yttrium-barium-copper-oxygen superconducting block in liquid-phase source coated infiltration growing manner |
CN104790036B (en) * | 2015-03-02 | 2017-06-16 | 天津师范大学 | The method that nano combined preparing YBCO superconducting blocks are grown with ytterbium base liquid phase source infiltration |
CN106348747B (en) * | 2016-08-19 | 2019-06-07 | 陕西师范大学 | Easily remove the remaining single domain yttrium barium copper oxide superconductor preparation method of liquid phase source |
CN106431403B (en) * | 2016-10-18 | 2019-10-22 | 天津师范大学 | A kind of preparation method of the preparing YBCO superconducting blocks of nanometer of bismuth ferrite doping |
CN107059127B (en) * | 2017-03-17 | 2019-04-16 | 陕西师范大学 | A kind of method of bottom seed crystal infiltration growth method preparation single domain rare earth barium copper oxide superconducting ring |
CN107287658B (en) * | 2017-04-28 | 2019-08-16 | 陕西师范大学 | A kind of method that pure-oxide pre-sintering method prepares single domain yttrium barium copper oxide superconductor |
US11107967B2 (en) | 2018-10-16 | 2021-08-31 | Imam Abdulrahman Bin Faisal University | Yttrium-based superconductors with tungsten nano-structures |
CN111768926B (en) * | 2020-07-31 | 2021-04-30 | 西北有色金属研究院 | Preparation method of Bi-2212 superconducting coating |
CN113443907A (en) * | 2021-04-26 | 2021-09-28 | 傲普(上海)新能源有限公司 | Material performance improvement method for high-temperature superconducting flywheel energy storage |
CN113912389B (en) * | 2021-10-25 | 2022-08-12 | 天津师范大学 | Method for improving performance of yttrium barium copper oxide superconducting block by adding 358 barium copper oxide into solid phase block |
CN114214728B (en) * | 2021-11-19 | 2024-04-02 | 陕西师范大学 | Method for improving seed crystal utilization rate by floor type SMG |
CN114057485B (en) * | 2021-12-10 | 2022-10-28 | 天津师范大学 | Method for improving performance of yttrium barium copper oxide superconducting block by co-doping nano ytterbium oxide and nano bismuth oxide |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101665980A (en) * | 2009-09-25 | 2010-03-10 | 陕西师范大学 | Infiltration method for preparing single-domain Gd-Ba-Cu-O superconducting block |
-
2012
- 2012-02-28 CN CN201210048104.0A patent/CN102534787B/en active Active
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101665980A (en) * | 2009-09-25 | 2010-03-10 | 陕西师范大学 | Infiltration method for preparing single-domain Gd-Ba-Cu-O superconducting block |
Non-Patent Citations (2)
Title |
---|
Y2Ba4CuWOx掺杂对单畴YBCO块材超导性能的影响;王高峰等;《西安邮电学院学报》;20111231;第16卷(第S2期);26-28 * |
纳米粒子掺杂对TS-MTG单畴YBCO超导块材性能的影响;高平;《中国优秀硕士学位论文全文数据库 工程科技Ⅱ辑》;20111015(第10期);C042-8 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US11858853B2 (en) | 2018-09-24 | 2024-01-02 | Imam Abdulrahman Bin Faisal University | Method for making a superconducting YBCO wire or tape |
Also Published As
Publication number | Publication date |
---|---|
CN102534787A (en) | 2012-07-04 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN102534787B (en) | The preparation method of single domain yttrium barium copper oxide superconductor | |
CN102925954B (en) | Method for preparing single domain yttrium barium copper oxide superconduction block by top seed infiltration process | |
CN102942359B (en) | Preparation method of single domain GdBaCuO superconductor block | |
CN102924075B (en) | Method for producing single domain yttrium barium copper oxide superconduction block | |
CN106205861B (en) | Preparation method for graphene-loaded multielement-doped magnesium diboride superconducting bulk material | |
Shalaby et al. | The impact of the addition of Bi2Te3 nanoparticles on the structural and the magnetic properties of the Bi-2223 high-Tc superconductor | |
CN104725035B (en) | A kind of preparation method of nano combined preparing YBCO superconducting blocks | |
CN107059127A (en) | A kind of bottom seed crystal infiltration growth method prepares the method for single domain rare earth barium copper oxide superconducting ring and its superconducting ring of preparation | |
CN103979951A (en) | Method for preparing single-domain yttrium barium copper oxide bulk superconductor by taking Y2BaCuO5 as base material | |
Hlásek et al. | Cost-effective isothermal top-seeded melt-growth of single-domain YBCO superconducting ceramics | |
CN101279847A (en) | Preparation for YBCO Superconducting bulk doped with trace rare-earth element | |
US8193122B2 (en) | Superconductor fabrication | |
CN103614775B (en) | The method of the accurate single crystal of a kind of embedded seeded growth REBCO | |
Belala et al. | Transport and magnetic properties of Bi (Pb) 2212 superconducting ceramics doped by low rate of potassium | |
CN104313692A (en) | Method for preparing single-domain (Gd/Y)-Ba-Cu-O superconductive bulk by liquid phase infiltration method | |
CN103396114B (en) | Simplified preparation method of single-domain YBCO (Yttrium Barium Copper Oxide) superconducting bulk material | |
CN103361710B (en) | Improve the method for single domain yttrium barium copper oxide superconductor preparation efficiency | |
CN103603043B (en) | The method of the accurate single crystal of a kind of embedded seeded growth calcium analysis YBCO | |
JP2007527350A (en) | Method for manufacturing a doped superconductor material | |
CN103060915B (en) | The preparation method of the single domain SmBCO oxygen bulk that crackle can be suppressed to produce | |
CN1328214C (en) | Method for preparing single domain Dy-Ba-Cu-O superconductive block | |
CN105236952A (en) | Preparation method of yttrium barium copper oxide superconductive block material doped with nano nickel ferrite | |
CN105177712A (en) | Method for growing REBCO high-temperature superconductor | |
Miryala | Development of MgB2 Superconducting Super-Magnets: Its Utilization towards Sustainable Development Goals | |
CN106431403B (en) | A kind of preparation method of the preparing YBCO superconducting blocks of nanometer of bismuth ferrite doping |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant |