CN102534787A - Preparation method of single domain yttrium barium copper oxide superconductor - Google Patents

Preparation method of single domain yttrium barium copper oxide superconductor Download PDF

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CN102534787A
CN102534787A CN2012100481040A CN201210048104A CN102534787A CN 102534787 A CN102534787 A CN 102534787A CN 2012100481040 A CN2012100481040 A CN 2012100481040A CN 201210048104 A CN201210048104 A CN 201210048104A CN 102534787 A CN102534787 A CN 102534787A
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bacuo
piece
block
oxygen
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CN102534787B (en
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杨万民
王妙
李国政
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Shaanxi Normal University
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Shaanxi Normal University
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Abstract

The invention relates to a preparation method of a single domain yttrium barium copper oxide superconductor; and the preparation method comprises the following steps: preparing Y2BaCuO5 precursor powder and liquid phase source powder, pressing a Y2BaCuO5 precursor block, a liquid phase block and a supporting bock, preparing a green body, growing a single domain yttrium barium copper oxide block in an infiltration manner, and carrying out oxygen permeation processing. A second phase nanoparticle Y2Ba4CuBiOx/Y2Ba4CuMOx (M is Bi or W) is successfully introduced for forming a flux pinning center by adopting a top seed crystal infiltration growing method and adding a metallic oxide (Bi2O3 powder and WO3 powder) for doping, thereby the powder preparation technology is simplified, the experimental period is shortened, the experiment cost is reduced, and the flux pinning capacity of the superconductor is increased. Y2O3 is used for preparing the supporting block which stably supports two briquettes above the supporting block in the slow cold growing process of an yttrium barium copper oxide block so as to prevent liquid phase from running off. The preparation method can be used for preparing the yttrium barium copper oxide superconductor and can also be used for preparing high-temperature superconductors of other series such as Gd, Sm, Nd, Eu and the like.

Description

The preparation method of single domain yttrium, barium, copper and oxygen superconductive block
Technical field
The invention belongs to high temperature cuprate superconductor material technology field, 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 superconducting block (RE-Ba-Cu-O, wherein RE is a REE, like Y, Gd, Nd etc.) has higher critical temperature and critical current density, and under high-intensity magnetic field, has stronger flux pinning ability.This advantage is that the application of said material aspect magnetic levitation technology laid a good foundation, and is particularly having a good application prospect aspect the developments such as super-conductive magnetic suspension bearing, accumulated energy flywheel and superconduction electricmachine and generator.In the process of preparation single domain cuprate superconductor bulk, use more technology and mainly contain two kinds, a kind of is traditional top seed crystal melting texture growing technology, another kind is the top seed crystal infiltration growth technique that grows up recent years.
Since top seed crystal infiltration growth technique is invented; Received more and more investigators' attention; Because it can solve the problem that exists in traditional melting texture growing technology effectively, for example the contraction of sample, distortion, inside exist a large amount of pores and macrocrack, liquid phase run off serious, Y 2BaCuO 5Spot segregation of particle or the like.But exist the inherent lattice defect in the superconductive block that goes out owing to the infiltration growth technique is prepared, as, the weak connection between crystal boundary, weak flux pinning ability etc., these are all restricting the further raising of superconductive block performance; In addition, because Y in the superconductive block prepared of top seed crystal infiltration process 2BaCuO 5The particle of particle has reached 1 μ m, promptly reaches its minimum grain size, therefore, further improve critical current density J cJust must in the YBCO superconductive block, introduce effective flux pinning center.Theoretically; Have only when the coherence length of the size of the second phase particle of introducing in the superconductive block and YBCO near the time; Just can play flux pinning effect effectively; And the coherence length of YBCO superconductor is a nanometer scale, so have only the non-superconducting particle of introducing nanometer scale as the flux pinning center, can control the oriented growth of superconductive block sheet tissue effectively and can eliminate the weak phenomenon that connects to greatest extent.Facts have proved that in improving the method that material internal component and structure aspects take effectively, doping is one of the most practical method of introducing useful effect pinning center, wherein, Y with structure of double perovskite 2Ba 4CuMO x(M is Nb, Zr, W, Ag, Mo, Bi etc.) nanoparticle is introduced in the YBCO superconductor as the second phase particle, can improve the magnetic suspension force and the critical current density J of YBCO superconductor effectively cBut introducing nanometer Y 2Ba 4CuMO xBefore the particle, we must prepare nanometer Y earlier through the method for sintering and ball milling repeatedly 2Ba 4CuMO xPowder has so just improved greatly at the YBCO superconductor and has introduced nanometer Y 2Ba 4CuMO xThe cost of particle, the present invention has then solved this technical barrier effectively.
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 and oxygen superconductive block that a kind of magnetic suspension force performance is high, the flux pinning ability is high.
Solving the problems of the technologies described above the technical scheme that is adopted is made up of following step:
1, preparation solid phase precursor powder
With Y 2O 3With BaCO 3, the CuO powder is 1: 1: 1 mixed in molar ratio, processes Y with solid state reaction 2BaCuO 5Powder is got 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 3The solid phase precursor powder.
0.001≤x in the following formula≤0.02,0.001≤y≤0.03.
2, preparation liquid phase source powder
With Y 2O 3With BaCO 3, CuO mixes at 1: 4: 6, sinters YBa into solid state reaction 2Cu 3O 7-δPowder, BaCO 3With CuO be 1: 1 in molar ratio, sinter BaCuO into solid state reaction 2Powder is with YBa 2Cu 3O 7-δPowder and CuO powder, BaCuO 2Powder is to mix at 1: 2: 3 in molar ratio, as liquid phase source powder.
0≤δ in the following formula≤1.
3, compacting solid phase pioneer's piece and liquid phase piece
Get (1-x) Y 2BaCuO 5+ xBi 2O 3Solid phase precursor powder and liquid phase source powder are pressed into different (1-x) Y of shape same thickness respectively 2BaCuO 5+ xBi 2O 3Solid phase pioneer's piece and liquid phase piece; 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 are pressed into different (1-y) Y of shape same thickness respectively 2BaCuO 5+ yWO 3Solid phase pioneer's piece and liquid phase piece; The mass ratio of solid phase precursor powder and liquid phase source powder is 1: 1.2～1.56.
4, compacting back-up block
With Y 2O 3Powder is pressed into and Y 2BaCuO 5Pioneer's piece and the block-shaped identical briquet of liquid phase are as back-up block.
5, preparation Nd-Ba-Cu oxygen seed crystal piece
Get 54.8586gNd 2O 3, 32.1727gBaCO 3, the 12.9687gCuO powder mixes Nd 2O 3With BaCO 3, the CuO powder mol ratio be 1: 1: 1, process Nd with solid state reaction 2BaCuO 5Powder.Get 20.9895g Y 2O 3, 49.2386gBaCO 3, 29.7719g CuO powder mixes Nd 2O 3With BaCO 3, the CuO powder mol ratio be 1: 4: 6, process NdBa with solid state reaction 2Cu 3O 7-δPowder.With Nd 2BaCuO 5Powder and NdBa 2Cu 3O 7-δPowder is to mix at 1: 3 according to mass ratio, as pioneer's piece, in stove, carries out sintering with top seed crystal melting texture method, and the dice of taking from right cleavage is as Nd-Ba-Cu oxygen seed crystal piece.
0≤δ in the following formula≤1.
6, base substrate assembling and laying method
At Al 2O 3The pad upper surface to down and on place MgO single-chip, back-up block, liquid phase piece, (1-x) Y successively 2BaCuO 5+ xBi 2O 3Solid phase pioneer's piece or (1-y) Y 2BaCuO 5+ yWO 3Solid phase pioneer's piece, Nd-Ba-Cu oxygen seed crystal piece.
7, infiltration growth single domain yttrium, barium, copper and oxygen block
The base substrate that assembles is put into tube furnace, be warming up to 900 ℃, be warming up to 1040～1045 ℃ with 40～60 ℃ temperature rise rate per hour again, be incubated 1～2.5 hour with 80～120 ℃ temperature rise rate per hour; Be cooled to 1015～1025 ℃ with 60 ℃ rate of temperature fall per hour,, naturally cool to room temperature, obtain single domain yttrium, barium, copper and oxygen block with stove with 0.1～0.5 ℃ rate of temperature fall slow cooling to 980～990 ℃ per hour.
8, oozing oxygen handles
Single domain yttrium, barium, copper and oxygen block is inserted in the quartz tube furnace, and in the circulation oxygen atmosphere, slow cooling is 200 hours in 440～410 ℃ the warm area, obtains the single domain yttrium, barium, copper and oxygen superconductive block.
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 3The solid phase precursor powder.At compacting (1-x) Y 2BaCuO 5+ xBi 2O 3Gu in pioneer's piece and the liquid phase piece 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 piece that assembles is put into tube furnace, bestly be warming up to 900 ℃ with 100 ℃ temperature rise rate per hour, be warming up to 1045 ℃ with 50 ℃ temperature rise rate per hour again, be incubated 2 hours; Best be cooled to 1020 ℃, with 0.3 ℃ rate of temperature fall slow cooling to 990 ℃ per hour, naturally cool to room temperature again, obtain the single domain yttrium, barium, copper and oxygen superconductive block with stove with 60 ℃ rate of temperature fall per hour.
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 3The solid phase precursor powder.At compacting (1-y) Y 2BaCuO 5+ yWO 3In solid phase pioneer's piece and the liquid phase piece 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 piece that assembles is put into tube furnace, bestly be warming up to 900 ℃ with 100 ℃ temperature rise rate per hour, be warming up to 1045 ℃ with 50 ℃ temperature rise rate per hour again, be incubated 2 hours; Best be cooled to 1020 ℃, with 0.3 ℃ rate of temperature fall slow cooling to 990 ℃ per hour, naturally cool to room temperature again, obtain the single domain yttrium, barium, copper and oxygen superconductive block with stove with 60 ℃ rate of temperature fall per hour.
In preparation base substrate 5 of the present invention, the MgO single-chip has etc. high 3～5.
Prepare in the base substrate 5 in the present invention, back-up block of the present invention, liquid phase piece, solid phase pioneer's piece are the identical right cylinder of external diameter.
The present invention adopts top seed crystal infiltration growth method, through adding Bi 2O 3Powder and other doped metallic oxide have successfully been introduced the second phase nanoparticle Y 2Ba 4CuBiO x/ Y 2Ba 4CuMO x(M is Bi, W) forms the flux pinning center, the present invention not only simplified powder preparing technology, shortened experimental period, reduced experimental cost, and further improved the flux pinning ability of superconductive block.In the present invention, adopted Y 2O 3The preparation back-up block, in the slow cooling process of growth of yttrium, barium, copper and oxygen block, two briquets above stably supporting stop the loss of liquid phase.The present invention can be used for preparing preparing YBCO superconducting blocks, also can be used for preparing other serial high-temperature superconducting blocks such as Y, Sm, Nd, Eu.
Description of drawings
Fig. 1 is the structural representation that sample is placed in the stove among the embodiment 1.
Fig. 2 is the surface topography map of the single domain yttrium, barium, copper and oxygen superconductive block of embodiment 1 preparation.
Fig. 3 is the magnetic suspension force graphic representation of the single domain yttrium, barium, copper and oxygen superconductive block of embodiment 1 preparation.
Fig. 4 is the magnetic suspension force graphic representation of the single domain yttrium, barium, copper and oxygen superconductive block of embodiment 4 preparations.
Fig. 5 is the environmental scanning electronic microscope figure of the single domain yttrium, barium, copper and oxygen superconductive block of embodiment 1
Embodiment
To further explain of the present invention, but the invention is not restricted to these embodiment below in conjunction with accompanying drawing and embodiment.
Embodiment 1
With used doped raw material Bi 2O 3Powder is that example prepares the single domain yttrium, barium, copper and oxygen superconductive block, and its preparation method is following:
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, the CuO powder mol ratio be 1: 1: 1, process 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, preparation liquid phase source powder
Get 106.9064g BaCO 3, 43.0936g CuO mixes BaCO 3With the mol ratio of CuO powder be 1: 1, process BaCuO with solid state reaction 2Powder.Get 22.6956g Y 2O 3, 79.3350g BaCO 3, 47.9695g CuO powder mixes Y 2O 3With BaCO 3, the CuO powder mol ratio be 1: 4: 6, process YBa with solid state reaction 2Cu 3O 7-δPowder.With 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 in the following formula≤1.
3, compacting doping Bi 2O 3The Y of powder 2BaCuO 5Pioneer's piece and liquid phase piece
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 that diameter is 20mm, thickness right cylinder inequality.
4, compacting back-up block
Get 2.5gY 2O 3Powder is pressed into the back-up block that diameter is 20mm.
5, preparation Nd-Ba-Cu oxygen seed crystal piece
Get 54.8586g Nd 2O 3, 32.1727g BaCO 3, 12.9687g CuO powder mixes Nd 2O 3With BCO 3, the 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 mixes Nd 2O 3With BaCO 3, the CuO powder mol ratio be 1: 4: 6, process NdBa with solid state reaction 2Cu 3O 7-δPowder.With Nd 2BaCuO 5Powder and NdBa 2Cu 3O 7-δPowder is to mix at 1: 3 according to mass ratio, as pioneer's piece, in stove, carries out sintering with top seed crystal melting texture method, and the dice of taking from right cleavage is as Nd-Ba-Cu oxygen seed crystal piece.
0≤δ in the following formula≤1.
6, base substrate assembling and laying method
As shown in Figure 1, at Al 2O 3Pad 6 upper surfaces to down and on place 4 MgO single-chips 5, back-up block 4, liquid phase piece 3, doping Bi successively 2O 3The Y of powder 2BaCuO 5The height of pioneer's piece 2,1,4 MgO single-chip 5 of Nd-Ba-Cu oxygen seed crystal piece is identical, and Nd-Ba-Cu oxygen seed crystal piece 1 is positioned at doping Bi 2O 3The Y of powder 2BaCuO 5The central position of pioneer's piece 2 upper surfaces.
7, infiltration growth single domain yttrium, barium, copper and oxygen block
The base substrate that assembles is put into tube furnace, be warming up to 900 ℃, be warming up to 1045 ℃ with 50 ℃ temperature rise rate per hour again, be incubated 2 hours with 100 ℃ temperature rise rate per hour; Be cooled to 1020 ℃ with 60 ℃ rate of temperature fall per hour,, naturally cool to room temperature, obtain single domain yttrium, barium, copper and oxygen block with stove with 0.3 ℃ rate of temperature fall slow cooling to 990 ℃ per hour.
8, oozing oxygen handles
Single domain yttrium, barium, copper and oxygen block is inserted in the quartz tube furnace, and in the circulation oxygen atmosphere, slow cooling is 200 hours in 410～440 ℃ the warm area, is prepared into the single domain yttrium, barium, copper and oxygen superconductive block.
Prepared single domain yttrium, barium, copper and oxygen superconductive block is used the camera surface topography, and the surface topography photo is seen Fig. 2.Adulterated Bi among a, b, c, d, e, the f among the figure 2O 3Particle content is followed successively by 0.1wt%, 0.3wt%, 0.5wt%, 0.7wt%, 0.9wt%, 2wt%, and visible by Fig. 2, it is four symmetrical sectors of central position with the seed crystal that its surface has all generated, and has tangible cross decorative pattern.Along with Bi 2O 3The continuation of particle doping increases, and trickle variation has taken place the pattern of sample, and yttrium barium copper oxide crystalline growth district demonstrates the trend that reduces.
To prepared single domain yttrium, barium, copper and oxygen superconductive block; Adopt three-dimensional magnetic field and magnetic force test set to measure its magnetic suspension force, test result is seen graphic representation 3, and the ratio of magnetic suspension force and single domain yttrium, barium, copper and oxygen superconduction piece top surface area (the upper surface diameter is 20mm) is a magnetic suspension force density; Visible by Fig. 3, Bi 2O 3The magnetic suspension force of doping prepared preparing YBCO superconducting blocks when being 0.7wt% be 24.48N to the maximum, corresponding magnetic suspension force density is 7.80N/cm 2
Embodiment 2
With used doped raw material Bi 2O 3Powder is that example prepares the single domain yttrium, barium, copper and oxygen superconductive block, and its preparation method is following:
At preparation doping Bi 2O 3The Y of powder 2BaCuO 5In the precursor powder step 1, preparation Y 2BaCuO 5Raw material that powder is used and preparation method are 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 piece and the liquid phase piece step 3, get 9g doping 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 different doping Bi of shape same thickness 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 that assembles is put into tube furnace, be warming up to 900 ℃ with 80 ℃ temperature rise rate per hour; Be warming up to 1045 ℃ with 40 ℃ temperature rise rate per hour again; Be incubated 1 hour, be cooled to 1015 ℃, with 0.1 ℃ rate of temperature fall slow cooling to 990 ℃ per hour with 60 ℃ rate of temperature fall 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 the single domain yttrium, barium, copper and oxygen superconductive block.
Embodiment 3
With used doped raw material Bi 2O 3Powder is that example prepares the single domain yttrium, barium, copper and oxygen superconductive block, and its preparation method is following:
At preparation doping Bi 2O 3The Y of powder 2BaCuO 5In the precursor powder step 1, preparation Y 2BaCuO 5Raw material that powder is used and preparation method are 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 piece and the liquid phase piece step 3, get 9g doping 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 different doping Bi of shape same thickness 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 that assembles is put into tube furnace, be warming up to 900 ℃ with 120 ℃ temperature rise rate per hour; Be warming up to 1040 ℃ with 60 ℃ temperature rise rate per hour again; Be incubated 2.5 hours, be cooled to 1025 ℃, with 0.5 ℃ rate of temperature fall slow cooling to 980 ℃ per hour with 60 ℃ rate of temperature fall 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 the single domain yttrium, barium, copper and oxygen superconductive block.
Embodiment 4
With used doped raw material WO 3Powder is that example prepares the single domain yttrium, barium, copper and oxygen superconductive block, and its preparation method is following:
Preparation Y at above embodiment 1～3 2BaCuO 5In the step 1 of precursor powder, preparation Y 2BaCuO 5Raw material that powder is used and preparation method are identical with embodiment 1.Get 100g Y 2BaCuO 5Powder joins ball mill, the Bi of interpolation 2O 3Powder is used Y 2BaCuO 5The WO of opaque amount 1.5% 3The powder replacement mixes, and is prepared into Y 2BaCuO 5Precursor powder.Other steps are identical with respective embodiments, are prepared into the single domain yttrium, barium, copper and oxygen superconductive block.
Prepared single domain yttrium, barium, copper and oxygen superconductive block adopts three-dimensional magnetic field and magnetic force test set that magnetic suspension force is tested; Test result is seen graphic representation 4; The ratio of magnetic suspension force and single domain yttrium, barium, copper and oxygen superconduction piece top surface area (the upper surface diameter is 20mm) is a magnetic suspension force density, and is visible by Fig. 4, WO 3The magnetic suspension force of doping prepared preparing YBCO superconducting blocks when being 1.5wt% be 25.76N to the maximum, corresponding magnetic suspension force density is 8.20N/cm 2
Embodiment 5
With used doped raw material WO 3Powder is that example prepares the single domain yttrium, barium, copper and oxygen superconductive block, and its preparation method is following:
Preparation Y at above embodiment 1～3 2BaCuO 5In the step 1 of pioneer's powder, preparation Y 2BaCuO 5Raw material that powder is used and preparation method are identical with embodiment 1.Get 100g Y 2BaCuO 5Powder joins ball mill, the Bi of interpolation 2O 3Powder is used Y 2BaCuO 5The WO of powder quality 0.1% 3The powder replacement mixes, and is prepared into Y 2BaCuO 5Precursor powder.Other steps are identical with respective embodiments, are prepared into the single domain yttrium, barium, copper and oxygen superconductive block, and prepared single domain yttrium, barium, copper and oxygen superconductive block adopts three-dimensional magnetic field and magnetic force test set that magnetic suspension force is tested, and test result is seen graphic representation 4.
Embodiment 6
With used doped raw material WO 3Powder is that example prepares the single domain yttrium, barium, copper and oxygen superconductive block, and its preparation method is following:
Preparation Y at above embodiment 1～3 2BaCuO 5In the step 1 of precursor powder, preparation Y 2BaCuO 5Raw material that powder is used and preparation method are identical with embodiment 1.Get 100g Y 2BaCuO 5Powder joins ball mill, the Bi of interpolation 2O 3Powder is used Y 2BaCuO 5The WO of opaque amount 3% 3The powder replacement mixes, and is prepared into Y 2BaCuO 5Precursor powder.Other steps are identical with respective embodiments, are prepared into the single domain yttrium, barium, copper and oxygen superconductive block, and prepared single domain yttrium, barium, copper and oxygen superconductive block adopts three-dimensional magnetic field and magnetic force test set that magnetic suspension force is tested, and test result is seen graphic representation 4.
In order to confirm optimum material proportion of the present invention, the contriver has carried out a large amount of laboratory study tests, and various experiment situation are following:
1, the different oxidation thing is to the influence of single domain yttrium, barium, copper and oxygen superconductive block pattern and magnetic suspension force
Adopt the preparation method of embodiment 1 to prepare the single domain yttrium, barium, copper and oxygen superconductive block.At preparation Y 2BaCuO 5In the precursor powder step 1, with analytically pure Y 2O 3(>=99.9%), BaCO 3(>=99.9%) and CuO (>=99.9%) powder is 1: 1: 1 mixed in molar ratio, processes Y with solid state reaction 2BaCuO 5Powder.Get Y 2BaCuO 5Powder joins ball mill, adds MOX, and oxide compound is selected Bi for use 2O 3Powder, WO 3In the powder any one mixes, and is prepared into Y 2BaCuO 5Precursor powder, Bi 2O 3Powder, WO 3The consumption of powder is following:
(1) adds Y 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 and oxygen superconductive block, adopt three-dimensional magnetic field and magnetic force test set that magnetic suspension force is tested to prepared single domain yttrium, barium, copper and oxygen superconductive block respectively.Test result is seen table 1 and Fig. 3, and in Fig. 3, curve a is 0.1wt%Bi 2O 3The magnetic suspension force curve of the adulterated single domain yttrium, barium, copper and oxygen superconductive block of particle, curve b are 0.3wt%Bi 2O 3The magnetic suspension force curve of the adulterated single domain yttrium, barium, copper and oxygen superconductive block of particle, curve c are 0.5wt%Bi 2O 3The magnetic suspension force curve of the adulterated single domain yttrium, barium, copper and oxygen superconductive block of particle, curve d are 0.7wt%Bi 2O 3The magnetic suspension force curve of the adulterated single domain yttrium, barium, copper and oxygen superconductive block of particle, curve e are 0.9wt%Bi 2O 3The magnetic suspension force curve of the adulterated single domain yttrium, barium, copper and oxygen superconductive block of particle, curve f are 2.0wt%Bi 2O 3The magnetic suspension force curve of the adulterated single domain yttrium, barium, copper and oxygen superconductive block of particle.See Fig. 2, adulterated Bi among a, b, c, d, e, the f among the figure with the take pictures surface topography map of single domain yttrium, barium, copper and oxygen superconductive block of photographic camera 2O 3Particle content is followed successively by 0.1wt%, 0.3wt%, 0.5wt%, 0.7wt%, 0.9wt%, 2wt%.With environmental scanning electronic microscope the structure of single domain yttrium, barium, copper and oxygen superconductive block is analyzed, stereoscan photograph is seen Fig. 5, adulterated Bi among a, b, c, d, e, the f among 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 the single domain yttrium, barium, copper and oxygen superconductive block of table 1 embodiment 1 preparation
Figure BSA00000675939600091
Visible by Fig. 2, it is four symmetrical sectors of central position that the surface of preparing YBCO superconducting blocks has all grown up to the Nd-Ba-Cu oxygen seed crystal, and has tangible cross decorative pattern.Along with Bi 2O 3The increase of doping, trickle variation has taken place in the surface topography of preparing YBCO superconducting blocks, and the growth district of preparing YBCO superconducting blocks demonstrates the trend that reduces.Visible by table 1 and Fig. 3, Bi 2O 3The magnetic suspension force that the particle doping is followed successively by the preparing YBCO superconducting blocks of 0.1wt%, 0.3wt%, 0.5wt%, 0.7wt%, 0.9wt%, 2wt% is respectively 6.84N, 18.48,21.72N, 24.48N, 12.42N, 5.76N, this shows, works as Bi 2O 3When the particle doping was 0.7wt%, the magnetic suspension force of preparing YBCO superconducting blocks was up to 24.48N.Visible by Fig. 5, in yttrium barium copper oxide superconduction matrix, be distributed with two kinds of particles, wherein bigger pearl particle is Y 2BaCuO 5Phase, it is evenly distributed in the middle of the yttrium barium copper oxide superconduction matrix, and the size of particle is 1.0 μ m～5.0 μ m; A kind of in addition particle of less point-like is by Bi 2O 3Particle reacts the nanometer Y that generates under the semi-melting state 2Ba 4CuMO xParticle, the size of particle compare Y between 80nm～160nm 2BaCuO 5One to two one magnitude that particle is little is with respect to Y 2BaCuO 5Particle, Y 2Ba 4CuBiO xBe on good terms and play the flux pinning effect better, thereby can improve the flux pinning ability and the magnetic suspension force of superconductive block effectively.
(2) add Y 2BaCuO 5The WO of opaque amount 0.1%, 0.5%, 0.8%, 1.5%, 2.0%, 3.0wt% 3Powder mixes, and is prepared into Y 2BaCuO 5Precursor powder.Other steps are identical with embodiment 1, are prepared into the single domain yttrium, barium, copper and oxygen superconductive block.Being prepared into diameter is the 20mm preparing YBCO superconducting blocks, and adopts three-dimensional magnetic field and magnetic force test set that magnetic suspension force is tested to prepared single domain yttrium, barium, copper and oxygen superconductive block respectively, and test result is seen table 2 and Fig. 4.In Fig. 4, curve a is 0.1wt%WO 3The magnetic suspension force curve of the adulterated single domain yttrium, barium, copper and oxygen superconductive block of particle, curve b are 0.5wt%WO 3The magnetic suspension force curve of the adulterated single domain yttrium, barium, copper and oxygen superconductive block of particle, curve c are 0.8wt%WO 3The magnetic suspension force curve of the adulterated single domain yttrium, barium, copper and oxygen superconductive block of particle, curve d are 1.5wt%WO 3The magnetic suspension force curve of the adulterated single domain yttrium, barium, copper and oxygen superconductive block of particle, curve e are 2.0wt%WO 3The magnetic suspension force curve of the adulterated single domain yttrium, barium, copper and oxygen superconductive block of particle, curve f are 3.0wt%WO 3The magnetic suspension force curve of the adulterated single domain yttrium, barium, copper and oxygen superconductive block of particle.
The magnetic suspension force test data of the single domain yttrium, barium, copper and oxygen superconductive block of table 2 embodiment 4 preparations
Figure BSA00000675939600101
Visible by table 2 and Fig. 4, WO 3The particle 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, this shows, works as WO 3When the particle doping was 1.5wt%, the magnetic suspension force of preparing YBCO superconducting blocks was up to 25.76N.

Claims (5)

1. the preparation method of a single domain yttrium, barium, copper and oxygen superconductive block is characterized in that it is made up of following step:
(1) preparation solid phase precursor powder
With Y 2O 3With BaCO 3, the CuO powder is 1: 1: 1 mixed in molar ratio, processes Y with solid state reaction 2BaCuO 5Powder is got 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 3The solid phase precursor powder;
0.001≤x in the following formula≤0.02,0.001≤y≤0.03;
(2) preparation liquid phase source powder
With Y 2O 3With BaCO 3, CuO mixes at 1: 4: 6, sinters YBa into solid state reaction 2Cu 3O 7-δPowder, BaCO 3With CuO be 1: 1 in molar ratio, sinter BaCuO into solid state reaction 2Powder is with YBa 2Cu 3O 7-δPowder and CuO powder, BaCuO 2Powder is to mix at 1: 2: 3 in molar ratio, as liquid phase source powder;
0≤δ in the following formula≤1;
(3) compacting solid phase pioneer's piece and liquid phase piece
Get (1-x) Y 2BaCuO 5+ xBi 2O 3Solid phase precursor powder and liquid phase source powder are pressed into different (1-x) Y of shape same thickness respectively 2BaCuO 5+ xBi 2O 3Solid phase pioneer's piece and liquid phase piece; 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 are pressed into different (1-y) Y of shape same thickness respectively 2BaCuO 5+ yWO 3Solid phase pioneer's piece and liquid phase piece; The mass ratio of solid phase precursor powder and liquid phase source powder is 1: 1.2～1.56;
(4) compacting back-up block
With Y 2O 3Powder is pressed into and Y 2BaCuO 5Pioneer's piece and the block-shaped identical briquet of liquid phase are as back-up block;
(5) preparation Nd-Ba-Cu oxygen seed crystal piece
Get 54.8586g Nd 2O 3, 32.1727g BaCO 3, 12.9687g CuO powder mixes Nd 2O 3With BaCO 3, the CuO powder mol ratio be 1: 1: 1, process Nd with solid state reaction 2BaCuO 5Powder; Get 20.9895g Y 2O 3, 49.2386gBaCO 3, 29.7719g CuO powder mixes Nd 2O 3With BaCO 3, the CuO powder mol ratio be 1: 4: 6, process NdBa with solid state reaction 2Cu 3O 7-δPowder; With Nd 2BaCuO 5Powder and NdBa 2Cu 3O 7-δPowder is to mix at 1: 3 according to mass ratio, as pioneer's piece, in stove, carries out sintering with top seed crystal melting texture method, and the dice of taking from right cleavage is as Nd-Ba-Cu oxygen seed crystal piece;
0≤δ in the following formula≤1;
(6) base substrate assembling and laying method
At Al 2O 3Pad (6) upper surface to down and on place MgO single-chip (5), back-up block (4), liquid phase piece (3), (1-x) Y successively 2BaCuO 5+ xBi 2O 3Solid phase pioneer's piece or (1-y) Y 2BaCuO 5+ yWO 3Solid phase pioneer's piece, Nd-Ba-Cu oxygen seed crystal piece (1);
(7) infiltration growth single domain yttrium, barium, copper and oxygen block
The base substrate that assembles is put into tube furnace, be warming up to 900 ℃, be warming up to 1040～1045 ℃ with 40～60 ℃ temperature rise rate per hour again, be incubated 1～2.5 hour with 80～120 ℃ temperature rise rate per hour; Be cooled to 1015～1025 ℃ with 60 ℃ rate of temperature fall per hour,, naturally cool to room temperature, obtain single domain yttrium, barium, copper and oxygen block with stove with 0.1～0.5 ℃ rate of temperature fall slow cooling to 980～990 ℃ per hour;
(8) oozing oxygen handles
Single domain yttrium, barium, copper and oxygen block is inserted in the quartz tube furnace, and in the circulation oxygen atmosphere, slow cooling is 200 hours in 440～410 ℃ the warm area, obtains the single domain yttrium, barium, copper and oxygen superconductive block.
2. according to the preparation method of the described single domain yttrium, barium, copper and oxygen superconductive block of claim 1, it is characterized in that: in preparation solid phase precursor powder step (1), 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 3The solid phase precursor powder; At compacting (1-x) Y 2BaCuO 5+ xBi 2O 3Gu in pioneer's piece and the liquid phase piece step (3), the mass 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 piece that assembles is put into tube furnace, be warming up to 900 ℃ with 100 ℃ temperature rise rate per hour, be warming up to 1045 ℃ with 50 ℃ temperature rise rate per hour again, be incubated 2 hours; Be cooled to 1020 ℃ with 60 ℃ rate of temperature fall per hour, with 0.3 ℃ rate of temperature fall slow cooling to 990 ℃ per hour, naturally cool to room temperature again, obtain the single domain yttrium, barium, copper and oxygen superconductive block with stove.
3. according to the preparation method of the described single domain yttrium, barium, copper and oxygen superconductive block of claim 1, it is characterized in that: in preparation solid phase precursor powder step (1), 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 3The solid phase precursor powder; At compacting (1-y) Y 2BaCuO 5+ yWO 3In solid phase pioneer's piece and the liquid phase piece step (3), the mass 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 piece that assembles is put into tube furnace, be warming up to 900 ℃ with 100 ℃ temperature rise rate per hour, be warming up to 1045 ℃ with 50 ℃ temperature rise rate per hour again, be incubated 2 hours; Be cooled to 1020 ℃ with 60 ℃ rate of temperature fall per hour, with 0.3 ℃ rate of temperature fall slow cooling to 990 ℃ per hour, naturally cool to room temperature again, obtain the single domain yttrium, barium, copper and oxygen superconductive block with stove.
4. according to the preparation method of the described single domain yttrium, barium, copper and oxygen superconductive block of claim 1, it is characterized in that: in preparation base substrate (5), described MgO single-chip has etc. high 3～5.
5. according to the preparation method of the described single domain yttrium, barium, copper and oxygen superconductive block of claim 1, it is characterized in that: in preparation base substrate (5), described back-up block, liquid phase piece, solid phase pioneer's piece are the identical right cylinder of external diameter.
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