CN101665980B - Infiltration method for preparing single-domain Gd-Ba-Cu-O superconducting block - Google Patents

Infiltration method for preparing single-domain Gd-Ba-Cu-O superconducting block Download PDF

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CN101665980B
CN101665980B CN2009100240343A CN200910024034A CN101665980B CN 101665980 B CN101665980 B CN 101665980B CN 2009100240343 A CN2009100240343 A CN 2009100240343A CN 200910024034 A CN200910024034 A CN 200910024034A CN 101665980 B CN101665980 B CN 101665980B
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CN101665980A (en
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杨万民
李国政
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Shaanxi Normal University
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Abstract

The invention relates to an infiltration method for preparing a single-domain Gd-Ba-Cu-O superconducting block. The method comprises the following steps: preparing pioneer powder of Gd2BaCuO5 and liquid-phase source powder; suppressing a pioneer block of Gd2BaCuO5 and a liquid-phase block; compressing a supporting block; assembling the pioneer block; infiltrating and growing the single-domain Gd-Ba-Cu-O block; and carrying out oxygen permeation treatment. The invention adopts a top seed crystal permeation growth method and enables the whole permeation growth process to only need two kinds of pioneer powder of Gd2BaCuO5 and BaCuO2 by changing components of the liquid-phase source powder used by the liquid-phase block, thereby simplifying the experimental links, shortening the experimental period, decreasing the experimental cost, saving power resources and improving the efficiency. The method adopts Yb2O3 to prepare the supporting block which stably supports the two blocks in a slow cold growth process of the Gd-Ba-Cu-O block to prevent liquid-phase loss; and the method not only can be used for preparing the Gd-Ba-Cu-O superconducting block but also can be used for preparing high-temperature superconducting blocks of other series, such as Y, Sm, Nd, Eu, and the like.

Description

The method for preparing single-domain Gd-Ba-Cu-O superconducting block with infiltration method
Technical field
The invention belongs to high temperature cuprate superconductor material technology field, be specifically related to top seed crystal infiltration growth method and prepare single-domain Gd-Ba-Cu-O superconducting block.
Background technology
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, Gd 2BaCuO 5Spot segregation of particle or the like.In the infiltration growth technique, use three isodiametric pioneer's briquets, comprise Gd 2BaCuO 5Pioneer's piece, liquid phase piece and back-up block, Gd 2BaCuO 5The Gd that pioneer's piece is high by phase purity, granularity is little 2BaCuO 5Precursor powder compacting forms, the liquid phase piece by etc. the GdBa of mol ratio 2Cu 3O 7-xAnd Ba 3Cu 5O 8(Ba 3Cu 5O 8Be BaCuO 2With the CuO mol ratio is 3: 2 mixture) mix compacting and form, back-up block is by initial powder oxide compound Gd 2O 3Directly compacting forms.Before thermal treatment, earlier with the liquid phase piece be placed into back-up block above, again with Gd 2BaCuO 5Pioneer's piece is put into above the liquid phase piece.In heat treatment process, the rich Ba in the liquid phase piece, the fusing of Cu liquid phase, the Gd above under the effect of capillary force, being penetrated into 2BaCuO 5In pioneer's piece, in slow temperature-fall period subsequently, the Gd of this liquid phase and pioneer's piece 2BaCuO 5Phase reaction generates GdBa 2Cu 3O 7-xPhase, and under the inducing of seed crystal, accomplish GdBa 2Cu 3O 7-xThe ordering growth of crystal grain.Back-up block also can absorb a part of liquid phase in heat treatment process, generates most Gd 2BaCuO 5Phase and a spot of GdBa 2Cu 3O 7-xPhase.Because a large amount of Gd 2BaCuO 5Two top pioneer's pieces can be at high temperature supported in the existence of solid particles, back-up block, make it in heat treatment process, keep erectting not fall, and can stop the loss of liquid phase.Can find out, top seed crystal infiltration growth method be a kind of than traditional method more complicated and time-consuming preparation method, this preparation method will use three kinds of pioneer's powder (Gd 2BaCuO 5, GdBa 2Cu 3O 7-x, BaCuO 2), and only need two kinds of (Gd in traditional texture method 2BaCuO 5, GdBa 2Cu 3O 7-x).And every kind of precursor powder makes by the traditional solid reaction method; That i.e. high-temperature calcination through repeatedly and grinding obtain is mutually pure, carbon content low and than pioneer's powder of small grain size (0.1～10 micron); Every kind of powder all needs week age to make; This makes the preparation cycle of infiltration growth method prolong greatly, has increased the expensive of experiment simultaneously.
Summary of the invention
Technical problem to be solved by this invention is to overcome above-mentioned single-domain Gd-Ba-Cu-O superconducting block preparing method's shortcoming, provides that a kind of preparation time is short, step is simple, good reproducibility, to be easy to the magnetic suspension force density of oriented growth, prepared single-domain Gd-Ba-Cu-O superconducting block big and critical temperature is high prepares the method for single-domain Gd-Ba-Cu-O superconducting block with infiltration method.
Solving the problems of the technologies described above the technical scheme that is adopted is made up of following step:
1, preparation Gd 2BaCuO 5Precursor powder
With Gd 2O 3With BaCO 3, the CuO powder is 1: 1: 1 mixed in molar ratio, processes Gd with solid state reaction 2BaCuO 5Powder.Get Ga 2BaCuO 5Powder joins ball mill, adds Gd 2BaCuO 5The CeO of opaque amount 1%～2% 2Powder mixes, and is prepared into Gd 2BaCuO 5Precursor powder.
CeO in the said ratio 2Powder directly adds Gd to 2BaCuO 5In the precursor powder, play and suppress Gd 2BaCuO 5Particle growth and refinement Gd 2BaCuO 5The effect of granularity is used to improve the flux pinning ability of single-domain Gd-Ba-Cu-O superconducting block.
2, preparation liquid phase source powder
With BaCO 3With the CuO powder is to mix at 1: 1 in molar ratio, processes BaCuO with solid state reaction 2Powder.With Gd 2BaCuO 5Precursor powder and BaCuO 2Powder, CuO powder are to mix at 1: 9: 6 in molar ratio, as liquid phase source powder.
3, compacting Gd 2BaCuO 5Pioneer's piece and liquid phase piece
Get Gd 2BaCuO 5Precursor powder, liquid phase source powder, being pressed into diameter respectively is that 20mm or 30mm thickness are the Gd of 8～12mm 2BaCuO 5Pioneer's piece and liquid phase piece, material therefor liquid phase source powder and Gd 2BaCuO 5The mass ratio of precursor powder is 1: 0.95～1.15.
4, compacting back-up block
With Yb 2O 3Powder is pressed into and Gd 2BaCuO 5Pioneer's piece is identical with liquid phase piece diameter, thickness is the briquet of 1～2mm, as back-up block.
5, assembling pioneer piece
The liquid phase piece be placed on back-up block directly over, Gd 2BaCuO 5Pioneer's piece is placed on the top of liquid phase piece, whole again being placed on the high MgO monocrystalline such as 3～10, and the MgO monocrystalline is placed on the Al of a circle 2O 3On the pad, a Nd-Ba-Cu oxygen seed crystal is placed Gd 2BaCuO 5The centre of surface of pioneer's piece.
Volume length * wide * the height of above-mentioned MgO monocrystalline is 5 * 5 * 5mm 3, Al 2O 3The pad diameter is that 4～6cm, thickness are 5～8mm.
6, infiltration growth single-domain Gd-Ba-Cu-O bulk
The pioneer's piece that assembles is put into tube furnace, be warming up to 800～900 ℃, be warming up to 1050～1060 ℃ with 40～60 ℃ temperature rise rate per hour again, be incubated 0.5～2 hour with 80～120 ℃ temperature rise rate per hour; Be cooled to 1040～1030 ℃ with 60 ℃ rate of temperature fall per hour,, naturally cool to room temperature, obtain the single-domain Gd-Ba-Cu-O bulk with stove with 0.1～0.5 ℃ rate of temperature fall slow cooling to 1020～1010 ℃ per hour.
7, oozing oxygen handles
The single-domain Gd-Ba-Cu-O bulk is inserted in the quartz tube furnace, and in the circulation oxygen atmosphere, slow cooling is 200 hours in 450～350 ℃ the warm area, obtains single-domain Gd-Ba-Cu-O superconducting block.
At preparation Gd of the present invention 2BaCuO 5In the precursor powder step 1, get Gd 2BaCuO 5Powder joins ball mill, the best Gd that adds 2BaCuO 5The CeO of opaque amount 2% 2Powder mixes, and is prepared into Gd 2BaCuO 5Precursor powder.At compacting Gd 2BaCuO 5In pioneer's piece and the liquid phase piece step 3, liquid phase source powder and Gd 2BaCuO 5The optimum quality ratio of precursor powder is 1: 1.09.In infiltration growth single-domain Gd-Ba-Cu-O bulk step 6, the pioneer's piece that assembles is put into tube furnace, bestly be warming up to 850 ℃ with 100 ℃ temperature rise rate per hour; Be warming up to 1055 ℃ with 50 ℃ temperature rise rate per hour again; Be incubated 1 hour, best be cooled to 1035 ℃, again with 0.3 ℃ rate of temperature fall slow cooling to 1015 ℃ per hour with 60 ℃ rate of temperature fall per hour; Naturally cool to room temperature with stove, obtain the single-domain Gd-Ba-Cu-O bulk.
The present invention adopts top seed crystal infiltration growth method, through changing the composition of the used liquid phase of liquid phase piece source powder, makes whole infiltration process of growth only need Gd 2BaCuO 5And BaCuO 2Two kinds of precursor powders have been simplified experiment link, have shortened experimental period, have reduced experimental cost, have saved the energy, have been improved efficient.Adopted Yb 2O 3The preparation back-up block, in the slow cooling process of growth of Gd-Ba-Cu-O bulk, two briquets above stably supporting stop the loss of liquid phase.The present invention can be used for preparing Gd-Ba-Cu-O superconducting block, 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 synoptic diagram of the assembling pioneer piece of embodiment 1.
Fig. 2 is the surface topography map of the single-domain Gd-Ba-Cu-O superconducting block of embodiment 1 preparation.
Fig. 3 is the resistance temperature curve of the single-domain Gd-Ba-Cu-O superconducting block of embodiment 1 preparation.
Fig. 4 is the magnetic suspension force curve of the single-domain Gd-Ba-Cu-O superconducting block of embodiment 1 preparation.
Fig. 5 is the surface topography map of the single-domain Gd-Ba-Cu-O superconducting block of embodiment 3 preparations.
Fig. 6 is the magnetic suspension force curve of the single-domain Gd-Ba-Cu-O superconducting block of embodiment 3 preparations.
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
1, preparation Gd 2BaCuO 5Precursor powder
Get 85.0421g Gd 2O 3, 46.2957g BaCO 3, 18.6622g CuO powder mixes, i.e. Gd 2O 3With BaCO 3, the CuO powder mol ratio be 1: 1: 1, process Gd with solid state reaction 2BaCuO 5Powder.Get 100g Gd 2BaCuO 5Powder joins ball mill, adds Gd 2BaCuO 5The CeO of opaque amount 2% 2Powder mixes, and is prepared into Gd 2BaCuO 5Precursor powder.
2, preparation liquid phase source powder
Get 106.9053g BaCO 3, 43.0947g CuO mixes, i.e. BaCO 3With the mol ratio of CuO powder be 1: 1, process BaCuO with solid state reaction 2Powder.With 34.0877g Gd 2BaCuO 5Precursor powder, 120g BaCuO 2Powder, 27.3274g CuO powder mix at ball mill, i.e. Gd 2BaCuO 5Precursor powder and BaCuO 2The mol ratio of powder, CuO powder is 1: 9: 6, as liquid phase source powder.
3, compacting Gd 2BaCuO 5Pioneer's piece and liquid phase piece
Get 11g liquid phase source powder, 12g Gd 2BaCuO 5Precursor powder, being pressed into diameter respectively is that 20mm, thickness are liquid phase piece and the Gd of 10mm 2BaCuO 5Pioneer's piece, material therefor liquid phase source powder and Gd 2BaCuO 5The mass ratio of precursor powder is 1: 1.09.
4, compacting back-up block
Get 2g Yb 2O 3Powder is pressed into and Gd 2BaCuO 5Pioneer's piece is identical with liquid phase piece diameter, thickness is the briquet of 2mm, as back-up block.
5, assembling pioneer piece
As shown in Figure 1, in Fig. 1, during assembling with liquid phase piece 2 be placed on back-up block 3 directly over, Gd 2BaCuO 5Pioneer's piece 1 is placed on the top of liquid phase piece 2, whole again being placed on the high MgO monocrystalline 4 such as 4, and MgO monocrystalline 4 is placed on the Al of a circle 2O 3On the pad 5, a Nd-Ba-Cu oxygen seed crystal 6 is placed Gd 2BaCuO 5The centre of surface of pioneer's piece 1.
Volume length * wide * the height of above-mentioned MgO monocrystalline is 5 * 5 * 5mm 3, Al 2O 3The pad diameter is that 4cm, thickness are 6mm.
6, infiltration growth single-domain Gd-Ba-Cu-O bulk
Pioneer's piece that device is good is put into tube furnace, is warming up to 850 ℃ with 100 ℃ temperature rise rate per hour, is warming up to 1055 ℃ with 50 ℃ temperature rise rate per hour again, is incubated 1 hour; Be cooled to 1035 ℃ with 60 ℃ rate of temperature fall per hour,, naturally cool to room temperature, obtain the single-domain Gd-Ba-Cu-O bulk with stove with 0.3 ℃ rate of temperature fall slow cooling to 1015 ℃ per hour.
7, oozing oxygen handles
The single-domain Gd-Ba-Cu-O bulk is inserted in the quartz tube furnace, and in the circulation oxygen atmosphere, slow cooling is 200 hours in 450～350 ℃ the warm area, obtains single-domain Gd-Ba-Cu-O superconducting block.
Prepared single-domain Gd-Ba-Cu-O superconducting block is used the camera surface topography, and the surface topography photo is seen Fig. 2.Visible by Fig. 2, sample surfaces four footpaths are clear, radial line radially, the angle between radial line and the radial line (segmental angle) is 90 degree, no sporadic nucleation phenomenon.
Prepared single-domain Gd-Ba-Cu-O superconducting block adopts critical temperature tester (being produced by Sichuan instrument four factories) that resistance temperature is tested; The resistance temperature curve of test is seen Fig. 3; Visible by figure, the width of transition Δ T＜5K of this superconductive block, superconducting transition temperature Tc reaches 92K.
Prepared single-domain Gd-Ba-Cu-O superconducting block adopts three-dimensional magnetic field and magnetic force test set that magnetic suspension force is tested; Test result is seen table 1 and graphic representation 4; The ratio of magnetic suspension force and single-domain Gd-Ba-Cu-O superconducting piece top surface area (the upper surface diameter is 20mm) is a magnetic suspension force density; Visible by table 1 and Fig. 4, the magnetic suspension force density of this superconductive block is up to 9N/cm 2
Embodiment 2
At preparation Gd 2BaCuO 5In the precursor powder step 1, preparation Gd 2BaCuO 5Raw material that powder is used and preparation method are identical with embodiment 1, get 100g Gd 2BaCuO 5Powder joins ball mill, adds Gd 2BaCuO 5The CeO of opaque amount 1% 2Powder mixes, and is prepared into Gd 2BaCuO 5Precursor powder.Other steps of this embodiment are identical with embodiment 1.Be prepared into the Gd-Ba-Cu-O superconducting block that diameter is 20mm, prepared single-domain Gd-Ba-Cu-O superconducting block adopts three-dimensional magnetic field and magnetic force test set that magnetic suspension force is tested, and magnetic suspension force density reaches and is 8.1N/cm 2
Embodiment 3
At compacting Gd 2BaCuO 5In pioneer's piece and the liquid phase piece step 3, get 30g Gd 2BaCuO 5Precursor powder, 30g liquid phase source powder are pressed into the Gd that diameter is 30mm respectively 2BaCuO 5Pioneer's piece and liquid phase piece.In compacting back-up block step 4, get 4.5g Yb 2O 3It is the briquet of 2mm for 30mm thickness that powder is pressed into diameter, as back-up block.In infiltration growth single-domain Gd-Ba-Cu-O bulk step 6, the pioneer's piece that assembles is put into tube furnace, be warming up to 800 ℃ with 100 ℃ temperature rise rate per hour, be warming up to 1055 ℃ with 50 ℃ temperature rise rate per hour again, be incubated 1.5 hours; Be cooled to 1035 ℃ with 60 ℃ rate of temperature fall per hour, with 0.2 ℃ rate of temperature fall slow cooling to 1015 ℃ per hour, naturally cool to room temperature with stove, obtaining diameter is the single-domain Gd-Ba-Cu-O bulk of 30mm.Other steps are identical with embodiment 1.Be prepared into single-domain Gd-Ba-Cu-O superconducting block.
Prepared single-domain Gd-Ba-Cu-O superconducting block adopts the camera surface topography, and the surface topography photo is seen Fig. 5.Visible by Fig. 5, four footpaths, macro morphology surface of single-domain Gd-Ba-Cu-O superconducting block are clear, radial line radially, the angle between radial line and the radial line (segmental angle) is 90 degree, no sporadic nucleation phenomenon.
Prepared single-domain Gd-Ba-Cu-O superconducting block adopts three-dimensional magnetic field and magnetic force test set that magnetic suspension force is tested; Test result is seen table 2 and graphic representation 6; The ratio of magnetic suspension force and single-domain Gd-Ba-Cu-O superconducting piece top surface area (the upper surface diameter is 30mm) is a magnetic suspension force density; Visible by table 2 and Fig. 6, the magnetic suspension force density of this superconductive block is up to 7N/cm 2
Embodiment 4
At preparation Gd 2BaCuO 5In the precursor powder step 1, preparation Gd 2BaCuO 5Raw material that powder is used and preparation method are identical with embodiment 1, get 100g Gd 2BaCuO 5Powder joins ball mill, adds Gd 2BaCuO 5The CeO of opaque amount 1.5% 2Powder mixes, and is prepared into Gd 2BaCuO 5Precursor powder.
At compacting Gd 2BaCuO 5In pioneer's piece and the liquid phase piece step 3, get 28.5g Gd 2BaCuO 5Precursor powder, 30g liquid phase source powder, being pressed into diameter respectively is the Gd of 8mm for 30mm thickness 2BaCuO 5Pioneer's piece and liquid phase piece, material therefor liquid phase source powder and Gd 2BaCuO 5The mass ratio of precursor powder is 1: 0.95.In compacting back-up block step 4, get 4.5g Yb 2O 3It is the briquet of 1.5mm for 30mm thickness that powder is pressed into diameter, as back-up block.In infiltration growth single-domain Gd-Ba-Cu-O bulk step 6, the pioneer's piece that assembles is put into tube furnace, be warming up to 900 ℃ with 80 ℃ temperature rise rate per hour, be warming up to 1060 ℃ with 40 ℃ temperature rise rate per hour again, be incubated 2 hours; Be cooled to 1040 ℃ with 60 ℃ rate of temperature fall per hour, with 0.1 ℃ rate of temperature fall slow cooling to 1020 ℃ per hour, naturally cool to room temperature with stove, obtaining diameter is the single-domain Gd-Ba-Cu-O bulk of 30mm.Other steps are identical with embodiment 1.Be prepared into single-domain Gd-Ba-Cu-O superconducting block.
Embodiment 5
At compacting Gd 2BaCuO 5In pioneer's piece and the liquid phase piece step 3, get 13.8g Gd 2BaCuO 5Precursor powder, 12g liquid phase source powder, being pressed into diameter respectively is the Gd of 12mm for 20mm thickness 2BaCuO 5Pioneer's piece and liquid phase piece, material therefor liquid phase source powder and Gd 2BaCuO 5The mass ratio of precursor powder is 1: 1.15.In compacting back-up block step 4, get 1.5g Yb 2O 3It is the briquet of 1mm for 20mm thickness that powder is pressed into diameter, as back-up block.In infiltration growth single-domain Gd-Ba-Cu-O bulk step 6, the pioneer's piece that assembles is put into tube furnace, be warming up to 850 ℃ with 120 ℃ temperature rise rate per hour, be warming up to 1050 ℃ with 60 ℃ temperature rise rate per hour again, be incubated 0.5 hour; Be cooled to 1030 ℃ with 60 ℃ rate of temperature fall per hour, with 0.5 ℃ rate of temperature fall slow cooling to 1010 ℃ per hour, naturally cool to room temperature with stove, obtaining diameter is the single-domain Gd-Ba-Cu-O bulk of 20mm.Other steps are identical with embodiment 1.Be prepared into single-domain Gd-Ba-Cu-O superconducting block.
The magnetic suspension force test result of the single-domain Gd-Ba-Cu-O superconducting block of table 1 embodiment 1 preparation
Figure G2009100240343D00081
The magnetic suspension force test result of the single-domain Gd-Ba-Cu-O superconducting block of table 2 embodiment 3 preparations
Figure G2009100240343D00091

Claims (2)

1. one kind prepares the method for single-domain Gd-Ba-Cu-O superconducting block with infiltration method, it is characterized in that he is made up of following step:
(1) preparation Gd 2BaCuO 5Precursor powder
With Gd 2O 3With BaCO 3, the CuO powder is 1: 1: 1 mixed in molar ratio, processes Gd with solid state reaction 2BaCuO 5Powder is got Gd 2BaCuO 5Powder joins ball mill, adds Gd 2BaCuO 5The CeO of opaque amount 1%～2% 2Powder mixes, and is prepared into Gd 2BaCuO 5Precursor powder;
(2) preparation liquid phase source powder
With BaCO 3With the CuO powder is to mix at 1: 1 in molar ratio, processes BaCuO with solid state reaction 2Powder is with Gd 2BaCuO 5Precursor powder and BaCuO 2Powder, CuO powder are to mix at 1: 9: 6 in molar ratio, as liquid phase source powder;
(3) compacting Gd 2BaCuO 5Pioneer's piece and liquid phase piece
Get Gd 2BaCuO 5Precursor powder, liquid phase source powder, being pressed into diameter respectively is that 20mm or 30mm thickness are the Gd of 8～12mm 2BaCuO 5Pioneer's piece and liquid phase piece, material therefor liquid phase source powder and Gd 2BaCuO 5The mass ratio of precursor powder is 1: 0.95～1.15;
(4) compacting back-up block
With Yb 2O 3Powder is pressed into and Gd 2BaCuO 5Pioneer's piece is identical with liquid phase piece diameter, thickness is the briquet of 1～2mm;
(5) assembling pioneer piece
The liquid phase piece be placed on back-up block directly over, Gd 2BaCuO 5Pioneer's piece is placed on the top of liquid phase piece, whole again being placed on the high MgO monocrystalline such as 3～10, and the MgO monocrystalline is placed on the Al of a circle 2O 3On the pad, a Nd-Ba-Cu oxygen seed crystal is placed Gd 2BaCuO 5The centre of surface of pioneer's piece;
(6) infiltration growth single-domain Gd-Ba-Cu-O bulk
The pioneer's piece that assembles is put into tube furnace; Be warming up to 800～900 ℃ with 80～120 ℃ temperature rise rate per hour, be warming up to 1050～1060 ℃ with 40～60 ℃ temperature rise rate per hour again, be incubated 0.5～2 hour; Be cooled to 1040～1030 ℃ with 60 ℃ rate of temperature fall per hour again; With 0.1～0.5 ℃ rate of temperature fall slow cooling to 1020～1010 ℃ per hour, naturally cool to room temperature with stove, obtain the single-domain Gd-Ba-Cu-O bulk;
(7) oozing oxygen handles
The single-domain Gd-Ba-Cu-O bulk is inserted in the quartz tube furnace, and in the circulation oxygen atmosphere, slow cooling is 200 hours in 450～350 ℃ the warm area, obtains single-domain Gd-Ba-Cu-O superconducting block.
2. prepare the method for single-domain Gd-Ba-Cu-O superconducting block according to claim 1 is described with infiltration method, it is characterized in that: at preparation Gd of the present invention 2BaCuO 5In the precursor powder step (1), get Gd 2BaCuO 5Powder joins ball mill, adds Gd 2BaCuO 5The CeO of opaque amount 2% 2Powder mixes, and is prepared into Gd 2BaCuO 5Precursor powder; At compacting Gd 2BaCuO 5In pioneer's piece and the liquid phase piece step (3), liquid phase source powder and Gd 2BaCuO 5The mass ratio of precursor powder is 1: 1.09; In infiltration growth single-domain Gd-Ba-Cu-O bulk step (6), the pioneer's piece that assembles is put into tube furnace, be warming up to 850 ℃ with 100 ℃ temperature rise rate per hour; Be warming up to 1055 ℃ with 50 ℃ temperature rise rate per hour again; Be incubated 1 hour, be cooled to 1035 ℃, again with 0.3 ℃ rate of temperature fall slow cooling to 1015 ℃ per hour with 60 ℃ rate of temperature fall per hour; Naturally cool to room temperature with stove, obtain the single-domain Gd-Ba-Cu-O bulk.
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