CN105236952A - Preparation method of yttrium barium copper oxide superconductive block material doped with nano nickel ferrite - Google Patents
Preparation method of yttrium barium copper oxide superconductive block material doped with nano nickel ferrite Download PDFInfo
- Publication number
- CN105236952A CN105236952A CN201510533794.2A CN201510533794A CN105236952A CN 105236952 A CN105236952 A CN 105236952A CN 201510533794 A CN201510533794 A CN 201510533794A CN 105236952 A CN105236952 A CN 105236952A
- Authority
- CN
- China
- Prior art keywords
- powder
- block
- nano
- solid phase
- copper oxide
- 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.)
- Granted
Links
Abstract
The invention discloses a preparation method of an yttrium barium copper oxide superconductive block material doped with nano nickel ferrite. The method includes the steps of preparing a solid phase powder, preparing a liquid phase source powder, press-moulding a precursor block, assembling the precursor block, growing a yttrium barium copper oxide single domain block material through infiltration, and performing oxygen permeation treatment. By means of doping of the nano particles of the nickel ferrite into the solid phase block and through high-temperature infiltration and slow-cooling growth, element replacement of nickel and iron to the element at copper position in the YBa<2>Cu<3>O<7-[delta]> phase is initiated in the yttrium barium copper oxide superconductive block material, so that component fluctuation and weak superconductive zones appear in the superconductive substrate, thereby increasing [delta]T<c>-typed pinning of the sample and further achieving better superconductive performances. In addition, there is only the BaCuO2 required as a precursor powder in the whole infiltration process, so that the preparation method is simple and efficient in process.
Description
Technical field
The invention belongs to high temperature cuprate superconductor field of material technology, be specifically related to the preparation method of the preparing YBCO superconducting blocks of a kind of nano nickel ferrite doping.
Background technology
High temperature superconducting materia and utilisation technology thereof have important or even irreplaceable using value in the energy, information, traffic, national defence, medical skill, major scientific projects etc., and it is one of focus in the world in new and high technology material and high-technology research field always.Wherein, owing to there is at liquid nitrogen temperature (77K) stronger flux pinning ability and higher critical current density (J can be kept under High-Field
c), yttrium barium copper oxide (Y-Ba-Cu-O) superconducting material is subject to extensive concern always, and being has application potential most and most possible one of superconductor dropping into practical application as early as possible in high temperature superconducting materia family.
When high-temperature superconductor works in liquid nitrogen temperature, inside there will be the flux creep produced because of hot activation, thus occurs that superconductivity (as trapped flux, magnetic suspension force etc.) decays serious problem in time.Therefore, in order to ensure the job stability of high-temperature superconductor, improving the practical value of superconducting material, more effective magnetic flux pinning center must be introduced in superconductor.
In high-temperature superconductor, there are two kinds of main Flux Pinning Mechanism, a kind of is caused by the normal core of non-superconducting (second-phase as insulation includes particle)
δ lsprig is pricked, and its major effect material is at null field and low outer J after the match
cperformance.Another kind is caused by chemical component fluctuation in superconduction matrix
δ T csprig is pricked, namely at YBa
2cu
3o
7-δthere is lower T in the weak superconduction district existed in matrix
cwith upper critical field H
c2, when foreign field increases, its weak superconductivity is damaged, and becomes normal state, thus produces effective magnetic flux pinning center, effectively improves material at the outer J after the match of height
cperformance, this pinning is also referred to as field and causes pinning.In our previous work, invent a kind of preparation method (201510091846.5) of nano combined preparing YBCO superconducting blocks, by using Y
2o
3nano powder and BaCuO
2front axle shell, CeO
2the mixture of initial powder serves as solid phase powder, in preparing YBCO superconducting blocks, successfully introduce nano level Y
2baCuO
5second phase particles is as effectively
δ ltype pinning center, significantly improves the superconductivity of sample.On this basis, we are necessary to invent new method to increase in superconductor
δ T csprig is pricked, to improve performance and the practical value of material further.
Summary of the invention
Technical problem to be solved by this invention is to provide one can introduce in superconduction matrix effectively
δ T ctype pinning center thus improve further sample superconductivity, the preparation method of the preparing YBCO superconducting blocks of nano nickel ferrite doping.
Solve the problems of the technologies described above adopted technical scheme to be made up of following step:
(1) solid phase powder is prepared:
By initial to BaO, CuO powder in molar ratio for the ratio of 1:1 mixes, make BaCuO with solid reaction process
2front axle shell; Again by the Y of median size 50nm
2o
3nano powder and BaCuO
2front axle shell be in molar ratio 1:1 ratio mixing, add 0.5% ~ 1.5%(w/w simultaneously) CeO
2initial powder and 0.1% ~ 0.4%(w/w), the NiFe of median size 50nm
2o
4nano powder, mixes, as solid phase powder;
(2) liquid phase source powder is prepared:
By Y
2o
3with the initial powder of BaO, CuO in molar ratio for the ratio of 1:10:16 mixes, as liquid phase source powder;
(3) predecessor block is suppressed:
Get solid phase powder and put into cylinder shape mould 1, be pressed into solid phase block; Get liquid phase source powder and put into cylinder shape mould 2, be pressed into liquid phase source block; Wherein the mass ratio of solid phase powder used and liquid phase source powder is 1:2.5 ~ 3.5, and the diameter of cylinder shape mould 2 is 10mm larger than cylinder shape mould 1; Get Yb again
2o
3initial powder puts into cylinder shape mould 2, is pressed into the thin slice of thick about 2mm, as back-up block;
(4) predecessor block is assembled:
Liquid phase source block, solid phase block are coaxially placed on directly over back-up block from bottom to top successively, then one piece of Nd-Ba-Cu oxygen seed crystal is placed in the upper surface central position of solid phase block, complete the assembling of predecessor block; Wherein Nd-Ba-Cu oxygen seed crystal used is the wafer from multidomain Nd-Ba-Cu oxygen bulk under cleavage, and its size is about 3mm × 3mm × 1.5mm;
(5) infiltration growth yttrium barium copper oxide single domain bulk:
The predecessor block assembled is placed on Al
2o
3on pad, middle interval is with 5 contour MgO single die, and then entirety puts into pit furnace, is warming up to 1030 ~ 1040 DEG C with the temperature rise rate of 240 DEG C per hour, is incubated 0.5 ~ 1.5 hour; Then be cooled to 1000 ~ 1010 DEG C with the rate of temperature fall of 60 DEG C per hour, then with rate of temperature fall slow cooling to 970 ~ 980 DEG C of 0.2 ~ 0.5 DEG C per hour, naturally cool to room temperature with stove, obtain yttrium barium copper oxide single domain bulk;
(6) oxygen process is oozed:
Yttrium barium copper oxide single domain bulk is put into quartz tube furnace, and in circulation oxygen atmosphere, slow cooling 200 hours in the warm area of 450 ~ 400 DEG C, obtains the preparing YBCO superconducting blocks of nano nickel ferrite doping.
In preparation solid phase powder step (1) of the present invention, by Y
2o
3nano powder and BaCuO
2front axle shell is the ratio mixing of 1:1 in molar ratio, best adds 1%(w/w) CeO
2initial powder and 0.2%(w/w) NiFe
2o
4nano powder; Drive in block step (3) before compaction, the optimum quality ratio of solid phase powder used and liquid phase source powder is 1:3; In infiltration growth yttrium barium copper oxide single domain bulk step (5), the best is warming up to 1035 DEG C with the temperature rise rate of 240 DEG C per hour, is incubated 1 hour; Then be cooled to 1005 DEG C with the rate of temperature fall of 60 DEG C per hour, then with the rate of temperature fall slow cooling to 975 DEG C of 0.33 DEG C per hour, naturally cool to room temperature with stove, obtain yttrium barium copper oxide single domain bulk.
High spot reviews of the present invention:
(1) impact of nano nickel ferrite doping on preparing YBCO superconducting blocks growing state; Result shows: a small amount of NiFe
2o
4doping can not affect the normal growth of yttrium barium copper oxide single domain bulk mutually.
(2) impact of nano nickel ferrite doping on preparing YBCO superconducting blocks magnetic levitation performance; Result shows: under optimum doping amount (0.2%), magnetic sample suspension property is significantly improved.
(3) impact of nano nickel ferrite doping on preparing YBCO superconducting blocks critical temperature; Result shows: nano-Ni/Fe
2o
4doping can cause sample T
cdecline, prove to occur weak superconduction district in sample.
The positively effect that the preparation method of the preparing YBCO superconducting blocks of nano nickel ferrite doping disclosed by the invention is compared with prior art had is:
The present invention adopts top seed crystal infiltration growth (TSIG) method, by ferrite-doping nickel nano particle in solid phase block, after high temperature infiltration and slow cooling growth, causes by Ni and Fe YBa in preparing YBCO superconducting blocks
2cu
3o
7-δthe element substitution of phase Cu position, thus in superconduction matrix, occur that component rises and falls and weak superconduction district, improve sample
δ T csprig is pricked, and obtains higher superconductivity.In addition, whole infiltration process of growth only needs BaCuO
2a kind of front axle shell, technique is simply efficient.
Accompanying drawing illustrates:
Fig. 1 is 0.1% nano-Ni/Fe prepared by embodiment 1
2o
4the surface topography map of the preparing YBCO superconducting blocks of doping;
Fig. 2 is 0.1% nano-Ni/Fe prepared by embodiment 1
2o
4the magnetic suspension force curve of the preparing YBCO superconducting blocks of doping;
Fig. 3 is 0.1% nano-Ni/Fe prepared by embodiment 1
2o
4the Critical Temperature Curve of the preparing YBCO superconducting blocks of doping;
Fig. 4 is 0.2% nano-Ni/Fe prepared by embodiment 2
2o
4the surface topography map of the preparing YBCO superconducting blocks of doping;
Fig. 5 is 0.2% nano-Ni/Fe prepared by embodiment 2
2o
4the magnetic suspension force curve of the preparing YBCO superconducting blocks of doping;
Fig. 6 is 0.2% nano-Ni/Fe prepared by embodiment 2
2o
4the Critical Temperature Curve of the preparing YBCO superconducting blocks of doping;
Fig. 7 is 0.3% nano-Ni/Fe prepared by embodiment 3
2o
4the surface topography map of the preparing YBCO superconducting blocks of doping;
Fig. 8 is 0.3% nano-Ni/Fe prepared by embodiment 3
2o
4the magnetic suspension force curve of the preparing YBCO superconducting blocks of doping;
Fig. 9 is 0.3% nano-Ni/Fe prepared by embodiment 3
2o
4the Critical Temperature Curve of the preparing YBCO superconducting blocks of doping;
Figure 10 is 0.4% nano-Ni/Fe prepared by embodiment 4
2o
4the surface topography map of the preparing YBCO superconducting blocks of doping;
Figure 11 is 0.4% nano-Ni/Fe prepared by embodiment 4
2o
4the magnetic suspension force curve of the preparing YBCO superconducting blocks of doping;
Figure 12 is 0.4% nano-Ni/Fe prepared by embodiment 4
2o
4the Critical Temperature Curve of the preparing YBCO superconducting blocks of doping.
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.Wherein used nanometer Y
2o
3and nano-Ni/Fe
2o
4(median size 50nm), Y
2o
3, Yb
2o
3, CeO
2, BaO and CuO chemical feedstocks all has commercially available, used Nd-Ba-Cu oxygen seed crystal is the wafer from multidomain Nd-Ba-Cu oxygen bulk under cleavage, and its size is about 3mm × 3mm × 1.5mm.
Embodiment 1
(1) solid phase powder is prepared:
Get the initial powder of 65.8415gBaO and 34.1585gCuO to mix, namely the mol ratio of the initial powder of BaO and CuO is 1:1, makes BaCuO with solid reaction process
2front axle shell; Get 49.2302gY again
2o
3nano powder and 50.7698gBaCuO
2front axle shell mixes, and adds 1gCeO simultaneously
2initial powder and 0.1gNiFe
2o
4nano powder, i.e. Y
2o
3nano powder and BaCuO
2the mol ratio of front axle shell is 1:1, adds 1%(w/w simultaneously) CeO
2initial powder and 0.1%(w/w) NiFe
2o
4nano powder, mixes, as solid phase powder;
(2) liquid phase source powder is prepared:
Get 7.4481gY
2o
3mix with the initial powder of 50.5727gBaO, 41.9792gCuO, i.e. Y
2o
3be 1:10:16 with the mol ratio of the initial powder of BaO, CuO, as liquid phase source powder;
(3) predecessor block is suppressed:
Get 5g solid phase powder and put into cylinder shape mould 1(diameter 16mm), be pressed into solid phase block; Get 15g liquid phase source powder and put into cylinder shape mould 2(diameter 26mm), be pressed into liquid phase source block; Namely the mass ratio of solid phase powder used and liquid phase source powder is 1:3, and the diameter of cylinder shape mould 2 is 10mm larger than cylinder shape mould 1; Get 3gYb again
2o
3initial powder puts into cylinder shape mould 2(diameter 26mm), be pressed into the thin slice of thick about 2mm, as back-up block;
(4) predecessor block is assembled:
Liquid phase source block, solid phase block are coaxially placed on directly over back-up block from bottom to top successively, then one piece of Nd-Ba-Cu oxygen seed crystal is placed in the upper surface central position of solid phase block, complete the assembling of predecessor block;
(5) infiltration growth yttrium barium copper oxide single domain bulk:
The predecessor block assembled is placed on Al
2o
3on pad, middle interval is with 5 contour MgO single die, and then entirety puts into pit furnace, is warming up to 1035 DEG C with the temperature rise rate of 240 DEG C per hour, is incubated 1 hour; Then be cooled to 1005 DEG C with the rate of temperature fall of 60 DEG C per hour, then with the rate of temperature fall slow cooling to 975 DEG C of 0.33 DEG C per hour, naturally cool to room temperature with stove, obtain yttrium barium copper oxide single domain bulk;
(6) oxygen process is oozed:
Yttrium barium copper oxide single domain bulk is put into quartz tube furnace, and in circulation oxygen atmosphere, in the warm area of 450 ~ 400 DEG C, slow cooling 200 hours, obtains 0.1% nano-Ni/Fe
2o
4the preparing YBCO superconducting blocks of doping.
0.1% prepared nano-Ni/Fe
2o
4the preparing YBCO superconducting blocks of doping, take surface topography with photographic camera, photo as shown in Figure 1.As seen from the figure, sample surfaces four footpath is clear, and without sporadic nucleation phenomenon, interpret sample successful growth is the superconductive block of single crystal domains.
Applying three-dimensional magnetic field and magnetic force test set are to 0.1% nano-Ni/Fe prepared
2o
4the preparing YBCO superconducting blocks of doping carries out levitation force test, and result as shown in Figure 2.As seen from the figure, the maximum magnetic flux suspending power of sample is 32.03N.
Application cutting machine is at 0.1% prepared nano-Ni/Fe
2o
4the preparing YBCO superconducting blocks of doping cuts the small sample that is of a size of 2mm × 2mm × 1mm, and its DC magnetic susceptibility in 95K to 77K temperature-fall period tested by recycling cryomagnetism test set, obtain sample critical temperature (T
c) curve, result is as shown in Figure 3.As seen from the figure, the initial transition temperature of sample is 89.1K, lower than non-impurity-doped sample (90.3K), proves to occur because Ni and Fe is to YBa in sample
2cu
3o
7-δthe element substitution of phase Cu position and the weak superconduction district caused.
Embodiment 2
In preparation solid phase powder step (1), preparation BaCuO
2the raw material that front axle shell is used and preparation method identical with embodiment 1, then get 49.2302gY
2o
3nano powder and 50.7698gBaCuO
2front axle shell mixes, and adds 1gCeO simultaneously
2initial powder and 0.2gNiFe
2o
4nano powder, i.e. Y
2o
3nano powder and BaCuO
2the mol ratio of front axle shell is 1:1, adds 1%(w/w simultaneously) CeO
2initial powder and 0.2%(w/w) NiFe
2o
4nano powder, mixes, as solid phase powder;
Other steps are identical with embodiment 1.Prepare 0.2% nano-Ni/Fe
2o
4the preparing YBCO superconducting blocks of doping.
0.2% prepared nano-Ni/Fe
2o
4the preparing YBCO superconducting blocks of doping, take surface topography with photographic camera, photo as shown in Figure 4.As seen from the figure, sample surfaces four footpath is clear, and without sporadic nucleation phenomenon, interpret sample successful growth is the superconductive block of single crystal domains.
Applying three-dimensional magnetic field and magnetic force test set are to 0.2% nano-Ni/Fe prepared
2o
4the preparing YBCO superconducting blocks of doping carries out levitation force test, and result as shown in Figure 5.As seen from the figure, the maximum magnetic flux suspending power of sample is 33.93N.
Application cutting machine is at 0.2% prepared nano-Ni/Fe
2o
4the preparing YBCO superconducting blocks of doping cuts the small sample that is of a size of 2mm × 2mm × 1mm, and its DC magnetic susceptibility in 95K to 77K temperature-fall period tested by recycling cryomagnetism test set, obtain sample critical temperature (T
c) curve, result is as shown in Figure 6.As seen from the figure, the initial transition temperature of sample is 87.8K, lower than non-impurity-doped sample (90.3K), proves to occur because Ni and Fe is to YBa in sample
2cu
3o
7-δthe element substitution of phase Cu position and the weak superconduction district caused.
Embodiment 3
In preparation solid phase powder step (1), preparation BaCuO
2the raw material that front axle shell is used and preparation method identical with embodiment 1, then get 49.2302gY
2o
3nano powder and 50.7698gBaCuO
2front axle shell mixes, and adds 1gCeO simultaneously
2initial powder and 0.3gNiFe
2o
4nano powder, i.e. Y
2o
3nano powder and BaCuO
2the mol ratio of front axle shell is 1:1, adds 1%(w/w simultaneously) CeO
2initial powder and 0.3%(w/w) NiFe
2o
4nano powder, mixes, as solid phase powder;
Other steps are identical with embodiment 1.Prepare 0.3% nano-Ni/Fe
2o
4the preparing YBCO superconducting blocks of doping.
0.3% prepared nano-Ni/Fe
2o
4the preparing YBCO superconducting blocks of doping, take surface topography with photographic camera, photo as shown in Figure 7.As seen from the figure, sample surfaces four footpath is clear, and without sporadic nucleation phenomenon, interpret sample successful growth is the superconductive block of single crystal domains.
Applying three-dimensional magnetic field and magnetic force test set are to 0.3% nano-Ni/Fe prepared
2o
4the preparing YBCO superconducting blocks of doping carries out levitation force test, and result as shown in Figure 8.As seen from the figure, the maximum magnetic flux suspending power of sample is 29.66N.
Application cutting machine is at 0.3% prepared nano-Ni/Fe
2o
4the preparing YBCO superconducting blocks of doping cuts the small sample that is of a size of 2mm × 2mm × 1mm, and its DC magnetic susceptibility in 95K to 77K temperature-fall period tested by recycling cryomagnetism test set, obtain sample critical temperature (T
c) curve, result is as shown in Figure 9.As seen from the figure, the initial transition temperature of sample is 86.4K, lower than non-impurity-doped sample (90.3K), proves to occur because Ni and Fe is to YBa in sample
2cu
3o
7-δthe element substitution of phase Cu position and the weak superconduction district caused.
Embodiment 4
In preparation solid phase powder step (1), preparation BaCuO
2the raw material that front axle shell is used and preparation method identical with embodiment 1, then get 49.2302gY
2o
3nano powder and 50.7698gBaCuO
2front axle shell mixes, and adds 1gCeO simultaneously
2initial powder and 0.4gNiFe
2o
4nano powder, i.e. Y
2o
3nano powder and BaCuO
2the mol ratio of front axle shell is 1:1, adds 1%(w/w simultaneously) CeO
2initial powder and 0.4%(w/w) NiFe
2o
4nano powder, mixes, as solid phase powder;
Other steps are identical with embodiment 1.Prepare 0.4% nano-Ni/Fe
2o
4the preparing YBCO superconducting blocks of doping.
0.4% prepared nano-Ni/Fe
2o
4the preparing YBCO superconducting blocks of doping, take surface topography with photographic camera, photo as shown in Figure 10.As seen from the figure, sample surfaces four footpath is clear, and without sporadic nucleation phenomenon, interpret sample successful growth is the superconductive block of single crystal domains.
Applying three-dimensional magnetic field and magnetic force test set are to 0.4% nano-Ni/Fe prepared
2o
4the preparing YBCO superconducting blocks of doping carries out levitation force test, and result as shown in figure 11.As seen from the figure, the maximum magnetic flux suspending power of sample is 26.24N.
Application cutting machine is at 0.4% prepared nano-Ni/Fe
2o
4the preparing YBCO superconducting blocks of doping cuts the small sample that is of a size of 2mm × 2mm × 1mm, and its DC magnetic susceptibility in 95K to 77K temperature-fall period tested by recycling cryomagnetism test set, obtain sample critical temperature (T
c) curve, result is as shown in figure 12.As seen from the figure, the initial transition temperature of sample is 85K, lower than non-impurity-doped sample (90.3K), proves to occur because Ni and Fe is to YBa in sample
2cu
3o
7-δthe element substitution of phase Cu position and the weak superconduction district caused.
Embodiment 5
In preparation solid phase powder step (1), preparation BaCuO
2the raw material that front axle shell is used and preparation method identical with embodiment 1, then get 49.2302gY
2o
3nano powder and 50.7698gBaCuO
2front axle shell mixes, and adds 0.5gCeO simultaneously
2initial powder and 0.2gNiFe
2o
4nano powder, i.e. Y
2o
3nano powder and BaCuO
2the mol ratio of front axle shell is 1:1, adds 0.5%(w/w simultaneously) CeO
2initial powder and 0.2%(w/w) NiFe
2o
4nano powder, mixes, as solid phase powder;
Drive before compaction in block step (3), get 5g solid phase powder and put into cylinder shape mould 1(diameter 16mm), be pressed into solid phase block; Get 12.5g liquid phase source powder and put into cylinder shape mould 2(diameter 26mm), be pressed into liquid phase source block; Namely the mass ratio of solid phase powder used and liquid phase source powder is 1:2.5, and the diameter of cylinder shape mould 2 is 10mm larger than cylinder shape mould 1; Get 3gYb again
2o
3initial powder puts into cylinder shape mould 2(diameter 26mm), be pressed into the thin slice of thick about 2mm, as back-up block.
In infiltration growth yttrium barium copper oxide single domain bulk step (5), the predecessor block assembled is placed on Al
2o
3on pad, middle interval is with 5 contour MgO single die, and then entirety puts into pit furnace, is warming up to 1030 DEG C with the temperature rise rate of 240 DEG C per hour, is incubated 1.5 hours; Then be cooled to 1000 DEG C with the rate of temperature fall of 60 DEG C per hour, then with the rate of temperature fall slow cooling to 970 DEG C of 0.5 DEG C per hour, naturally cool to room temperature with stove, obtain yttrium barium copper oxide single domain bulk.
Other steps are identical with embodiment 1.Prepare 0.2% nano-Ni/Fe
2o
4the preparing YBCO superconducting blocks of doping.
Embodiment 6
In preparation solid phase powder step (1), preparation BaCuO
2the raw material that front axle shell is used and preparation method identical with embodiment 1, then get 49.2302gY
2o
3nano powder and 50.7698gBaCuO
2front axle shell mixes, and adds 1.5gCeO simultaneously
2initial powder and 0.2gNiFe
2o
4nano powder, i.e. Y
2o
3nano powder and BaCuO
2the mol ratio of front axle shell is 1:1, adds 1.5%(w/w simultaneously) CeO
2initial powder and 0.2%(w/w) NiFe
2o
4nano powder, mixes, as solid phase powder;
Drive before compaction in block step (3), get 5g solid phase powder and put into cylinder shape mould 1(diameter 16mm), be pressed into solid phase block; Get 17.5g liquid phase source powder and put into cylinder shape mould 2(diameter 26mm), be pressed into liquid phase source block; Namely the mass ratio of solid phase powder used and liquid phase source powder is 1:3.5, and the diameter of cylinder shape mould 2 is 10mm larger than cylinder shape mould 1; Get 3gYb again
2o
3initial powder puts into cylinder shape mould 2(diameter 26mm), be pressed into the thin slice of thick about 2mm, as back-up block.
In infiltration growth yttrium barium copper oxide single domain bulk step (5), the predecessor block assembled is placed on Al
2o
3on pad, middle interval is with 5 contour MgO single die, and then entirety puts into pit furnace, is warming up to 1040 DEG C with the temperature rise rate of 240 DEG C per hour, is incubated 0.5 hour; Then be cooled to 1010 DEG C with the rate of temperature fall of 60 DEG C per hour, then with the rate of temperature fall slow cooling to 980 DEG C of 0.2 DEG C per hour, naturally cool to room temperature with stove, obtain yttrium barium copper oxide single domain bulk.
Other steps are identical with embodiment 1.Prepare 0.2% nano-Ni/Fe
2o
4the preparing YBCO superconducting blocks of doping.
Embodiment 7
Simultaneous test
Conclusion:
(1) a small amount of NiFe
2o
4doping can not affect the normal growth of yttrium barium copper oxide single domain bulk mutually;
(2) under optimum doping amount (0.2%), magnetic sample suspension property is significantly improved;
(3) nano-Ni/Fe
2o
4doping can cause sample T
cdecline, prove to occur weak superconduction district in sample.
Claims (2)
1. a preparation method for the preparing YBCO superconducting blocks of nano nickel ferrite doping, is characterized in that it carries out in the steps below:
(1) solid phase powder is prepared:
By initial to BaO, CuO powder in molar ratio for the ratio of 1:1 mixes, make BaCuO with solid reaction process
2front axle shell; Again by the Y of median size 50nm
2o
3nano powder and BaCuO
2front axle shell be in molar ratio 1:1 ratio mixing, add 0.5% ~ 1.5%(w/w simultaneously) CeO
2initial powder and 0.1% ~ 0.4%(w/w), the NiFe of median size 50nm
2o
4nano powder, mixes, as solid phase powder;
(2) liquid phase source powder is prepared:
By Y
2o
3with the initial powder of BaO, CuO in molar ratio for the ratio of 1:10:16 mixes, as liquid phase source powder;
(3) predecessor block is suppressed:
Get solid phase powder and put into cylinder shape mould 1, be pressed into solid phase block; Get liquid phase source powder and put into cylinder shape mould 2, be pressed into liquid phase source block; Wherein the mass ratio of solid phase powder used and liquid phase source powder is 1:2.5 ~ 3.5, and the diameter of cylinder shape mould 2 is 10mm larger than cylinder shape mould 1; Get Yb again
2o
3initial powder puts into cylinder shape mould 2, is pressed into the thin slice of thick about 2mm, as back-up block;
(4) predecessor block is assembled:
Liquid phase source block, solid phase block are coaxially placed on directly over back-up block from bottom to top successively, then one piece of Nd-Ba-Cu oxygen seed crystal is placed in the upper surface central position of solid phase block, complete the assembling of predecessor block; Wherein Nd-Ba-Cu oxygen seed crystal used is the wafer from multidomain Nd-Ba-Cu oxygen bulk under cleavage, and its size is about 3mm × 3mm × 1.5mm;
(5) infiltration growth yttrium barium copper oxide single domain bulk:
The predecessor block assembled is placed on Al
2o
3on pad, middle interval is with 5 contour MgO single die, and then entirety puts into pit furnace, is warming up to 1030 ~ 1040 DEG C with the temperature rise rate of 240 DEG C per hour, is incubated 0.5 ~ 1.5 hour; Then be cooled to 1000 ~ 1010 DEG C with the rate of temperature fall of 60 DEG C per hour, then with rate of temperature fall slow cooling to 970 ~ 980 DEG C of 0.2 ~ 0.5 DEG C per hour, naturally cool to room temperature with stove, obtain yttrium barium copper oxide single domain bulk;
(6) oxygen process is oozed:
Yttrium barium copper oxide single domain bulk is put into quartz tube furnace, and in circulation oxygen atmosphere, slow cooling 200 hours in the warm area of 450 ~ 400 DEG C, obtains the preparing YBCO superconducting blocks of nano nickel ferrite doping.
2. the preparation method of the preparing YBCO superconducting blocks of nano nickel ferrite doping according to claim 1, is characterized in that: in preparation solid phase powder step (1), by Y
2o
3nano powder and BaCuO
2front axle shell be in molar ratio 1:1 ratio mixing, add 1%(w/w simultaneously) CeO
2initial powder and 0.2%(w/w) NiFe
2o
4nano powder, mixes, as solid phase powder; Drive in block step (3) before compaction, the mass ratio of solid phase powder used and liquid phase source powder is 1:3; In infiltration growth yttrium barium copper oxide single domain bulk step (5), the predecessor block assembled is placed on Al
2o
3on pad, middle interval is with 5 contour MgO single die, and then entirety puts into pit furnace, is warming up to 1035 DEG C with the temperature rise rate of 240 DEG C per hour, is incubated 1 hour; Then be cooled to 1005 DEG C with the rate of temperature fall of 60 DEG C per hour, then with the rate of temperature fall slow cooling to 975 DEG C of 0.33 DEG C per hour, naturally cool to room temperature with stove, obtain yttrium barium copper oxide single domain bulk.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510533794.2A CN105236952B (en) | 2015-08-27 | 2015-08-27 | The preparation method of the preparing YBCO superconducting blocks of nano nickel ferrite doping |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510533794.2A CN105236952B (en) | 2015-08-27 | 2015-08-27 | The preparation method of the preparing YBCO superconducting blocks of nano nickel ferrite doping |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105236952A true CN105236952A (en) | 2016-01-13 |
| CN105236952B CN105236952B (en) | 2017-09-22 |
Family
ID=55034833
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510533794.2A Expired - Fee Related CN105236952B (en) | 2015-08-27 | 2015-08-27 | The preparation method of the preparing YBCO superconducting blocks of nano nickel ferrite doping |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105236952B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106431403A (en) * | 2016-10-18 | 2017-02-22 | 天津师范大学 | Preparation method of yttrium-barium-copper-oxide superconductive block doped with nano bismuth ferrite |
| CN113818071A (en) * | 2021-10-25 | 2021-12-21 | 天津师范大学 | Method for preventing top seed crystal from moving in growth process of nano composite yttrium barium copper oxide superconducting block |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456726A (en) * | 2009-01-07 | 2009-06-17 | 西南交通大学 | Method for preparing high critical current density yttrium barium copper oxide superconducting film |
| CN104725035A (en) * | 2015-03-02 | 2015-06-24 | 天津师范大学 | Preparation method of nano composite ytrium barium copper oxide superconducting bulks |
-
2015
- 2015-08-27 CN CN201510533794.2A patent/CN105236952B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456726A (en) * | 2009-01-07 | 2009-06-17 | 西南交通大学 | Method for preparing high critical current density yttrium barium copper oxide superconducting film |
| CN104725035A (en) * | 2015-03-02 | 2015-06-24 | 天津师范大学 | Preparation method of nano composite ytrium barium copper oxide superconducting bulks |
Non-Patent Citations (1)
| Title |
|---|
| JINCANG ZHANG 等: "Magnetic Ion Fe and Ni Doping in the Cu-O Chain and the CuO2 Plane in YBa2Cu3O7-δ: A Positron Study", 《IEEE TRANSACTIONS ON APPLIED SUPERCONDUCTIVITY》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106431403A (en) * | 2016-10-18 | 2017-02-22 | 天津师范大学 | Preparation method of yttrium-barium-copper-oxide superconductive block doped with nano bismuth ferrite |
| 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 |
| CN113818071A (en) * | 2021-10-25 | 2021-12-21 | 天津师范大学 | Method for preventing top seed crystal from moving in growth process of nano composite yttrium barium copper oxide superconducting block |
| CN113818071B (en) * | 2021-10-25 | 2024-01-26 | 天津师范大学 | Method for preventing top seed crystal from moving in growth process of nano composite yttrium barium copper oxide superconducting bulk material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105236952B (en) | 2017-09-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| 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 | |
| CN107059127B (en) | A kind of method of bottom seed crystal infiltration growth method preparation single domain rare earth barium copper oxide superconducting ring | |
| CN103979951B (en) | Method for preparing single-domain yttrium barium copper oxide bulk superconductor by taking Y2BaCuO5 as base material | |
| CN102924075B (en) | Method for producing single domain yttrium barium copper oxide superconduction block | |
| CN104725035A (en) | Preparation method of nano composite ytrium barium copper oxide superconducting bulks | |
| CN102877124B (en) | Method for preparing wide-crack spacing REBCO high-temperature superconducting thick films using YBCO/LAO seed films | |
| CN104313691A (en) | Method for preparing single domain (Gd/Y)-Ba-Cu-O superconductivity block | |
| WO2022148214A1 (en) | Method for uniformly doping nanoparticles in high-temperature superconducting material | |
| CN105236952A (en) | Preparation method of yttrium barium copper oxide superconductive block material doped with nano nickel ferrite | |
| CN104313692A (en) | Method for preparing single-domain (Gd/Y)-Ba-Cu-O superconductive bulk by liquid phase infiltration method | |
| CN103541011B (en) | The method of the accurate single crystal of a kind of growing RE BCO high-temperature superconductor | |
| CN103614775B (en) | The method of the accurate single crystal of a kind of embedded seeded growth REBCO | |
| CN103603043B (en) | The method of the accurate single crystal of a kind of embedded seeded growth calcium analysis YBCO | |
| CN113430646B (en) | Method for inducing growth of REBCO superconducting block by using single seed crystal bridge structure | |
| CN103526283A (en) | Method for preparing pure-a-axis-direction YBCO liquid phase epitaxy film | |
| CN110373717A (en) | A method of REBCO high-temperature superconducting block is grown using component hierarchical control method | |
| CN103361710B (en) | Improve the method for single domain yttrium barium copper oxide superconductor preparation efficiency | |
| CN103396114B (en) | Simplified preparation method of single-domain YBCO (Yttrium Barium Copper Oxide) superconducting bulk material | |
| CN106087034B (en) | A method of utilizing corrosion seed crystal induced growth REBCO high-temperature superconducting block | |
| CN1328214C (en) | Method for preparing single domain Dy-Ba-Cu-O superconductive block | |
| CN109626987A (en) | A kind of preparation method of Bismuth-system superconductor | |
| CN106348747B (en) | Easily remove the remaining single domain yttrium barium copper oxide superconductor preparation method of liquid phase source | |
| Gauss et al. | Properties of large-scale melt-processed YBCO samples | |
| CN105177712A (en) | Method for growing REBCO high-temperature superconductor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170922 Termination date: 20180827 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |