CN103420675B - A kind of Nd 2-xce xcuO 4-δthe low temperature preparation method of superconducting nano porcelain powder - Google Patents
A kind of Nd 2-xce xcuO 4-δthe low temperature preparation method of superconducting nano porcelain powder Download PDFInfo
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- CN103420675B CN103420675B CN201310347257.XA CN201310347257A CN103420675B CN 103420675 B CN103420675 B CN 103420675B CN 201310347257 A CN201310347257 A CN 201310347257A CN 103420675 B CN103420675 B CN 103420675B
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- 239000000843 powder Substances 0.000 title claims abstract description 35
- 229910052573 porcelain Inorganic materials 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 32
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 238000001704 evaporation Methods 0.000 claims abstract description 9
- 230000008020 evaporation Effects 0.000 claims abstract description 9
- 238000010992 reflux Methods 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 15
- 238000003786 synthesis reaction Methods 0.000 abstract description 15
- 239000002245 particle Substances 0.000 abstract description 6
- 238000001035 drying Methods 0.000 abstract description 4
- 238000003980 solgel method Methods 0.000 abstract description 4
- 229910052779 Neodymium Inorganic materials 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 229910052684 Cerium Inorganic materials 0.000 abstract description 2
- 229910052802 copper Inorganic materials 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 19
- 239000010949 copper Substances 0.000 description 17
- 238000011160 research Methods 0.000 description 11
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 5
- 230000005290 antiferromagnetic effect Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000010532 solid phase synthesis reaction Methods 0.000 description 4
- 239000005751 Copper oxide Substances 0.000 description 3
- 229910000431 copper oxide Inorganic materials 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 239000002887 superconductor Substances 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical group [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 239000003352 sequestering agent Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention provides a kind of Nd
2-xce
xcuO
4- δthe low temperature preparation method of superconducting nano porcelain powder, by Nd (NO
3)
3nH
2o, Ce (NO
3)
36H
2o, Cu (NO
3)
23H
2o and EDTA is that 2-x:x:1:3 weighs by the mol ratio of Nd:Ce:Cu:EDTA, wherein x=0 ~ 0.17; First EDTA is placed in deionized water, adds quadrol adjust ph simultaneously, then add Nd (NO
3)
3nH
2o, Ce (NO
3)
36H
2o and Cu (NO
3)
23H
2o, adds quadrol adjust ph simultaneously, obtains colloidal sol, reheat evaporation concentration and obtain gel, and gel drying is obtained xerogel through 60 ~ 80 DEG C of reflux, and then calcining obtains Nd
2-xce
xcuO
4- δsuperconducting nano porcelain powder, its particle diameter is 20 ~ 70nm.The present invention adopts sol-gel process that Nd, Ce and Cu are mixed in atomic level, thus achieves pure phase nanometer Nd
2-xce
xcuO
4- δthe low temperature synthesis of superconduction porcelain powder, and greatly reduce energy consumption.
Description
Technical field
The invention belongs to supercondutive powder body technique field, relate to a kind of Nd
1.85ce
0.15cuO
4-δthe preparation method of superconducting nano porcelain powder.
Background technology
Switzerland physicist A. M ü ller in 1986 and Germany physicist G. Bednorz have found zero resistance transition temperature T
cfor the copper oxide La of 35K
2-xba
xcuO, thus the new era of having started the research of high temperature critical temperature and superconductivity.Carrying out in a large number and carrying out in a deep going way along with research, in this high-temperature superconductor research field, new phenomenon, new effect, new theory, new technology, novel material emerge in an endless stream, the fast development of great impellent fundamental research and application technical research.Since the copper oxygen face of electronics or cavity type doping is found in copper oxide high temperature superconduction, copper oxide high temperature superconduction obtains further development.But in the preparation of numerous superconduction systems and property Quality Research, electron type superconducting phase is little for the research of cavity type superconduction, and research in this respect in several years is up to date just gradually more and more, especially to RE
2-xce
xcuO
4the research of (RE=Nd, Pr, Sm, Eu) system, concentrate on its physical property Quality Research in these a lot of researchs on the one hand, and this may be for the reason swashing mechanism in order to illustrate superconductor superconduction.Electron-doped Superconductors and cavity type superconduction have following different physical properties, and the scope of the antiferromagnetic phase that cavity type superconduction table goes out is very wide, and in low-doped lower acquisition, the interaction energy of superconduction is simultaneously distinguished very easily from antiferromagnetic performance; Contrary to electron type superconduction, the narrow range of antiferromagnetic phase, and also antiferromagnetic phase and superconducting phase are often higher than T
ccoexisting state is there is when point.Cavity type superconduction and the difference of electron type superconduction in physical properties also have much relations with preparation method.As document S. Uthayakumar, R. Fittipaldi, A. Guarino, A. Vecchione, A. Romano, A. Nigro, H.-U. Habermeier, S. Pace, Physica C 468 (2008) 2271 and Y. Tokura, described in H.Takagi, S.Uhida, Nature 337 (1989) 345: at present for superconduction system (particularly RE
2-xce
xcuO
4superconduction system) preparation method mainly adopt solid-phase synthesis, by rare earth oxide after the abundant ground and mixed of certain hour at a certain temperature sintering synthesis phase.The synthesis temperature of this method is high, and being difficult to simultaneously due to Ce diffusion in this system, causes the mutually impure of synthesis, simultaneously because synthesis temperature is very high, causes being difficult to close nano superconductive porcelain powder.
For Nd
2-xce
xcuO
4-δ(NCCO) superconduction system, the main preparation process adopted is at present: by Ce
2o
3, Nd
2o
3put into mortar after weighing by the mol ratio analytical balance of 2-x:x:1 with CuO, the stove putting into 1150 DEG C after abundant ground and mixed at 950 DEG C after pre-burning sinters Nd into
2-xce
xcuO
4-δphase.The synthesis temperature of its most last phase is 1150 DEG C, needs to consume a large amount of energy, and cannot synthesis of nano powder, simultaneously because the diffusion problem of Ce time the phase of synthesizing still there is certain dephasign.
Summary of the invention
The object of the invention is to propose a kind of Nd
2-xce
xcuO
4-δthe low temperature preparation method of superconducting nano porcelain powder, this method adopts sol-gel process to achieve and prepare the Nd that particle diameter is 20 ~ 70nm under low temperature (600 ~ 900 DEG C)
2-xce
xcuO
4-δ(δ=0 ~ 0.6) superconducting nano porcelain powder pure phase.
The present invention is realized by following technical proposal: a kind of Nd
2-xce
xcuO
4-δthe low temperature preparation method of superconducting nano porcelain powder, through following each step:
(1) by Nd (NO
3)
3nH
2o, Ce (NO
3)
36H
2o, Cu (NO
3)
23H
2o and EDTA(ethylenediamine tetraacetic acid (EDTA)) be that 2-x:x:1:3 weighs by the mol ratio of Nd:Ce:Cu:EDTA, wherein x=0 ~ 0.17;
(2) be 5 ~ 40:1 by liquid-solid ratio (L/Kg), standby for step (1) institute EDTA be placed in deionized water, add quadrol adjust ph simultaneously, obtain mixing solutions;
(3) in step (2) gained mixing solutions, the standby Nd (NO of step (1) is added
3)
3nH
2o, Ce (NO
3)
36H
2o and Cu (NO
3)
23H
2o, adds quadrol adjust ph simultaneously, obtains mixture;
(4) step (3) gained mixture is obtained colloidal sol through 60 ~ 80 DEG C of reflux, reheat evaporation concentration and obtain gel, and gel drying is obtained xerogel;
(5) calcining of step (4) gained xerogel is obtained Nd
2-xce
xcuO
4-δsuperconducting nano porcelain powder.
Described step (2) pH value range is 3.5 ~ 8.
Described step (3) pH value range is 4 ~ 10.
The time of described step (4) reflux is 1 ~ 4h, and the time of evaporation concentration is 3 ~ 7h.
The temperature of described step (4) drying is 70 ~ 150 DEG C, and drying conditions is normal pressure.
The temperature that described step (5) is calcined is 600 ~ 900 DEG C, time 2 ~ 16h, and calcination atmosphere is air.
The present invention Nd of Nano grade that adopted sol-gel method to prepare
2-xce
xcuO
4-δsuperconducting nano porcelain powder, the Nd for having Lacking oxygen of synthesis
2-xce
xcuO
4-δ(δ=0 ~ 0.6) pure phase, crystalline structure is tetragonal, and the particle diameter of powder is 20 ~ 70nm.The preparation Nd that the present invention proposes
2-xce
xcuO
4-δthe method of superconducting nano porcelain powder compared with prior art has following advantages: the present invention can at low temperatures with the nanometer Nd becoming pure phase
2-xce
xcuO
4-δpowder.Because the present invention adopts EDTA to be sequestrant, quadrol is linking agent, the Nd-Ce-Cu system colloid that success is made, thus achieves the mixing of Nd, Ce and Cu three in atomic level, solve the problem that rare earth element (particularly Ce) is difficult to spread, and then synthesize the nanometer Nd of pure phase for low temperature
2-xce
xcuO
4-δpowder creates condition, greatly reduces the energy consumption of materials synthesis simultaneously.
Accompanying drawing explanation
Fig. 1 is embodiment 1 gained Nd
2cuO
4-δthe XRD figure spectrum of superconducting nano porcelain powder;
Fig. 2 is embodiment 2 gained Nd
1.85ce
0.15cuO
4-δthe XRD figure spectrum of superconducting nano porcelain powder;
Fig. 3 is embodiment 2 gained Nd
1.85ce
0.15cuO
4-δthe TEM photo of superconducting nano porcelain powder;
Fig. 4 is embodiment 2 gained Nd
1.85ce
0.15cuO
4-δthe HRTEM photo of superconducting nano porcelain powder;
Fig. 5 is embodiment 3 gained Nd
1.83ce
0.17cuO
4-δthe XRD figure spectrum of superconducting nano porcelain powder;
Fig. 6 is the Nd that embodiment 2 obtains with solid phase method
2-xce
xcuO
4-δthe XRD of powder contrasts collection of illustrative plates.
Embodiment
Below in conjunction with accompanying drawing the present invention done and be described further.
Embodiment 1
(1) by Nd (NO
3)
3nH
2o, Cu (NO
3)
23H
2o and EDTA(ethylenediamine tetraacetic acid (EDTA)) be that 2:1:3 weighs by the mol ratio of Nd:Ce:Cu:EDTA;
(2) be 5:1 by liquid-solid ratio (L/Kg), standby for step (1) institute EDTA is placed in deionized water, and add quadrol adjust ph is 4 simultaneously, obtains mixing solutions;
(3) in step (2) gained mixing solutions, the standby Nd (NO of step (1) is added
3)
3nH
2o and Cu (NO
3)
23H
2o, add quadrol adjust ph is 8 simultaneously, obtains mixture;
(4) step (3) gained mixture is obtained colloidal sol through 60 DEG C of reflux 1h, reheats evaporation concentration 7h and obtain gel, and by gel in baking oven with 120 DEG C, constant pressure and dry obtains xerogel;
(5) step (4) gained xerogel is obtained Nd with 600 DEG C of calcining 8h in air atmosphere
2cuO
4-δsuperconducting nano porcelain powder.
Embodiment 2
(1) by Nd (NO
3)
3nH
2o, Ce (NO
3)
36H
2o, Cu (NO
3)
23H
2o and EDTA(ethylenediamine tetraacetic acid (EDTA)) be that 1.85:0.15:1:3 weighs by the mol ratio of Nd:Ce:Cu:EDTA;
(2) be 20:1 by liquid-solid ratio (L/Kg), standby for step (1) institute EDTA is placed in deionized water, and add quadrol adjust ph is 6 simultaneously, obtains mixing solutions;
(3) in step (2) gained mixing solutions, the standby Nd (NO of step (1) is added
3)
3nH
2o, Ce (NO
3)
36H
2o and Cu (NO
3)
23H
2o, add quadrol adjust ph is 6 simultaneously, obtains mixture;
(4) step (3) gained mixture is obtained colloidal sol through 75 DEG C of reflux 4h, reheats evaporation concentration 6h and obtain gel, and by gel in baking oven with 90 DEG C, constant pressure and dry obtains xerogel;
(5) step (4) gained xerogel is obtained Nd with 700 DEG C of calcining 8h in air atmosphere
1.85ce
0.15cuO
4-δsuperconducting nano porcelain powder.
Embodiment 3
(1) by Nd (NO
3)
3nH
2o, Ce (NO
3)
36H
2o, Cu (NO
3)
23H
2o and EDTA(ethylenediamine tetraacetic acid (EDTA)) be that 1.83:0.17:1:3 weighs by the mol ratio of Nd:Ce:Cu:EDTA;
(2) be 40:1 by liquid-solid ratio (L/Kg), standby for step (1) institute EDTA is placed in deionized water, and add quadrol adjust ph is 8 simultaneously, obtains mixing solutions;
(3) in step (2) gained mixing solutions, the standby Nd (NO of step (1) is added
3)
3nH
2o, Ce (NO
3)
36H
2o and Cu (NO
3)
23H
2o, add quadrol adjust ph is 10 simultaneously, obtains mixture;
(4) step (3) gained mixture is obtained colloidal sol through 80 DEG C of reflux 2h, reheats evaporation concentration 3h and obtain gel, and by gel in baking oven with 70 ~ 150 DEG C, constant pressure and dry obtains xerogel;
(5) step (4) gained xerogel is obtained Nd with 600 DEG C of calcining 16h in air atmosphere
1.83ce
0.17cuO
4-δsuperconducting nano porcelain powder.
Embodiment 4
(1) by Nd (NO
3)
3nH
2o, Ce (NO
3)
36H
2o, Cu (NO
3)
23H
2o and EDTA(ethylenediamine tetraacetic acid (EDTA)) be that 1.9:0.1:1:3 weighs by the mol ratio of Nd:Ce:Cu:EDTA;
(2) be 30:1 by liquid-solid ratio (L/Kg), standby for step (1) institute EDTA is placed in deionized water, and add quadrol adjust ph is 3.5 simultaneously, obtains mixing solutions;
(3) in step (2) gained mixing solutions, the standby Nd (NO of step (1) is added
3)
3nH
2o, Ce (NO
3)
36H
2o and Cu (NO
3)
23H
2o, add quadrol adjust ph is 4 simultaneously, obtains mixture;
(4) step (3) gained mixture is obtained colloidal sol through 80 DEG C of reflux 1h, reheats evaporation concentration 3 ~ 6h and obtain gel, and by gel in baking oven with 70 DEG C, constant pressure and dry obtains xerogel;
(5) step (4) gained xerogel is obtained Nd with 900 DEG C of calcining 2h in air atmosphere
1.9ce
0.1cuO
4-δsuperconducting nano porcelain powder.
That can find out employing the present invention synthesis from the XRD figure shown in Fig. 1 is Nd mutually
2cuO
4pure phase, 2 θ corresponding halfwidth (FWHM) 31.501 °, 31.497 °, 45.89 ° 9,56.78 ° time can be obtained be respectively 0.0078,0.0078,0.0062,0.0061 XRD figure spectrum, utilize to thank and strangle formula and try to achieve corresponding powder grain size and be: 170.8,170.8,223.1,240.2, its median size is 20nm as can be seen here.That can find out synthesis from the XRD figure shown in Fig. 2 is Nd mutually
1.85ce
0.15cuO
4-δpure phase, Fig. 3 shows the Nd calcining synthesis at 700 DEG C
1.85ce
0.15cuO
4-δtEM photo, as can be seen from the figure the particle diameter of powder is at about 50nm, crystal grain distribution uniform simultaneously, as can be seen from the lattice of the HRTEM of Fig. 4 mutually in, calcine the primary particle size of the powder obtained at about 15nm, Fig. 5 is the XRD figure spectrum of powder after calcining in embodiment 3, and that as can be seen from the figure synthesize is Nd mutually
1.83ce
0.17cuO
4pure phase, utilizes to thank and strangles formula and can try to achieve its average particle size particle size for 17nm.In addition, as can be seen from Fig. 6 the synthetic method that solid phase method and the present invention propose XRD comparison diagram in, still there is a lot of Ce in the powder that solid phase method calcines synthesis at 700 DEG C
2o
3, Nd
2o
3with the phase of CuO, only there is a small amount of Nd
1.85ce
0.15cuO
4-δphase, the sol-gel method that the present invention proposes as can be seen here achieves pure phase Nd
1.85ce
0.15cuO
4-δthe low temperature synthesis of nano-powder, greatly reduces synthesis energy consumption simultaneously.
Claims (2)
1. a Nd
2-xce
xcuO
4-δthe low temperature preparation method of superconducting nano porcelain powder, is characterized in that through following each step:
(1) by Nd (NO
3)
3nH
2o, Ce (NO
3)
36H
2o, Cu (NO
3)
23H
2o and EDTA is that 2-x:x:1:3 weighs by the mol ratio of Nd:Ce:Cu:EDTA, wherein x=0 ~ 0.17;
(2) be 5 ~ 40:1 by liquid-solid ratio, standby for step (1) institute EDTA is placed in deionized water, and add quadrol adjust ph scope is 3.5 ~ 8 simultaneously, obtains mixing solutions;
(3) in step (2) gained mixing solutions, the standby Nd (NO of step (1) is added
3)
3nH
2o, Ce (NO
3)
36H
2o and Cu (NO
3)
23H
2o, add quadrol adjust ph scope is 4 ~ 10 simultaneously, obtains mixture;
(4) step (3) gained mixture is obtained colloidal sol through 60 ~ 80 DEG C of reflux, reheat evaporation concentration and obtain gel, and be dry xerogel under the normal pressure of 70 ~ 150 DEG C in temperature by gel;
(5) be that under the air atmosphere of 600 ~ 900 DEG C, calcining 2 ~ 16h obtains Nd in temperature by step (4) gained xerogel
2-xce
xcuO
4-δsuperconducting nano porcelain powder.
2. Nd according to claim 1
2-xce
xcuO
4-δthe low temperature preparation method of superconducting nano porcelain powder, is characterized in that: the time of described step (4) reflux is 1 ~ 4h, and the time of evaporation concentration is 3 ~ 7h.
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| CN104003708A (en) * | 2014-05-20 | 2014-08-27 | 昆明理工大学 | Preparation method of Nd1.85Ce0.15CuO4-detal superconducting target with preferred orientation |
| CN106663502B (en) * | 2014-11-05 | 2018-09-04 | 株式会社藤仓 | Oxide superconductor, superconducting wire and their manufacturing method |
| CN106268835B (en) * | 2015-06-08 | 2018-09-25 | 中国石油化工股份有限公司 | A kind of catalyst and preparation method thereof of maleic anhydride Hydrogenation gamma-butyrolacton |
| CN107777719B (en) * | 2017-10-24 | 2019-04-23 | 东北大学秦皇岛分校 | A kind of preparation method and applications of copper acid praseodymium nano adsorption material |
| CN107673392B (en) * | 2017-10-24 | 2019-04-23 | 东北大学秦皇岛分校 | A kind of preparation method and applications of copper acid neodymium nano-powder |
| CN107758723B (en) * | 2017-11-13 | 2019-04-12 | 东北大学 | A kind of copper acid samarium nano-photo catalytic raw powder's production technology and its application |
| CN112811893A (en) * | 2021-01-09 | 2021-05-18 | 浙江大学台州研究院 | Method for uniformly doping nanoparticles in high-temperature superconducting material |
| CN114368776A (en) * | 2022-01-12 | 2022-04-19 | 扬州大学 | Nano polycrystalline powder of electron-doped copper oxide high-temperature superconducting material NCCO and preparation method thereof |
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|---|---|---|---|---|
| CN1686817A (en) * | 2005-04-29 | 2005-10-26 | 中国科学院上海光学精密机械研究所 | Direct synthesis of Y by citric acid combustion method2O3Method for preparing nano material |
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