CN100434365C - YBa2Cu3O7 multicrystal nano-wire array and its preparation method - Google Patents

YBa2Cu3O7 multicrystal nano-wire array and its preparation method Download PDF

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CN100434365C
CN100434365C CNB2005100948185A CN200510094818A CN100434365C CN 100434365 C CN100434365 C CN 100434365C CN B2005100948185 A CNB2005100948185 A CN B2005100948185A CN 200510094818 A CN200510094818 A CN 200510094818A CN 100434365 C CN100434365 C CN 100434365C
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yba
aluminium
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array
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CN1948160A (en
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章根强
陆小力
张涛
李晓光
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University of Science and Technology of China USTC
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Abstract

The present invention relates to a YBa2Cu3O7 nano wire ordered array and its preparation method. It is characterized by that it uses complexing agent ethylenediamine tetraacetic acid and cross-linking agent ethylene glycol, and utilizes the ethylenediamine tetraacetic acid aqueous solution whose pH value is 7-8 and mole concentration is 0.6-1.2, and adds the Y(NO3)3 and Cu(NO3)2 mixed solution obtained by using nitric acid to dissolve Y2O3 and CuO according to the mole ratio of Y:Ba:Cu=1:2:3 and Ba(NO3)2 powder so as to make the molar weight of the contained ethylenediamine tetraacetic acid be twice that of CuO; after the ethylene glycol is added, heats them to obtain a dark brown sol solution; under the condition of low vacuum makes the sol solution be injected into the micropore aluminium oxide template obtained by adopting secondary anodic oxidation process, then makes said template undergo the processes of sintering and pure oxygen atmosphere annealing treatment so as to obtain multicrystal YBa2Cu3O7 nano wire ordered array which is contained in the multipore aluminium oxide template interior and whose diameter is 50-60 nm and length is micrometer-grade. Said YBa2Cu3O7 multicrystal nano wire array has high-temperature superconductivity.

Description

YBa 2Cu 3O 7Multicrystal nano-wire array and preparation method thereof
Technical field:
The invention belongs to oxide high-temperature superconducting material and preparing technical field thereof, particularly relate to YBa 2Cu 3O 7High temperature superconducting materia nanometer line ordered array and preparation method thereof.
Background technology:
U.S.'s " physical comment bulletin " magazine (1987,58 the volume, the 908th page) reported first YBa 2Cu 3O 7-δOxide high temperature superconductor, superconducting transition temperature are 93K, and this is the oxide superconductor that first superconducting temperature is higher than liquid nitrogen temperature.At present, the method for preparing Y-Ba-Cu-O system high-temperature superconducting material mainly is ceramic post sintering method and organic metal salt chemical Vapor deposition process.For example " American Chemical Society's meeting will " magazine is (1998,120 the volume, the 2733rd page) report solid reaction process, U.S.'s " superconduction science and technology " magazine (2003,16 volumes, the 1202nd page) report sol-gel method, U.S.'s " Applied Physics wall bulletin " magazine (1991,120 the volume, the 2426th page) report coprecipitation method, the chemical Vapor deposition process of Germany's " advanced material " magazine (2000,12 volumes, the 116th page) report.Existing solid reaction process and coprecipitation method are owing to the restriction of its raw material and preparation means, and its product can only be the random powder of micron dimension and nanometer scale, and need higher sintering temperature; Chemical Vapor deposition process is because equipment and technology, and product mostly is film greatly, and method program complexity, expense costliness, is unfavorable for applying.
One peacekeeping quasi-one-dimensional nanometer material is widely studied because of having unique character, and nanometer line ordered array more has a lot of unusual character and application prospects.At present, the ordered nano linear array that a lot of metals, alloy, oxide compound and Ferrite Material arranged is being synthesized by success, for example: a series of metal nano-wire arrays such as Au, the Ag of American Chemical Society's " nanometer wall bulletin " magazine (2003,3 volumes, the 919th page) report, Cu, American Chemical Society's " chemical material " magazine (2003,15 volumes, the 664th page) the Ni-Cu alloy nano linear array of report, Germany's " Applied Physics A " magazine (2003,78 the volume, the 1197th page) report Fe 2O 3Nano-wire array.But do not see preparation high temperature superconducting materia YBa so far 2Cu 3O 7The relevant report of nanometer line ordered array.
Summary of the invention:
The present invention proposes a kind of high temperature superconducting materia YBa 2Cu 3O 7Nanometer line ordered array and preparation method thereof.
YBa of the present invention 2Cu 3O 7The preparation method of nanometer line ordered array is characterized in that: getting the pH value is the edta solution of 0.6-1.2M for 7-8, volumetric molar concentration, and by Y: Ba: the Cu mol ratio is that adding in 1: 2: 3 is by nitric acid dissolve Y 2O 3Y (the NO that obtains with CuO 3) 3And Cu (NO 3) 2Mixing solutions and Ba (NO 3) 2Powder, the molar weight that makes wherein contained ethylenediamine tetraacetic acid (EDTA) is the twice of CuO; Add this liquor capacity 1-3 ethylene glycol doubly, the system that is heated to becomes the Vandyke brown sol solution by blue solution; Purity is not less than 99.9% aluminium flake and is not less than 10 in vacuum tightness -3Pa, temperature is annealing after 4-7 hour in 500-600 ℃ the environment, place the electrolyzer anode place of the oxalic acid electrolytic solution that 0.3M ± 0.05M is housed, the one side of aluminium flake is contacted with electrolytic solution, another side contacts with the anode copper sheet, at 30-45V, corrosion is 8-10 hour under the 0-5 ℃ of condition, aluminium flake after the corrosion is placed in the mixed acid solution of 6 ± 1wt% phosphoric acid and 1.5 ± 0.5wt% chromic acid composition, soaked 10-20 hour at 40-60 ℃, then this aluminium flake is placed on the anode place of the electrolyzer that 0.3 ± 0.05M oxalic acid solution is housed, the one side that was corroded is contacted with electrolytic solution, another side contacts with the copper sheet anode, at 30-45V, carried out corroding the second time 18-24 hour under the 0-5 ℃ of condition; With removing the remaining aluminium lamination of the side that does not contact with the solution of aluminium generation replacement(metathesis)reaction with electrolytic solution; To face down except that this of intact aluminium, float on 2-4 hour through hole on the 4-6wt% phosphoric acid solution; Porous alumina formwork behind the through hole is placed above-mentioned sol solution, be evacuated to and be not less than 10 -1Pa; Take out the porous alumina formwork that this has filled colloidal sol, more than 10 hours, obtain being included in the YBa in the template 700-800 ℃ of insulation 2Cu 3O 7-δNanometer line ordered array; Through the pure oxygen atmosphere anneal, promptly obtain YBa again 2Cu 3O 7Nanometer line ordered array.
Described energy comprises CuCl with aluminium generation replacement(metathesis)reaction with the solution of removing the side residue aluminium lamination that does not contact with electrolytic solution 2Or SnCl 2
Adopt the YBa of method for preparing among the present invention 2Cu 3O 7Nanometer line ordered array is characterised in that it is to be contained in polycrystalline YBa in the porous alumina formwork that the aperture is 50-60nm, that be arranged parallel to each other 2Cu 3O 7The oldered array that nano wire is formed, lattice is an orthohormbic structure, it is electrical to possess high-temperature superconductor.
Method among the present invention utilizes ethylenediamine tetraacetic acid (EDTA) as complexing agent, and ethylene glycol obtains the colloidal sol of stable homogeneous as linking agent, and equipment used is simple, and operation is easily gone; The speed and the degree of control rate of heating and adjustable ethylene glycol of time and ethylenediamine tetraacetic acid (EDTA) polyreaction are grasped the sol-gel transition process; Can in order to pouring into the alumina formwork in different apertures, thereby can obtain the nano wire of different diameter by the viscosity of allotment colloidal sol; Because aluminum oxide is 800 ℃ of beginning crystallization, the aluminum oxide after the crystallization is insoluble to bronsted lowry acids and bases bronsted lowry, causes resulting nano wire to deal and characterizes, so be defined as 800 ℃ on the sintering temperature; Traditional sol-gel process for preparing adopts organic metal salt as precursor more, the expense costliness, complicated operation, and can not effectively control the transition process of collosol and gel, can not realize the regulation and control to the colloidal sol viscosity, the colloidal sol that makes traditional method obtain is unsuitable for pouring porous alumina formwork and prepares nano wire; With traditional solid state reaction, coprecipitation method synthesis temperature is to compare more than 900 ℃, and the precursor sol thing in the inventive method is a molecular level uniform mixing system, and reaction activity reduces greatly, makes the inventive method synthesize YBa 2Cu 3O 7Temperature be reduced to 700 ℃; Traditional solid reaction process can only obtain the random granular powder of micron order, and constraint can obtain large-area nano line oldered array as hard template with porous alumina formwork in the inventive method.This method is at present known in the world synthesizing high temperature superconducting material YBa simple, cheap, that easily go 2Cu 3O 7The method of nanometer line ordered array.
YBa among the present invention 2Cu 3O 7Be by diameter be 50-60nm, the nanometer line ordered array that constitutes of the polycrystalline compounds vertically arranged of being parallel to each other, be successfully to synthesize big area, densification, continuously and YBa in the world first with high-temperature superconductor characteristic 2Cu 3O 7The one-dimensional nano line oldered array helps further understanding the origin of high-temperature superconductor, is exploitation highly sensitive infrared detector, and Josephson saves very-high speed computer, and high-resolution superconducting quantum interference device (SQUID) provides important material foundation.
Description of drawings:
Fig. 1 is the surface topography photo of the porous alumina formwork of JSM-6700F field emission scanning electron microscope (FE-SEM) observation;
Fig. 2 is the cross section pattern photo of the porous alumina formwork of JSM-6700F field emission scanning electron microscope observation.
Fig. 3 is the YBa that is filled in the porous alumina formwork 2Cu 3O 7-δThe copper target X-ray diffraction style figure of nano-wire array.
Fig. 4 is the surface topography photo that is contained in the nano-wire array in the porous alumina formwork of JSM-6700F field emission scanning electron microscope observation;
Fig. 5, Fig. 6 and Fig. 7 are the YBa behind the partial oxidation aluminum alloy pattern plate of removing of JSM-6700F field emission scanning electron microscope observation 2Cu 3O 7-δThe surface topography photo of nano-wire array different amplification.
Fig. 8 is the YBa behind whole alumina formworks of removing of H-800 transmission electron microscope (TEM) observation 2Cu 3O 7-δThe pattern photo of nano wire.
Fig. 9 is the YBa of JEOL-2010 high resolution transmission electron microscopy (HRTEM) observation 2Cu 3O 7-δSingle nano-wire and pairing selected area electron diffraction pattern thereof.
Figure 10 goes up measured YBa in superconducting quantum interference device (SQUID) (SQUID) 2Cu 3O 7The specific magnetising moment of nano-wire array and the curve relation figure of temperature.
Embodiment:
Embodiment 1:YBa 2Cu 3O 7The preparation of nanometer line ordered array
1), adopt the two-step anodization legal system to be equipped with porous alumina formwork:
The aluminium flake that will be not less than 99.9% (used aluminium flake purity is 99.999% in the present embodiment) through the purity of ultrasonic cleaning, polishing and anneal is packed in the electrolyzer, adopting the oxalic acid of 0.3mol/L is electrolytic solution, in temperature is under the 0--5 ℃ of condition, and the oxidation voltage that adds 40V carried out once oxidation 8-10 hour; With the aluminium flake behind the once oxidation by H 3PO4 and H 2CrO 4Soak after 10-20 hour in the nitration mixture of forming and take out, under the condition identical, carried out secondary oxidation 20 hours with once oxidation; To seal through oxide film one side of the aluminium flake behind the secondary oxidation, opposite side is immersed the CuCl of 1mol/L 2When having bubble to produce, do not take out in the solution, to remove the aluminum substrate of this side;
Its chemical process can be expressed as:
2Al+3CuCl 2→3Cu+2AlCl 3
At last aluminium flake being swum in the phosphoric acid solution of 5 ± 1wt% has the globule to ooze out until upper surface, and this step is used to remove the blocking layer of pellumina.
2), the required sol solution of sol-gel method preparation:
According to compound YBa 2Cu 3O 7Composition, take by weighing 0.4516g (0.002mol) Y respectively 2O 3, 2.0904g (0.008mol) Ba (NO 3) 2, 0.9546g (0.012mol) CuO; With Y 2O 3With CuO HNO 3Obtain Y (NO after the solution dissolving 3) 3And Cu (NO 3) 2Mixing solutions 20ml; Take by weighing 7.02g (0.024mol) ethylenediamine tetraacetic acid (EDTA), be dissolved in the distilled water of 30ml, and regulate the pH value to 7-8 with quadrol; Add the Ba (NO that has weighed up 3) 2And be stirred to it and dissolve fully; Pour the Y (NO of above-mentioned 20ml into 3) 3And Cu (NO 3) 2Mixing solutions, and add in the quadrol and dissolving Y 2O 3With nitric acid unnecessary in the CuO process, be 7-8 with the pH value that keeps solution, stir the blue solution that obtains stable homogeneous; Adding 50ml-150ml ethylene glycol and stirring make it to mix with solution in this 50ml blue solution, heat mixing solutions 40-60 minute that obtains, and obtain the sol solution of brown stable homogeneous.The volume of ethylene glycol is many more, and resulting sol solution viscosity is big more, and needed heat-up time is few more.
3), YBa 2Cu 3O 7The preparation of nano-wire array:
Porous alumina formwork is immersed in the wide-necked bottle of the sol solution that fills step 2 preparation, is not less than 10 in vacuum tightness -1Kept 10-30 minute under the condition of Pa; The insulation in air, under 700 ℃ the condition of the alumina formwork that fills up sol solution in the hole was obtained being filled in the YBa in the alumina formwork hole after 12 hours 2Cu 3O 7-δNanometer line ordered array.
4), the processing of sample
Earlier the cotton balls that dips in a small amount of dehydrated alcohol with tweezers gripping wiping template surface gently dips in the Al that takes a morsel with cotton balls then 2O 3Ultrafine powder wiping template surface 5-10 minute is removed the YBa of surface adhesion 2Cu 3O 7-δPowder separates the aluminum substrate of pellumina with peripheral support with pincet again; 8-10 the alumina formwork grind into powder through above-mentioned processing can be carried out the XRD test, with resulting powder in pure oxygen atmosphere, through program be: be warming up to 500 ℃ through 30 hours from 300 ℃, after being cooled to 300 ℃ anneal by 500 ℃ in 30 hours, can go up the relation curve of measuring its specific magnetising moment and temperature again in superconducting quantum interference device (SQUID) (SQUID).
YBa is handled and be filled with to NaOH solution with 6mol/L to passing through surperficial wiping 2Cu 3O 7-δAfter the alumina formwork of nano wire carries out in various degree corrosion, can carry out FE-SEM, TEM, HRTEM test.
Fig. 1 is the surperficial FE-SEM figure of self-control porous alumina formwork, the diameter of as can be seen from the figure prepared porous alumina formwork hole evenly, regular shape, arrangement high-sequential;
Fig. 2 is the cross section FE-SEM figure of porous alumina formwork, the hole vertical film surface of as can be seen from the figure prepared porous alumina formwork and being arranged parallel to each other.
Fig. 3 is with the prepared YBa that is filled with among the embodiment 2Cu 3O 7-δThe X-ray diffraction style of the alumina formwork of nano-wire array after milled processed, its X-coordinate are diffraction angle (2 θ), and ordinate zou is relative diffracted intensity; Diffraction peaks all among the figure is consistent with the JCPDS-89-5842 in the international standard powder X-ray RD diffraction card, can change into (103), (102), (103), (110) by the orthohomic lattice index ... because used alumina formwork is a kind of anoxic structure in the present embodiment, so the YBCO sample that burns out at general air atmosphere all can show anoxic structure in various degree, the YBa of the indexing as a result of Fig. 3 2Cu 3O 6.94It is exactly a kind of anoxic structure.Sample is carried out anneal can obtain not anoxybiotic YBCO nano wire, i.e. YBa under pure oxygen atmosphere 2Cu 3O 7Nano wire.
Fig. 4 wipes to be filled with YBa 2Cu 3O 7-δSurperficial FE-SEM observed behind the alumina formwork surface attachments of nano wire schemes, and this figure reflects the YBa that the method that adopts among the embodiment can obtain high fill-ratio intuitively 2Cu 3O 7-δNano-wire array, this is consistent with result among Fig. 4 and Fig. 5.
Fig. 5, Fig. 6 and Fig. 7 are respectively the YBa that removes behind the partial oxidation aluminum alloy pattern plate 2Cu 3O 7-δThe FE-SEM figure of nano-wire array different amplification, Fig. 4 and Fig. 5 reflect that the prepared nano wire of method that adopts among the embodiment is large-area, its filling ratio is very high; It is full that Fig. 6 illustrates that prepared nano wire has, and diameter is even, and the characteristics that length-to-diameter ratio is bigger, its length are micron dimension.
Fig. 8 removes the TEM shape appearance figure of being observed behind whole alumina formworks, as can be seen from the figure, adopts the prepared YBa of method in implementing 2Cu 3O 7-δNanowire diameter evenly, smooth surface and nano wire be fine and close, and length is micron dimension.
Fig. 9 is the YBa in high resolution transmission electron microscopy (HRTEM) observation 2Cu 3O 7-δThe shape appearance figure of single nano-wire and corresponding selected area electron diffraction pattern thereof, this figure has proved that further the diameter of nano wire is even, smooth surface and densification; Its electron diffraction pattern is a ring-type, proves prepared YBa 2Cu 3O 7Nano wire is a polycrystalline, but and index turn to (104), (020), (205) crystal face, this result is consistent with XRD indexing result.
Figure 10 is the YBa through the pure oxygen atmosphere anneal that utilizes superconducting quantum interference device (SQUID) to measure 2Cu 3O 7The specific magnetising moment of nano-wire array and the graph of relation of temperature, sample reveals diamagnetism in the 91.8K following table as can be seen; " Superconductor Physics " book (Zhang Liyuan, Zhang Jinlong, the 7th page, Electronic Industry Press) is mentioned and is looped around the diamagnetism that high-temperature superconductor surperficial screen current has on every side caused whole system; This is one of characteristic of having of high-temperature superconductor material, and the Magnetic Measurement result in the present embodiment is that system shows diamagnetism in the 10-91.8K scope, illustrate that the screen current of system this moment is set up, and superconductor is at superconducting transition temperature (T c) below do not have resistance, screen current can exist always, all will show diamagnetism so the sample among the embodiment is lower than 91.8K in temperature, with the YBa that is reported 2Cu 3O 7The superconducting transition temperature unanimity of bulk.
Measuring result and the literature search of XRD, FE-SEM, TEM, HRTEM, SQUID show: adopt the inventive method successfully to prepare high temperature superconducting materia YBa first 2Cu 3O 7The multicrystal nano-wire oldered array, the required instrument of this method is simple, and expense is cheap; Prepared YBa 2Cu 3O 7The multicrystal nano-wire oldered array possesses supraconductivity, has certain pushing effect for the further mechanism of understanding high-temperature superconductor and for the development and application of nano-device.

Claims (3)

1, a kind of YBa 2Cu 3O 7The preparation method of nanometer line ordered array is characterized in that: getting the pH value is the edta solution of 0.6-1.2M for 7-8, volumetric molar concentration, and by Y: Ba: the Cu mol ratio is that adding in 1: 2: 3 is by nitric acid dissolve Y 2O 3Y (the NO that obtains with CuO 3) 3And Cu (NO 3) 2Mixing solutions and Ba (NO 3) 2Powder, the molar weight that makes wherein contained ethylenediamine tetraacetic acid (EDTA) is the twice of CuO; Add this liquor capacity 1-3 ethylene glycol doubly, the system that is heated to becomes the Vandyke brown sol solution by blue solution; Purity is not less than 99.9% aluminium flake and is not less than 10 in vacuum tightness -3Pa, temperature is annealing after 4-7 hour in 500-600 ℃ the environment, place the electrolyzer anode place of the oxalic acid electrolytic solution that 0.3M ± 0.05M is housed, the one side of aluminium flake is contacted with electrolytic solution, another side contacts with the anode copper sheet, at 30-45V, corrosion is 8-10 hour under the 0-5 ℃ of condition, aluminium flake after the corrosion is placed in the mixed acid solution of 6 ± 1wt% phosphoric acid and 1.5 ± 0.5wt% chromic acid composition, soaked 10-20 hour at 40-60 ℃, then this aluminium flake is placed on the anode place of the electrolyzer that 0.3 ± 0.05M oxalic acid solution is housed, the one side that was corroded is contacted with electrolytic solution, another side contacts with the copper sheet anode, at 30-45V, carried out corroding the second time 18-24 hour under the 0-5 ℃ of condition; With removing the remaining aluminium lamination of the side that does not contact with the solution of aluminium generation replacement(metathesis)reaction with electrolytic solution; To face down except that this of intact aluminium, float on 2-4 hour through hole on the 4-6wt% phosphoric acid solution; Porous alumina formwork behind the through hole is placed above-mentioned sol solution, be evacuated to and be not less than 10 -1Pa; Take out the porous alumina formwork that this has filled colloidal sol, more than 10 hours, obtain being included in the YBa in the template 700-800 ℃ of insulation 2Cu 3O 7-δNanometer line ordered array; Through the pure oxygen atmosphere anneal, promptly obtain YBa again 2Cu 3O 7Nanometer line ordered array.
2, YBa according to claim 1 2Cu 3O 7The preparation method of nanometer line ordered array is characterised in that described energy comprises CuCl with aluminium generation replacement(metathesis)reaction with the solution of removing the side residue aluminium lamination that does not contact with electrolytic solution 2Or SnCl 2
3, adopt the YBa of the described method preparation of claim 1 2Cu 3O 7Nanometer line ordered array is characterised in that it is to be contained in polycrystalline YBa in the porous alumina formwork that the aperture is 50-60nm, that be arranged parallel to each other 2Cu 3O 7The oldered array that nano wire is formed, lattice is an orthohormbic structure, it is electrical to possess high-temperature superconductor.
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CN102050423B (en) * 2009-11-06 2013-04-03 国家纳米科学中心 Nickel-bismuth hybridized nanowire and preparation method thereof
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CN109295325B (en) * 2018-09-27 2020-10-30 江苏师范大学 Preparation method of high-strength high-conductivity Cu-Cr-Zn alloy material
CN112456538B (en) * 2020-11-30 2022-02-08 西北有色金属研究院 Preparation method of REBCO nano particle composite YBCO superconducting layer

Citations (2)

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Publication number Priority date Publication date Assignee Title
CN1031296A (en) * 1987-06-09 1989-02-22 纳幕尔杜邦有限公司 The method of improved manufacturing 90K superconductor
JPH07126068A (en) * 1993-04-13 1995-05-16 Kyocera Corp Production of oxide superconductor

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Publication number Priority date Publication date Assignee Title
CN1031296A (en) * 1987-06-09 1989-02-22 纳幕尔杜邦有限公司 The method of improved manufacturing 90K superconductor
JPH07126068A (en) * 1993-04-13 1995-05-16 Kyocera Corp Production of oxide superconductor

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