CN101307489A - Halogen-containing high temperature superconductor crystal and method for making same - Google Patents

Halogen-containing high temperature superconductor crystal and method for making same Download PDF

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CN101307489A
CN101307489A CNA2008100575183A CN200810057518A CN101307489A CN 101307489 A CN101307489 A CN 101307489A CN A2008100575183 A CNA2008100575183 A CN A2008100575183A CN 200810057518 A CN200810057518 A CN 200810057518A CN 101307489 A CN101307489 A CN 101307489A
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刘青清
李凤英
靳常青
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Institute of Physics of CAS
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Abstract

The invention relates to a halogen-containing high-temperature superconducting crystal material and a high-pressure preparation method thereof. The halogen-containing high-temperature superconducting crystal material is Sr2CuO2+deltaCl2-y, the crystal is apical oxygen doped, wherein, the delta is more than 0 and less than 2, the y is more than 0 and less than 2, an a-axis lattice parameter is between 3.8 and 3.94, and a current carrier of the crystal is a p-type current carrier. The invention also provides a high-pressure synthetic method for the Sr2CuO2+deltaCl2-y crystal. The method adopts an apical oxygen doped mechanism, utilizes SrO2 as an oxygen source, and uses a precursor method to prepare the p-type high-temperature superconducting crystal material under high temperature and high pressure by controlling oxygen pressure and changing chloride content. The material has good two-dimensional characteristics, so the material is the ideal material for researching an electronic structure of the plane of CuO2.

Description

A kind of halogen-containing high temperature superconductor crystal and preparation method thereof
Technical field
The present invention relates to a kind of high-temperature superconductor, particularly relate to a kind of a kind of Sr of drift angle oxygen mechanism of doping effect High Temperature High Pressure synthetic that utilizes 2CuO 2+ δCl 2-yHigh temperature superconductor crystal and high temperature and high pressure preparation process thereof.
Background technology
High-temperature superconductor research is the important front edge field of condensed matter science.High-temperature superconductor belongs to deutero-perovskite copper oxide on crystalline structure, and pressure is fit to the uhligite material of Metacentre Height densification very much.Pressure is being brought into play in the research of high-temperature superconductor and important effect, is the important means of development new high temperature superconductor.
On crystalline structure, high-temperature superconductor is made of two portions: charge reservoir layer and [CuO 2] the plane conductive layer, the connection between them is " drift angle oxygen " normally.Go up from directly perceived, drift angle oxygen and high-temperature superconductor origin have close association.If keep basic [CuO 2] plane, and change interlayer structure into halogenide by common oxide compound, then form a kind of new superconduction system---oxyhalogenide high-temperature superconductor.The oxyhalogenide high-temperature superconductor provides an ideal system for research drift angle oxygen problem.People such as Jin (C.Q.Jin, et al., Nature (London) 375,301 (1995)) in this system, propose and set up a kind of unconventional mechanism of doping effect first---" doping of drift angle oxygen ", promptly partly substitute drift angle monovalence chlorine with divalence oxygen, introduce the middle mutually drift angle oxygen that this does not have of parent in adulterated mode, under High Temperature High Pressure, successfully synthesize T first c=80K contains bilayer [CuO 2] planar (Sr, Ca) 3Cu 2O 4+ δCl 2-xSuperconductor produces p type current carrier in different valency negatively charged ion alternate mode.Corner position is occupied fully by oxygen and chlorine in the adulterated Cl-system high-temperature superconducting of drift angle oxygen body, regulates hole by the relative content that changes oxygen and chlorine, and it is electrical to produce high-temperature superconductor, is the ideal system of carrying out structure and Correlation of Physical research.On the other hand, chlorine copper oxygen compound is fit to the experimental study of angular resolution photoelectron spectrum (ARPES) and scanning tunnel spectrum (STM) as a kind of ideal two-dimensional model system material very much.Therefore, by optimize the synthesis technique development simple in structure contain individual layer [CuO 2] this type of new type high temperature superconductor of planar, understanding drift angle oxygen problem and high-temperature superconductor mechanism are had positive effect.
Summary of the invention
One of purpose of the present invention is to utilize a kind of unconventional mechanism of doping effect---and drift angle oxygen mixes, the synthetic individual layer [CuO that contains of High Temperature High Pressure 2] planar Cl-system high-temperature superconducting body crystal.
Another object of the present invention provides a kind of preparation and contains individual layer [CuO 2] planar Cl-system high-temperature superconducting body crystalline High Temperature High Pressure synthetic method.
To achieve these goals, the present invention adopts following technical scheme:
The invention provides a kind of Sr 2CuO 2+ δCl 2-yHigh temperature superconductor crystal, this crystal drift angle oxygen mixes, 0＜δ＜2,0＜y＜2 wherein, a axialite lattice parameter is
Figure A20081005751800051
Above-mentioned Sr 2CuO 2+ δCl 2-yHigh temperature superconductor crystal, its superconducting transition temperature are 10-60K.
Above-mentioned Sr 2CuO 2+ δCl 2-yHigh temperature superconductor crystal, its corner position are occupied fully by oxygen and chlorine and current carrier is a p type current carrier.
Above-mentioned Sr 2CuO 2+ δCl 2-yHigh temperature superconductor crystal, its spacer are I4/mmm, and lattice parameter is
Figure A20081005751800052
Figure A20081005751800053
The invention provides a kind of Sr 2CuO 2+ δCl 2-yThe preparation method of high-temperature superconductor, this method utilize drift angle oxygen mechanism of doping effect, utilize SrO 2Make oxygen source, press and the change cl content by control oxygen, wherein, SrO 2In the oxygen source of excess of oxygen in being pressed into as height, this is to induce in height is pressed into that to produce drift angle oxygen necessary.Prepare 0201-Cl new type high temperature superconductor (Sr by presoma method high pressure 2CuO 2+ δCl 2-yHigh-temperature superconductor), may further comprise the steps:
1) under normal pressure, preparation Sr 2CuO 2Cl 2And Sr 2CuO 3Precursor samples;
2) with presoma Sr 2CuO 2Cl 2And Sr 2CuO 3, SrO 2With CuO by (2-y)/2: (p/2): q: (the Sr wherein of mol ratio (y-p)/2 2CuO 3With SrO 2Mole number be respectively p and q, y=p+q, 0＜p＜1,0＜q＜1) at rare gas element, weighing in the preferred argon gas, mixing, also grinding, compressing tablet then, with goldleaf or platinum foil parcel, and be encapsulated in the NaCl, and the sample that presses is put into the graphite furnace that places the high pressure assembly, carry out height and be pressed into, obtain Sr 2CuO 2+ δCl 2-yHigh temperature superconductor crystal, its mesohigh synthetic pressure is 3-8GPa, and temperature is 850-1200 ℃, and soaking time is more than 20 minutes.
Wherein, the preferred 4-7GPa of pressure, further preferred 5-6GPa.
Wherein, the preferred 900-1200 of temperature ℃, further preferred 950-1100 ℃.
Above-mentioned Sr 2CuO 2+ δCl 2-yAmong the preparation method of high-temperature superconductor, step 1) is synthesized Sr 2CuO 2Cl 2The concrete steps of presoma are technique known, and with document L.L.Miller, et al. is among full content introducing the application of Phys.Rev.B 41,1921 (1990) at this.
Above-mentioned Sr 2CuO 2+ δCl 2-yAmong the preparation method of high-temperature superconductor, step 1) is synthesized Sr 2CuO 3The concrete steps of presoma comprise:
Adopt solid phase reaction method under the normal pressure, with 99.9% or the SrCO of above purity 3With of mixed in molar ratio, the grinding of CuO powder with 2: 1, and under 950 ℃ condition sintering, be incubated 24 hours, preferably repeat sintering three times, obtain monophasic Sr 2CuO 3Compound.
Above-mentioned Sr 2CuO 2+ δCl 2-yAmong the preparation method of high-temperature superconductor, step 2) synthetic Sr 2CuO 2+ δCl 2-yThe concrete steps of high temperature superconductor crystal comprise:
With synthetic presoma Sr 2CuO 2Cl 2, Sr 2CuO 3With SrO 2With CuO by the weighing in being filled with the glove box of rare gas element, for example argon gas of above-mentioned mol ratio, mixing, evenly grind; Be pressed into the sequin of diameter 5mm then,, and be encapsulated in the NaCl cylinder of Φ 8 * 15mm with the goldleaf parcel; The sample that presses is put into graphite furnace, pack into and carry out height in the high pressure assembly and be pressed into, sample synthesizes on the big press of cubic apparatus and carries out, at room temperature slowly boost to earlier 6GPa, restart heating schedule and be heated to 950-1100 ℃, insulation is 20-150 minute under high-temperature and high-pressure conditions, is quenched to room temperature, release then (1GP,a=1 ten thousand normal atmosphere).
Wherein, before High-Voltage Experimentation, at first carry out the demarcation of temperature and pressure, with the method control Heating temperature of control heating power.
Description of drawings
Below in conjunction with drawings and Examples the present invention is described further:
Fig. 1 is the device synoptic diagram of High Temperature High Pressure synthetic sample of the present invention.
Fig. 2 is the Sr of high pressure preparation of the present invention 2CuO 2+ δCl 1.2X ray diffracting spectrum.The different symbol of mark is represented CuO (o), SrCl respectively among the figure 2Sr (OH) 2H 2O (*) with unknown mutually (?).
Fig. 3 is the Sr of high pressure preparation of the present invention 2CuO 2+ δCl 1.2The dc magnetization rate and the relation of temperature.Illustration is represented Sr 2CuO 2+ δCl 1.2Resistance and the relation of temperature.
Embodiment
Embodiment 1 utilizes drift angle oxygen mechanism of doping effect height to be pressed into Sr 2CuO 2+ δCl 2-yHigh temperature superconductor crystal.
Sr 2CuO 2Cl 2The preparation of precursor samples
Referring to reference L.L.Miller, et al., Phys.Rev.B 41,1921 (1990).
Sr 2CuO 3The preparation of precursor samples
Adopt solid phase reaction method under the normal pressure, with the SrCO of 99.9% purity 3With mixed in molar ratio, the grinding of CuO powder with 2: 1, sintering under 950 ℃ condition, be incubated 24 hours or repeat this sintering three times, just can prepare monophasic Sr 2CuO 3Compound.
Sr 2CuO 2+ δCl 2-yThe crystalline preparation
Utilize SrO 2Make oxygen source, press and the change cl content, carry out Sr by control oxygen 2CuO 2+ δCl 2- yThe crystalline preparation.With Sr 2CuO 2Cl 2, Sr 2CuO 3, SrO 2Press (2-y)/2 with CuO: (p/2): q: mol ratio (y-p)/2 (p=0.4, q=0.4, y=0.8) weighing in being filled with the glove box of argon gas, mixing, evenly grinding.Be pressed into the sequin of diameter 5mm then,, and be encapsulated in the NaCl cylinder of Φ 8 * 15mm with the goldleaf parcel.The sample that presses is put into graphite furnace, and the high pressure assembly interior (device as shown in Figure 1) of packing into carries out height and is pressed into.Sample synthesizes on the big press of cubic apparatus and carries out, and at first carries out the demarcation of temperature and pressure before the High-Voltage Experimentation, with the method control Heating temperature of control heating power.Earlier at room temperature slowly boost to 5GPa, restart heating schedule and be heated to 1200 ℃, insulation is 20 minutes under high-temperature and high-pressure conditions, is quenched to room temperature, and release then obtains Sr 2CuO 2+ δCl 2-yCrystal prototype.
Sample is carried out X-ray diffraction measures, the result as shown in Figure 2, the result confirms that sample is monophasic Sr 2CuO 2+ δCl 2-yCrystal, through indexing as can be known its spacer be I4/mmm, lattice constant is
Figure A20081005751800081
Figure A20081005751800082
Simultaneously its susceptibility and resistivity are measured with variation of temperature, be the results are shown among Fig. 3, as shown in Figure 3, this Sr 2CuO 2+ δCl 2-yThe crystalline superconducting transition temperature is about 30K.
Embodiment 2 utilizes drift angle oxygen mechanism of doping effect height to be pressed into Sr 2CuO 2+ δCl 2-yHigh temperature superconductor crystal.
Sr 2CuO 2Cl 2And Sr 2CuO 3The preparation of precursor samples is identical with embodiment 1.
Sr 2CuO 2+ δCl 2-yThe crystalline preparation:
Utilize SrO 2Make oxygen source, press and the change cl content, carry out Sr by control oxygen 2CuO 2+ δCl 2- yThe crystalline preparation.With Sr 2CuO 2Cl 2, Sr 2CuO 3, SrO 2Press (2-y)/2 with CuO: (p/2): q: mol ratio (y-p)/2 (p=0.2, q=0.4, y=0.6) weighing in being filled with the glove box of argon gas, mixing, evenly grinding.Be pressed into the sequin of diameter 5mm then,, and be encapsulated in the NaCl cylinder of Φ 8 * 15mm with the goldleaf parcel.The sample that presses is put into graphite furnace, and the high pressure assembly interior (device as shown in Figure 1) of packing into carries out height and is pressed into.Sample synthesizes on the big press of cubic apparatus and carries out, and at first carries out the demarcation of temperature and pressure before the High-Voltage Experimentation, with the method control Heating temperature of control heating power.Earlier at room temperature slowly boost to 6GPa, restart heating schedule and be heated to 1150 ℃, insulation is 30 minutes under high-temperature and high-pressure conditions, is quenched to room temperature, and release then obtains Sr equally 2CuO 2+ δCl 2 -yCrystal prototype.
Embodiment 3 utilizes drift angle oxygen mechanism of doping effect height to be pressed into Sr 2CuO 2+ δCl 2-yHigh temperature superconductor crystal.Sr 2CuO 2Cl 2And Sr 2CuO 3The preparation of precursor samples is identical with embodiment 1.
Sr 2CuO 2+ δCl 2-yThe crystalline preparation
Utilize SrO 2Make oxygen source, press and the change cl content, carry out Sr by control oxygen 2CuO 2+ δCl 2- yThe crystalline preparation.With Sr 2CuO 2Cl 2, Sr 2CuO 3, SrO 2Press (2-y)/2 with CuO: (p/2): q: mol ratio (y-p)/2 (p=0.15, q=0.4, y=1.0) weighing in being filled with the glove box of argon gas, mixing, evenly grinding.Be pressed into the sequin of diameter 5mm then,, and be encapsulated in the NaCl cylinder of Φ 8 * 15mm with the goldleaf parcel.The sample that presses is put into graphite furnace, and the high pressure assembly interior (device as shown in Figure 1) of packing into carries out height and is pressed into.Sample synthesizes on the big press of cubic apparatus and carries out, and at first carries out the demarcation of temperature and pressure before the High-Voltage Experimentation, with the method control Heating temperature of control heating power.Earlier at room temperature slowly boost to 7GPa, restart heating schedule and be heated to 1100 ℃, insulation is 80 minutes under High Temperature High Pressure, is quenched to room temperature, and release then obtains Sr equally 2CuO 2+ δCl 2-yCrystal prototype.
Embodiment 4 utilizes drift angle oxygen mechanism of doping effect height to be pressed into Sr 2CuO 2+ δCl 2-yHigh temperature superconductor crystal.
Sr 2CuO 2Cl 2And Sr 2CuO 3The preparation of precursor samples is identical with embodiment 1.
Sr 2CuO 2+ δCl 2-yThe crystalline preparation
Utilize SrO 2Make oxygen source, press and the change cl content, carry out Sr by control oxygen 2CuO 2+ δCl 2- yThe crystalline preparation.With Sr 2CuO 2Cl 2, Sr 2CuO 3, SrO 2Press (2-y)/2 with CuO: (p/2): q: mol ratio (y-p)/2 (p=0.8, q=0.4, y=1.2) weighing in being filled with the glove box of argon gas, mixing, evenly grinding.Be pressed into the sequin of diameter 5mm then,, and be encapsulated in the NaCl cylinder of Φ 8 * 15mm with the goldleaf parcel.The sample that presses is put into graphite furnace, and the high pressure assembly interior (device as shown in Figure 1) of packing into carries out height and is pressed into.Sample synthesizes on the big press of cubic apparatus and carries out, and at first carries out the demarcation of temperature and pressure before the High-Voltage Experimentation, with the method control Heating temperature of control heating power.Earlier at room temperature slowly boost to 7GPa, restart heating schedule and be heated to 950 ℃, insulation is 120 minutes under High Temperature High Pressure, is quenched to room temperature, and release then obtains Sr equally 2CuO 2+ δCl 2-yCrystal prototype.
It should be noted that; above in conjunction with the embodiments technical scheme of the present invention is had been described in detail; but those skilled in the art will find apparent that; on the technical solution of the present invention basis; can carry out variations and modifications to technical scheme of the present invention, but not break away from the generalized scope of the present invention's claims required for protection.

Claims (9)

1, a kind of Sr 2CuO 2+ δCl 2-yHigh temperature superconductor crystal, this crystal drift angle oxygen mix and have a unusual big a axialite lattice parameter, 0＜δ＜2,0.4≤y≤1.2 wherein, and a is not less than
Figure A2008100575180002C1
2, high temperature superconductor crystal as claimed in claim 1 is characterized in that, this crystalline superconducting transition temperature is 10-60K.
3, high temperature superconductor crystal as claimed in claim 1 is characterized in that, its corner position is occupied fully by oxygen and chlorine and current carrier is a p type current carrier.
4, each described high temperature superconductor crystal of claim 1-3 is characterized in that, this crystalline spacer is I4/mmm, and lattice parameter is
Figure A2008100575180002C2
5, each described Sr of a kind of claim 1-4 2CuO 2+ δCl 2-yThe preparation method of high temperature superconductor crystal, this method utilize drift angle oxygen mechanism of doping effect, under high pressure prepare Sr by the presoma method 2CuO 2+ δCl 2-yHigh-temperature superconductor may further comprise the steps:
1) under normal pressure, preparation Sr 2CuO 2Cl 2And Sr 2CuO 3Precursor samples;
2) with presoma Sr 2CuO 2Cl 2And Sr 2CuO 3With SrO 2With CuO by (2-y)/2: (p/2): q: (the Sr wherein of mol ratio (y-p)/2 2CuO 3With SrO 2Mole number be respectively p and q, y=p+q, 0＜p＜1,0＜q＜1) weighing in rare gas element, mixing and grinding, compressing tablet with goldleaf or platinum foil parcel, and is encapsulated in the NaCl then, and the sample that presses put into the graphite furnace that places the high pressure assembly, and carry out height and be pressed into, obtain Sr 2CuO 2+ δCl 2-yHigh temperature superconductor crystal, its mesohigh synthetic pressure is 3-8GPa, and temperature is 850-1200 ℃, and insulation is more than 20 minutes.
6, the preparation method of high-temperature superconductor as claimed in claim 5 is characterized in that, described pressure is 4-7GPa, and described temperature is 950-1100 ℃, and described rare gas element is an argon gas.
7, the preparation method of high-temperature superconductor as claimed in claim 5 is characterized in that, step 1) is synthesized Sr 2CuO 3The concrete steps of presoma comprise:
Adopt solid phase reaction method under the normal pressure, with 99.9% or the SrCO of above purity 3With of mixed in molar ratio, the grinding of CuO powder with 2: 1, and under 950 ℃ condition sintering, be incubated 24 hours, perhaps repeat this sintering three times, obtain monophasic Sr 2CuO 3Compound.
8, the preparation method of high-temperature superconductor as claimed in claim 5 is characterized in that step 2) synthetic Sr 2CuO 2+ δCl 2-yThe concrete steps of high temperature superconductor crystal comprise:
With synthetic presoma Sr 2CuO 2Cl 2, Sr 2CuO 3With SrO 2With CuO by the weighing in being filled with the glove box of argon gas of described mol ratio, mixing, evenly grind; Be pressed into the sequin of diameter 5mm then,, and be encapsulated in the NaCl cylinder of Φ 8 * 15mm with goldleaf or platinum foil parcel; The sample that presses is put into graphite furnace, pack into and carry out height in the high pressure assembly and be pressed into, sample synthesizes on the big press of cubic apparatus and carries out, at room temperature slowly boost to earlier 6GPa, restart heating schedule and be heated to 900-1100 ℃, insulation is 20-60 minute under high-temperature and high-pressure conditions, is quenched to room temperature, release then obtains Sr 2CuO 2+ δCl 2-yHigh temperature superconductor crystal.
9, the preparation method of high-temperature superconductor as claimed in claim 8 is characterized in that, at first carries out the demarcation of temperature and pressure before High-Voltage Experimentation, and controls Heating temperature with the method for control heating power.
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Cited By (3)

* Cited by examiner, † Cited by third party
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CN106083053A (en) * 2016-06-24 2016-11-09 中国科学院地球化学研究所 A kind of preparation method of marmatite electrode
CN106205857A (en) * 2016-06-24 2016-12-07 中国科学院地球化学研究所 A kind of preparation method of magnetic iron ore electrode
CN107817003A (en) * 2016-09-14 2018-03-20 西安航通测控技术有限责任公司 A kind of external parameters calibration method of distributed large scale space positioning system

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106083053A (en) * 2016-06-24 2016-11-09 中国科学院地球化学研究所 A kind of preparation method of marmatite electrode
CN106205857A (en) * 2016-06-24 2016-12-07 中国科学院地球化学研究所 A kind of preparation method of magnetic iron ore electrode
CN106205857B (en) * 2016-06-24 2018-02-13 中国科学院地球化学研究所 A kind of preparation method of magnetic iron ore electrode
CN106083053B (en) * 2016-06-24 2018-10-19 中国科学院地球化学研究所 A kind of preparation method of marmatite electrode
CN107817003A (en) * 2016-09-14 2018-03-20 西安航通测控技术有限责任公司 A kind of external parameters calibration method of distributed large scale space positioning system

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