CN102191543A - Iron arsenide high-temperature superconducting crystal, and preparation method thereof - Google Patents
Iron arsenide high-temperature superconducting crystal, and preparation method thereof Download PDFInfo
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- CN102191543A CN102191543A CN 201110115203 CN201110115203A CN102191543A CN 102191543 A CN102191543 A CN 102191543A CN 201110115203 CN201110115203 CN 201110115203 CN 201110115203 A CN201110115203 A CN 201110115203A CN 102191543 A CN102191543 A CN 102191543A
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Abstract
The invention discloses an iron arsenide high-temperature superconducting crystal, and a preparation method thereof. The high-temperature superconducting crystal is NaxFeAs, wherein 0 < x < 2. A superhigh-pressure synthesis method for the NaxFeAs crystal is provided by the invention, and utilizes high-pressure synchrotron radiation to prepare the high-temperature superconducting crystal. The material presents obvious crystal structure characteristic change along with pressure increase.
Description
Technical field
The present invention relates to a kind of iron arsenic compound high temperature superconductor crystal and preparation method thereof.
Background technology
Since iron-based superconductor LaFeOAs(Tc=26K) find since [Y. Kamihara, et al., J. Am. Chem. Soc.128,10012 (2006)], a series of iron arsenic super conductors are found, and comprise the LnOFeAs (L n=La of " 1111 " type, Sm, Pr, Nd etc.), the RFFeAs (R=Ca of " 122 " type, Sr, Ba, Eu), " 111 " type (Li, Na) FeAs and " 11 " type Fe (Se, Te) superconductor, and superconducting transition temperature is brought up to 55K rapidly.Iron arsenide superconductor presents copper oxide superconductor discovery another the big type high temp superconducting material after 22 years of being adopted as a child.The supraconductivity of iron arsenide is relevant with its laminate structure, and the FeAs layer is considered to supraconductivity is played an important role, and is similar to the CuO2 plane of copper oxide high-temperature superconductor.Compare with strong related charge transfer type Mott copper oxide parent, iron arsenide parent is the metal/semiconductor metallic compound of cruising mutually, presents the behavior of Pauli paramagnetic.Therefore, the iron arsenide that has a higher superconducting transition temperature has proposed challenge to traditional electroacoustic coupling BCS theory.The iron arsenide superconductor of seeking the FeAs of containing layer simple in structure has significant physical meaning to the superconducting mechanism of studying its iron arsenide superconductor.
Summary of the invention
For achieving the above object, the invention provides a kind of iron arsenic compound high temperature superconductor crystal, this crystal is cubic phase NaxFeAs superconductor crystal, and its spacer is P4/nmm, and lattice parameter is a=3.0-4.0, c=6.0-7.1.
Further, among the described NaxFeAs, 0＜x＜2.
Further, described NaxFeAs superconductor crystal presents bigger compression along c direction of principal axis [FeAs4] tetrahedron, trends towards [FeAs4] positive tetrahedron of rule, and the As-Fe-As bond angle reaches 109.4
oThe pressure phase transition of new cubic phase NaxFeAs superconductor crystal is 2-6GPa.
A kind of preparation method of above-mentioned iron arsenic compound high temperature superconductor crystal, be specially: the cubic phase NaxFeAs superconductor crystal that utilizes normal pressure synthesis is as precursor, precursor under the pressure of 0-20GPa, is carried out high pressure and obtains the cubic phase NaxFeAs superconductor crystal that structure is caved in.
Further, described precursor adopts the normal pressure direct sintering to make, its concrete steps are: with 99.9% or the Na of above purity, Fe and As powder be with mol ratio mixing in the glove box that is filled with Ar gas, grinding, the compressing tablet of x:1:1, and the alumina crucible of packing into is encapsulated in then and is filled with in argon gas or the vitreosil pipe, slowly be warmed up to 800-1100 ℃, be incubated 10-24 hour, preferably repeat sintering twice, obtain monophasic NaxFeAs compound.
Further, described precursor adopts normal pressure presoma sintering process to make, and its concrete steps are:
1) under normal pressure, preparation FeAs or Na3As precursor samples;
2) presoma FeAs and Na are pressed 1:x, the weighing in the glove box that is filled with Ar gas of the mol ratio of 0＜x＜2, mixed grinding, compressing tablet, the alumina crucible of packing into, be encapsulated in then and be filled with in argon gas or the vitreosil pipe, slowly be warmed up to 800-1100 ℃, insulation preferably repeated sintering twice more than 5 hours, obtained monophasic NaxFeAs compound.
Further, described temperature is 900-1050 ℃, more preferably 950-1000 ℃.
Further, described precursor adopts the original position High-Voltage Experimentation to obtain the cubic phase NaxFeAs superconductor crystal that structure is caved in, and it utilizes the original position high pressure synchrotron radiation angle x-ray diffraction experiment technology of loosing, and employing diamond anvil high-tension unit carries out the original position High-Voltage Experimentation.
Further, the diamond anvil mesa diameter of described diamond anvil high-tension unit is 500 μ m, and the high pressure packing adopts T301 Stainless Steel sheet, and transmission medium is a silicone oil, and pressing the mark material is ruby, determines pressure by ruby fluorescence peak.
Further, the wavelength of used incident X ray is 0.368 in the described experiment, effective 2
θAngular region is 0-25
o
The invention provides NaxFeAs crystal and ultra-high voltage synthetic method thereof, this method utilizes the high pressure synchrotron radiation to prepare this high-temperature superconductive crystal material.This material shows tangible crystal structure characteristic variation with the increase of pressure.
Description of drawings
Fig. 1 is the NaxFeAs superconductor crystal structure that obtains at the 0-20GPa uht conditions of the present invention;
Fig. 2 is NaxFeAs superconductor crystal [FeAs4] the tetrahedral structure figure (b) that obtains at the 0-20GPa uht conditions of the present invention;
Fig. 3 is the XRD figure spectrum of the NaxFeAs superconductor crystal sample that obtains at the 0-20GPa uht conditions of the present invention;
Fig. 4 is the variation of the lattice parameter of 0-20GPa uht conditions NaxFeAs superconductor crystal of the present invention;
Fig. 5 is the variation of the unit-cell volume of 0-20GPa uht conditions NaxFeAs superconductor crystal of the present invention with pressure;
Fig. 6 is the variation relation figure of the superconducting transition temperature of NaxFeAs superconductor crystal of the present invention with pressure.
Embodiment
Extremely shown in Figure 6 as Fig. 1, technical solution of the present invention is: utilize the precursor method by the NaxFeAs superconductor crystal in normal pressure synthesis four directions phase, then utilize the NaxFeAs superconductor crystal of the cubic phase that ultra-high voltage development structure caves in, characterize at 0-20GPa in conjunction with the synchrotron radiation X ray technology and obtain the ultra-high voltage structure evolution.
A kind of NaxFeAs superconductor crystal by normal pressure preparation of the present invention may further comprise the steps as the method that the precursor height is pressed into the cubic phase NaxFeAs superconductor crystal that a kind of structure caves in:
(1) the normal pressure tube sealing prepares the NaxFeAs high-temperature superconductor, can be divided into normal pressure direct sintering, normal pressure presoma sintering process.It also can adopt other ordinary method to make, and disclosed concrete grammar step is not intended to limit the scope of the invention among the embodiment.
The normal pressure direct sintering prepares new type high temperature superconductor (NaxFeAs high-temperature superconductor) by changing sodium content normal pressure tube sealing, may further comprise the steps:
With 99.9% or the Na of above purity, Fe and As powder are with mol ratio mixing in the glove box that is filled with Ar gas, grinding, the compressing tablet of x:1:1, the alumina crucible of packing into, be encapsulated in then and be filled with in argon gas or the vitreosil pipe, slowly be warmed up to 800-1100 ℃, be incubated 10-24 hour, preferably repeat sintering twice, obtain monophasic NaxFeAs compound.
Normal pressure-sintered method can also prepare the NaxFeAs high-temperature superconductor by presoma method normal pressure tube sealing, and concrete steps comprise:
1) under normal pressure, preparation FeAs or Na3As precursor samples;
2) with presoma FeAs and Na by 1:x(0＜x＜2) mol ratio weighing in the glove box that is filled with Ar gas, mixed grinding, compressing tablet, the alumina crucible of packing into, be encapsulated in then and be filled with in argon gas or the vitreosil pipe, slowly be warmed up to 800-1100 ℃, insulation is more than 5 hours, the preferred sintering twice that repeats obtains monophasic NaxFeAs compound.
Wherein, the preferred 900-1050 of temperature ℃, further preferred 950-1000 ℃.
(2) under the uht conditions of 0-20GPa, obtain the cubic phase NaxFeAs superconductor crystal that a kind of structure is caved in by the NaxFeAs superconductor crystal of normal pressure synthesis:
Utilize the original position high pressure synchrotron radiation angle x-ray diffraction experiment technology of loosing, adopt diamond anvil (DAC) high-tension unit to carry out the original position High-Voltage Experimentation.The diamond anvil mesa diameter is 500 μ m, and the high pressure packing adopts T301 Stainless Steel sheet.Transmission medium is a silicone oil.Pressing the mark material is ruby, determines pressure by ruby fluorescence peak.The pressure range of experiment is 0-20GPa.The wavelength of used incident X ray is 0.368 in the experiment, effective 2
θAngular region is 0-25
oReach about 3GPa at pressure, the new cubic phase NaxFeAs superconductor crystal that caves in that causes by the electronic structure phase transformation occurs.Compare with the NaxFeAs superconductor crystal structure of normal pressure synthesis, present bigger compression along c direction of principal axis [FeAs4] tetrahedron, trend towards [FeAs4] positive tetrahedron of rule, the As-Fe-As bond angle reaches 109.4
o
Embodiment 1: utilize normal pressure direct sintering method to synthesize the NaxFeAs high temperature superconductor crystal.
With 99.9% or the Na of above purity, Fe and As powder are with x:1:1(x=0.8) mol ratio mixing in the glove box that is filled with Ar gas, grinding, compressing tablet, the alumina crucible of packing into, be encapsulated in then and be filled with in argon gas or the vitreosil pipe, slowly be warmed up to 800 ℃, be incubated 40 hours, preferably repeat sintering twice, obtain monophasic NaxFeAs compound.
Embodiment 2: utilize normal pressure direct sintering method to synthesize the NaxFeAs high temperature superconductor crystal.
With 99.9% or the Na of above purity, Fe and As powder are with x:1:1(x=1.1) mol ratio mixing in the glove box that is filled with Ar gas, grinding, compressing tablet, the alumina crucible of packing into, be encapsulated in then and be filled with in argon gas or the vitreosil pipe, slowly be warmed up to 900 ℃, be incubated 24 hours, preferably repeat sintering twice, obtain monophasic NaxFeAs compound.
Embodiment 3: utilize normal pressure direct sintering method to synthesize the NaxFeAs high temperature superconductor crystal.
With 99.9% or the Na of above purity, Fe and As powder are with x:1:1(x=1.6) mol ratio mixing in the glove box that is filled with Ar gas, grinding, compressing tablet, the alumina crucible of packing into, be encapsulated in then and be filled with in argon gas or the vitreosil pipe, slowly be warmed up to 1000 ℃, be incubated 20 hours, preferably repeat sintering twice, obtain monophasic NaxFeAs compound.
Embodiment 4: utilize normal pressure presoma method to synthesize the NaxFeAs high temperature superconductor crystal.
The preparation of FeAs precursor samples:
Adopt solid phase reaction method under the normal pressure, with 99.9% or the Fe of above purity and As powder with mol ratio mixing in being filled with the glove box of argon gas, grinding, the compressing tablet of 1:1, be sealed in the vitreosil pipe sintering under 1000 ℃ condition then, be incubated 48 hours, obtain monophasic FeAs compound.
The preparation of NaxFeAs high temperature superconductor crystal:
With presoma FeAs and Na by 1:x(x=0.8) mol ratio weighing in the glove box that is filled with Ar gas, mixed grinding, compressing tablet, the alumina crucible of packing into, be encapsulated in then and be filled with in argon gas or the vitreosil pipe, slowly be warmed up to 850 ℃, be incubated 60 hours, the preferred sintering twice that repeats obtains monophasic NaxFeAs compound.
Embodiment 5: utilize normal pressure presoma method to synthesize the NaxFeAs high temperature superconductor crystal.
The preparation of FeAs precursor samples is identical with implementing 4;
The preparation of NaxFeAs high temperature superconductor crystal:
With presoma FeAs and Na by 1:x(x=1.2) mol ratio weighing in the glove box that is filled with Ar gas, mixed grinding, compressing tablet, the alumina crucible of packing into, be encapsulated in then and be filled with in argon gas or the vitreosil pipe, slowly be warmed up to 900 ℃, be incubated 24 hours, the preferred sintering twice that repeats obtains monophasic NaxFeAs compound.
Embodiment 6: utilize normal pressure presoma method to synthesize the NaxFeAs high temperature superconductor crystal.
The preparation of FeAs precursor samples is identical with implementing 4;
The preparation of NaxFeAs high temperature superconductor crystal:
With presoma FeAs and Na by 1:x(x=1.4) mol ratio weighing in the glove box that is filled with Ar gas, mixed grinding, compressing tablet, the alumina crucible of packing into, be encapsulated in then and be filled with in argon gas or the vitreosil pipe, slowly be warmed up to 950 ℃, be incubated 15 hours, the preferred sintering twice that repeats obtains monophasic NaxFeAs compound.
Embodiment 7: ultra-high voltage prepares the cubic phase NaxFeAs superconductor crystal that structure is caved in down.
With the direct synthetic NaxFeAs of normal pressure (x=0.8) high temperature superconductor crystal, utilize the original position high pressure synchrotron radiation angle x-ray diffraction experiment technology of loosing, adopt diamond anvil (DAC) high-tension unit to carry out the original position High-Voltage Experimentation.Diamond anvil mesa diameter 500 μ m, high pressure packing adopt T301 Stainless Steel sheet.Transmission medium is a silicone oil.Pressing the mark material is ruby, determines pressure by ruby fluorescence peak.The pressure range of experiment is 0-20GPa.The wavelength of used incident X ray is 0.368 in the experiment, effective 2
θAngular region is 0-25
oReach about 2.5GPa at pressure, the new cubic phase NaxFeAs superconductor crystal that caves in that causes by the electronic structure phase transformation occurs.
Embodiment 8: ultra-high voltage prepares the cubic phase NaxFeAs superconductor crystal that structure is caved in down.
With the direct synthetic NaxFeAs of normal pressure (x=1.4) high temperature superconductor crystal, utilize the original position high pressure synchrotron radiation angle x-ray diffraction experiment technology of loosing, adopt diamond anvil (DAC) high-tension unit to carry out the original position High-Voltage Experimentation.Diamond anvil mesa diameter 500 μ m, high pressure packing adopt T301 Stainless Steel sheet.Transmission medium is a silicone oil.Pressing the mark material is ruby, determines pressure by ruby fluorescence peak.The pressure range of experiment is 0-20GPa.The wavelength of used incident X ray is 0.368 in the experiment, effective 2
θAngular region is 0-25
oReach about 3.0 GPa at pressure, the new cubic phase NaxFeAs superconductor crystal that caves in that causes by the electronic structure phase transformation occurs.
Embodiment 9: ultra-high voltage prepares the cubic phase NaxFeAs superconductor crystal that structure is caved in down.
With normal pressure precursor method synthetic NaxFeAs (x=1.2) high temperature superconductor crystal, utilize the original position high pressure synchrotron radiation angle x-ray diffraction experiment technology of loosing, adopt diamond anvil (DAC) high-tension unit to carry out the original position High-Voltage Experimentation.Diamond anvil mesa diameter 500 μ m, high pressure packing adopt T301 Stainless Steel sheet.Transmission medium is a silicone oil.Pressing the mark material is ruby, determines pressure by ruby fluorescence peak.The pressure range of experiment is 0-20GPa.The wavelength of used incident X ray is 0.368 in the experiment, effective 2
θAngular region is 0-25
oReach 3.5GPa at pressure, the new cubic phase NaxFeAs superconductor crystal that caves in that causes by the electronic structure phase transformation occurs.
Embodiment 10: ultra-high voltage prepares the cubic phase NaxFeAs superconductor crystal that structure is caved in down.
With normal pressure precursor method synthetic NaxFeAs (x=1.6) high temperature superconductor crystal, utilize the original position high pressure synchrotron radiation angle x-ray diffraction experiment technology of loosing, adopt diamond anvil (DAC) high-tension unit to carry out the original position High-Voltage Experimentation.Diamond anvil mesa diameter 500 μ m, high pressure packing adopt T301 Stainless Steel sheet.Transmission medium is a silicone oil.Pressing the mark material is ruby, determines pressure by ruby fluorescence peak.The pressure range of experiment is 0-20GPa.The wavelength of used incident X ray is 0.368 in the experiment, effective 2
θAngular region is 0-25
oReach 2-5GPa at pressure, the new cubic phase NaxFeAs superconductor crystal that caves in that causes by the electronic structure phase transformation occurs.
Claims (10)
1. an iron arsenic compound high temperature superconductor crystal is characterized in that, this crystal is cubic phase NaxFeAs superconductor crystal, and its spacer is P4/nmm, and lattice parameter is a=3.0-4.0, c=6.0-7.1.
2. iron arsenic compound high temperature superconductor crystal as claimed in claim 1 is characterized in that, among the described NaxFeAs, and 0＜x＜2.
3. iron arsenic compound high temperature superconductor crystal as claimed in claim 1, it is characterized in that, described NaxFeAs superconductor crystal presents bigger compression along c direction of principal axis [FeAs4] tetrahedron, trends towards [FeAs4] positive tetrahedron of rule, and the As-Fe-As bond angle reaches 109.4
oThe pressure phase transition of new cubic phase NaxFeAs superconductor crystal is 2-6GPa.
4. the preparation method of the described iron arsenic compound high temperature superconductor crystal of claim 1, it is characterized in that, this method is specially: the cubic phase NaxFeAs superconductor crystal that utilizes normal pressure synthesis is as precursor, precursor under the pressure of 0-20GPa, is carried out high pressure and obtains the cubic phase NaxFeAs superconductor crystal that structure is caved in.
5. preparation method as claimed in claim 4, it is characterized in that, described precursor adopts the normal pressure direct sintering to make, and its concrete steps are: with 99.9% or the Na of above purity, Fe and As powder are with mol ratio mixing in the glove box that is filled with Ar gas, grinding, the compressing tablet of x:1:1, the alumina crucible of packing into, be encapsulated in then and be filled with in argon gas or the vitreosil pipe, slowly be warmed up to 800-1100 ℃, be incubated 10-24 hour, the preferred sintering twice that repeats obtains monophasic NaxFeAs compound.
6. preparation method as claimed in claim 4 is characterized in that, described precursor adopts normal pressure presoma sintering process to make, and its concrete steps are:
1) under normal pressure, preparation FeAs or Na3As precursor samples;
2) presoma FeAs and Na are pressed 1:x, the weighing in the glove box that is filled with Ar gas of the mol ratio of 0＜x＜2, mixed grinding, compressing tablet, the alumina crucible of packing into, be encapsulated in then and be filled with in argon gas or the vitreosil pipe, slowly be warmed up to 800-1100 ℃, insulation preferably repeated sintering twice more than 5 hours, obtained monophasic NaxFeAs compound.
7. preparation method as claimed in claim 6 is characterized in that, described temperature is 900-1050 ℃, more preferably 950-1000 ℃.
8. preparation method as claimed in claim 4, it is characterized in that, described precursor adopts the original position High-Voltage Experimentation to obtain the cubic phase NaxFeAs superconductor crystal that structure is caved in, it utilizes the original position high pressure synchrotron radiation angle x-ray diffraction experiment technology of loosing, and adopts the diamond anvil high-tension unit to carry out the original position High-Voltage Experimentation.
9. preparation method as claimed in claim 8 is characterized in that, the diamond anvil mesa diameter of described diamond anvil high-tension unit is 500 μ m, the high pressure packing adopts T301 Stainless Steel sheet, transmission medium is a silicone oil, and pressing the mark material is ruby, determines pressure by ruby fluorescence peak.
10. preparation method as claimed in claim 8 is characterized in that, the wavelength of used incident X ray is 0.368 in the described experiment, effective 2
θAngular region is 0-25
o
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104764761A (en) * | 2015-04-23 | 2015-07-08 | 中国工程物理研究院材料研究所 | Method for measuring phase transition of substance under high static pressure |
| CN105651578B (en) * | 2016-04-01 | 2018-04-13 | 扬州大学 | A kind of preparation method of synchrotron radiation X-ray Absorption Fine Structure test sample |
| CN113113184A (en) * | 2021-03-29 | 2021-07-13 | 深圳先进技术研究院 | Carbon-based superconducting material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101407340A (en) * | 2008-11-11 | 2009-04-15 | 中国科学院物理研究所 | Iron arsenic compound high temperature superconductor crystal and preparation thereof |
| CN101608340A (en) * | 2009-01-21 | 2009-12-23 | 中国科学院物理研究所 | A kind of iron-based high-temperature superconductive crystal and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101407340A (en) * | 2008-11-11 | 2009-04-15 | 中国科学院物理研究所 | Iron arsenic compound high temperature superconductor crystal and preparation thereof |
| CN101608340A (en) * | 2009-01-21 | 2009-12-23 | 中国科学院物理研究所 | A kind of iron-based high-temperature superconductive crystal and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 《Journal of the American Chemical Society》 20110429 Qingqing Liu等 Pressure-Induced Isostructural Phase Transition and Correlation of FeAs Coordination with the Superconducting Properties of 111-Type Na1-xFeAs 7892-7896 第133卷, * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104764761A (en) * | 2015-04-23 | 2015-07-08 | 中国工程物理研究院材料研究所 | Method for measuring phase transition of substance under high static pressure |
| CN104764761B (en) * | 2015-04-23 | 2017-05-10 | 中国工程物理研究院材料研究所 | Method for measuring phase transition of substance under high static pressure |
| CN105651578B (en) * | 2016-04-01 | 2018-04-13 | 扬州大学 | A kind of preparation method of synchrotron radiation X-ray Absorption Fine Structure test sample |
| CN113113184A (en) * | 2021-03-29 | 2021-07-13 | 深圳先进技术研究院 | Carbon-based superconducting material and preparation method thereof |
| CN113113184B (en) * | 2021-03-29 | 2023-04-18 | 深圳先进技术研究院 | Carbon-based superconducting material and preparation method thereof |
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Application publication date: 20110921 |