CN115893316A - High pressure preparation of ternary La 0.75+x Ce 0.25-x H 10 Method for high temperature superconductors - Google Patents
High pressure preparation of ternary La 0.75+x Ce 0.25-x H 10 Method for high temperature superconductors Download PDFInfo
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- CN115893316A CN115893316A CN202310020193.6A CN202310020193A CN115893316A CN 115893316 A CN115893316 A CN 115893316A CN 202310020193 A CN202310020193 A CN 202310020193A CN 115893316 A CN115893316 A CN 115893316A
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- 239000002887 superconductor Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 26
- 239000000956 alloy Substances 0.000 claims abstract description 26
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 20
- 239000010432 diamond Substances 0.000 claims abstract description 20
- 230000007704 transition Effects 0.000 claims abstract description 14
- 238000011065 in-situ storage Methods 0.000 claims abstract description 10
- 238000004093 laser heating Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 9
- 150000004678 hydrides Chemical class 0.000 claims abstract description 8
- JBANFLSTOJPTFW-UHFFFAOYSA-N azane;boron Chemical compound [B].N JBANFLSTOJPTFW-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 6
- 229910020785 La—Ce Inorganic materials 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 10
- 229910052684 Cerium Inorganic materials 0.000 claims description 5
- 238000001069 Raman spectroscopy Methods 0.000 claims description 5
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 5
- 229910002056 binary alloy Inorganic materials 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- 229910000636 Ce alloy Inorganic materials 0.000 abstract description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 1
- 238000005259 measurement Methods 0.000 description 13
- 150000001875 compounds Chemical class 0.000 description 9
- 230000001276 controlling effect Effects 0.000 description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000001000 micrograph Methods 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 230000005469 synchrotron radiation Effects 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000002216 synchrotron radiation X-ray diffraction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E40/00—Technologies for an efficient electrical power generation, transmission or distribution
- Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment
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- Inorganic Compounds Of Heavy Metals (AREA)
- Superconductors And Manufacturing Methods Therefor (AREA)
Abstract
High pressure preparation of ternary La of the invention 0.75+x Ce 0.25‑x H 10 A method for preparing a high-temperature superconductor belongs to the technical field of preparation of superconducting materials, and comprises the steps of taking metal lanthanum, metal cerium alloy and ammonia borane as raw materials, utilizing a diamond anvil cell device, and adopting high-pressure in-situ laser heating to synthesize La-Ce-H ternary superconducting hydride; the superconducting hydride prepared by the invention has lower synthetic pressure intensity and stable interval, higher superconducting transition temperature and upper critical magnetic field; the superconducting property of the sample can be regulated and controlled within a certain range by selecting initial alloys with different element ratios. The superconductor prepared by the method has the potential of becoming a candidate material of a superconducting micro-nano device.
Description
Technical Field
The invention belongs to the technical field of preparation of superconducting materials, and particularly relates to a method for preparing ternary high-temperature superconducting hydride.
Background
The superconductor is a special material with zero resistance and complete diamagnetism, and has wide application prospect in the fields of energy, traffic, medical treatment, electric power, quantum computation and the like. The achievement of the superconducting state requires a cryogenic environment at a temperature below the superconducting transition temperature. Therefore, it is the researchers to raise the superconducting transition temperature of the materialThe aim is constantly being pursued. Hydrogen-rich compounds are potentially high temperature superconductors due to the minimal atomic mass of hydrogen and the relatively high debye temperature. In recent years, hydrogen-rich compound superconductors have attracted much attention and achieved a series of innovative results. For example: the British journal of Nature (2015, 525, 73-76) reports: under 155 ten thousand atmospheric pressure, H is successfully synthesized by experiments 3 S high-temperature superconductor, the superconducting transition temperature of which can reach 203K. Another type of binary hydride, laH, was reported again in 2019, nature,2019,569,528-531 10 . The superconducting transition temperature can reach 250K under 170 ten thousand atmospheric pressure. If the ternary hydrogen-rich compound with adjustable components is prepared, the pressure required by superconducting transformation of the material is effectively reduced. The synthesis pressure of the ternary hydrogen-rich compounds reported so far is still higher than 150GPa. Therefore, designing and preparing the H with adjustable components at lower pressure 10 The high-temperature superconductor containing the ternary hydrogen-rich compound greatly promotes the application prospect of the superconducting material.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the problems and the defects existing in the background technology and provides a simple method for preparing the ternary hydrogen-rich compound La 0.75+x Ce 0.25-x H 10 By controlling the element proportion of the initial La-Ce alloy, the La is regulated and controlled 0.75+x Ce 0.25-x H 10 Superconducting transition temperature and stable pressure.
The method takes metal lanthanum, metal cerium and ammonia borane as initial reactants, utilizes a diamond anvil cell device, and adopts high-pressure in-situ laser heating to synthesize La 0.75+x Ce 0.25-x H 10 A ternary superconducting hydride. The specific technical scheme is as follows:
high-pressure preparation of ternary La 0.75+x Ce 0.25-x H 10 The method of the high-temperature superconductor firstly utilizes multi-target magnetron sputtering to synthesize La-Ce binary alloy, and the atomic ratio of La to Ce is (0.75 + x): (0.25-x), x is more than or equal to 0 and less than or equal to 0.03. Then taking a small piece of La-Ce alloy with the diameter of 20-30 microns in a glove box protected by inert gas, and mixing with ammonia boraneLoading the sample into a diamond anvil cell pressing cavity, calibrating pressure by using the variation relation of a diamond Raman peak along with the pressure, pressurizing the sample to 110-132GPa, finally uniformly carrying out high-pressure in-situ laser heating on the sample by using a 1070nm infrared laser, controlling the heating time of each part within 3 seconds, and controlling the heating temperature to be 1000-1500K to finally obtain La 0.75+x Ce 0.25-x H 10 A high temperature superconductor.
In the preparation process, la-Ce alloys with different proportions can be selected as initial reactants, and the La/Ce atomic ratio is preferably 3:1.
in the preparation process of the invention, the ternary hydride (La) with different La/Ce ratios 0.75 Ce 0.25 H 10 、La 0.77 Ce 0.23 H 10 、La 0.78 Ce 0.22 H 10 ) The initial superconducting transition temperatures obtained were 175K (113 GPa), 190K (123 GPa) and 188K (132 GPa), respectively. The high-temperature superconductivity of the superconducting material can be kept to lower pressure, namely 95GPa (155K), 101GPa (167K) and 107GPa (172K). For La 0.75 Ce 0.25 H 10 The upper critical magnetic field is 235T at 100 GPa.
Has the beneficial effects that:
la prepared by the invention 0.75+x Ce 0.25-x H 10 The advantages of high temperature superconductors are: the synthesis and stable pressure is low; the superconducting transition temperature and the upper critical magnetic field are higher; the superconducting property of the sample can be regulated and controlled within a certain range by selecting the initial alloys with different proportions. The superconductor prepared by the method has the potential of becoming a candidate material of a superconducting micro-nano device.
Drawings
FIG. 1 is a flow chart of diamond anvil preparation and sample loading for electrical measurements.
FIG. 2 is La prepared in example 1 0.75 Ce 0.25 Scanning electron micrographs of the alloy.
FIG. 3 is La prepared in example 1 0.75 Ce 0.25 Energy spectrum of the alloy.
FIG. 4 is La in diamond anvil cell prepared in example 1 0.75 Ce 0.25 H 10 Sample and four electrode micrographs.
FIG. 5 is La prepared in example 1 0.75 Ce 0.25 H 10 And (5) refining the result of the synchrotron radiation XRD of the sample.
FIG. 6 is La prepared in example 1 0.75 Ce 0.25 H 10 The resistance-temperature curve of the sample is obtained by the super conductivity measurement under different pressures.
FIG. 7 is La prepared in example 1 0.75 Ce 0.25 H 10 The resulting upper critical field was fitted to the sample at 100 GPa.
FIG. 8 is La prepared by example 2 0.77 Ce 0.23 Scanning electron micrographs of the alloy.
FIG. 9 is La prepared in example 2 0.77 Ce 0.23 Energy spectrum of the alloy.
FIG. 10 is La in diamond anvil cell prepared in example 2 0.77 Ce 0.23 H 10 Sample and four electrode micrographs.
FIG. 11 is La prepared in example 2 0.77 Ce 0.23 H 10 The resistance-temperature curve of the sample is obtained by the super conductivity measurement under different pressures.
FIG. 12 is La prepared in example 3 0.78 Ce 0.22 Scanning electron micrographs of the alloys.
FIG. 13 is La prepared in example 3 0.78 Ce 0.22 Energy spectrum of the alloy.
FIG. 14 is La in diamond anvil cell prepared in example 3 0.78 Ce 0.22 H 10 Sample and four electrode micrographs.
FIG. 15 is La prepared in example 3 0.78 Ce 0.22 H 10 The resistance-temperature curve of the sample is obtained by the super conductivity measurement under different pressures.
Detailed Description
The invention will now be described in more detail with reference to the following examples, in which the reagents are, unless otherwise specified, commercially available products and are used without further purification.
Example 1 hydration at 113GPaInto high-temperature superconducting La 0.75 Ce 0.25 H 10 Compound (I)
Firstly, synthesizing La-Ce binary alloy by utilizing multi-target magnetron sputtering, wherein the atomic ratio of La to Ce is 3: FIG. 2 is a scanning electron micrograph of the La-Ce alloy prepared in example 1, showing that the deposited La-Ce alloy is in the form of clusters with a cluster size of less than 1 μm. Fig. 3 is a spectrum of the La-Ce alloy prepared in example 1, showing that the atomic percentages of La and Ce are 75% and 25%, respectively. A small piece of La-Ce alloy with a diameter of 20 μm was then taken in an inert gas-protected glove box and loaded into a diamond anvil cell together with ammonia borane, and the initial sample was packaged and prepared for electrical measurements according to the procedure shown in fig. 1. Calibrating the pressure by using the change relation of the diamond Raman peak along with the pressure, pressurizing the sample to 113GPa, finally uniformly carrying out high-pressure in-situ laser heating on the sample by using a 1070nm infrared laser, controlling the heating time of each part within 3 seconds, and controlling the heating temperature to be 1500K to finally obtain La 0.75 Ce 0.25 H 10 A high temperature superconductor. The properties of the product were characterized by low temperature electrical measurements during pressure relief and synchrotron XRD diffraction. FIG. 4 is La in diamond anvil cell prepared in example 1 0.75 Ce 0.25 H 10 And (4) micrographs of the sample and the four electrodes show that the surface appearance of the initial sample is changed after the initial sample is subjected to high-pressure in-situ laser heating. FIG. 5 is La prepared in example 1 0.75 Ce 0.25 H 10 The result of the synchrotron radiation XRD fine modification of the sample shows that the structure of the superconducting phase is P6 3 And/mmc. Meanwhile, the hydrogen content can be estimated as H according to the volume of the unit cell 10 . FIG. 6 is La prepared in example 1 0.75 Ce 0.25 H 10 The resistance-temperature curve of the sample obtained by the super-conductivity measurement under different pressures shows that La 0.75 Ce 0.25 H 10 The sample has a high superconducting transition temperature between the pressure after synthesis and the pressure before decomposition. At a minimum stable pressure of 95GPa, the superconducting transition temperature is 155K. FIG. 7 is La prepared in example 1 0.75 Ce 0.25 H 10 Fitting the sample at 100GPa to obtain an upper critical magnetic field, and fitting by a WHH formula to show that the upper critical magnetic field reachesTo 235T.
Example 2 Synthesis of high temperature superconducting La at 123GPa 0.77 Ce 0.23 H 10 Compound (I)
Firstly, preparing La-Ce alloy by utilizing multi-target magnetron sputtering, wherein the atomic ratio of La to Ce is 0.77:0.23. FIG. 8 is a scanning electron micrograph of the La-Ce alloy of example 2, showing that its surface is relatively flat and the cluster size is less than 1 μm. FIG. 9 is a spectrum of the La-Ce alloy of example 2 showing that the atomic percentages of La and Ce in the alloy are 77% and 23%, respectively. A small piece of La-Ce alloy with a diameter of 20 μm was then taken in an inert gas-protected glove box and loaded into a diamond anvil cell together with ammonia borane, and the initial sample was packaged and prepared for electrical measurements according to the procedure shown in fig. 1. Calibrating the pressure by using the change relation of the diamond Raman peak along with the pressure, pressurizing the sample to 123GPa, finally uniformly carrying out high-pressure in-situ laser heating on the sample by using a 1070nm infrared laser, controlling the heating time of each part within 3 seconds, and controlling the heating temperature to be 1500K to finally obtain La 0.77 Ce 0.23 H 10 A high temperature superconductor. The superconducting properties of the product were characterized by low temperature electrical measurements during pressure relief. FIG. 10 is La in diamond anvil cell prepared in example 2 0.77 Ce 0.23 H 10 And the micrographs of the sample and the four electrodes show that the surface appearance of the initial sample is changed after the initial sample is subjected to high-pressure in-situ laser heating, so that a target product is generated. FIG. 11 is La prepared in example 2 0.77 Ce 0.23 H 10 The resistance-temperature curve of the sample is obtained by the super conductivity measurement under different pressures. Shows La 0.77 Ce 0.23 H 10 The sample has a high superconducting transition temperature between the pressure after synthesis and the pressure before decomposition. Comparative example 1 shows that the minimum stable pressure increases with increasing La content, being 101GPa.
Example 3 Synthesis of high temperature superconducting La at 132GPa 0.78 Ce 0.22 H 10 Compound (I)
Firstly, preparing La-Ce alloy by utilizing multi-target magnetron sputtering, wherein the atomic ratio of La to Ce is 0.78:0.22. FIG. 12 is a scanning electron microscope of the alloy of example 3And a mirror image shows that the surface is relatively flat, and the cluster size is less than 1 micron. Fig. 13 is a spectrum of the alloy of example 3, showing that the atomic percentages of La and Ce in the alloy are 78% and 22%, respectively. A small piece of La-Ce alloy with a diameter of 20 μm was then taken in an inert gas-protected glove box and loaded into a diamond anvil cell together with ammonia borane, and the initial sample was packaged and prepared for electrical measurements according to the procedure shown in fig. 1. Calibrating the pressure by using the variation relation of the diamond Raman peak along with the pressure, pressurizing the sample to 132GPa, finally uniformly carrying out high-pressure in-situ laser heating on the sample by using a 1070nm infrared laser, controlling the heating time of each part within 3 seconds, and controlling the heating temperature to be 1500K to finally obtain La 0.78 Ce 0.22 H 10 A high temperature superconductor. The superconducting properties of the product were characterized by low temperature electrical measurements during pressure relief. FIG. 14 is La in diamond anvil cell prepared in example 3 0.78 Ce 0.22 H 10 And micrographs of the sample and the four electrodes show that the surface appearance of the initial sample is changed after the initial sample is heated by high-pressure in-situ laser, and a target product is generated. FIG. 15 is La prepared by example 3 0.78 Ce 0.22 H 10 The resistance-temperature curves of the sample obtained by the superconductivity measurement under different pressures show that the minimum stable pressure of the ternary hydride is further increased with the further increase of the La content, and the minimum stable pressure is 107GPa. At the same time, the transition around the 50K temperature indicates that the sample contains a small amount of other superconducting phases. Comparative examples 1, 2 and 3 show that the molar ratio of La/Ce in the case of an atomic ratio of 3:1, ternary La 0.75+x Ce 0.25-x H 10 High temperature superconductors have the lowest stable pressure.
Claims (3)
1. High-pressure preparation of ternary La 0.75+x Ce 0.25-x H 10 The method of the high-temperature superconductor firstly utilizes multi-target magnetron sputtering to synthesize La-Ce binary alloy, and the atomic ratio of La to Ce is (0.75 + x): (0.25-x), x is more than or equal to 0 and less than or equal to 0.03; then taking a small piece of La-Ce alloy with the diameter of 20-30 microns in a glove box protected by inert gas, loading the La-Ce alloy and ammonia borane into a diamond anvil cell chamber, and closing the diamond anvil cell by utilizing the change of a diamond Raman peak along with the pressureCalibrating pressure, pressurizing a sample to 110-132GPa, uniformly carrying out high-pressure in-situ laser heating on the sample by using a 1070nm infrared laser, controlling the heating time of each part within 3 seconds, and heating at 1000-1500K to finally obtain La 0.75+x Ce 0.25-x H 10 A high temperature superconductor.
2. High pressure preparation of ternary La according to claim 1 0.75+x Ce 0.25-x H 10 A method for producing a high temperature superconductor, characterized in that the atomic ratio of La and Ce is 3:1.
3. high pressure preparation of ternary La according to claim 1 0.75+x Ce 0.25-x H 10 Method for high-temperature superconductors, characterized in that for ternary hydrides of different La/Ce ratios La 0.75 Ce 0.25 H 10 、La 0.77 Ce 0.23 H 10 、La 0.78 Ce 0.22 H 10 Pressurizing to 113GPa, 123GPa and 132GPa respectively in the anvil pressing cavity to obtain initial superconducting transition temperatures of 175K, 190K and 188K respectively; the superconducting transition temperatures of the superconducting material which can retain the high-temperature superconductivity to the lowest pressure and the lowest pressure are 95GPa/155K, 101GPa/167K and 107GPa/172K respectively.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101747041A (en) * | 2008-11-27 | 2010-06-23 | 中国科学院物理研究所 | Single-phase iron-based superconducting material based on fluoride and preparation method thereof |
| JP2022082013A (en) * | 2020-11-20 | 2022-06-01 | 国立研究開発法人物質・材料研究機構 | Cerium 12 boride and method for producing the same |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101747041A (en) * | 2008-11-27 | 2010-06-23 | 中国科学院物理研究所 | Single-phase iron-based superconducting material based on fluoride and preparation method thereof |
| JP2022082013A (en) * | 2020-11-20 | 2022-06-01 | 国立研究開発法人物質・材料研究機構 | Cerium 12 boride and method for producing the same |
Non-Patent Citations (1)
| Title |
|---|
| WUHAO CHEN ET AL: ""Enhancement of the superconducting critical temperature realized in the La–Ce–H system at moderate pressures"", 《ARXIV》, 12 April 2022 (2022-04-12), pages 1 - 30 * |
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