CN113371686A - Novel quasi-two-dimensional selenium-doped tellurium-containing superconducting material and preparation method thereof - Google Patents
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/002—Compounds containing, besides selenium or tellurium, more than one other element, with -O- and -OH not being considered as anions
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
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Abstract
The invention relates to a novel quasi-two-dimensional selenium-doped tellurium-containing superconducting material and a preparation method thereof, belonging to the technical field of functional material manufacturing. The chemical general formula of the novel quasi-two-dimensional selenium-doped tellurium-containing superconducting material is CuIr2Te4‑xSex(x is more than or equal to 0.0 and less than or equal to 0.5). The invention uses the traditional high-temperature solid phase method, high-purity Cu, Ir, Te and Se powder (the purity is more than or equal to 99.9%) with corresponding stoichiometric ratio is fully ground and then placed in a quartz tube, then the quartz tube is vacuumized and sealed, the sealed quartz tube filled with raw materials is placed in a furnace and sintered for 120h at 850 ℃ to obtain CuIr2Te4‑xSex(x is more than or equal to 0.0 and less than or equal to 0.5) is added. Fully grinding the polycrystalline powder, tabletting, putting the flaky sample into a vacuum-sealed quartz tube, and sintering at 850 ℃ for 240h to obtain a sheetForm CuIr2Te4‑xSex(x is more than or equal to 0.0 and less than or equal to 0.5) sample. And finally determining that the target product has superconductivity by measuring the low-temperature performance of physical properties such as conductivity, magnetic property, specific heat capacity and the like of the sample by using a comprehensive physical property testing system (PPMS).
Description
Technical Field
The invention belongs to the technical field of functional material manufacturing, and particularly relates to a series of CuIr with a chemical general formula2Te4-xSex(x is more than or equal to 0.0 and less than or equal to 0.5) and a preparation method thereof.
Background
The superconducting material is a special material which has the property of a superconductor at a critical temperature, and the material in a superconducting state not only has the ideal characteristic of zero resistance, but also has the unique properties of complete diamagnetism and magnetic flux quantization. The characteristics enable the application prospect of the superconducting material to be very wide, and the superconducting material can be widely and heterosceptically applied to the fields of energy transmission, long-distance traffic transportation, special equipment, high-energy physics and the like.
In 1908, Onens successfully liquefied helium, and a low-temperature environment of 1.5K was obtained by a liquid helium throttling expansion technology, and a superconducting phenomenon of mercury was found for the first time after 3 years, so that the superconductor formally entered the visual field of scientists. Since the discovery of superconductors in 1911, scientific interest has been attracted by virtue of their unique zero-resistance effect and perfect diamagnetism. The interest in the superconducting field in the school has not been reduced, and scientists are paving the way for superconducting materials from laboratories to practical applications from the search for systems with higher superconducting critical temperatures to the study of the mechanism of superconducting phenomena. The superconductor has nearly ideal electromagnetic performance, so that the superconductor has extremely attractive application prospect in the energy fields of power generation, power transmission, energy storage and the like, and has the potential of a novel high-performance device.
In 1986, the Chinese scientist Zhao Zhi Xian academy finds the YBCO system, and by virtue of the fact that the temperature of the YBCO system is higher than the superconducting transition temperature of a liquid nitrogen temperature zone (77K), a copper-based superconducting material becomes a first high-temperature superconducting material, attracts the attention of the academic world to a great extent, and pushes the research on the superconducting material to a high tide. Until 2008, copper-based superconducting materials were the mainstream materials in the field of superconducting materials, and scientists urgently wanted to find out a new superconducting microscopic action mechanism from the superconducting materials which can not be predicted and described by the conventional BCS theory, but the mechanism is largeAll without work. In the ongoing research on copper-based superconducting materials, scientists have also found copper oxides as ceramic materials whose high brittleness makes them difficult to process. This property greatly limits the application of copper-based superconducting materials in the industry, and compels scientists to shift their eyes to find new high-temperature superconducting systems. Subsequently, japanese scientist h.hosono discovered LaFeAs1-xFxThe critical temperature of the system is up to about 55K through doping or introducing defects and the like, and the limit of McMilan predicted by BCS theory is exceeded, which proves that another high-temperature superconducting system worthy of being researched is discovered. In addition, due to the layered material structure, the higher upper critical field and the lower electron carrier concentration of the iron-based superconductor material, various superconducting properties are very similar to those of a copper-based high-temperature superconductor. Then the LaFeAsO is found by the Tanpheng research group of the university of Tennessee of America1-xFxThe antiferromagnetic ordered state in the sample shows that the carrier doping effect of the antiferromagnetic matrix in the sample is the reason that the iron-based material generates the superconducting phenomenon, and further proves that the copper-based high-temperature superconducting material and the iron-based high-temperature superconducting material possibly have the same physical action mechanism. Although iron-based superconductors have extremely high research potential, the field of iron-based high-temperature superconductors has not yet formed a systematic and complete theoretical system to date.
Two-dimensional layered Transition Metal Sulfides (TMDs) have been long paid attention to by researchers in the fields of energy, sensing, environment, electronics, and the like, because of their unique physical properties such as tunable band gap. Among them, charge density waves and superconductivity are two important collective quantum phenomena as condensed substances, and have been important research subjects of condensed physics. The 1T and 2H structure type compounds are widely concerned at present, the 2H type transition metal sulfur compound generally has the property of simultaneously appearing charge density wave and superconductivity, and the 1T type transition metal sulfur compound can only observe the charge density wave. In 2006, Cava research group at university of Princeton, USA found that 1T-TiSe can be inhibited by introducing Cu intercalation2The formation temperature of the medium charge density wave enables the superconducting transition temperature of the system to be greatly improved. This means thatThe formation of charge density wave can be inhibited by means of doping, introducing defects and the like, and the purposeful regulation and control of the superconductivity of the material are realized. However, the transition metal sulfide superconducting material is not perfect at present, a specific mechanism of a competitive relationship between a formation mechanism of a charge density wave and superconductivity does not form a system theory, and the superconducting temperature of the system is generally low. Therefore, the development of novel transition metal sulfide superconductors still has important scientific significance and potential application value.
Disclosure of Invention
Aiming at the defects of the existing materials, the invention aims to provide a method for doping Se into CuIr2Te4In the layered compound, a series of novel Se-doped telluride superconductors are obtained by substituting Te and the preparation method thereof is simple, low in preparation cost and high in safety.
In order to achieve the purpose, the invention adopts the following technical scheme:
a novel quasi-two-dimensional selenium-doped tellurium-containing superconducting material has the following characteristic chemical formula:
CuIr2Te4-xSex(0.0≤x≤0.5)
the novel Se-doped telluride superconducting material and the preparation method thereof are characterized by comprising the following processes and steps:
(1) weighing corresponding high-purity Cu, Ir, Te and Se powder (the purity is more than or equal to 99.9%) according to the stoichiometric ratio, fully grinding the raw material powder to uniformly mix the raw material powder, transferring the ground powder into a quartz tube, and pumping the quartz tube under a vacuum system until the vacuum degree is 1 multiplied by 10-5Torr, sealing the tube by acetylene flame;
(2) placing the sealed quartz tube in a box furnace at 850 ℃, heating to 850 ℃ at the speed of 1 ℃/min, calcining for 120h, cooling to room temperature along with the furnace, opening the quartz tube, and fully grinding the obtained powder again;
(3) tabletting the powder obtained in the step (2) to obtain a flaky sample, putting the flaky sample into a quartz tube, and vacuumizing the quartz tube again to 1 x 10-5Torr, and sealing the quartz tube by acetylene flame under continuous vacuum-pumping;
(4) placing the sealed quartz tube in a box furnace again, heating to 850 ℃ at the speed of 1 ℃/min, calcining for 240h, cooling to room temperature along with the furnace, and opening the quartz tube to obtain the sheet CuIr2Te4-xSex(x is more than or equal to 0.0 and less than or equal to 0.5) sample.
(5) After the components of the sample are determined by using a powder X-ray diffraction method (PXRD), the structure model function of Fullprof software is used for fitting to obtain specific parameters such as the crystal structure of each component;
(6) the samples were finally tested by the integrated physical testing system (PPMS): and obtaining low-temperature performance of physical properties such as conductivity, magnetism, specific heat capacity and the like, and finally determining the superconductivity of the sample.
Compared with the prior art, the invention has the following beneficial effects:
(1) the first example of the invention is to dope a tellurium-containing layered structure superconductor with Se to obtain novel CuIr2Te4-xSex(x is more than or equal to 0 and less than or equal to 0.5), thereby playing an important guiding role in disclosing the influence rule of the change of the crystal structure, the phase change structure and the electronic energy band structure of the material on the superconductivity and other physical properties and the competitive mechanism of the superconductivity and the instability of charge density waves;
(2) the Se-doped telluride superconducting material is easy to prepare, has low requirement on equipment and is suitable for large-scale popularization;
(3) the polycrystalline material prepared by the preparation method disclosed by the invention is uniform in property, stable in property in air and convenient to store;
(4) the optimal doped superconducting CuIr prepared by the preparation method of the invention2Te3.9Se0.1Superconducting transition temperature T ofc2.83K, the superconducting transition temperature is improved by doping.
Drawings
FIG. 1 shows a series of CuIr prepared by the method of the present invention2Te4-xSex(x is more than or equal to 0.0 and less than or equal to 0.5) XRD pattern and CuIr2Te3.9Se0.1Polycrystalline material X-ray powder diffraction pattern fitted using fullpref software;
FIG. 2 is a graph of a polymer prepared by the method of the present inventionA series of CuIr2Te4-xSex(x is more than or equal to 0.0 and less than or equal to 0.5) a conductivity and magnetic susceptibility curve chart of the polycrystalline material;
FIG. 3 is a series of (a) CuIr prepared according to the method of the present invention2Te3.9Se0.1Specific heat capacity of polycrystalline material, (b) CuIr2Te3.9Se0.1Lower critical magnetic field intensity curve of polycrystalline material, (c) CuIr2Te3.9Se0.1And (d) CuIr2Te3.8Se0.2Upper critical magnetic field strength profile of polycrystalline material;
FIG. 4 shows a series of CuIr prepared by the method of the present invention2Te4-xSex(0.0. ltoreq. x. ltoreq.0.5) T of samplecAnd TCDWElectron phase diagram as a function of doping concentration.
Fig. 5 is a comparison of superconductivity of the multiple telluride superconducting materials.
Detailed Description
The invention will be further elucidated by means of the following figures and examples, without the scope of protection of the invention being limited to the ones shown.
Example 1:
accurately weighing 0.0066g Cu, 0.0398g Ir, 0.0528g Te and 0.0008g Se raw materials, fully grinding, placing in a quartz tube, and pumping the quartz tube filled with the fully ground raw materials to a vacuum degree of 1 × 10-5Torr and sealing the tube by acetylene flame; then, placing the sealed quartz tube in a box furnace at 850 ℃ for calcining for 120h, then opening the quartz tube, fully grinding the obtained powder, and tabletting; the pressed sheet was again placed in a quartz tube, which was evacuated to a vacuum of 1X 10- 5Torr and sealing the tube by acetylene flame; then placing the sealed quartz tube in a box furnace at 850 ℃ again for calcining for 240 hours to obtain CuIr2Te3.9Se0.1A sample; then determining the purity of the sample by X-ray powder diffraction (PXRD); the resulting polycrystalline sample material will finally be tested for physical properties by a physical testing system (PPMS): mainly comprises conductivity, magnetic properties, heat capacity and the like, and finally determines that the target product has superconductivity.
Example 2:
accurately weighing 0.0066g Cu, 0.0400g Ir, 0.0518g Te and 0.0016g Se raw materials, fully grinding, placing in a quartz tube, pumping the quartz tube filled with the fully ground raw materials to a vacuum degree of 1 × 10-5Torr and sealing the tube by acetylene flame; then, placing the sealed quartz tube in a box furnace at 850 ℃ for calcining for 120h, then opening the quartz tube, fully grinding the obtained powder, and tabletting; the pressed sheet was again placed in a quartz tube, which was evacuated to a vacuum of 1X 10- 5Torr and sealing the tube by acetylene flame; then placing the sealed quartz tube in a box furnace at 850 ℃ again for calcining for 240 hours to obtain CuIr2Te3.8Se0.2A sample; then determining the purity of the sample by X-ray powder diffraction (PXRD); the resulting polycrystalline sample material will finally be tested for physical properties by a physical testing system (PPMS): mainly comprises conductivity, magnetic properties, heat capacity and the like, and finally determines that the target product has superconductivity.
Example 3:
accurately weighing 0.0068g Cu, 0.0412g Ir, 0.0452g Te and 0.0068g Se raw materials, fully grinding, placing in a quartz tube, pumping the quartz tube filled with the fully ground raw materials to a vacuum degree of 1 × 10-5Torr and sealing the tube by acetylene flame; then, placing the sealed quartz tube in a box furnace at 850 ℃ for calcining for 120h, then opening the quartz tube, fully grinding the obtained powder, and tabletting; the pressed sheet was again placed in a quartz tube, which was evacuated to a vacuum of 1X 10- 5Torr and sealing the tube by acetylene flame; then placing the sealed quartz tube in a box furnace at 850 ℃ again for calcining for 240 hours to obtain CuIr2Te3.5Se0.5A sample; then determining the purity of the sample by X-ray powder diffraction (PXRD); the resulting polycrystalline sample material will finally be tested for physical properties by a physical testing system (PPMS): mainly comprises conductivity, magnetic properties, heat capacity and the like, and finally determines that the target product has superconductivity.
Evaluation experiment:
CuIr prepared by the preparation method2Te3.9Se0.1Superconducting transition temperature T of samplecIt was 2.83K. The series of CuIr of the invention2Te4-xSex(x is more than or equal to 0.0 and less than or equal to 0.5) is the Se-doped tellurium-containing layered structure superconductor which is reported for the first time. The powder fitting proves that the material has uniform phase and stable quality in air.
Claims (5)
1. The series of novel Se-doped telluride-containing superconducting materials have the following characteristic chemical formula:
CuIr2Te4-xSex(0.0≤x≤0.5)。
2. the novel Se-doped telluride-containing superconducting material and the preparation method thereof are characterized by comprising the following processes and steps:
(1) weighing corresponding high-purity Cu, Ir, Te and Se powder (the purity is more than or equal to 99.9%) according to the stoichiometric ratio, fully grinding the raw material powder to uniformly mix the raw material powder, transferring the ground powder into a quartz tube, and pumping the quartz tube under a vacuum system until the vacuum degree is 1 multiplied by 10-5Torr, sealing the tube by acetylene flame;
(2) placing the sealed quartz tube in a box furnace at 850 ℃, heating to 850 ℃ at the speed of 1 ℃/min, calcining for 120h, cooling to room temperature along with the furnace, opening the quartz tube, and fully grinding the obtained powder again;
(3) tabletting the powder obtained in the step (2) to obtain a flaky sample, putting the flaky sample into a quartz tube, and vacuumizing the quartz tube again to 1 x 10-5Torr, and sealing the quartz tube by acetylene flame under continuous vacuum-pumping;
(4) placing the sealed quartz tube in a box furnace again, heating to 850 ℃ at the speed of 1 ℃/min, calcining for 240h, cooling to room temperature along with the furnace, and opening the quartz tube to obtain the sheet CuIr2Te4-xSex(x is more than or equal to 0.0 and less than or equal to 0.5) sample.
(5) After the components of the sample are determined by using a powder X-ray diffraction method (PXRD), the structure model function of Fullprof software is used for fitting to obtain specific parameters such as the crystal structure of each component;
(6) the samples were finally tested by the integrated physical testing system (PPMS): and obtaining low-temperature performance of physical properties such as conductivity, magnetism, heat capacity and the like, and finally determining the superconductivity of the sample.
3. The 850 ℃ calcination procedure of claim 2- (2): the heating rate is 1 ℃/min, the temperature is preserved for 7200min at 850 ℃, and the furnace is cooled after the temperature preservation is finished.
4. The 850 ℃ calcination procedure of claim 2- (4): the temperature rising speed is 1 ℃/min, the temperature is kept for 14400min at 850 ℃, and the furnace cooling is carried out after the temperature keeping is finished.
5. The novel Se-doped telluride superconducting material prepared by the method according to the claims 1-2 is found to add a new member to a novel disulfide superconducting family, provides an ideal material platform for revealing the competitive relationship between charge density wave phase transition and superconductivity, and is expected to be stripped to further construct a photoelectric thin film device, a miniature detector and the like.
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| CN109797430A (en) * | 2018-12-28 | 2019-05-24 | 中山大学 | A kind of novel codope chalcogen superconductor and preparation method thereof |
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| 沈少喜;曹世勋;陈腊;袁淑娟;康保娟;张金仓;: "Fe_(1.01)Se_(0.4)Te_(0.6)单晶的超导电性研究", 低温物理学报 * |
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