CN114380340B - Unlimited layer nickel-based superconductor precursor Nd 1-x Sr x NiO 3 Is prepared by the preparation method of (2) - Google Patents

Unlimited layer nickel-based superconductor precursor Nd 1-x Sr x NiO 3 Is prepared by the preparation method of (2) Download PDF

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CN114380340B
CN114380340B CN202111438410.0A CN202111438410A CN114380340B CN 114380340 B CN114380340 B CN 114380340B CN 202111438410 A CN202111438410 A CN 202111438410A CN 114380340 B CN114380340 B CN 114380340B
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金奎娟
杨明卫
杨镇
郭尔佳
葛琛
王灿
何萌
杨国桢
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    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/40—Nickelates
    • C01G53/66—Nickelates containing alkaline earth metals, e.g. SrNiO3, SrNiO2
    • C01G53/68—Nickelates containing alkaline earth metals, e.g. SrNiO3, SrNiO2 containing rare earth, e.g. La1.62 Sr0.38NiO4
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Abstract

The invention provides an infinite layer nickel-based superconductor precursor Nd 1‑x Sr x NiO 3 The preparation method of (2) comprises the following steps: (1) Heating an infinite layer nickel-based superconductor precursor perovskite oxide film prepared by pulse laser deposition and placing the film in an oxygen-enriched environment so as to carry out annealing treatment; (2) Cooling the product annealed in the step (1) to obtain an infinite layer nickel-based superconductor precursor Nd 1‑ x Sr x NiO 3 Wherein x is greater than 0 and less than or equal to 0.33. The method has simple and convenient operation, can improve the stability of the sample property, and ensures the high repeatability of the grown sample.

Description

Unlimited layer nickel-based superconductor precursor Nd 1-x Sr x NiO 3 Is prepared by the preparation method of (2)
Technical Field
The invention belongs to the field of materials. In particular, the present invention relates to an infinite layer nickel-based superconductor precursor Nd 1-x Sr x NiO 3 Is prepared by the preparation method of (1).
Background
Unlimited layer nickel-based superconductor Nd 0.8 Sr 0.2 NiO 2 Reduction of perovskite oxide thin film Nd by hydrogenation 0.8 Sr 0.2 NiO 3 Realizing superconductivity, but growing to obtain the Nd 0.8 Sr 0.2 NiO 3 The precursors are very difficult and often very easy to obtain Ruddlesden-Popper (RP) phase (Nd 0.8 Sr 0.2 ) 2 NiO 4 Even severely segregated NiO forms in the structure. Synthesis of Nd is generally confirmed by judging that the peak position of X-ray diffraction (002) of a pulsed laser deposited film is more than 48 DEG and that a (001) diffraction peak exists 0.8 Sr 0.2 NiO 3 Is a structure of (a). By changing the oxygen atmosphere during growth, or by modifyingVarying the area size of the laser spot, or ensuring the stoichiometry during growth by polishing the polycrystalline target, e.g., lee, k.; goodge, B.H.estimates of the synthesis of thin film superconducting infinite-layers, APL Mater,2020,8, (041107) discloses that Nd is obtained by polishing a polycrystalline target, changing the area of the laser spot 0.8 Sr 0.2 NiO 3 . The prior art means have complex processes, the obtained samples have low repeatability and the quality of the samples is not uniform.
Based on this, there is a need for a new method for obtaining an infinite layer nickel-based superconductor precursor Nd that can greatly reduce the complexity of the operation and improve the stability of the sample properties and ensure high reproducibility of the grown sample 0.8 Sr 0.2 NiO 3 。
Disclosure of Invention
The invention aims to provide an Nd precursor for obtaining an infinite layer nickel-based superconductor, which has simple and convenient operation, can improve the stability of sample properties and ensure high repeatability of a grown sample 0.8 Sr 0.2 NiO 3 Is a method of (2).
The above object of the present invention is achieved by the following means.
The invention provides an infinite layer nickel-based superconductor precursor Nd 1-x Sr x NiO 3 The preparation method of (2) comprises the following steps:
(1) Heating an infinite layer nickel-based superconductor precursor perovskite oxide film prepared by pulse laser deposition and placing the film in an oxygen-enriched environment so as to carry out annealing treatment;
(2) Cooling the product annealed in the step (1) to obtain an infinite layer nickel-based superconductor precursor Nd 1- x Sr x NiO 3 Wherein x is greater than 0 and less than or equal to 0.33.
The inventors of the present application have unexpectedly found that by exposing an infinite layer nickel-based superconductor precursor perovskite oxide film prepared by pulsed laser deposition to a high temperature oxygen-rich environment, an infinite layer nickel-based superconductor precursor Nd can be obtained 1- x Sr x NiO 3 . Without wishing to be bound by theory, this may be due to the high temperature oxygen-rich environment causing oxygen to enter the perovskite oxide film, being able to oxidize the low valence metal element in the film, so that the impurity phase with multivalent states in the film is easily oxidized to higher valence states, thereby facilitating the oxidation relative to (Nd 1-x Sr x ) 2 NiO 4 Nd with high valence state of Ni in phase and NiO 1-x Sr x NiO 3 Is formed and stabilized.
In the specific embodiment of the present invention, the pulsed laser deposition method is not particularly limited, and methods known to those skilled in the art may be employed. In particular embodiments of the present invention, pulsed laser deposition methods employed are well known and commonly used by those skilled in the art, such as Li, D.et al, superconduction Dome in Nd 1- x Sr x NiO 2 Infinite Layer films Phys Rev Lett.2020, 125,027001, which discloses the preparation of Nd using pulsed laser deposition methods 1-x Sr x NiO 3 (0.125<x<0.25 A) a film.
Preferably, in the method of the present invention, the temperature increase in the step (1) is performed under the following conditions:
heating the precursor perovskite oxide film of the infinite layer nickel-based superconductor prepared by pulse laser deposition to 450-550 ℃ and keeping for 5-20 minutes.
Preferably, in the method of the present invention, the temperature increase in the step (1) is performed under the following conditions:
heating the precursor perovskite oxide film of the infinite layer nickel-based superconductor prepared by pulse laser deposition to 500-550 ℃ and keeping for 10-15 minutes.
Preferably, in the method of the present invention, the temperature increase in the step (1) is performed under the following conditions:
the infinite layer nickel-based superconductor precursor perovskite oxide film prepared by pulse laser deposition is heated to 500 ℃ and maintained for 10 minutes.
Preferably, in the method of the present invention, the oxygen pressure of the oxygen-enriched environment is 500-5000Pa.
The inventors of the present application have unexpectedly found that a desired structural phase Nd can be obtained when the oxygen pressure of the oxygen-enriched environment is 500-5000Pa 1-x Sr x NiO 3 . When the oxygen pressure is too low, formation of Ruddlesden-Popper (RP) phase such as 214 and NiO is caused, and a desired structural phase cannot be obtained. When the oxygen pressure is too high, the physical properties of the 113 phase are easily changed, and the phase is deviated from intrinsic full-metallic state, and becomes insulated.
Preferably, in the method of the present invention, the oxygen pressure of the oxygen-enriched environment is 500-1000Pa.
Preferably, in the method of the present invention, the annealing treatment in the step (1) is performed for 30 minutes to 3 hours.
Preferably, in the method of the present invention, the annealing treatment in the step (1) is performed for 1 to 2 hours.
Preferably, in the method of the present invention, the cooling in the step (2) is performed under the following conditions: the cooling rate is 5-20deg.C/min, preferably 10-15deg.C/min.
Preferably, in the method of the present invention, the cooling in the step (2) is performed under the following conditions: the cooling rate is 10-15 ℃/min.
In a specific embodiment of the invention, the positioning of the precursor perovskite oxide film material of the infinite layer nickel-based superconductor in the sample chamber in the high temperature oxygen-rich environment is performed in situ in the sample chamber.
In a specific embodiment of the present invention, the size of the grown sample and the thickness of the sample are not particularly limited, and may be in a range that can be heated uniformly by a heater.
The invention has the following beneficial effects:
the method of the invention adopts an in-situ high-temperature oxygen-enriched method to change the structure of the precursor perovskite oxide film of the infinite layer nickel-based superconductor, so the method of the invention is simple and convenient, clean and pollution-free. Meanwhile, the invention avoids the complicated operations of adjusting the size of light spots, polishing a polycrystalline target material, regulating and controlling oxygen pressure and the like after each pulse laser deposition is finished, and can quantitatively realize the synthesis of the precursor perovskite oxide film material of the infinite layer nickel-based superconductor.
The invention has no special regulation on the size of the sample, can deposit in a range of uniform heating, can produce the sample amount which is 5-10 times of the common operation at one time, and has high repeatability and uniform sample quality.
In the method, the structure of the precursor perovskite oxide film material of the infinite layer nickel-based superconductor can be controlled by adjusting the oxygen pressure, so that the artificial controllable laser method growth operation is realized.
The precursor perovskite oxide Nd of the infinite layer nickel-based superconductor with stable structure, which is obtained by the method of the invention 1- x Sr x NiO 3 Can be used for subsequent hydrogenation reduction reaction to obtain an infinite layer nickel-based superconductor Nd 1-x Sr x NiO 2 Provides a good material foundation for the research of nickel-based superconductors in the field of unconventional superconducting physics and the application of superconducting coils.
Drawings
Embodiments of the present invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 is a schematic diagram of an apparatus for producing a precursor perovskite oxide of an infinite layer nickel-based superconductor at high temperature and oxygen enrichment in accordance with an embodiment of the invention;
FIG. 2 is an X-ray diffraction pattern of a precursor perovskite oxide thin film material of an infinite layer nickel-based superconductor having a structural transition in examples 4-5, 7-8 and comparative examples 1-2 of the present invention;
FIG. 3 is an X-ray diffraction chart of the samples prepared in example 5 and example 6 of the present invention;
FIG. 4 shows Nd at different Sr doping concentrations in examples 9 and 10 of the present invention 0.85 Sr 0.15 NiO 3 ，Nd 0.75 Sr 0.25 NiO 3 An X-ray diffraction pattern of the prepared sample;
wherein, the reference numerals:
1-laser deposition of a sample cavity; 2-a heater; precursor Nd of 3-infinite layer nickel-base superconductor 1-x Sr x NiO 3 The method comprises the steps of carrying out a first treatment on the surface of the 4-oxygen pipeline; 5-oxygen switch.
Detailed Description
The following detailed description of the invention is provided in connection with the accompanying drawings that are presented to illustrate the invention and not to limit the scope thereof.
Example 1
20% strontium doped neodymium nickelate perovskite Nd 0.8 Sr 0.2 NiO 3 Single crystal film pulse laser preparation:
NiO and Nd 2 O 3 SrCO 3 Three raw materials are according to 5:2:1, and weighing and mixing the mixture. Then, a pre-sintering operation at 1250 ℃ is performed to achieve carbon removal. Then sintering the fixed and molded raw material into Nd at high temperature of 1350 DEG C 0.8 Sr 0.2 NiO 3 Is a target material of (a). SrTiO of (001) oriented TiO surface cut-off layer 3 A substrate. The perovskite oxide film material is obtained by adopting a pulse laser deposition method and utilizing pulse laser to bombard the target material and sputtering deposition, wherein the bombarding frequency is 4Hz, and the energy density of the pulse laser bombarding the target material is 1.8J/cm 2 . In SrTiO 3 Intermediate product (i.e., original sample 1) is formed after deposition on the substrate. The deposition conditions are as follows: the deposition temperature was 600℃and the deposition oxygen pressure was 20Pa.
Example 2
15% strontium doped neodymium nickelate perovskite Nd 0.85 Sr 0.15 NiO 3 Single crystal film pulse laser preparation:
NiO and Nd 2 O 3 SrCO 3 Three raw materials are according to 40:17:6 molar ratio, and weighing and mixing. The remaining operating conditions were the same as in example 1, to obtain original sample 2. The prepared original sample 2 is stored in vacuum.
Example 3
25% strontium doped neodymium nickelate perovskite Nd 0.75 Sr 0.25 NiO 3 Single crystal film pulse laser preparation:
NiO and Nd 2 O 3 SrCO 3 Three raw materials are according to 8:3: molar ratio of 2Weighing and mixing are carried out. The remaining operating conditions were the same as in example 1, to obtain original sample 3. The prepared original sample 3 is stored in vacuum.
Example 4
The original sample 1, where the deposition of example 1 was completed, was warmed to 500 ℃. After the temperature is stabilized for 10 minutes, 500Pa of oxygen is introduced through an oxygen pipeline, and after standing is carried out for 1 hour, the temperature is reduced to room temperature at a cooling rate of 10 ℃/min, and a sample 1 is obtained. The prepared sample 1 was then stored in vacuo.
Example 5
Sample 2 was obtained in the same manner as in example 4, except that the original sample 1 obtained by the deposition of example 1 was subjected to an oxygen pressure of 1000Pa. And (5) preserving the prepared sample 2 in vacuum.
Example 6
Sample 2 prepared in example 5 was subjected to a process such as Li, d.f.; lee, K.superconductivity in an index-layer laminate, nature 2019, 572,624 627 reports on the use of CaH 2 The hydrogenation reduction reaction is carried out to obtain a sample 3, namely an infinite layer of nickel-based superconducting material Nd 0.8 Sr 0.2 NiO 2 . And (5) preserving the prepared sample 3 in vacuum.
Comparative example 1
Sample 4 was obtained in the same manner as in example 4, except that the original sample 1 obtained by the deposition of example 1 was subjected to an oxygen pressure of 20Pa. And (5) preserving the prepared sample 4 in vacuum.
Comparative example 2
Sample 5 was obtained in the same manner as in example 4, except that the original sample 1 obtained by the deposition of example 1 was subjected to an oxygen pressure of 100 Pa. The prepared sample 5 was stored in vacuum.
Example 7
Sample 6 was obtained in the same manner as in example 4, except that the original sample 1 obtained by the deposition of example 1 was subjected to an oxygen pressure of 3000 Pa. The prepared sample 6 was stored in vacuum.
Example 8
Sample 7 was obtained in the same manner as in example 4, except that the original sample 1 obtained by the deposition of example 1 was subjected to an oxygen pressure of 5000Pa. The prepared sample 7 was stored in vacuum.
Example 9
Sample 8 was obtained in the same manner as in example 4, except that the original sample 2, on which the deposition of example 2 was completed, was subjected to an oxygen pressure of 1000Pa. The prepared sample 8 was stored in vacuum.
Example 10
Sample 9 was obtained in the same manner as in example 4, except that the original sample 3 obtained by the deposition of example 3 was subjected to an oxygen pressure of 1000Pa. The prepared sample 9 was stored in vacuum.
Example 11
The macroscopic change of the sample structure can be measured by performing X-ray diffraction characterization operation on the samples 1, 2, 4, 5, 6 and 7 and the original sample 1.
FIG. 2 is an X-ray diffraction pattern of a precursor perovskite oxide thin film material of an infinite layer nickel-based superconductor having a structural transition in examples 4-5, 7-8 and comparative examples 1-2 of the present invention. The sample that had not been subjected to the high temperature oxygen evolution operation after pulse deposition was designated as original sample 1 (i.e., the sample of example 1). The angle of the (002) diffraction peak and the presence or absence of the (001) diffraction peak by contrast X-ray diffraction can be used to determine that the original sample 1, sample 4 and sample 5 are (Nd 0.8 Sr 0.2 ) 2 NiO 4 Phase, sample 1, sample 2, sample 6 and sample 7 were Nd 0.8 Sr 0.2 NiO 3 And (3) phase (C). The 2θ angles of the original sample 1, sample 4, and sample 5 were 47.49 °, 47.52 °, 47.72 °, respectively. Although it is (Nd 0.8 Sr 0.2 ) 2 NiO 4 The phase, however, was seen to increase monotonically with increasing 2 theta angle as the temperature was maintained at 500 ℃, samples 1, 2,6 and 7 were maintained at higher oxygen pressures, distinct (001) diffraction peaks were seen, and the 2 theta angles were 48.24 °, 48.43 °, 48.51 ° and 48.58 °, respectively, with the four samples having infinite layers of nickel-based superconductor precursor Nd 0.8 Sr 0.2 NiO 3 I.e. having a (001) diffraction peak and a (002) diffraction peak with a peak position of more than 48 °. Sample 1, sample 2, sample 6 and sample 7 also have a law that the 2θ angle increases with the increase of the introduced oxygen pressure. It can be derived thatConclusion, the 2 theta angle is not limited to (Nd 0.8 Sr 0.2 ) 2 NiO 4 Whether the phase is Nd 0.8 Sr 0.2 NiO 3 With the structure, along with the rise of the pressure of the heat preservation and oxygen introduction at 500 ℃, the monotonous increase of the 2 theta angle can be seen, and when the oxygen pressure reaches a certain value, (Nd 0.8 Sr 0.2 ) 2 NiO 4 Phase vanishes, nd 0.8 Sr 0.2 NiO 3 The structure appears. Through the high-temperature oxygen-introducing operation, the growth of the precursor perovskite oxide film material of the infinite layer nickel-based superconductor is stably and controllably realized.
Example 12
Sample 2 and sample 3 were subjected to an X-ray diffraction characterization operation. Macroscopic changes in the structure of the sample can be measured. FIG. 3 perovskite oxide Nd as precursor for infinite layer nickel-based superconductors in example 5 and example 6 of the present invention 0.8 Sr 0.2 NiO 3 Unlimited layer nickel-based superconductor Nd 0.8 Sr 0.2 NiO 2 Is an X-ray diffraction pattern of (2). Sample 3 is a precursor perovskite oxide thin film material Nd of an infinite layer nickel-based superconductor grown in the same manner as sample 2 0.8 Sr 0.2 NiO 3 Infinite layer nickel-base superconductor Nd obtained by hydrogenation reduction reaction 0.8 Sr 0.2 NiO 2 And (3) a sample. It can be seen that Nd 0.8 Sr 0.2 NiO 2 (001) and (002) peak positions relative to the precursor perovskite oxide film material Nd of the infinite layer nickel-based superconductor 0.8 Sr 0.2 NiO 3 All shift to high angle, and quantitatively see that the 2 theta angle of the diffraction peak position (002) is from Nd 0.8 Sr 0.2 NiO 3 48.43 DEG of (2) is shifted to Nd 0.8 Sr 0.2 NiO 2 54.47 deg.. In addition to the shift of peak position, an infinite layer of nickel-based superconductor Nd can be seen 0.8 Sr 0.2 NiO 2 (001) and (002) peak intensities relative to the precursor perovskite oxide Nd of an infinite layer nickel-based superconductor 0.8 Sr 0.2 NiO 3 The weakening is evident. This can be seen as the peak oxygen from Nd 0.8 Sr 0.2 NiO 3 Is removed to obtain the C-axis lattice constant relative to Nd 0.8 Sr 0.2 NiO 3 The angle 2 theta is shifted to a high angle. This is in conjunction with Li, d.f.; nd reported by Lee, K.superconductivity in an index-layer nickel, nature 2019, 572,624-627 0.8 Sr 0.2 NiO 2 (001) and (002) peak positions relative to the precursor perovskite oxide Nd of the infinite layer nickel-based superconductor 0.8 Sr 0.2 NiO 3 The phenomenon of high angle deviation is consistent. Indicating that the precursor perovskite oxide film material Nd of the infinite layer nickel-based superconductor obtained by growth of the invention 0.8 Sr 0.2 NiO 3 Can be subjected to hydrogenation reduction reaction to obtain Nd 0.8 Sr 0.2 NiO 2 。
Example 13
Sample 8 and sample 9 were subjected to an X-ray diffraction characterization procedure. FIG. 4 shows perovskite oxide Nd as a precursor for infinite layer nickel-based superconductors in examples 9 and 10 of the present invention 0.85 Sr 0.15 NiO 3 And Nd 0.75 Sr 0.25 NiO 3 Is an X-ray diffraction pattern of (2). From the two characteristics of (001) diffraction peak and (002) diffraction peak with peak position greater than 48 deg. judging that we have obtained the precursor perovskite oxide 113 phase of infinite layer nickel-base superconductor, it can be seen that the high temperature oxygen-introducing operation is performed in other proportion Nd 1- x Sr x NiO 3 The perovskite oxide thin film material 113 phase may also be obtained, demonstrating the versatility of this approach.

Claims (7)

1. Infinite layer nickel-based superconductor precursor Nd 1-x Sr x NiO 3 The preparation method of (2) comprises the following steps:
(1) Heating an infinite layer nickel-based superconductor precursor perovskite oxide film prepared by pulse laser deposition and placing the film in an oxygen-enriched environment so as to carry out annealing treatment;
(2) Cooling the product annealed in the step (1) to obtain an infinite layer nickel-based superconductor precursor Nd 1- x Sr x NiO 3 Wherein x is greater than 0 and less than or equal to 0.33;
the temperature rise in the step (1) is performed under the following conditions:
heating the infinite layer nickel-based superconductor precursor perovskite oxide film prepared by pulse laser deposition to 450-550 ℃ and keeping for 5-20 minutes;
the oxygen pressure of the oxygen-enriched environment is 500-5000Pa;
the annealing treatment in the step (1) is performed for 30 minutes to 3 hours.
2. The method of claim 1, wherein the heating in step (1) is performed under the following conditions:
heating the precursor perovskite oxide film of the infinite layer nickel-based superconductor prepared by pulse laser deposition to 500-550 ℃ and keeping for 10-15 minutes.
3. The method of claim 2, wherein the heating in step (1) is performed under the following conditions:
the infinite layer nickel-based superconductor precursor perovskite oxide film prepared by pulse laser deposition is heated to 500 ℃ and maintained for 10 minutes.
4. The method of claim 1, wherein the oxygen-enriched environment has an oxygen pressure of 500-1000Pa.
5. The method of claim 1, wherein the annealing treatment in step (1) is performed for 1 to 2 hours.
6. The method of claim 1, wherein the cooling in step (2) is performed under the following conditions: the cooling rate is 5-20 ℃/min.
7. The method of claim 6, wherein the cooling in step (2) is performed under the following conditions: the cooling rate is 10-15 ℃/min.
CN202111438410.0A 2021-11-30 2021-11-30 Unlimited layer nickel-based superconductor precursor Nd 1-x Sr x NiO 3 Is prepared by the preparation method of (2) Active CN114380340B (en)

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