CN109182981B - Preparation method of strontium cobaltate film material - Google Patents
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- CN109182981B CN109182981B CN201811368751.3A CN201811368751A CN109182981B CN 109182981 B CN109182981 B CN 109182981B CN 201811368751 A CN201811368751 A CN 201811368751A CN 109182981 B CN109182981 B CN 109182981B
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Abstract
The invention discloses a preparation method of a strontium cobaltate film material, which is used for researching the magnetic and electrical properties of the strontium cobaltate film material. Firstly, preparing a strontium cobaltate powder sample by adopting a ball milling method, then drying the powder sample and preparing a blocky target material, and finally depositing the blocky target material on a substrate by adopting a pulse laser deposition method and annealing to obtain the strontium cobaltate film material. The strontium cobaltate powder prepared by the ball milling method is uniform in mixing and high in particle size uniformity, and the ball milling method has the characteristics of simplicity in operation, mild conditions, easiness in control and the like; the strontium cobaltate film deposited by the pulse laser deposition method has the characteristics of good quality, high uniformity, stable material components and the like, and meanwhile, the strontium cobaltate film prepared on the substrate with the similar lattice constant and the perovskite structure is more stable in structure, and the metal-semiconductor conversion process of the strontium cobaltate film is observed on a strontium cobaltate film sample.
Description
Technical Field
The invention belongs to the technical field of film materials, and particularly relates to a preparation method of a strontium cobaltate film material.
Background
Magnetic materials are an old and very versatile material. In the process of continuous development and progress of modern electronic information technology, various components made of magnetic materials are indispensable. Since the 50 s of the last century, perovskite-type ABO was started3The properties of oxides in terms of structural features, electromagnetic properties, and the like have been studied. Because cobalt has multiple oxidation states (Co)2+,Co3+,Co4+) Therefore, the strontium cobaltate has special electromagnetic performance. Meanwhile, because of the particularity of the film material, new performances which some bulk materials do not have can be derived. Because of good electronic and oxygen ion conductivity and good electrochemical activity, the material is used as an excellent functional material and applied to synthesis of oxygen-permeable ceramic membranes, solid electrodes, solid oxidation batteries, electrocatalysis reactors and the like. At present, relatively few research reports on strontium cobaltate at home and abroad exist, and the preparation of the strontium cobaltate film and the research on the magnetic and electrical properties of the strontium cobaltate film are more rarely reported, so that the development and application of the special properties of the material are limited.
Disclosure of Invention
The invention aims to overcome the defects of the existing research and provides a preparation method of a strontium cobaltate film material.
The technical scheme adopted by the invention is as follows:
a preparation method of strontium cobaltate thin film material comprises the following steps:
step 1: preparing strontium cobaltate powder by adopting a ball milling method;
step 2: calcining strontium cobaltate powder at high temperature to prepare a strontium cobaltate block target material;
and step 3: and depositing the blocky target material on the perovskite structure single crystal substrate by using a pulse laser deposition method to obtain the strontium cobaltate thin film material.
The materials used in the step 1 of preparing the strontium cobaltate powder by using the ball milling method comprise a cobalt source material and a strontium source material, wherein the cobalt source material and the strontium source material are cobaltosic oxide and strontium carbonate respectively.
Further, the step 1: the method comprises the following specific steps:
1-1: mixing cobaltosic oxide and strontium carbonate according to SrCoO3Accurately weighing the mass ratio of the medium-cation substances, adding a proper amount of absolute ethyl alcohol, and fully grinding by using an agate mortar to obtain powder A;
the amount of the absolute ethyl alcohol is determined according to the dryness degree of the powder A;
1-2: pouring the powder A into a ball milling tank, and placing the ball milling tank into a ball mill with 7-8 revolutions per minute for ball milling for 24-28 hours to obtain powder B;
1-3: and (3) placing the powder B in a porcelain crucible, placing the porcelain crucible in a muffle furnace at 850-950 ℃ for 6-6.5 hours, and removing organic matters to obtain dry black strontium cobaltate powder.
Further, in the step 2, strontium cobaltate powder is calcined at a high temperature to prepare a strontium cobaltate block target material, which specifically comprises the following steps:
2-1: grinding the dried black strontium cobaltate powder into granular-feeling-free powder C;
2-2: placing the powder C in a corundum boat, and calcining the powder C in a tubular furnace at the high temperature of 1100-1200 ℃ for 10-11 hours to obtain black strontium cobaltate powder D;
2-3: pressing the strontium cobaltate powder D into a cylindrical target material with the diameter of 30-35mm by using a metal die, wherein the pressure is 20-22 MPa;
2-4: and (3) annealing the cylindrical target material in a muffle furnace at 650-680 ℃ for 6-6.5 hours to obtain the strontium cobaltate bulk target material.
Further, in the step 3, the bulk target material is deposited on the perovskite structure single crystal substrate by using a pulsed laser deposition method to obtain the strontium cobaltate thin film material, which specifically comprises the following steps:
3-1: respectively placing the strontium cobaltate blocky target material and the perovskite structure single crystal substrate at corresponding positions in a vacuum chamber of a pulse laser deposition system, closing the vacuum chamber, and successively starting a mechanical pump and a molecular pump to vacuumize the vacuum chamber;
3-2: when the vacuum degree of the vacuum chamber reaches 10-4When Pa, the molecular pump is closed, the oxygen valve is opened, and the oxygen pressure of the vacuum chamber is adjusted to 14-14.5 Pa;
3-3: setting the temperature of the substrate at 650-700 ℃, and covering the perovskite structure single crystal substrate by using a baffle plate;
3-4: setting the voltage of a pulse laser to be 19-20kV and the frequency to be 1-1.2Hz, and pre-striking;
3-5: and removing the baffle, starting deposition, depositing for 30-40min, carrying out in-situ heat preservation for 15-20min, and cooling to room temperature to obtain the perovskite strontium cobaltate thin film material.
The deposition time of the prepared strontium cobaltate film material is adjusted according to the thickness of the target film, and the adjustment rate is 300-320 nm/h.
Further, the perovskite structure single crystal substrate includes, but is not limited to, SrTiO3Single crystal, LaAlO3And (3) single crystal. The crystal orientation of the perovskite single crystal substrate is (100), (110) and (111).
According to the invention, the strontium cobaltate film material is prepared by adopting the technical scheme, and the comprehensive magnetic and electrical performance test is carried out on the strontium cobaltate film by utilizing the QD comprehensive physical property measurement system and the magnetic measurement system, so that the metal-semiconductor transition phenomenon is found in the temperature change process. The strontium cobaltate powder is prepared by adopting a ball milling method, the prepared strontium cobaltate powder is uniform in mixing ratio and high in particle size uniformity, in addition, the ball milling method has the characteristics of simplicity in operation, mild condition, easiness in control and the like, and finally, a pulse laser deposition method is used for depositing to obtain the strontium cobaltate film. The method of the invention can not only ensure the uniformity of the thickness of the film, but also improve the quality of the film material.
Drawings
The invention is described in further detail below with reference to the following figures and detailed description:
FIG. 1 shows SrCoO on STO (001) substrate3-δA thin film XRD diffraction pattern;
FIG. 2 is SrCoO3-δThe resistivity of the film changes with the temperature under different currents;
FIG. 3 is SrCoO3-δThe resistivity of the film varies with the magnetic field under different temperatures.
Detailed Description
Example 1
A preparation method of strontium cobaltate thin film material comprises the following steps:
step 1: preparing strontium cobaltate powder by adopting a ball milling method, which comprises the following steps of;
1-1: mixing cobaltosic oxide and strontium carbonate according to SrCoO3Accurately weighing the mass ratio of the medium-cation substances, adding a proper amount of absolute ethyl alcohol, and fully grinding by using an agate mortar to obtain powder A;
1-2: pouring the powder A into a ball milling tank, and placing the powder A into a ball mill with 8 revolutions per minute for ball milling for 28 hours to obtain powder B;
1-3: placing the powder B in a porcelain crucible, placing the porcelain crucible in a muffle furnace at 950 ℃ for 6 hours, and removing organic matters to obtain dry black strontium cobaltate powder;
step 2: calcining strontium cobaltate powder at high temperature to prepare a strontium cobaltate block target material, which is as follows;
2-1: grinding the dried black strontium cobaltate powder into granular-feeling-free powder C;
2-2: placing the powder C in a corundum boat, and calcining the powder C in a tubular furnace at the high temperature of 1200 ℃ for 10 hours to obtain black strontium cobaltate powder D;
2-3: pressing the strontium cobaltate powder D into a cylindrical target material with the diameter of 35mm by using a metal die, wherein the pressure is 22 MPa;
2-4: placing the cylindrical target material in a muffle furnace at 680 ℃ for annealing for 6 hours to obtain a strontium cobaltate block target material;
and step 3: depositing the blocky target material on the perovskite structure single crystal substrate by using a pulse laser deposition method to obtain the strontium cobaltate thin film material, which comprises the following specific steps:
3-1: respectively placing the strontium cobaltate blocky target material and the perovskite structure single crystal substrate at corresponding positions in a vacuum chamber of a pulse laser deposition system, closing the vacuum chamber, and successively starting a mechanical pump and a molecular pump to vacuumize the vacuum chamber;
3-2: when the vacuum degree of the vacuum chamber reaches 10-4When Pa, the molecular pump is closed, the oxygen valve is opened, and the oxygen pressure of the vacuum chamber is adjusted to 14.5 Pa;
3-3: setting the temperature of the substrate to 700 ℃, and covering the perovskite structure single crystal substrate by using a baffle;
3-4: setting the voltage of a pulse laser to be 20kV and the frequency to be 1Hz, and performing pre-striking;
3-5: and removing the baffle, starting deposition, depositing for 40min, carrying out in-situ heat preservation for 15min, and cooling to room temperature to obtain the perovskite strontium cobaltate thin film material.
Example 2
A preparation method of strontium cobaltate thin film material comprises the following steps:
step 1: preparing strontium cobaltate powder by adopting a ball milling method, which comprises the following steps of;
1-1: mixing cobaltosic oxide and strontium carbonate according to SrCoO3Accurately weighing the mass ratio of the medium-cation substances, adding a proper amount of absolute ethyl alcohol, and fully grinding by using an agate mortar to obtain powder A;
1-2: pouring the powder A into a ball milling tank, and placing the powder A into a ball mill with 7 revolutions per minute for ball milling for 26 hours to obtain powder B;
1-3: placing the powder B in a porcelain crucible, placing the porcelain crucible in a muffle furnace at 850 ℃ for 6.5 hours, and removing organic matters to obtain dry black strontium cobaltate powder;
step 2: calcining strontium cobaltate powder at high temperature to prepare a strontium cobaltate block target material, which is as follows;
2-1: grinding the dried black strontium cobaltate powder into granular-feeling-free powder C;
2-2: placing the powder C in a corundum boat, and placing the corundum boat in a tubular furnace to be calcined at the high temperature of 1100 ℃ for 10.5 hours to obtain black strontium cobaltate powder D;
2-3: pressing the strontium cobaltate powder D into a cylindrical target material with the diameter of 30mm by using a metal die, wherein the pressure is 20 MPa;
2-4: placing the cylindrical target material in a muffle furnace at 650 ℃ for annealing for 6.5 hours to obtain a strontium cobaltate bulk target material;
and step 3: depositing the blocky target material on the perovskite structure single crystal substrate by using a pulse laser deposition method to obtain the strontium cobaltate thin film material, which comprises the following specific steps:
3-1: respectively placing the strontium cobaltate blocky target material and the perovskite structure single crystal substrate at corresponding positions in a vacuum chamber of a pulse laser deposition system, closing the vacuum chamber, and successively starting a mechanical pump and a molecular pump to vacuumize the vacuum chamber;
3-2: when the vacuum degree of the vacuum chamber reaches 10-4When Pa, the molecular pump is closed, the oxygen valve is opened, and the oxygen pressure of the vacuum chamber is adjusted to 14 Pa;
3-3: setting the temperature of the substrate to 680 ℃, and covering the perovskite structure single crystal substrate by using a baffle;
3-4: setting the voltage of a pulse laser to be 19.5kV and the frequency to be 1.1Hz, and performing pre-striking;
3-5: and removing the baffle, starting deposition, depositing for 35min, carrying out in-situ heat preservation for 20min, and cooling to room temperature to obtain the perovskite strontium cobaltate thin film material.
Example 3
A preparation method of strontium cobaltate thin film material comprises the following steps:
step 1: preparing strontium cobaltate powder by adopting a ball milling method, which comprises the following steps of;
1-1: mixing cobaltosic oxide and strontium carbonate according to SrCoO3Accurately weighing the mass ratio of the medium-cation substances, adding a proper amount of absolute ethyl alcohol, and fully grinding by using an agate mortar to obtain powder A;
1-2: pouring the powder A into a ball milling tank, and placing the powder A into a ball mill with the speed of 7.6 revolutions per minute for ball milling for 24 hours to obtain powder B;
1-3: placing the powder B in a porcelain crucible, placing the porcelain crucible in a muffle furnace at 900 ℃ for 6 hours, and removing organic matters to obtain dry black strontium cobaltate powder;
step 2: calcining strontium cobaltate powder at high temperature to prepare a strontium cobaltate block target material, which is as follows;
2-1: grinding the dried black strontium cobaltate powder into granular-feeling-free powder C;
2-2: placing the powder C in a corundum boat, and placing the corundum boat in a tubular furnace to be calcined at the high temperature of 1150 ℃ for 10 hours to obtain black strontium cobaltate powder D;
2-3: pressing the strontium cobaltate powder D into a cylindrical target material with the diameter of 30mm by using a metal die, wherein the pressure is 20 MPa;
2-4: annealing the cylindrical target material in a muffle furnace at 650 ℃ for 6 hours to obtain a strontium cobaltate block target material;
and step 3: depositing the blocky target material on the perovskite structure single crystal substrate by using a pulse laser deposition method to obtain the strontium cobaltate thin film material, which comprises the following specific steps:
3-1: respectively placing the strontium cobaltate blocky target material and the perovskite structure single crystal substrate at corresponding positions in a vacuum chamber of a pulse laser deposition system, closing the vacuum chamber, and successively starting a mechanical pump and a molecular pump to vacuumize the vacuum chamber;
3-2: when the vacuum degree of the vacuum chamber reaches 10-4When Pa, the molecular pump is closed, the oxygen valve is opened, and the oxygen pressure of the vacuum chamber is adjusted to 14 Pa;
3-3: setting the temperature of the substrate to 650 ℃, and covering the perovskite structure single crystal substrate by using a baffle;
3-4: setting the voltage of a pulse laser to be 19kV and the frequency to be 1Hz, and performing pre-striking;
3-5: and removing the baffle, starting deposition, depositing for 30min, carrying out in-situ heat preservation for 15min, and cooling to room temperature to obtain the perovskite strontium cobaltate thin film material.
FIG. 1 shows SrCoO on STO (001) substrate3-δA thin film XRD diffraction pattern; FIG. 2 is SrCoO3-δThe resistivity of the film changes with the temperature under different currents; FIG. 3 is SrCoO3-δThe resistivity of the film varies with the magnetic field under different temperatures.
As can be seen in FIG. 1, XRD of a SrCoO 3-delta thin film sample showed it to grow epitaxially in the STO (200) direction. This time, a SrCoO 3-delta film was successfully prepared on the STO (100) substrate by a pulsed laser deposition system (PLD).
As can be seen from FIG. 2, the SrCoO 3-delta film undergoes a metallic-semiconductor reversible transformation process at a temperature in the range of 10K to 300K. The prepared SrCoO 3-delta film is shown to have reversible resistivity change with temperature.
As can be seen from FIG. 3, at 149K, the resistivity of the SrCoO 3-delta film increases with the increase of the magnetic field during the increase of the magnetic field from 0T to 9T. At 300K, the resistivity of the magnetic field increases from 0T to 9T, and becomes smaller as the magnetic field increases. The prepared SrCoO 3-delta film is shown to have variable resistivity with temperature under varying magnetic field.
Claims (5)
1. A preparation method of strontium cobaltate film material is characterized by comprising the following steps: which comprises the following steps:
step 1: preparing strontium cobaltate powder by adopting a ball milling method:
1-1: mixing cobaltosic oxide and strontium carbonate according to SrCoO3Accurately weighing the mass ratio of the medium-cation substances, adding absolute ethyl alcohol, and fully grinding to obtain powder A;
1-2: pouring the powder A into a ball milling tank, and placing the ball milling tank into a ball mill with 7-8 revolutions per minute for ball milling for 24-28 hours to obtain powder B;
1-3: placing the powder B in a muffle furnace at 850-950 ℃ for 6-6.5 hours, and removing organic matters to obtain strontium cobaltate powder;
step 2: calcining strontium cobaltate powder at high temperature to prepare a strontium cobaltate block target material:
2-1: grinding strontium cobaltate powder into non-granular powder C;
2-2: calcining the powder C in a tube furnace at the high temperature of 1100-1200 ℃ for 10-11 hours to obtain strontium cobaltate powder D;
2-3: pressing the strontium cobaltate powder D into a cylindrical target material with the diameter of 30-35mm by using a metal die, wherein the pressure is 20-22 MPa;
2-4: placing the cylindrical target material in a muffle furnace at 650-680 ℃ for annealing for 6-6.5 hours to obtain a strontium cobaltate block target material;
and step 3: depositing the blocky target material on the perovskite structure single crystal substrate by using a pulse laser deposition method to obtain a strontium cobaltate thin film material:
3-1: respectively placing the strontium cobaltate blocky target material and the perovskite structure single crystal substrate at corresponding positions in a vacuum chamber of a pulse laser deposition system, closing the vacuum chamber, and successively starting a mechanical pump and a molecular pump to vacuumize the vacuum chamber;
3-2: when the vacuum degree of the vacuum chamber reaches 10-4When Pa, the molecular pump is closed, the oxygen valve is opened, and the oxygen pressure of the vacuum chamber is adjusted to 14-14.5 Pa;
3-3: setting the temperature of the substrate at 650-700 ℃, and covering the perovskite structure single crystal substrate by using a baffle plate;
3-4: setting the voltage of a pulse laser to be 19-20kV and the frequency to be 1-1.2Hz, and pre-striking;
3-5: removing the baffle, starting deposition, depositing for 30-40min, carrying out in-situ heat preservation for 15-20min, and cooling to room temperature to obtain the perovskite strontium cobaltate thin film material;
the prepared strontium cobaltate film material has a metallic-semiconductor reversible transformation process within the temperature range of 10K-300K, the resistivity of the strontium cobaltate film material increases along with the enhancement of a magnetic field in the process of increasing the magnetic field from 0T-9T at 149K, and the resistivity of the strontium cobaltate film material decreases along with the enhancement of the magnetic field in the process of increasing the magnetic field from 0T-9T at 300K.
2. The method for preparing the strontium cobaltate thin film material according to claim 1, wherein the method comprises the following steps: the amount of the absolute ethyl alcohol described in step 1-1 is determined according to the degree of drying of the powder A.
3. The method for preparing the strontium cobaltate thin film material according to claim 1, wherein the method comprises the following steps: the deposition time of the prepared strontium cobaltate film material is adjusted according to the thickness of the target film, and the adjustment rate is 300-320 nm/h.
4. The method for preparing the strontium cobaltate thin film material according to claim 1, wherein the method comprises the following steps: the perovskite structure single crystal substrate includes but is not limited to SrTiO3Single crystal, LaAlO3And (3) single crystal.
5. Strontium cobaltate thin film material obtained by the preparation method according to any one of claims 1 to 4.
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