CN112537799A - Method for regulating oxygen vacancy sequence phase of perovskite phase cobalt oxide material - Google Patents
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Abstract
A method for controlling the oxygen vacancy phase of a perovskite phase cobalt oxide material comprises applying to a perovskite phase cobalt oxide in the form of a thin film of ACoO3Applying an electric field or applying an electric field and a stress field such that the perovskite phase cobalt oxide thin film is formed from the original perovskite phase ACoO3Conversion to oxygen vacancy ordered phase ACoO2.5(ii) a Wherein A is selected from one or more of La, Sr and Ca. By applying electric field and stress field to the perovskite phase cobalt oxide thin film at the same time, a transverse oxygen vacancy phase parallel to the substrate is generated in the perovskite phase cobalt oxide thin film. By applying only an electric field but not a stress field to the perovskite-phase cobalt oxide thin film, a longitudinal oxygen vacancy sequence phase perpendicular to the substrate is generated in the perovskite-phase cobalt oxide thin film, and meanwhile, a small amount of transverse oxygen vacancy sequence phases exist on two sides of the longitudinal oxygen vacancy sequence phase. The oxygen vacancy phase obtained by the method has a wide application prospect in the fields of solid oxide fuel cells, catalysts, oxygen separation membranes, gas sensors and the like.
Description
Technical Field
The invention relates to the field of materials. In particular, the invention relates to a method for regulating the oxygen vacancy sequence phase of a perovskite phase cobalt oxide material.
Background
With the development of the times and the progress of science and technology, material science plays an increasingly important role, and the regulation, control and development of materials with excellent performance are always the targets pursued by the majority of scientific researchers. Among them, perovskite-type transition metal oxide materials have attracted much attention in the fields of catalysis, gas sensors, oxygen separation membranes, solid oxide fuel cell electrode materials, and the like, because of their high oxygen ion transfer activity. The migration and transmission of oxygen ions also become the core process of the perovskite transition metal oxide work.
In the perovskite transition metal oxide, the efficiency of oxygen ion migration and transmission processes directly determines the working efficiency of catalysis, gas sensors, oxygen separation membranes and solid oxide fuel cell electrode materials. The migration and transport process of oxygen ions is an important issue of close attention, and is greatly related to the oxygen vacancy phase formed in the material. At present, in perovskite cobalt oxide, a thin film can be mainly irradiated by high-energy electron beams to generate oxygen vacancy sequences (electron beams are accelerated to 0.5MeV by an electron accelerator and then bombard the surface of a sample), or the size of lattice mismatch between a substrate and the thin film is adjusted by substrates with different lattice constants, so that the adjustment of oxygen vacancy sequence phases in the thin film is realized, but the methods are relatively complex and have higher cost, so that a new means and a method for manufacturing and controlling the oxygen vacancy sequence phases are urgently required to be explored.
In the invention, oxygen ions in the perovskite type cobalt oxide can be migrated by utilizing an electric field to form an oxygen vacancy sequence phase with a one-dimensional oxygen vacancy channel, and simultaneously, the direction of the oxygen vacancy channel in the oxygen vacancy sequence phase can be regulated and controlled by combining a stress field. The method for inducing oxygen ion migration in the perovskite type cobalt oxide to form the phase with the specific oxygen vacancy sequence by utilizing the complex interaction of the electric field and the stress field has the advantages of simple operation and low cost, and has important practical significance for the fields of catalysis, gas sensors and the like.
Disclosure of Invention
The invention aims to provide a method for regulating and controlling an oxygen vacancy sequence phase of a perovskite phase cobalt oxide material. The method provided by the invention can regulate and control the direction of the oxygen vacancy sequence phase in the material.
The purpose of the invention is realized by the following technical scheme.
A method for regulating and controlling an oxygen vacancy sequence phase of a perovskite phase cobalt oxide material comprises the following steps: for perovskite phase cobalt oxide ACoO in the form of a thin film3Applying an electric field or applying an electric field and a stress field such that the perovskite phase cobalt oxide thin film is formed from the original perovskite phase ACoO3Conversion to oxygen vacancy ordered phase ACoO2.5(ii) a Wherein A is selected from one or more of La, Sr and Ca.
Preferably, in the method of the present invention, the voltage of the electric field is 1-5V, and the current is 1X 10-7-2×10- 6A. More preferably, in the method of the present invention, the voltage of the electric field is 2-3V and the current is 1X 10-7-6×10-7A。
Preferably, in the method of the present invention, the pressure of the stress field is 3-5 Gpa.
Preferably, in the method of the present invention, the applying of the electric field is performed by a method comprising the steps of:
(1) preparing a perovskite phase cobalt oxide thin film grown on a substrate into a transmission electron microscope cross-section sample, and mounting the sample on one end of a sample rod of a transmission electron microscope;
(2) fixing a metal tungsten needle tip on the other end of the sample rod, and enabling the metal tungsten needle tip to be just contacted with the perovskite phase cobalt oxide film without stress; and then applying an electric field to the sample through an external power supply device connected with the sample rod, wherein the metal tungsten needle point is connected with the anode, and the substrate is grounded.
Preferably, in the method of the present invention, the applying the electric field and the stress field is performed by a method comprising the steps of:
(1) preparing a perovskite phase cobalt oxide thin film grown on a substrate into a transmission electron microscope cross-section sample, and mounting the sample on one end of a sample rod of a transmission electron microscope;
(2) fixing a metal tungsten needle point on the other end of the sample rod, and driving the metal tungsten needle point through piezoelectric ceramics so as to apply a stress field to the sample; and then applying an electric field to the sample through an external power supply device connected with the sample rod, wherein the metal tungsten needle point is connected with the anode, and the substrate is grounded.
Preferably, in the method of the present invention, the metal tungsten tip is pretreated by electrochemical corrosion.
Preferably, in the method of the present invention, the step (1) of preparing the transmission electron microscope cross-section sample is performed by a method including the following steps:
adhering the perovskite phase cobalt oxide film grown on the substrate to a silicon wafer, heating and curing, and cutting into pieces with the thickness of 5 mm; and grinding the silicon wafer to the thickness of 2-3 microns, fixing the silicon wafer on a molybdenum ring, moving the silicon wafer upwards to an ion thinning instrument for thinning.
Preferably, in the method of the present invention, the cross-sectional thickness of the TEM cross-sectional sample is 30-70 nm.
Preferably, in the method of the present invention, the substrate is made of Nb-doped SrTiO3Forming; wherein the mass fraction of Nb is 0.5-1% based on the total mass of the substrate.
The principle of the invention is as follows: in the perovskite-phase cobalt oxide thin film, oxygen ions have a certain activity, and therefore, are likely to migrate by an external driving force, thereby forming an oxygen-deficient phase having an oxygen vacancy phase. The electric field can reduce the migration barrier of oxygen ions, and the oxygen ions in the perovskite phase cobalt oxide film are induced to migrate as a strong driving force to form an oxygen defect phase with an oxygen vacancy sequence phase. On the contrary, the stress field can effectively inhibit the chemical expansion caused by oxygen migration, thereby playing a pinning role on the structure of the perovskite phase cobalt oxide film and inhibiting the perovskite phase cobalt oxide film from forming an oxygen defect phase with an oxygen vacancy sequence phase. Therefore, the direction of the generation of the oxygen vacancy sequence phase in the perovskite phase cobalt oxide film can be effectively regulated and controlled by combining the electric field and the stress field.
The invention has the following beneficial effects:
the method provided by the invention can regulate and control the direction of the oxygen vacancy sequence phase in the material. By applying electric field and stress field to the perovskite phase cobalt oxide thin film at the same time, a transverse oxygen vacancy phase parallel to the substrate is generated in the perovskite phase cobalt oxide thin film. By applying only an electric field but not a stress field to the perovskite-phase cobalt oxide thin film, a longitudinal oxygen vacancy sequence phase perpendicular to the substrate is generated in the perovskite-phase cobalt oxide thin film, and meanwhile, a small amount of transverse oxygen vacancy sequence phases exist on two sides of the longitudinal oxygen vacancy sequence phase. The transverse oxygen vacancy sequence phase and the longitudinal oxygen vacancy sequence correspond to oxygen vacancy channel directions with different orientations, so that the transverse oxygen vacancy sequence phase and the longitudinal oxygen vacancy sequence have important influence on the migration, the transmission efficiency and the direction of oxygen ions.
The oxygen vacancy sequence phase obtained by the method has a wide application prospect in the fields of solid oxide fuel electric fields, catalysts, oxygen separation membranes, gas sensors and the like.
Drawings
Embodiments of the invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1a shows the regulation of LaCoO according to the present invention3A schematic diagram of one embodiment of an apparatus for oxygen vacancy phase experiment in thin films;
FIG. 1b shows the regulation of LaCoO according to the present invention3Low power transmission electron micrographs of one embodiment of an oxygen vacancy ordered phase in the film;
FIG. 2a shows original LaCoO in example 1 of the present invention3A high-resolution transmission electron microscope image of the film;
FIG. 2b shows LaCoO under the combined action of external electric field and stress field in example 1 of the present invention3The film forms a high-resolution transmission electron microscope image of a transverse (parallel to the substrate) oxygen vacancy sequence phase on two sides of the tungsten needle tip;
FIG. 2c shows LaCoO in example 1 of the present invention3A profile of the electric field in the film;
FIG. 3a shows original LaCoO in example 2 of the present invention3A high-resolution transmission electron microscope image of the film;
FIG. 3b shows LaCoO under the action of external electric field only in example 2 of the present invention3The film forms a high-resolution transmission electron microscope image of an oxygen vacancy sequence phase in the longitudinal direction (vertical to the substrate) in front of the tungsten needle;
FIG. 3c shows LaCoO in example 2 of the present invention3A profile of the electric field in the film;
FIG. 4a shows original LaCoO in example 1 of the present invention3Electron energy loss spectra of the O-K edge of the phase and oxygen vacancy sequence phases;
FIG. 4b shows original LaCoO in example 1 of the present invention3Co-L of phase and oxygen vacancy ordered phase2,3Electron energy loss spectra of the edges;
FIG. 5a shows that the present invention regulates LaCoO under the combined action of external electric field and stress field3Schematic representation of one embodiment of an oxygen vacancy ordering phase in a film;
FIG. 5b shows the control of LaCoO under the independent action of external electric field according to the present invention3Schematic representation of one embodiment of the oxygen vacancy phase in the film.
Detailed Description
The present invention is described in further detail below with reference to specific embodiments, which are given for the purpose of illustration only and are not intended to limit the scope of the invention.
The preparation method of the invention forms the oxygen defect phase with the oxygen vacancy sequence phase by means of the migration of oxygen ions in the perovskite phase cobalt oxide film which can induce epitaxial growth by an electric field and pins the characteristic that the local structure can inhibit the formation of the oxygen defect phase by a stress field, and controls the position and the direction of the oxygen vacancy sequence phase by adjusting the complex interaction of the electric field and the stress field. The principle of the method of the invention is shown in fig. 1a and 1 b. As shown in FIG. 1a, the W tip and LaCoO are constructed in an electron microscope3Thin film, conductive SrTiO3A sandwich structure of substrates; wherein the W needle point is used as a movable electrode, an electric field and a stress field are applied to the film, and simultaneously, the conductive SrTiO3The substrate is grounded as a cathode. FIG. 1b is a low power transmission electron micrograph of the experimental setup.
Example 1
(1) The traditional preparation of a transmission electron microscope section sample is utilized:
growing Nb doped SrTiO by using epoxy resin glue (M-bond 610)3LaCoO on a substrate3The film was bonded to a clean-surfaced Si wafer and heated for 3 hours. After the adhesive was firmly bonded, the resultant was cut into a long strip having a length of 3mm and a width of 0.6 mm. The strips were ground and polished with diamond sandpaper until the thickness of the strips was below 3 μm. And further thinning the sample by using ion thinning equipment to ensure that the final thickness of the film is between 30 and 70 nm. Then the sample rod is placed at one end of a transmission electron microscope sample rod and fixed. Then fixing the electrochemically corroded metal tungsten needle tip at the moving end of the sample rod, thereby constructing a W needle tip and LaCoO on the sample rod of the in-situ electrical probe of the transmission electron microscope3Film, 0.7% Nb SrTiO3Substrate "sandwich structure.
(2) The metallic W tip was driven by a piezoelectric ceramic to apply a force of 4GPa to the sample, and then a positive voltage, 0.7% Nb: SrTiO, was applied to one end of the metallic W tip by an external power supply connected to the sample rod3The substrate is grounded, the voltage is 2V, and the current is 3 x 10-7A. LaCoO right in front of the needle tip due to local pinning of stress field3The film keeps the original perovskite structure, and oxygen ions in the film close to the substrate on two sides of the needle point gradually migrate under the driving of an external electric field to form a transverse oxygen vacancy sequence phase.
Characterization and testing
From the high-resolution transmission electron microscopy images (as shown in FIG. 2b and FIG. 3b), it can be determined that the formed transverse and longitudinal oxygen vacancy phases are LaCoO2.5And (4) phase(s).
FIG. 2a shows LaCoO without any applied electric and stress fields3FIG. 2b shows that when an electric field and a stress field are applied simultaneously to the thin film, oxygen ions in the thin film on both sides of the thin film, which are not completely inhibited by the stress of the needle tip, are induced to migrate to form oxygen vacancy sequences parallel to the substrate-thin film interface due to the complex effects of the electric field and the stress field, i.e., the stress field inhibits the migration of oxygen ions in the thin film directly in front of the needle tipAnd (4) phase(s). Figure 2c shows the electric field profile in the film.
Fig. 4a and 4b show that the oxygen content of the oxygen vacancy-ordered phase region is significantly lower than the stress-pinned region, and the valence state of the corresponding transition metal Co ion is also lower.
Example 2
(1) The traditional preparation of a transmission electron microscope section sample is utilized:
growing Nb doped SrTiO by using epoxy resin glue (M-bond 610)3LaCoO on a substrate3The film was bonded to a clean-surfaced Si wafer and heated for 3 hours. After the adhesive was firmly bonded, the resultant was cut into a long strip having a length of 3mm and a width of 0.6 mm. The strips were ground and polished with diamond sandpaper until the thickness of the strips was below 3 μm. And further thinning the sample by using ion thinning equipment to ensure that the final thickness of the film is between 30 and 70 nm. Then the sample rod is placed at one end of a transmission electron microscope sample rod and fixed. Then fixing the electrochemically corroded metal tungsten needle tip at the moving end of the sample rod, thereby constructing a W needle tip and LaCoO on the sample rod of the in-situ electrical probe of the transmission electron microscope3Film, 0.7% Nb SrTiO3Substrate "sandwich structure.
(2) The piezoelectric ceramic drives the metal W needle point to be connected with the LaCoO3The film just contacted but without significant stress interaction, then a positive voltage, 0.7% Nb: SrTiO, was applied to one end of the metallic W tip by an external power supply connected to the sample rod3The substrate is grounded, the voltage is 1V, and the current is 2 x 10-7A. At this time, under the driving action of the external electric field, the LaCoO right in front of the needle point3Oxygen ions in the film gradually migrate to form a longitudinal oxygen vacancy sequence phase on the surface of the film, and a little transverse oxygen vacancy sequence phase is formed on the surfaces of the films on two sides of the needle point.
Characterization and testing
FIGS. 3a to 3c show the LaCoO tip pair at W in step (2) of the present embodiment3The film is located in front of the needle tip when only external electric field but not stress field is applied3The oxygen in the film gradually migrates outward and forms longitudinal oxygen vacancy sequencesAnd (4) phase(s). When only an electric field is applied to the film without applying a stress field, the electric field induces oxygen ion migration in the film, forming a longitudinal oxygen vacancy phase structure directly in front of the tip and a small amount of transverse oxygen vacancy phase at the sides of the film, as shown in fig. 3 b.
Claims (10)
1. A method for regulating and controlling an oxygen vacancy sequence phase of a perovskite phase cobalt oxide material comprises the following steps: for perovskite phase cobalt oxide ACoO in the form of a thin film3Applying an electric field or applying an electric field and a stress field such that the perovskite phase cobalt oxide thin film is formed from the original perovskite phase ACoO3Conversion to oxygen vacancy ordered phase ACoO2.5(ii) a Wherein A is selected from one or more of La, Sr and Ca.
2. The method of claim 1, wherein the electric field has a voltage of 1-5V and a current of 1 x 10-7-2×10-6A。
3. The method of claim 2, wherein the electric field has a voltage of 2-3V and a current of 1 x 10-7-6×10-7A。
4. The method of claim 1, wherein the stress field has a pressure of 3-5 GPa.
5. The method of claim 1, wherein the applying the electric field is performed by a method comprising:
(1) preparing a perovskite phase cobalt oxide thin film grown on a substrate into a transmission electron microscope cross-section sample, and mounting the sample on one end of a sample rod of a transmission electron microscope;
(2) fixing a metal tungsten needle tip on the other end of the sample rod, and enabling the metal tungsten needle tip to be just contacted with the perovskite phase cobalt oxide film without stress; and then applying an electric field to the sample through an external power supply device connected with the sample rod, wherein the metal tungsten needle point is connected with the anode, and the substrate is grounded.
6. The method of claim 1, wherein the applying the electric field and the stress field is performed by a method comprising:
(1) preparing a perovskite phase cobalt oxide thin film grown on a substrate into a transmission electron microscope cross-section sample, and mounting the sample on one end of a sample rod of a transmission electron microscope;
(2) fixing a metal tungsten needle point on the other end of the sample rod, and driving the metal tungsten needle point through piezoelectric ceramics so as to apply a stress field to the sample; and then applying an electric field to the sample through an external power supply device connected with the sample rod, wherein the metal tungsten needle point is connected with the anode, and the substrate is grounded.
7. The method of claim 5 or 6, wherein the metal tungsten tip is pre-treated with electrochemical etching.
8. The method according to claim 5 or 6, wherein the step (1) of producing the transmission electron microscope cross-sectional sample is performed by a method comprising the following steps:
adhering the perovskite phase cobalt oxide film grown on the substrate to a silicon wafer, heating and curing, and cutting into pieces with the thickness of 5 mm; and grinding the silicon wafer to the thickness of 2-3 microns, fixing the silicon wafer on a molybdenum ring, moving the silicon wafer upwards to an ion thinning instrument for thinning.
9. The method according to claim 5 or 6, wherein the cross-sectional thickness of the TEM cross-sectional sample is 30-70 nm.
10. The method of claim 5 or 6, wherein the substrate is formed from Nb doped SrTiO3Forming; wherein the mass fraction of Nb is 0.5-1% based on the total mass of the substrate.
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