CN113106398B - Preparation method of lanthanum strontium manganese oxygen film - Google Patents

Preparation method of lanthanum strontium manganese oxygen film Download PDF

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CN113106398B
CN113106398B CN202110389349.9A CN202110389349A CN113106398B CN 113106398 B CN113106398 B CN 113106398B CN 202110389349 A CN202110389349 A CN 202110389349A CN 113106398 B CN113106398 B CN 113106398B
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lanthanum
film
lanthanum strontium
strontium manganese
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CN113106398A (en
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王学锋
袁霄
陈勇达
刘汝新
张�荣
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Nanjing University
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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    • C23C14/5806—Thermal treatment

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Abstract

The invention discloses a lanthanum strontium manganese oxygen film preparation method, which comprises the steps of firstly depositing a strontium aluminate film on a processed substrate by using a pulse laser deposition system under the conditions of certain temperature and pressure in a vacuum chamber of the pulse laser deposition system, carrying out in-situ annealing on the substrate, then depositing a lanthanum strontium manganese oxygen film on the substrate in the same way, and then carrying out in-situ annealing, wherein the preparation process is monitored in situ by using the pulse laser deposition system. In the invention, strontium aluminate is used as a buffer layer in the preparation process of the strontium aluminate film, the stress can be quickly released in a thinner thickness, the prepared lanthanum strontium manganese oxide film has good ferromagnetic metal characteristics and meets the requirements of a spinning electronic device, the method effectively solves the problem that a dead layer is thicker on a large lattice mismatched substrate in the preparation of the lanthanum strontium manganese oxide film in the prior art, and the method can be further popularized and applied to the preparation of other types of films.

Description

Preparation method of lanthanum strontium manganese oxygen film
Technical Field
The invention discloses a preparation method of a lanthanum strontium manganese oxygen film, belonging to the technical field of electronic materials.
Background
With the coming of the fourth industrial revolution and the evolution of emerging technologies such as 5G and big data, the requirements for the information storage field are higher and higher, and the traditional materials applied to the information storage field still have the defects of low storage density, limited erasing times, large energy consumption and the like, and a novel material is urgently needed to meet the requirements of low energy consumption and long service life of a storage device. In the novel storage material, the lanthanum strontium manganese oxygen film has physical properties such as exchange bias effect, room-temperature ferromagnetism, colossal magnetoresistance effect, metal insulator transformation and the like, is used as a spin injection source to be applied to a spin electronic device, and has the advantages of high reading speed, low energy consumption, long service life and the like.
At present, along with the gradual reduction of thickness, the interface of lanthanum strontium manganese oxygen film in-process of preparing can appear the dead layer with the substrate, and the nature of lanthanum strontium manganese oxygen film can become anti-ferromagnetic insulating nature by ferromagnetic metal nature in dead layer region to produce extremely high resistivity. The occurrence of dead layers is not beneficial to the miniaturization of devices, and the further application of the novel lanthanum strontium manganese oxide film is limited. The main reasons for generating the dead layer of the lanthanum strontium manganese oxygen film prepared on the traditional perovskite substrate are as follows: stress caused by lattice mismatch of the substrate and the lanthanum strontium manganese oxygen film, electronic orbit reconstruction caused by discontinuous polarity of the lanthanum strontium manganese oxygen film, disorder caused by interface diffusion of the substrate and the lanthanum strontium manganese oxygen film and the like. In the prior art, elimination of track reconstruction caused by polarity discontinuity of lanthanum strontium manganese oxygen through interface engineering and doping of lanthanum strontium manganese oxygen to change or inhibit diffusion of a lanthanum strontium manganese oxygen thin film at an interface are effective means, but in practical engineering application, interface engineering operation is relatively complex, reduction range of thickness of a dead layer is small, partial properties of the lanthanum strontium manganese oxygen thin film can be reduced through doping, particularly on a large substrate with lattice mismatch, thickness of the lanthanum strontium manganese oxygen dead layer can often reach 10nm, and influence of the means on thickness of the dead layer is small.
Therefore, a simple and effective method is designed to reduce the thickness of a dead layer in the preparation process of the lanthanum strontium manganese oxygen thin film, and especially under the condition of certain larger lattice-mismatched substrates, the method has important significance for the miniaturization, popularization and application of lanthanum strontium manganese oxygen thin film devices.
Disclosure of Invention
Technical problem to be solved by the invention
In order to solve the problem that a dead layer is thicker on a large lattice mismatched substrate during the preparation of the lanthanum strontium manganese oxygen film in the prior art, the invention provides the preparation method of the lanthanum strontium manganese oxygen film, which can effectively reduce the thickness of the generated dead layer.
Technical scheme
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a preparation method of a lanthanum strontium manganese oxygen film comprises the following steps:
step 1, treating a lanthanum aluminate substrate by using acetone, alcohol and deionized water;
step 2, placing the treated lanthanum aluminate substrate into a vacuum chamber of a pulse laser deposition system, introducing protective mixed gas, and heating the substrate;
step 3, preparing a strontium aluminate target material in a vacuum chamber, irradiating the strontium aluminate target material by using laser to generate plasma plume, depositing a strontium aluminate film on a lanthanum aluminate substrate, and carrying out in-situ monitoring through a fluorescent screen of a deposition system;
step 4, keeping the temperature and air pressure environment in the vacuum chamber unchanged, and carrying out in-situ annealing on the substrate obtained in the step 3;
step 5, replacing the lanthanum strontium manganese oxygen target, depositing a lanthanum strontium manganese oxygen film on the substrate obtained in the step 4 in the same way as the step 3, and carrying out in-situ monitoring through a fluorescent screen of a deposition system;
step 6, keeping the temperature and the air pressure environment of the vacuum chamber unchanged, carrying out in-situ annealing on the substrate obtained in the step 5, and stopping introducing protective gas after the film is naturally cooled to the room temperature;
and 7, closing the pulse laser deposition system, taking out the substrate, and finishing the preparation of the lanthanum strontium manganese oxygen film.
Further, the method for processing the lanthanum aluminate substrate in the step 1 comprises the following steps: firstly, ultrasonically cleaning a lanthanum aluminate substrate in acetone and absolute ethyl alcohol respectively, and then soaking the cleaned substrate in deionized water.
Further, the protective mixed gas in step 2 is a mixed gas of oxygen and ozone.
Further, the laser source in step 3 is a KrF excimer laser.
Advantageous effects
By adopting the technical scheme of the invention, the following beneficial effects can be produced:
in the preparation process of the lanthanum strontium manganese oxide film, strontium aluminate is used as a buffer layer, and compared with the traditional interface engineering and perovskite structure buffer layer, the lanthanum strontium manganese oxide film has smaller elastic modulus and can quickly release stress at thinner thickness, and experiments show that the thickness of a dead layer on a large-lattice-mismatched substrate can be reduced by 60%;
the method can accurately control the thickness of the prepared lanthanum strontium manganese oxygen film, the lanthanum strontium manganese oxygen film after dead layer reduction is a single crystal film, has good ferromagnetic metal characteristics, meets the requirements of spin electronic devices, and can be further popularized and applied to the preparation of other types of films.
Drawings
FIG. 1 is a schematic diagram of a pulsed laser deposition system according to the present invention;
FIG. 2 is a schematic view showing the steps of the process for producing a strontium aluminate film according to the present invention;
FIG. 3 is a graph showing the change of the atomic magnetic moment of the lanthanum strontium manganese oxygen thin film according to the temperature in the comparative example;
FIG. 4 is a graph of the change of the atomic magnetic moment of the lanthanum strontium manganese oxygen film with temperature according to the embodiment of the present invention;
FIG. 5 is a graph showing the change of resistivity of a lanthanum strontium manganese oxygen thin film prepared according to a comparative example of the present invention with temperature;
FIG. 6 is a graph of the resistivity of a lanthanum strontium manganese oxygen thin film prepared according to an embodiment of the present invention varying with temperature;
FIG. 7 is reciprocal space diffraction pattern of lanthanum strontium manganese oxygen thin film prepared by comparison example of the present invention;
FIG. 8 is a reciprocal space diffraction pattern of a lanthanum strontium manganese oxygen thin film prepared according to an embodiment of the present invention;
the reference numerals in the figures illustrate: 1-a vacuum chamber; 2-a substrate; 3-a target material rotary table; 4-reflection high-energy electron diffractometer; 5-mixed gas input device; 6-fluorescent screen; 7-laser incidence device, 8-air extraction opening.
Detailed Description
For a further understanding of the invention, reference should be made to the following detailed description taken in conjunction with the accompanying drawings.
FIG. 1 is a schematic structural diagram of a pulsed laser deposition system for implementing the method of the present invention, wherein when the system is in operation, a deposition target is placed on a target turntable 3, the replacement of strontium aluminate and lanthanum strontium manganese oxide targets is realized by the rotation of the turntable, a substrate 2 is fixed above the target turntable 3, a reflective high-energy electron diffractometer 4 is used for generating an electron beam irradiated on the substrate and forming a diffraction stripe on a fluorescent screen 6 to realize the in-situ monitoring of the deposition process, a mixed gas required in the deposition process is input into a vacuum chamber through a mixed gas input device 5, a laser input device 7 generates laser and irradiates the target on the target turntable 3, and an air exhaust port 8 realizes the control of the air pressure in the vacuum chamber 1.
As shown in FIG. 2, the method of the present invention first treats lanthanum aluminate (LaAlO)3) The substrate is processed, and the processing method in the embodiment is as follows: firstly, ultrasonically cleaning a lanthanum aluminate substrate in acetone and absolute ethyl alcohol for 5 minutes respectively; then soaking the cleaned substrate in deionized water at 70 ℃ for 20 minutes, and then putting the substrate into a vacuum chamber of a pulse laser deposition system, wherein the air pressure in the chamber is set to be less than or equal to 8.6 multiplied by 10-8mbar; to prevent the substrate from oxygen deficiency, the pressure in the vacuum chamber is 1.4 × 10-3mbar protective gas is heated simultaneously, and the protective gas comprises the following components: 90 plus or minus 2 percent of oxygen and 10 plus or minus 2 percent of ozone.
Preparing a strontium aluminate target material in a vacuum chamber of a pulse laser deposition system, irradiating the strontium aluminate target material by using laser to generate plasma plume, and depositing a strontium aluminate film on a lanthanum aluminate substrate at the deposition temperature of 750 +/-5 ℃ and the air pressure of 1.4 +/-0.2 multiplied by 10-5mbar, the deposition thickness of the strontium aluminate layer is 2.4nm, and the deposition process is monitored in situ through a system fluorescent screen; the temperature and the air pressure environment in the vacuum chamber are kept unchanged (the temperature is 750 +/-5 ℃, and the air pressure is 1.4 +/-0.2 multiplied by 10)-5mbar) was applied to the substrate in situ for an annealing time of 30 minutes.
The lanthanum strontium manganese oxygen target material is replaced in a pulse laser deposition system, the deposition of the lanthanum strontium manganese oxygen film is carried out on the substrate after in-situ annealing by adopting the same mode, the deposition temperature is 750 +/-5 ℃, and the air pressure is 1.4 +/-0.2 multiplied by 10-5mbar, the deposition thickness of the lanthanum strontium manganese oxygen layer is more than or equal to 4.8 nm; and (3) keeping the temperature and the air pressure environment of the vacuum chamber, carrying out in-situ annealing on the substrate for 15 minutes, stopping introducing protective gas after the film is naturally cooled to room temperature, closing the pulse laser deposition system, taking out the substrate, and completing the preparation of the lanthanum strontium manganese oxide film.
In this embodiment, the laser source used in the pulsed laser deposition system is a KrF excimer laser, the wavelength is 248nm, the angle between the target and the laser beam is about 45 °, and the average energy density of the laser beam: 1.7 +/-0.2J/cm2And the distance between the substrate and the target material is as follows: 5cm, laser repetition frequency: 1 Hz.
In order to verify the lanthanum strontium manganese oxygen film prepared by the invention, a comparative example is provided, and the method comprises the following steps: the step of depositing the strontium aluminate film in the embodiment is removed, and the lanthanum strontium manganese oxide film is directly prepared on the lanthanum aluminate substrate, and other preparation conditions are the same as the embodiment.
The magnetic performance of the lanthanum strontium manganese oxygen thin film prepared in the comparative example is mainly judged by using a superconducting quantum interferometer (SQUID) to characterize the lanthanum strontium manganese oxygen thin film prepared in the comparative example, as can be seen from figure 3, the lanthanum strontium manganese oxygen thin film prepared in the comparative example has extremely low ferromagnetic performance at 10K, and compared with the saturated atomic magnetic moment of a block material which is as high as 4 mu B, the saturated atomic magnetic moment of the lanthanum strontium manganese oxygen thin film is only 0.6 mu B, the Curie temperature is about 100K, and even the saturated atomic magnetic moment is difficult to distinguish from the background and is far lower than the Curie temperature 367K of the block.
As shown in FIG. 4, the magnetic properties of the lanthanum strontium manganese oxygen thin film prepared by the method of the present invention are characterized by a superconducting quantum interferometer, and compared with the comparative example in which the original thickness is not increased by a buffer layer, the saturated magnetic moment of the lanthanum strontium manganese oxygen thin film prepared by the method of the present invention is 3.7 μ B at 10K, the Curie temperature is higher than 280K, and is much higher than the saturated magnetic moment and the Curie temperature in the comparative example, which are already close to the properties of the bulk material.
The transport performance of the lanthanum strontium manganese oxygen thin film is characterized by a comprehensive physical property measurement system for the thin film prepared in the comparative example, fig. 5 is a change curve of the resistivity of the thin film prepared in the comparative example along with the temperature, and as can be seen from the graph, the larger resistivity of the lanthanum strontium manganese oxygen thin film is shown as the reason, which is opposite to the half-metallic property of the bulk material, which shows that the lanthanum strontium manganese oxygen thin film is in a dead layer at the moment.
Fig. 6 is a graph showing the change of resistivity with temperature of the thin film manufactured by the method of the present invention, and it can be seen from the graph that the lanthanum strontium manganese oxygen thin film is metallic, and the lower resistivity, contrary to the insulation in the comparative example, also indicates excellent properties in the interior of the material.
The structure of the lanthanum strontium manganese oxide thin film was characterized by an X-ray diffractometer, and fig. 7 is a reciprocal space diagram of the lanthanum strontium manganese oxide thin film along the direction 103 of the comparative example, where it can be seen that the thin film made by the comparative example method is completely bounded by the substrate, and the almost invisible diffraction peak indicates that the stress of the lanthanum strontium manganese oxide thin film is hardly released.
As shown in fig. 8, in contrast to the comparative example, the significant diffraction peaks of the lanthanum strontium manganese oxide film produced by the method of the present invention indicate the good quality of the film (in the figure the LSMO represents the lanthanum strontium manganese oxide film and the arrows point to the central diffraction point) and the perpendicular distance from the central diffraction point of the substrate (in the figure the white line represents the central diffraction point) indicates that the stress of the lanthanum strontium manganese oxide film has been released.
The pulse laser deposition method has the advantages of simple preparation process, controllable atomic-scale precision and adjustable parameters in the preparation process, and the used substrates are all commercial products, are easy to obtain and have good repeatability. The prepared lanthanum strontium manganese oxygen film is ferromagnetic metal, and the method can be extended to the preparation of other perovskite structure films.
The present invention and its embodiments have been described above schematically, without limitation, and what is shown in the drawings is only one of the embodiments of the present invention, and the actual structure is not limited thereto. Therefore, if the person skilled in the art receives the teaching, without departing from the spirit of the invention, the person skilled in the art shall not inventively design the similar structural modes and embodiments to the technical solution, but shall fall within the scope of the invention.

Claims (4)

1. The preparation method of the lanthanum strontium manganese oxygen film is characterized by comprising the following steps of:
step 1, treating a lanthanum aluminate substrate by using acetone, alcohol and deionized water;
step 2, placing the treated lanthanum aluminate substrate into a vacuum chamber of a pulse laser deposition system, introducing protective mixed gas, and heating the substrate;
step 3, preparing a strontium aluminate target material in a vacuum chamber, irradiating the strontium aluminate target material by using laser to generate plasma plume, depositing a strontium aluminate film on a lanthanum aluminate substrate, and carrying out in-situ monitoring on the deposition process through a system fluorescent screen;
step 4, keeping the temperature and air pressure environment in the vacuum chamber unchanged, and carrying out in-situ annealing on the substrate obtained in the step 3;
step 5, replacing the lanthanum strontium manganese oxygen target, depositing a lanthanum strontium manganese oxygen film on the substrate obtained in the step 4 in the same way as the step 3, and carrying out in-situ monitoring on the deposition process through a system fluorescent screen;
step 6, keeping the temperature and the air pressure environment of the vacuum chamber unchanged, carrying out in-situ annealing on the substrate obtained in the step 5, and stopping introducing protective gas after the film is naturally cooled to the room temperature;
and 7, closing the pulse laser deposition system, taking out the substrate, and finishing the preparation of the lanthanum strontium manganese oxygen film.
2. The method for preparing a lanthanum strontium manganese oxygen thin film according to claim 1, wherein the method for processing the lanthanum aluminate substrate in the step 1 comprises: firstly, ultrasonically cleaning a lanthanum aluminate substrate in acetone and absolute ethyl alcohol respectively, and then soaking the cleaned substrate in deionized water.
3. The method of claim 1, wherein the protective mixture gas in step 2 is a mixture gas of oxygen and ozone.
4. The method of claim 1, wherein the laser source in step 3 is a KrF excimer laser.
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CN106591781A (en) * 2017-01-10 2017-04-26 河北大学 Improvement method for interface dead layer of ultrathin lanthanum-strontium-manganese oxide film

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Publication number Priority date Publication date Assignee Title
CN106591781A (en) * 2017-01-10 2017-04-26 河北大学 Improvement method for interface dead layer of ultrathin lanthanum-strontium-manganese oxide film

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