CN109023261B - Preparation method of transferable perovskite oxide piezoelectric texture film with crystallization promoted by graphene - Google Patents

Preparation method of transferable perovskite oxide piezoelectric texture film with crystallization promoted by graphene Download PDF

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CN109023261B
CN109023261B CN201810849978.3A CN201810849978A CN109023261B CN 109023261 B CN109023261 B CN 109023261B CN 201810849978 A CN201810849978 A CN 201810849978A CN 109023261 B CN109023261 B CN 109023261B
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CN109023261A (en
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牛刚
代立言
赵金燕
任巍
王玲艳
白炜
史鹏
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Xian Jiaotong University
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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
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Abstract

The invention discloses a preparation method of a transferable perovskite oxide piezoelectric texture film with crystallization promoted by graphene, which comprises the following steps: 1) selecting graphiteAlkene is used as an intermediate layer material of the oxide and the substrate; 2) selecting a pulsed laser deposition technology as a film growth means, and controlling the growth temperature to be 500-800 ℃; controlling the oxygen partial pressure to be 10-20 Pa; controlling the laser energy at 1.5J/cm2～3J/cm2The frequency is 1 Hz-10 Hz; the film with the perovskite structure prepared by the invention is analyzed by X-ray diffraction (XRD), an Atomic Force Microscope (AFM) and a Piezoelectric Force Microscope (PFM), the grown film has good texture crystallization characteristic, and the thickness of the film layer is controllable within 300 nm; the surface of the film is flat, and the root mean square roughness is within 1 nm; the grown thin film is piezoelectric and has the potential to be transferred to any substrate.

Description

Preparation method of transferable perovskite oxide piezoelectric texture film with crystallization promoted by graphene
Technical Field
The invention relates to a perovskite oxide film growth method, in particular to a preparation method of a transferable perovskite oxide piezoelectric texture film with crystallization promoted by graphene.
Background
The ferroelectric oxide film is used for preparing energy conversion, information storage, temperature detection and other types of devices due to the characteristics of ferroelectricity, piezoelectricity, pyroelectricity and the like, and has wide application in various fields of national defense, education, medical treatment, aerospace, information and the like.
Currently, many people have realized the preparation of ferroelectric piezoelectric thin films with better crystalline quality on some specific substrates, such as strontium titanate and other oxide substrates. However, in order to satisfy more various functional requirements, it is desirable to grow ferroelectric piezoelectric thin films on more various substrates. For example, it is desired to grow a ferroelectric piezoelectric thin film on a silicon substrate by means of a semiconductor silicon process line which has been widely established, but since the silicon surface is easily oxidized, a thin film in a polycrystalline or amorphous state is obtained; for another example, it is desirable to combine the ferroelectric piezoelectric thin film with a flexible substrate, but since the melting point of common flexible substrates such as polyimide thin film (PI), polyethylene terephthalate (PET) and other organic materials is generally within 300 ℃, it is difficult to satisfy the crystallization temperature as high as 500 ℃ required in the growth process of the ferroelectric piezoelectric thin film, and thus the thin film obtained on the flexible substrate can only be a poor quality amorphous thin film which is not crystallized. At present, no technology can finish the work of preparing a high-quality texture ferroelectric piezoelectric film on any substrate.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a transferable perovskite oxide piezoelectric textured film with graphene promoted crystallization, which can integrate the perovskite oxide piezoelectric textured film on a silicon substrate conveniently.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a preparation method of a transferable perovskite oxide piezoelectric texture film with crystallization promoted by graphene comprises the following steps:
step 1: selecting graphene as an interlayer material of an oxide and a substrate;
step 2: growing a film by using a pulse laser deposition method; wherein the growth temperature is 500-800 ℃; the oxygen partial pressure is 10Pa to 20 Pa; the laser energy is 1.5J/cm2～3J/cm2The frequency is 1 Hz-10 Hz.
The invention further improves the following steps:
step 2, the specific method for growing the film by using the pulse laser deposition method is as follows:
2-1) placing the perovskite oxide target material to be grown and the graphene substrate in a vacuum chamber, and pumping the pressure in the vacuum chamber to 5 × 10-4Pa below to remove the contaminant impurities adsorbed on the surface of the graphene;
2-2) heating the graphene substrate to 500-800 ℃, introducing oxygen into the vacuum cavity, and controlling the air pressure to be 10-20 Pa;
2-3) using a pulse laser, controlling the laser energy density to be 1.5J/cm2～3J/cm2Converging laser on the surface of the barium titanate ceramic target by using a lens, and controlling the laser frequency to be between 1Hz and 10 Hz;
2-4) adjusting the distance between the substrate and the target material to be between 3cm and 10cm, and ensuring that the plasma plume tip part struck by the pulse laser can be positioned on the surface of the substrate;
2-5) keeping the above state to grow the film, after the film grows to the preset thickness, closing the laser, introducing oxygen into the vacuum cavity, and controlling the air pressure to be 1 × 104Pa is above;
2-6) cooling the substrate to room temperature, introducing air into the vacuum cavity, and opening the cavity to obtain a film/graphene substrate sample.
Compared with the prior art, the invention has the following beneficial effects:
the film with the perovskite structure prepared by the invention has texture crystallization through analysis of X-ray diffraction (XRD), Atomic Force Microscope (AFM) and Piezoelectric Force Microscope (PFM), and the film thickness is controllable within 300 nm; the surface of the film is flat, and the root mean square roughness is within 1 nm; finally, the film prepared by the invention has piezoelectricity.
Drawings
Fig. 1 is an out-of-plane XRD pattern of a barium titanate thin film on silicon-based graphene prepared in example 1;
fig. 2 is an out-of-plane XRD pattern of the same thickness of the graphene-free silicon-based barium titanate thin film prepared under the same conditions as in example 1;
FIG. 3 is an AFM observation film surface topography of the barium titanate film on the silicon-based graphene prepared in example 1;
fig. 4 is a PFM observed film compressive stress response plot of the barium titanate film on silicon-based graphene prepared in example 1;
wherein the abscissa of FIG. 1-2 represents the out-of-plane diffraction angle of X-rays and the ordinate represents the diffraction intensity, and the scan area of FIG. 3 is 2 × 2 μm2(ii) a The abscissa of FIG. 4 represents the intensity of the applied voltage and the ordinate in the upper graph represents the piezoelectric response produced by the membraneThe corresponding phase shift is in degrees, and the ordinate of the lower half of the graph shows the strength of the piezoelectric response generated by the membrane.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
referring to fig. 1, the preparation method of the transferable perovskite oxide piezoelectric textured thin film with graphene promoted crystallization of the invention comprises the following steps:
step 1: selecting graphene as an interlayer material of an oxide and a substrate;
step 2: the method for growing the film by using the pulse laser deposition method comprises the following steps:
2-1) loading the perovskite oxide target material to be grown and the graphene substrate in a vacuum chamber, and using the vacuum chamberThe air pressure in the cavity is pumped to 5 × 10-4Pa below to remove the contaminant impurities adsorbed on the surface of the graphene;
2-2) heating the graphene substrate to 500-800 ℃, introducing oxygen into the vacuum cavity, and controlling the air pressure to be 10-20 Pa;
2-3) using a pulse laser, controlling the laser energy density to be 1.5J/cm2～3J/cm2Converging laser on the surface of the barium titanate ceramic target by using a lens, and controlling the laser frequency to be between 1Hz and 10 Hz;
2-4) adjusting the distance between the substrate and the target material to be between 3cm and 10cm, and ensuring that the plasma plume tip part struck by the pulse laser can be positioned on the surface of the substrate;
2-5) keeping the above state to grow the film, after the film grows to the preset thickness, closing the laser, introducing oxygen into the vacuum cavity, and controlling the air pressure to be 1 × 104Pa is above;
2-6) cooling the substrate to room temperature, introducing air into the vacuum cavity, and opening the cavity to obtain a film/graphene substrate sample.
Example 1
1) Barium titanate ceramic target material and SiO coated with graphene2the/Si substrate is arranged in the cavity of the pulse laser deposition equipment;
2) the chamber pressure was pumped down to background pressure 5 × 10 using a vacuum pump-4Pa；
3) Heating the silicon-based graphene substrate to 650 ℃;
4) introducing high-purity oxygen, and adjusting the air pressure to 10 Pa;
5) shielding the substrate by using a baffle, opening a laser, adjusting laser focus on the surface of the barium titanate ceramic target, and carrying out pre-sputtering to remove impurities on the surface of the target;
6) the laser energy density is adjusted to be 1.8J/cm2Controlling the frequency to be 5Hz, opening a baffle plate in front of the substrate, and starting film growth;
7) according to the required film thickness, after waiting for a certain growth time, closing the laser and stopping the film growth;
8) closing the vacuum pump, filling sufficient oxygen into the cavity, and adjusting the air pressure to be within1×104Pa is above;
9) and closing the substrate heater, after the substrate is cooled to room temperature, communicating the cavity with the atmosphere, opening a cavity door, and taking out the grown barium titanate film on the silicon-based graphene.
As shown in fig. 1, the obtained barium titanate thin film on si-based graphene was subjected to an out-of-plane structure test by XRD (the japanese Rigaku SmartLab type X-ray diffractometer, X-ray source is Cu target, Ge (220) single crystal with 2 refractions is used as monochromator), and it was found that the obtained thin film was mainly grown in the (001) direction. As shown in fig. 2, the prepared graphene-free covered SiO grown2The barium titanate film on the Si substrate is subjected to an out-of-plane structure test by XRD (a Rigaku SmartLab type X-ray diffractometer in Japan, an X-ray source is a Cu target, and Ge (220) single crystal with 2 refractions is used as a monochromator), and the diffraction peak intensity of the prepared film is obviously lower than that of a film growing on the substrate covered with graphene, which shows that the crystallization quality of the film on the substrate without the graphene is poor, and the crystallization quality of the film can be improved by using the graphene as the substrate. As shown in FIG. 3, the surface of the thin film was smooth and the root mean square roughness was 0.96 nm. As shown in fig. 4, by using PFM to characterize the piezoelectric response of the barium titanate thin film on the silicon-based graphene, a typical phase-flip curve and a strain "butterfly curve" can be detected, which indicates that the thin film has piezoelectricity.
Example 2
1) Barium titanate ceramic target material and SiO coated with graphene2the/Si substrate is arranged in the cavity of the pulse laser deposition equipment;
2) the chamber pressure was pumped down to background pressure 5 × 10 using a vacuum pump-4Pa；
3) Heating the silicon-based graphene substrate to 500 ℃;
4) introducing high-purity oxygen, and adjusting the air pressure to 10 Pa;
5) shielding the substrate by using a baffle, opening a laser, adjusting laser focus on the surface of the barium titanate ceramic target, and carrying out pre-sputtering to remove impurities on the surface of the target;
6) the laser energy density is adjusted to be 1.5J/cm2Controlling the frequency to be 1Hz, opening a baffle plate in front of the substrate, and starting film growth;
7) according to the required film thickness, after waiting for a certain growth time, closing the laser and stopping the film growth;
8) the vacuum pump is closed, sufficient oxygen is filled into the cavity, and the air pressure is adjusted to be 1 × 104Pa is above;
9) and closing the substrate heater, after the substrate is cooled to room temperature, communicating the cavity with the atmosphere, opening a cavity door, and taking out the grown barium titanate film on the silicon-based graphene.
Example 3
1) Barium titanate ceramic target material and SiO coated with graphene2the/Si substrate is arranged in the cavity of the pulse laser deposition equipment;
2) the chamber pressure was pumped down to background pressure 5 × 10 using a vacuum pump-4Pa；
3) Heating the silicon-based graphene substrate to 600 ℃;
4) introducing high-purity oxygen, and adjusting the air pressure to 15 Pa;
5) shielding the substrate by using a baffle, opening a laser, adjusting laser focus on the surface of the barium titanate ceramic target, and carrying out pre-sputtering to remove impurities on the surface of the target;
6) the laser energy density is adjusted to be 2.0J/cm2Controlling the frequency to be 3Hz, opening a baffle plate in front of the substrate, and starting film growth;
7) according to the required film thickness, after waiting for a certain growth time, closing the laser and stopping the film growth;
8) the vacuum pump is closed, sufficient oxygen is filled into the cavity, and the air pressure is adjusted to be 1 × 104Pa is above;
9) and closing the substrate heater, after the substrate is cooled to room temperature, communicating the cavity with the atmosphere, opening a cavity door, and taking out the grown barium titanate film on the silicon-based graphene.
Example 4
1) Barium titanate ceramic target material and SiO coated with graphene2the/Si substrate is arranged in the cavity of the pulse laser deposition equipment;
2) the chamber pressure was pumped down to background pressure 5 × 10 using a vacuum pump-4Pa；
3) Heating the silicon-based graphene substrate to 700 ℃;
4) introducing high-purity oxygen, and adjusting the air pressure to 18 Pa;
5) shielding the substrate by using a baffle, opening a laser, adjusting laser focus on the surface of the barium titanate ceramic target, and carrying out pre-sputtering to remove impurities on the surface of the target;
6) the laser energy density is adjusted to be 2.5J/cm2Controlling the frequency to be 8Hz, opening a baffle plate in front of the substrate, and starting film growth;
7) according to the required film thickness, after waiting for a certain growth time, closing the laser and stopping the film growth;
8) the vacuum pump is closed, sufficient oxygen is filled into the cavity, and the air pressure is adjusted to be 1 × 104Pa is above;
9) and closing the substrate heater, after the substrate is cooled to room temperature, communicating the cavity with the atmosphere, opening a cavity door, and taking out the grown barium titanate film on the silicon-based graphene.
Example 5
1) Barium titanate ceramic target material and SiO coated with graphene2the/Si substrate is arranged in the cavity of the pulse laser deposition equipment;
2) the chamber pressure was pumped down to background pressure 5 × 10 using a vacuum pump-4Pa；
3) Heating the silicon-based graphene substrate to 800 ℃;
4) introducing high-purity oxygen, and adjusting the air pressure to be 20 Pa;
5) shielding the substrate by using a baffle, opening a laser, adjusting laser focus on the surface of the barium titanate ceramic target, and carrying out pre-sputtering to remove impurities on the surface of the target;
6) the laser energy density is adjusted to be 3.0J/cm2Controlling the frequency to be 10Hz, opening a baffle plate in front of the substrate, and starting film growth;
7) according to the required film thickness, after waiting for a certain growth time, closing the laser and stopping the film growth;
8) the vacuum pump is closed, sufficient oxygen is filled into the cavity, and the air pressure is adjusted to be 1 × 104Pa is above;
9) and closing the substrate heater, after the substrate is cooled to room temperature, communicating the cavity with the atmosphere, opening a cavity door, and taking out the grown barium titanate film on the silicon-based graphene.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.

Claims (1)

1. A preparation method of a transferable perovskite oxide piezoelectric texture film with crystallization promoted by graphene is characterized by comprising the following steps:
step 1: selecting graphene as an interlayer material of an oxide and a substrate;
step 2: growing a film by using a pulse laser deposition method; wherein the growth temperature is 500-800 ℃; the oxygen partial pressure is 10Pa to 20 Pa; the laser energy is 1.5J/cm2～3J/cm2The frequency is 1 Hz-10 Hz; the specific method comprises the following steps:
2-1) placing the perovskite oxide target material to be grown and the graphene substrate in a vacuum chamber, and pumping the pressure in the vacuum chamber to 5 × 10-4Pa below to remove the contaminant impurities adsorbed on the surface of the graphene;
2-2) heating the graphene substrate to 500-800 ℃, introducing oxygen into the vacuum cavity, and controlling the air pressure to be 10-20 Pa;
2-3) using a pulse laser, controlling the laser energy density to be 1.5J/cm2～3J/cm2Converging laser on the surface of the barium titanate ceramic target by using a lens, and controlling the laser frequency to be between 1Hz and 10 Hz;
2-4) adjusting the distance between the substrate and the target material to be between 3cm and 10cm, and ensuring that the plasma plume tip part struck by the pulse laser can be positioned on the surface of the substrate;
2-5) keeping the above state to grow the film, after the film grows to the preset thickness, closing the laser, introducing oxygen into the vacuum cavity, and controlling the air pressure to be 1 × 104Pa is above;
2-6) cooling the substrate to room temperature, introducing air into the vacuum cavity, and opening the cavity to obtain a film/graphene substrate sample.
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CN109898138B (en) * 2019-02-28 2020-09-29 西安交通大学 Method for epitaxial growth of single-crystal barium titanate film on germanium substrate
CN109896543B (en) * 2019-02-28 2020-07-28 西安交通大学 Method for long-distance epitaxial growth of transferable barium titanate single crystal film
CN110010769B (en) * 2019-03-26 2020-12-25 浙江大学 Preparation method of oriented growth organic-inorganic hybrid perovskite film
CN113371703A (en) * 2021-05-21 2021-09-10 西安交通大学 Graphene-improved silicon integrated energy storage thin film and preparation method thereof

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