CN109166790B - Method for stripping perovskite oxide piezoelectric film on graphene by using metal stress layer - Google Patents
Method for stripping perovskite oxide piezoelectric film on graphene by using metal stress layer Download PDFInfo
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- CN109166790B CN109166790B CN201810849986.8A CN201810849986A CN109166790B CN 109166790 B CN109166790 B CN 109166790B CN 201810849986 A CN201810849986 A CN 201810849986A CN 109166790 B CN109166790 B CN 109166790B
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Abstract
The invention discloses a method for stripping a perovskite oxide piezoelectric film on graphene by utilizing a metal stress layer, which comprises the following steps: 1) selecting a perovskite oxide piezoelectric film growing on the graphene layer; 2) selecting metal Cr as a metal stress layer material; 3) controlling the pressure of argon at 0.3-1.0 Pa in the growth process of the Cr metal stress layer; controlling the growth of the Cr metal stress layer to be 40-100W of low-power growth for 5-10 minutes, and then using 150-200W of high-power growth for 2 hours; 4) and 3) adhering the Cr stress layer/film/graphene/substrate with the adhesive tape obtained in the step 3), and tearing the adhesive tape off the substrate to realize the stripping of the piezoelectric film. In order to simply and conveniently prepare the high-quality perovskite oxide piezoelectric film on any flexible substrate, the separation of the perovskite oxide piezoelectric film is realized by utilizing weak van der Waals force formed by the contact of graphene and a three-dimensional material and a metal stress layer, and the transfer of the film is further completed.
Description
Technical Field
The invention relates to a method for stripping a perovskite oxide piezoelectric film grown on graphene by utilizing a metal stress layer.
Background
The film growth technology is a foundation stone of modern electronic products, and the realization of miniaturization and function diversification of devices of the electronic products does not depart from the development of the film technology. At present, people have increasingly strong demand for producing flexible electronic products, but the conventional film growth and processing means at present are difficult to meet the requirement of completing material integration on various flexible substrates. In order to integrate a functional oxide thin film, particularly an oxide piezoelectric thin film with a perovskite structure, on a flexible substrate, film growth is directly carried out on a substrate such as mica with flexibility, but the method limits an electronic device on a specific substrate such as mica, and various actual requirements are difficult to meet; one method is to grow a sacrificial layer which is easy to corrode on a hard substrate, then grow a thin film layer which is expected to meet the function of an electronic device on the sacrificial layer, corrode the sacrificial layer by using a corrosive liquid, so that the thin film floats on the corrosive liquid and is finally transferred to a flexible substrate.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for stripping a perovskite oxide piezoelectric film on graphene by using a metal stress layer, which can simply strip the perovskite oxide piezoelectric film from a substrate.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a method for stripping a perovskite oxide piezoelectric film on graphene by using a metal stress layer is characterized by comprising the following steps:
step 1: selecting a structure of an oxide/graphene/substrate growing on the graphene layer;
step 2: growing a Cr metal stress layer on the surface of the oxide/graphene/substrate structure by adopting a magnetron sputtering method to obtain a Cr metal stress layer/film/graphene/substrate structure;
and step 3: and (3) adhering the structure surface obtained by growth in the step (2) to an adhesive tape to form an adhesive tape/Cr metal stress layer/film/graphene/substrate structure, and peeling off the film by tearing off the adhesive tape.
The invention further improves the following steps:
in the step 1, the oxide/graphene/substrate structure is a perovskite oxide piezoelectric film, and the substrate and the perovskite oxide film are separated by graphene.
In step 2, the thickness of Cr metal as a stress layer is 1 μm.
In the step 2, the magnetron sputtering method comprises the following specific steps:
the sample and the Cr target material are put into a magnetron sputtering film growth cavity, and the air pressure in the vacuum cavity is pumped to 5 multiplied by 10-4Removing pollutants adsorbed on the surface of the film under Pa, introducing argon into the vacuum chamber, turning on a pulse power supply, controlling the power to be 40-100W, growing for 5-10 minutes, increasing the power to 150-200W, growing for 2 hours, introducing air into the chamber, and taking out a sample.
When argon is introduced into the vacuum cavity, the air pressure is controlled between 0.3Pa and 1.0 Pa.
Compared with the prior art, the invention has the following beneficial effects:
in order to simply and conveniently prepare the high-quality perovskite oxide piezoelectric film on any flexible substrate, the invention realizes the stripping of the perovskite oxide piezoelectric film by utilizing weak van der Waals force formed by the contact of graphene and a three-dimensional material and a metal stress layer. Compared with the prior art, the method can realize the stripping of the perovskite oxide piezoelectric film from any substrate, and provides possibility for realizing the integration of the perovskite oxide piezoelectric film on any substrate. According to the analysis of a Scanning Electron Microscope (SEM) and a Piezoelectric Force Microscope (PFM) of the prepared peeled solid film, the surface of the peeled solid film is flat and smooth; the release film has piezoelectricity.
Drawings
FIG. 1 is a schematic view of a peeling process in example 1;
FIG. 2 is a surface SEM image of an oxide film stripped in example 1;
FIG. 3 is a PFM graph of the oxide film stripped in example 1.
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 method for peeling the perovskite oxide piezoelectric film on the graphene by using the metal stress layer is characterized by comprising the following steps:
step 1: selecting a perovskite oxide piezoelectric film growing on the graphene layer, namely an oxide/graphene/substrate structure;
step 2: growing a Cr metal stress layer on the surface of the oxide/graphene/substrate structure by adopting a magnetron sputtering method to obtain a Cr metal stress layer/film/graphene/substrate structure; the thickness of Cr metal as a stress layer is 1 μm; the magnetron sputtering method comprises the following specific steps:
the sample and the Cr target material are put into a magnetron sputtering film growth cavity, and the air pressure in the vacuum cavity is pumped to 5 multiplied by 10-4Removing pollutants adsorbed on the surface of the film below Pa, introducing argon into the vacuum cavity, and controlling the air pressure to be between 0.3Pa and 1.0 Pa; turning on a pulse power supply, controlling the power to be 40-100W, growing for 5-10 minutes, and increasing the power to 150-20W0W, growing for 2 hours, introducing air into the cavity, and taking out a sample.
And step 3: and (3) adhering the structure surface obtained by growth in the step (2) to an adhesive tape to form an adhesive tape/Cr metal stress layer/film/graphene/substrate structure, and peeling off the film by tearing off the adhesive tape.
The Scanning Electron Microscope (SEM) and the Piezoelectric Force Microscope (PFM) analysis of the peeled solid film prepared by the invention determine that the peeled solid film has the following properties:
(1) the surface of the stripped film is flat and smooth;
(2) the release film has piezoelectricity.
Example 1
1) Selection of graphene-segregated SiO2Barium titanate (BaTiO) grown on Si substrate3BTO) thin films;
2) loading a sample and a Cr target material into a magnetron sputtering film growth cavity;
3) pumping the air pressure in the vacuum chamber to 5 × 10-4Removing pollutants adsorbed on the surface of the film below Pa;
4) introducing high-purity argon into the vacuum cavity, and controlling the air pressure to be 0.5 Pa;
5) turning on a pulse power supply, controlling the power at 50W, growing for 5 minutes, increasing the power to 150W, and growing for 2 hours;
6) closing the pulse power supply, introducing air into the cavity, and taking out the sample;
7) and 6) adhering an adhesive tape on the surface of the sample obtained in the step 6), and tearing the adhesive tape off the substrate to realize the peeling of the film.
The stripping process is illustrated as follows, as in fig. 1. As shown in fig. 2, the peeled film was observed by SEM, and it was found that the surface was flat and smooth. As shown in FIG. 3, a typical write domain pattern can be obtained by utilizing the compressive stress response of the film under PFM peeling, which indicates that the film has piezoelectricity.
Example 2
1) Selection of graphene-segregated SiO2Barium titanate (BaTiO) grown on Si substrate3BTO) thin films;
2) loading a sample and a Cr target material into a magnetron sputtering film growth cavity;
3) pumping the air pressure in the vacuum chamber to 5 × 10-4Removing pollutants adsorbed on the surface of the film below Pa;
4) introducing high-purity argon into the vacuum cavity, and controlling the air pressure to be 0.3 Pa;
5) turning on a pulse power supply, controlling the power at 40W, growing for 5 minutes, increasing the power to 150W, and growing for 2 hours;
6) closing the pulse power supply, introducing air into the cavity, and taking out the sample;
7) and 6) adhering an adhesive tape on the surface of the sample obtained in the step 6), and tearing the adhesive tape off the substrate to realize the peeling of the film.
Example 3
1) Selection of graphene-segregated SiO2Barium titanate (BaTiO) grown on Si substrate3BTO) thin films;
2) loading a sample and a Cr target material into a magnetron sputtering film growth cavity;
3) pumping the air pressure in the vacuum chamber to 5 × 10-4Removing pollutants adsorbed on the surface of the film below Pa;
4) introducing high-purity argon into the vacuum cavity, and controlling the air pressure to be 1.0 Pa;
5) turning on a pulse power supply, controlling the power at 100W, growing for 10 minutes, increasing the power to 200W, and growing for 2 hours;
6) closing the pulse power supply, introducing air into the cavity, and taking out the sample;
7) and 6) adhering an adhesive tape on the surface of the sample obtained in the step 6), and tearing the adhesive tape off the substrate to realize the peeling of the film.
Example 4
1) Selection of graphene-segregated SiO2Barium titanate (BaTiO) grown on Si substrate3BTO) thin films;
2) loading a sample and a Cr target material into a magnetron sputtering film growth cavity;
3) pumping the air pressure in the vacuum chamber to 5 × 10-4Removing pollutants adsorbed on the surface of the film below Pa;
4) introducing high-purity argon into the vacuum cavity, and controlling the air pressure to be 0.8 Pa;
5) turning on a pulse power supply, controlling the power at 60W, growing for 8 minutes, increasing the power to 180W, and growing for 2 hours;
6) closing the pulse power supply, introducing air into the cavity, and taking out the sample;
7) and 6) adhering an adhesive tape on the surface of the sample obtained in the step 6), and tearing the adhesive tape off the substrate to realize the peeling of the film.
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 method for stripping a perovskite oxide piezoelectric film on graphene by using a metal stress layer is characterized by comprising the following steps:
step 1: selecting a structure of an oxide/graphene/substrate growing on the graphene layer; the oxide/graphene/substrate is a perovskite oxide piezoelectric film, and the substrate and the perovskite oxide film are separated by graphene;
step 2: growing a Cr metal stress layer on the surface of the oxide/graphene/substrate structure by adopting a magnetron sputtering method to obtain a Cr metal stress layer/film/graphene/substrate structure; the thickness of Cr metal as a stress layer is 1 μm; the magnetron sputtering method comprises the following specific steps:
the sample and the Cr target material are put into a magnetron sputtering film growth cavity, and the air pressure in the vacuum cavity is pumped to 5 multiplied by 10-4Removing pollutants adsorbed on the surface of the film below Pa, introducing argon into the vacuum chamber, turning on a pulse power supply, controlling the power to be 40-100W, growing for 5-10 minutes, increasing the power to 150-200W, growing for 2 hours, introducing air into the chamber, and taking out a sample; controlling the air pressure between 0.3Pa and 1.0Pa when argon is introduced into the vacuum cavity;
and step 3: and (3) adhering the structure surface obtained by growth in the step (2) to an adhesive tape to form an adhesive tape/Cr metal stress layer/film/graphene/substrate structure, and peeling off the film by tearing off the adhesive tape.
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