CN113529032A - Preparation method of flexible lead zirconate titanate film - Google Patents

Preparation method of flexible lead zirconate titanate film Download PDF

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CN113529032A
CN113529032A CN202010321551.3A CN202010321551A CN113529032A CN 113529032 A CN113529032 A CN 113529032A CN 202010321551 A CN202010321551 A CN 202010321551A CN 113529032 A CN113529032 A CN 113529032A
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lead zirconate
zirconate titanate
deposition
film
transition layer
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徐小科
李效民
刘茜
周真真
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3457—Sputtering using other particles than noble gas ions
    • 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
    • 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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • 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
    • 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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
    • C23C14/025—Metallic sublayers
    • 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
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • 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
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/20—Metallic material, boron or silicon on organic substrates
    • 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
    • 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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/28—Vacuum evaporation by wave energy or particle radiation

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Abstract

The invention discloses a preparation method of a flexible lead zirconate titanate film, which is characterized in that a metal platinum transition layer is deposited on a flexible substrate before the lead zirconate titanate film is deposited, the deposition mode of the lead zirconate titanate film is magnetron sputtering, and the deposition temperature of the lead zirconate titanate film is 160-200 ℃.

Description

Preparation method of flexible lead zirconate titanate film
Technical Field
The invention relates to a preparation method of a flexible lead zirconate titanate film, belongs to the field of piezoelectric materials, and particularly relates to a preparation method of a low-temperature deposited polycrystalline lead zirconate titanate film on a flexible substrate.
Background
The piezoelectric material is a material with piezoelectric effect, and the material can generate an electric signal under the action of pressure or generate mechanical deformation under the action of an electric field, so that the piezoelectric material can be widely applied to multiple fields such as transducers, drivers, piezoelectric sensors and the like. The piezoelectric material comprises an inorganic piezoelectric material and an organic piezoelectric material, wherein the inorganic piezoelectric material is represented by barium titanate and lead zirconate titanate and has the characteristics of strong piezoelectricity and high dielectric constant, and the organic piezoelectric material is represented by polyvinylidene fluoride (PVDF) and has the advantages of good flexibility, low density, low impedance and the like.
In recent years, electronic devices are being flexible and wearable, which brings new opportunities for application of piezoelectric materials and also faces new challenges. On one hand, the frequent deformation of the flexible electronic device can lead the piezoelectric material to have more chances to generate and store electric energy, thereby becoming a new hotspot research direction in the field of energy research; on the other hand, because the traditional inorganic piezoelectric material mainly comprises crystals and ceramics, the preparation process of the traditional inorganic piezoelectric material usually needs a crystallization temperature of more than 500 ℃, and the crystallization temperature cannot be effectively combined with the process temperature below 200 ℃ needed by the flexible electronic device process, while the organic piezoelectric material can be obtained at a lower temperature, but has the defects of low piezoelectric strain constant, high driving voltage and the like, and the performance is usually not satisfactory. Therefore, how to obtain an inorganic flexible piezoelectric material with good crystallinity at a relatively low temperature is a significant problem in the field of current piezoelectric materials.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a method for preparing a flexible lead zirconate titanate thin film, wherein before depositing the lead zirconate titanate thin film, a metal platinum transition layer is deposited on a flexible substrate, the deposition manner of the lead zirconate titanate thin film is magnetron sputtering, and the deposition temperature of the lead zirconate titanate thin film is 160 to 200 ℃.
The method prepares a transition layer of metal platinum between a flexible substrate and the lead zirconate titanate film, and the transition layer not only can be used as a bottom electrode of a flexible piezoelectric device, but also can induce the lead zirconate titanate film to crystallize at a lower temperature.
Preferably, the deposition mode of the metal platinum transition layer comprises pulsed laser deposition, magnetron sputtering and electron beam evaporation, and preferably pulsed laser deposition.
Preferably, the deposition temperature of the metal platinum transition layer is room temperature to 200 ℃.
Preferably, the thickness of the platinum transition layer is 25 to 100 nm.
Preferably, the target material for depositing the lead zirconate titanate film is Pb (Zr) with 5-20% excess Pb element0.52Ti0.48)O3A target material.
Preferably, the sputtering power density is 8-15 w/cm in the deposition process of the lead zirconate titanate film2Ar and O2The flow ratio of (3): 1-1: 1, the deposition pressure is 0.5-3 Pa, and the deposition time is 1-5 hours.
Preferably, the thickness of the lead zirconate titanate thin film is 200 to 500 nm.
Preferably, the flexible substrate is any one of a polyimide film and a polyethylene terephthalate film.
Preferably, the flexible substrate is pretreated before the metal platinum transition layer is deposited, and the pretreatment step comprises organic solvent cleaning and deionized water cleaning.
Preferably, the pretreatment step further comprises an oxygen plasma surface treatment.
The method has the advantages that the whole preparation process flow has no process condition of more than 200 ℃, so that adverse factors such as deformation, embrittlement and the like of the flexible substrate at high temperature can be avoided, the process is simple and feasible, and the prepared lead zirconate titanate film has good density, high crystallization degree, strong bonding force and excellent piezoelectric performance.
Drawings
FIG. 1 is a sample of a flexible lead zirconate titanate film obtained in example 1 of the present invention;
FIG. 2 is an X-ray diffraction pattern of a flexible lead zirconate titanate thin film obtained in example 2 of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
The following is an exemplary description of the method for preparing the flexible lead zirconate titanate thin film according to the present invention.
First, a suitable flexible substrate is selected and pre-processed. Common flexible substrates comprise polyethylene terephthalate (PET) and Polyimide (PI), the two of which can bear the process temperature of about 200 ℃, wherein the PET is colorless and transparent and can be used for photoelectric functional devices, the PI has better thermal stability, and piezoelectric functional layers with better performance can be obtained. In some embodiments, the thickness of the polyimide film may be 25 to 100 μm, and the thickness of the polyethylene terephthalate film may be 100 to 200 μm.
The pretreatment of the substrate is generally the cleaning of organic solvent and deionized water. For example, ultrasonic cleaning is performed for 5 minutes with acetone, ethanol, and deionized water, respectively.
For flexible substrates, it is preferred to bombard the surface of the substrate with plasma to reduce its surface energy in order to enhance the bonding force between the substrate and the film. In some embodiments, the pretreatment steps of the flexible substrate before deposition sequentially comprise organic solvent cleaning, deionized water cleaning and oxygen plasma surface treatment. For example, the substrate surface is ultrasonically cleaned with acetone, ethanol, and deionized water for 5 minutes, respectively, and then bombarded with oxygen plasma generated by an oxygen plasma generator. The bias voltage of the oxygen plasma surface treatment can be 1500-2300V, the bombardment time can be 0.5-5 minutes, and the oxygen flow can be 5-20 mL/min.
Next, a metal platinum transition layer is deposited on the flexible substrate. The thickness of the metal platinum transition layer can be 25-100 nm.
The deposition method of the metal platinum transition layer can be a physical deposition method such as pulse laser deposition, magnetron sputtering, electron beam evaporation and the like. Preferably, the deposition mode is pulsed laser deposition. In some embodiments, the laser energy is 160mJ, the laser frequency is 3-5 Hz, and the backing vacuum pressure is not higher than 5 × 10-4Pa, and the deposition time is 0.2-1 hour.
The deposition temperature of the metal platinum transition layer can be room temperature to 200 ℃. In some embodiments, the deposition temperature is room temperature. In some embodiments, the deposition temperature is 100 to 200 ℃.
And then, depositing the lead zirconate titanate film layer by adopting a magnetron sputtering method. The target material component for magnetron sputtering is Pb (Zr)0.52Ti0.48)O3And the Pb element is excessive by 5-20% so as to prevent the deviation of the stoichiometric ratio caused by Pb volatilization in the sputtering process.
The deposition temperature of the lead zirconate titanate thin film can be 160-200 ℃. The invention can be used as a bottom electrode of a flexible piezoelectric device and can induce the lead zirconate titanate film to crystallize at a lower temperature by constructing the metal platinum transition layer. The reasons are the following two points: firstly, the metal platinum and the lead zirconate titanate are both in a cubic crystal system and have close lattice constants, and a lattice matching relationship exists, so that the lead zirconate titanate film can be induced to crystallize; secondly, the crystallization of the material needs a certain amount of energy, and platinum, as a common catalytic material, may play a certain activating role in the film formation process of lead zirconate titanate to promote the transition of the lead zirconate titanate to the crystalline state.
In some embodiments, the process parameters for magnetron sputtering the lead zirconate titanate thin film may be: the sputtering power density is 8-15 w/cm2Ar and O2The flow ratio of (2): 1, the deposition pressure is 0.5-3 Pa, and the deposition time is 1-5 hours.
The preparation method of the flexible lead zirconate titanate film adopts a laminated film type structure, firstly deposits a platinum transition layer on a flexible substrate, and then deposits a lead zirconate titanate film layer, which is a layer-by-layer physical deposition mode. In addition, the present invention addresses primarily low temperature deposition of lead zirconate titanate films on flexible substrates to meet the requirements of ferroelectric loudspeaker applications alike. It is noted that the present invention does not need to use metal (e.g. platinum) nanoparticles dispersed in the lead zirconate titanate thin film, but rather, can realize the purpose of inducing the crystallization of the lead zirconate titanate thin film at a lower temperature by preparing an important buffer layer of the lead zirconate titanate ferroelectric layer, namely a platinum layer, at a low temperature and using the platinum layer as an indispensable functional layer.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1
The preparation method of the flexible lead zirconate titanate film comprises the following steps:
(1) using a polyimide film with the thickness of 25 mu m as a substrate, sequentially using acetone, ethanol and deionized water to perform ultrasonic cleaning for 5 minutes respectively, then bombarding the surface of the substrate by using oxygen plasma generated by an oxygen plasma generator, wherein the voltage is 2000V, the bombardment time is 2 minutes, and the oxygen flow is 5-20 mL/min;
(2) depositing a metal platinum transition layer on a polyimide substrate by adopting a pulse laser deposition method, wherein the adopted laser is a 248nm helium-neon excimer laser, the laser energy is 160mJ, the laser frequency is 5Hz, and the back bottom vacuum is 5 multiplied by 10-4Pa, the substrate temperature is room temperature, the deposition time is 1 hour, and the thickness of the obtained metal platinum transition layer is 30 nm;
(3) continuously depositing a lead zirconate titanate piezoelectric functional layer by adopting a magnetron sputtering method, wherein the substrate temperature is 180 ℃, the deposition pressure is 1Pa, the Ar flow is 10sccm, and O is2The flow rate is 5sccm, and the sputtering power density is 10w/cm2The deposition time was 3 hours.
Fig. 1 is a schematic diagram of a sample obtained in this example, in which a polyimide substrate is in a dark yellow color, a platinum transition layer is formed on the polyimide substrate in a silver white color, and a lead zirconate titanate piezoelectric functional layer is formed in a square portion in a green color in the middle. The substrate is polyimide, a metal platinum transition layer is uniformly covered on the polyimide, and the middle square part is a lead zirconate titanate piezoelectric function layer. As can be seen, each film layer of the obtained sample is dense and glossy, is well combined with the substrate, has no sign of shedding or cracking when the substrate is bent, and can be used for flexible devices.
Example 2
The preparation method of the flexible lead zirconate titanate film comprises the following steps:
(1) taking a polyimide film with the thickness of 50 mu m as a substrate, and sequentially ultrasonically cleaning the substrate for 5 minutes by using acetone, ethanol and deionized water;
(2) depositing a metal platinum transition layer on a polyimide substrate by adopting a pulse laser deposition method, wherein the adopted laser is a 248nm helium-neon excimer laser, the laser energy is 160mJ, the laser frequency is 5Hz, and the back bottom vacuum is 5 multiplied by 10-4Pa, the substrate temperature is 200 ℃, the deposition time is 1.5 hours, and the thickness of the obtained metal platinum transition layer is 50 nm;
(3) continuously depositing the lead zirconate titanate piezoelectric functional layer by adopting a magnetron sputtering method, wherein the substrate temperature is 200 ℃, the deposition pressure is 2Pa, the Ar flow is 10sccm, the O2 flow is 5sccm, and the sputtering power density is 12w/cm2The deposition time was 4 hours.
FIG. 2 is an X-ray diffraction pattern of a sample obtained in this example, in which the low-angle broad peak is derived from substrate polyimide and the rest are diffraction peaks of a lead zirconate titanate thin film. By comparison with the PDF # card, it can be seen that the diffraction peaks of lead zirconate titanate include a plurality of orientations such as (111), (200), (220), (311), indicating that the lead zirconate titanate thin film is a polycrystalline thin film and the full width at half maximum of each diffraction peak is narrow, indicating that the degree of crystallization of lead zirconate titanate is high.
The above description is illustrative of the present invention and is not intended to be limiting, and other embodiments based on the spirit of the present invention are within the scope of the present invention.

Claims (10)

1. The preparation method of the flexible lead zirconate titanate film is characterized in that a metal platinum transition layer is deposited on a flexible substrate before the lead zirconate titanate film is deposited, the deposition mode of the lead zirconate titanate film is magnetron sputtering, and the deposition temperature of the lead zirconate titanate film is 160-200 ℃.
2. The preparation method according to claim 1, wherein the metal platinum transition layer is deposited by pulsed laser deposition, magnetron sputtering, electron beam evaporation, preferably pulsed laser deposition.
3. The method according to claim 1 or 2, wherein the deposition temperature of the metal platinum transition layer is room temperature to 200 ℃.
4. The method according to any one of claims 1 to 3, wherein the thickness of the metal platinum transition layer is 25 to 100 nm.
5. The method according to any one of claims 1 to 4, wherein the target material for depositing the lead zirconate titanate thin film is Pb (Zr) with 5 to 20 percent excess Pb element0.52Ti0.48)O3A target material.
6. The method according to any one of claims 1 to 5, wherein a sputtering power density during the deposition of the lead zirconate titanate thin film is 8 to 15w/cm2Ar and O2The flow ratio of (3): 1-1: 1, the deposition pressure is 0.5-3 Pa, and the deposition time is 1-5 hours.
7. The method according to any one of claims 1 to 6, wherein the thickness of the lead zirconate titanate thin film is 200 to 500 nm.
8. The production method according to any one of claims 1 to 7, wherein the flexible substrate is any one of polyimide and polyethylene terephthalate.
9. The preparation method according to any one of claims 1 to 8, wherein the flexible substrate is subjected to pretreatment before the metal platinum transition layer is deposited, and the pretreatment comprises organic solvent cleaning and deionized water cleaning.
10. The method of claim 9, wherein the pre-treating step further comprises an oxygen plasma surface treatment.
CN202010321551.3A 2020-04-22 2020-04-22 Preparation method of flexible lead zirconate titanate film Pending CN113529032A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1779923A (en) * 2005-09-23 2006-05-31 中国科学院上海技术物理研究所 Production of thin-film ferroelectric materials with lead zirconate-titanate with reading circuit integration
JP2007154275A (en) * 2005-12-07 2007-06-21 Canon Inc Deposition method and thin piezoelectric substance film
CN102157682A (en) * 2010-11-25 2011-08-17 南京理工大学 One-phase ferroelectric film and preparing method thereof as well as effective resistance regulation mode
CN108517503A (en) * 2018-05-22 2018-09-11 苏州大学 A kind of preparation method of PZT thin film

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1779923A (en) * 2005-09-23 2006-05-31 中国科学院上海技术物理研究所 Production of thin-film ferroelectric materials with lead zirconate-titanate with reading circuit integration
JP2007154275A (en) * 2005-12-07 2007-06-21 Canon Inc Deposition method and thin piezoelectric substance film
CN102157682A (en) * 2010-11-25 2011-08-17 南京理工大学 One-phase ferroelectric film and preparing method thereof as well as effective resistance regulation mode
CN108517503A (en) * 2018-05-22 2018-09-11 苏州大学 A kind of preparation method of PZT thin film

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
曾晟等: "溅射工艺参数对PZT铁电薄膜相变过程的影响", 《无机材料学报》 *

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