CN110660583A - Thin film capacitor - Google Patents

Thin film capacitor Download PDF

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CN110660583A
CN110660583A CN201811196824.5A CN201811196824A CN110660583A CN 110660583 A CN110660583 A CN 110660583A CN 201811196824 A CN201811196824 A CN 201811196824A CN 110660583 A CN110660583 A CN 110660583A
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film
strontium titanate
energy storage
thin film
dielectric
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CN110660583B (en
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冯雪
王志建
陈颖
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Tsinghua University
Institute of Flexible Electronics Technology of THU Zhejiang
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Tsinghua University
Institute of Flexible Electronics Technology of THU Zhejiang
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/018—Dielectrics
    • H01G4/06—Solid dielectrics
    • H01G4/08—Inorganic dielectrics
    • H01G4/12—Ceramic dielectrics
    • H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
    • H01G4/1218—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates
    • H01G4/1227—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates based on alkaline earth titanates
    • 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
    • C23C14/088—Oxides of the type ABO3 with A representing alkali, alkaline earth metal or Pb and B representing a refractory or rare earth metal
    • 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
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/005—Electrodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/33—Thin- or thick-film capacitors 
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13—Energy storage using capacitors

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  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The present invention relates to a film capacitor. The thin film capacitor comprises a dielectric thin film and an electrode layer, wherein the dielectric thin film comprises a flexible metal substrate and a strontium titanate thin film formed on the flexible metal substrate, and the electrode layer is formed on the strontium titanate layer. The dielectric film of the film capacitor is a ceramic film, has high dielectric constant, low dielectric loss, high breakdown field strength and high energy storage density, has good flexibility, and can replace a high molecular film to be used as the dielectric film of the film capacitor, thereby promoting the development of the film capacitor towards the trend of miniaturization, lightness and thinness, high integration and multiple functions.

Description

Thin film capacitor
The application is that the application number is: 201810713410.9, having application date of 2018, 6 and 29, and having the name of: the invention discloses a flexible energy storage film, a preparation method thereof and a divisional application of the invention application of a film capacitor.
Technical Field
The invention relates to the field of energy sources, in particular to a film capacitor.
Background
With the gradual trend toward miniaturization, multi-functionality, and light weight of electronic devices, electronic components constituting the electronic devices also need to be developed toward miniaturization, light weight, high integration, and multi-functionality.
For a thin film capacitor, a desirable approach to achieve miniaturization is to increase the capacitance by increasing the dielectric constant of the dielectric thin film. The dielectric film mainly comprises a high-molecular energy storage film and a ceramic energy storage film, and in the traditional film capacitor, the used dielectric film is mainly the high-molecular energy storage film. Because the dielectric constant of the ceramic energy storage film is far higher than that of the polymer energy storage film, the ceramic energy storage film is used for replacing the polymer energy storage film, and the development trend of the film capacitor is met. However, ceramic energy storage films lack the flexibility of polymeric energy storage films.
Disclosure of Invention
In view of the above, it is necessary to provide a thin film capacitor in response to the problem of the dielectric thin film of the thin film capacitor; the dielectric film of the film capacitor is a ceramic film, and thus the development of the film capacitor toward miniaturization, lightness, thinness, high integration and multi-functionalization is promoted.
A thin film capacitor includes a dielectric thin film including a flexible metal substrate and a strontium titanate thin film formed on the flexible metal substrate, and an electrode layer formed on the strontium titanate layer.
In one embodiment, the minimum bending radius of the dielectric film is 2 mm-20 mm; and/or
The dielectric constant of the dielectric film is 280-310; and/or
The dielectric loss of the dielectric film is 0.003-0.05; and/or
The breakdown field strength of the dielectric film is 1000 kV/cm-3000 kV/cm; and/or
The energy storage density of the dielectric film is 12J/cm3～55J/cm3。
In one embodiment, the thickness of the strontium titanate film is 10 nm-2 μm, and the grain size is 30 nm-500 nm.
In one embodiment, the thickness of the flexible metal substrate is 12-18 μm; and/or
The surface roughness of the flexible metal substrate is 0.4-0.8 μm; and/or
The surface tension of the flexible metal substrate is more than or equal to 60 dynes; and/or
The flexible metal substrate includes a copper foil.
In one embodiment, the thickness of the electrode layer is 100nm to 3 μm.
In one embodiment, the sheet resistance of the electrode layer is 0.001 mO/□ -0.5 omega/□.
In one embodiment, the material of the electrode layer comprises at least one of copper, platinum, gold, silver, and aluminum.
The dielectric film is a ceramic film, has high dielectric constant, low dielectric loss, high breakdown field strength and high energy storage density, has good flexibility, and can replace a high polymer film to be used as the dielectric film of the film capacitor, so that the development of the film capacitor towards the trend of miniaturization, lightness and thinness, high integration and multiple functions can be promoted. Meanwhile, the film capacitor has the advantages of no polarity, high insulation resistance, excellent frequency characteristics (wide frequency response), small dielectric loss and the like. The method can be applied to a plurality of industries such as electronics, household appliances, communication, electric power, electrified railways, new energy vehicles, wind power generation, solar power generation and the like. Especially in the signal cross connection part, the thin film capacitor with good frequency characteristic and low dielectric loss of the invention can ensure that the signal is not distorted too much when being transmitted, and has good electrical performance and high reliability.
Drawings
FIG. 1 is a flow chart of a process for preparing a flexible energy storage thin film according to the present invention, wherein (a) is a flexible metal substrate, (b, c) is a strontium titanate thin film formed on the flexible metal substrate, and (d) is an electrode layer formed on the strontium titanate thin film;
fig. 2 is a schematic diagram of the energy storage thin films of example 1, example 10 and comparative example 1 of the present invention, in which (g) is the flexible energy storage thin film of example 1, (f) is the flexible energy storage thin film of example 10, and (e) is the strontium titanate energy storage thin film of comparative example 1.
Detailed Description
The thin film capacitor provided by the present invention will be further explained below.
As shown in fig. 1, the preparation method of the flexible energy storage thin film provided by the invention comprises the following steps:
(a) providing a flexible metal substrate;
(b) depositing a strontium titanate film prefabricated layer on the flexible metal substrate by using a magnetron sputtering method by taking strontium titanate as a target material;
(c) carrying out heat treatment on the flexible metal substrate deposited with the strontium titanate film prefabricated layer to obtain a strontium titanate film; and
(d) and forming an electrode layer on the strontium titanate film to obtain the flexible energy storage film.
In the step (a), the flexible metal substrate is not limited to any material, as long as the flexible metal substrate has good flexibility, strong high-temperature oxidation resistance, conductivity and no reaction with the ceramic film, and the flexible metal substrate comprises one of Pt, Au, Ag, Cu, Ni, Ti and Al.
Considering that copper foil is the most cost-effective metal material in the field of electronics industry, its resistivity is 1.75X 10-8Omega. m, second only to silver (1.65X 10)-8Ω · m), a thermal conductivity 401W/(m · K), second only to silver (420W/(m · K)), while the price of copper is far greaterLower than the price of silver. Secondly, industrial copper foil is mature, the copper foil is divided into rolled copper foil and electrolytic copper foil, and the rolled copper foil and the electrolytic copper foil are both subjected to electroplating treatment to prevent oxidation and high-temperature oxidation resistance, and cannot be oxidized when being calcined in air at 400-500 ℃. Therefore, the flexible metal substrate is preferably a copper foil.
Further, the rolled copper foil is composed of rod-shaped grains parallel to the surface of the copper foil and has superior bending resistance, and the electrolytic copper foil is composed of rod-shaped grains perpendicular to the surface of the copper foil and has lower bending resistance than the rolled copper foil, and therefore, the copper foil is preferably a rolled copper foil.
The thinner the flexible substrate is, the better the flexibility is, and therefore, the thickness of the flexible substrate is 12 to 18 μm, and more preferably, a rolled copper foil of 12 μm.
In the film capacitor, the flexible substrate is used as an electrode, the actual contact area of the strontium titanate film and the electrode is related to the surface roughness of the flexible substrate, and the larger the surface roughness is, the larger the actual contact area is, and the larger the capacitance value per unit geometric area is. However, the surface roughness of the flexible substrate is too large, which easily causes the generation of holes on the surface of the strontium titanate film and affects the energy storage performance of the flexible energy storage film. Therefore, the surface roughness of the flexible substrate is 0.4 μm to 0.8 μm.
The surface tension of the flexible substrate is more than or equal to 60 dynes, preferably more than 60 dynes, and the higher the surface tension of the flexible substrate is, the stronger the bonding force between the strontium titanate film and the flexible substrate is.
The surface activity can be increased by treating the surface of the flexible substrate, thereby increasing the surface tension. Preferably, the treatment method comprises the following steps: the method comprises the steps of heating a flexible substrate, setting the temperature to be 100-300 ℃, preserving heat for 10-30 minutes, and then processing the flexible substrate by using a Hall ion source, wherein the voltage of the Hall ion source is 800-2000V, the current is 0.5-2A, and the processing time is 1-10 min.
And (b) depositing a strontium titanate film prefabricated layer on the flexible metal substrate by adopting a magnetron sputtering process. The ions which spirally move at high speed under the action of an electric field and a magnetic field bombard the strontium titanate target material, and atoms or ion groups bombarded from the strontium titanate target material are deposited on the flexible metal substrate to form a strontium titanate film prefabricated layer. Because the magnetron sputtering particles have energy as high as 1eV to 10eV, and can maintain higher surface mobility on the surface of the flexible metal substrate, the formed strontium titanate film prefabricated layer has better crystallization performance and high deposition efficiency, the temperature of the flexible metal substrate required for forming the strontium titanate film prefabricated layer is lower, and the compatibility with an integration process is better.
Compared with PLD, sol-gel and hydrothermal methods and the like, the method for forming the strontium titanate film prefabricated layer on the flexible metal substrate by deposition through the magnetron sputtering process has the advantages of high deposition efficiency, good film forming crystallinity and the like, and is beneficial to improving the energy storage performance of the flexible energy storage film. And the whole process is a physical process, and oxygen cooling protection is not needed when film forming is finished, so that the flexible metal substrate is protected from being oxidized and has high conductivity.
If the compactness of the strontium titanate target material is not high, the surface and the inner air holes of the strontium titanate target material are more, and the strontium titanate target material is easy to generate microcracks under the action of high pressure and high temperature during magnetron sputtering, and the microcracks are expanded to cause the cracking of the strontium titanate target material. Therefore, the compactness of the strontium titanate target is preferably equal to or more than 96 percent, and more preferably more than 96 percent, so that the target is convenient for magnetron sputtering and works stably.
In the magnetron sputtering process, the working atmosphere of the magnetron sputtering is argon, the flow rate of the argon is 30 sccm-120 sccm, and the vacuum degree is 0.1 Pa-0.5 Pa. The magnetron sputtering power is 50W-200W, and the deposition time is 1 min-60 min.
Furthermore, the thickness of the deposited strontium titanate film prefabricated layer is 30 nm-3 μm, the grain size is 10 nm-450 nm, and the film structure is compact.
In the step (c), the flexible metal substrate deposited with the strontium titanate thin film pre-fabricated layer is subjected to a heat treatment, which is an annealing heat treatment. When annealing at 300-400 deg.C, SrTiO3Sr, Ti and O atoms in the ceramic can exchange energy with each other by virtue of lattice vibration, and some atoms in distorted positions can be restored to be positiveNormal state, and thus internal stress is reduced accordingly. When annealing is carried out at 400 ℃ to 500 ℃, the mobility of Sr, Ti and O atoms is increased, so that some vacancies, interstitial atoms and dislocations which are originally frozen are recombined in the film, or move to the surface and grain boundaries to disappear, or are combined into a defect configuration with lower energy (such as dislocation loops, vacancy clusters and the like). In this case, the internal stress of the film will be greatly reduced. When annealing is carried out at 500-600 ℃, the diffusion of Sr, Ti and O atoms is intensified, the frozen defects can be further eliminated, and various recrystallization can also occur, so that the grain boundary is reduced, and the internal stress of the film is obviously reduced. Preferably, the temperature of the heat treatment of the invention is 300-600 ℃ and the time is 20-60 minutes. By adopting annealing heat treatment at different temperatures and for different time, the non-equilibrium defects such as lattice mismatch, lattice reconstruction, impurities, phase change and the like in the strontium titanate film prefabricated layer disappear greatly, and the strontium titanate film is obtained. Compared with the strontium titanate film prefabricated layer, the internal stress of the strontium titanate film is obviously reduced.
Preferably, oxygen is introduced during the heat treatment, the flow rate of the oxygen is 30sccm to 150sccm, and the vacuum degree is 0.1Pa to 1 Pa. The oxygen can eliminate oxygen vacancy generated in the deposition process of the strontium titanate ceramic film, and can further reduce the defects of the strontium titanate ceramic film.
In the step (d), the electrode layer can be formed by deposition through a magnetron sputtering process, namely, the electrode layer is formed by deposition on the strontium titanate film through the magnetron sputtering process after the heat treatment, and the working efficiency is high.
Considering that the thinner the electrode layer is, the higher the sheet resistance of the electrode layer is, and correspondingly, the higher the voltage resistance of the electrode layer is; the thicker the electrode layer, the lower the sheet resistance of the electrode layer, and correspondingly, the higher the current resistance of the electrode layer. Moreover, the thinner the electrode layer, the more easily it is oxidized, resulting in a loss of capacity; the thicker the electrode layer is, the lower the voltage resistance of the electrode layer is, resulting in the electrode layer being easily broken down. Preferably, the thickness of the electrode layer is 100nm to 3 μm, and the sheet resistance of the electrode layer is 0.001 mOhm/□ to 0.5 Ohm/□.
Preferably, the material of the electrode layer includes at least one of copper, platinum, gold, silver, and aluminum, and is more preferably copper.
According to the invention, the flexible metal substrate is adopted, the strontium titanate film is formed on the flexible metal substrate through the magnetron sputtering process, and then the electrode layer is formed on the strontium titanate film to form the ceramic energy storage film, so that the ceramic energy storage film is not only flexible, but also high in preparation efficiency, good in microstructure such as crystallinity and grain size and low in internal stress, and the energy storage performance of the flexible energy storage film is improved.
The invention also provides a flexible energy storage film which comprises a flexible metal substrate, and a strontium titanate film and an electrode layer which are sequentially formed on the flexible metal substrate.
The thickness of the strontium titanate film is 10 nm-2 mu m, and the grain size is 30-500 nm; the thickness of the electrode layer is 100 nm-3 mu m.
The flexible metal substrate comprises a copper foil, and the thickness of the copper foil is 12-18 mu m; and/or
The surface roughness of the copper foil is 0.4-0.8 μm; and/or
The surface tension of the copper foil is not less than 60 dyne.
The minimum bending radius of the flexible energy storage film is 2-20 mm; and/or
The dielectric constant of the flexible energy storage film is 280-310; and/or
The dielectric loss of the flexible energy storage film is 0.003-0.05; and/or
The breakdown field strength of the flexible energy storage film is 1000 kV/cm-3000 kV/cm; and/or
The energy storage density of the flexible energy storage film is 12J/cm3～55J/cm3。
The energy storage film is composed of a flexible metal substrate, a strontium titanate material and an electrode layer, not only is the flexibility of the energy storage film realized, but also the energy storage film has high dielectric constant, low dielectric loss, high breakdown field strength and high energy storage density.
The invention also provides a film capacitor, which comprises the flexible energy storage film.
The flexible energy storage film provided by the invention is used for replacing a high polymer film, and the development of a film capacitor towards the trends of miniaturization, lightness, thinness, high integration and multiple functions can be promoted. Meanwhile, the film capacitor has the advantages of no polarity, high insulation resistance, excellent frequency characteristics (wide frequency response), small dielectric loss and the like. The method can be applied to a plurality of industries such as electronics, household appliances, communication, electric power, electrified railways, new energy vehicles, wind power generation, solar power generation and the like. Especially in the signal cross connection part, the thin film capacitor with good frequency characteristic and low dielectric loss of the invention can ensure that the signal is not distorted too much when being transmitted, and has good electrical performance and high reliability.
Hereinafter, the film capacitor will be further described by the following specific examples.
Example 1:
as shown in FIG. 1, a rolled copper foil having a thickness of 18 μm and a surface roughness of 0.5 μm was placed in a vacuum chamber and evacuated to a vacuum of 3X 10-3Pa. The vacuum chamber is heated to 150 ℃, the heat preservation time is 10min, argon is filled, and the flow of the argon is 30 sccm. And (3) opening the Hall ion source, setting the voltage of the Hall ion source to be 1000v and the current to be 0.5A, and treating for 1min to enable the surface tension of the copper foil to reach 60 dynes.
Closing the gate valve until the vacuum degree is 0.4Pa, keeping the argon flow at 30sccm, starting a magnetron sputtering power supply to 80w, taking strontium titanate with the density of 96% as a target material, depositing for 3 minutes, and forming a strontium titanate film prefabricated layer with the grain size of 130nm on the copper foil, wherein the grain size of the strontium titanate film prefabricated layer is 80nm, and the structure is compact.
And (3) closing the argon, filling oxygen, ensuring the vacuum degree to be 0.1Pa, setting the heating temperature to be 300 ℃, and keeping the temperature for 30min, wherein the oxygen flow is 30 sccm.
And (3) closing an oxygen valve, opening an argon valve, ensuring the vacuum degree to be 0.4Pa, opening a magnetron sputtering power supply, setting magnetron sputtering current 4A, taking metal copper as a target material, depositing for 10 minutes to form a copper electrode layer, wherein the thickness of the copper electrode layer is 100nm, and the sheet resistance is 0.5 omega/□, so as to obtain the flexible energy storage film shown in (g) in figure 2.
Tests prove that the thickness of the strontium titanate film in the obtained flexible energy storage film is 100nm, the minimum bending radius of the flexible energy storage film is 4mm, the grain size is 120nm, the dielectric constant is 300, the dielectric loss is 0.008, the breakdown field strength is 1800kV/cm, and the energy storage density is 30J/cm3The method can be applied to film capacitors.
Example 2:
as shown in FIG. 1, a rolled copper foil as a substrate, which had a thickness of 12 μm and a surface roughness of 0.5 μm, was placed in a vacuum chamber and evacuated to a vacuum of 3X 10-3Pa. The vacuum chamber is heated to 150 ℃, the heat preservation time is 10min, argon is filled, and the flow of the argon is 30 sccm. And opening the Hall ion source, setting the voltage of the Hall ion source to be 1000v and the current to be 0.5A, and treating for 1min to enable the surface tension of the copper foil to reach 65 dynes.
Closing the gate valve until the vacuum degree is 0.4Pa, keeping the argon flow at 30sccm, starting a magnetron sputtering power supply to 80w, taking strontium titanate with the density of 97% as a target material, depositing for 4 minutes, and forming a 150nm strontium titanate film prefabricated layer on the copper foil, wherein the grain size of the strontium titanate film prefabricated layer is 80nm, and the structure is compact.
And (3) closing the argon, filling oxygen with the flow rate of 60sccm, ensuring the vacuum degree to be 0.2Pa, setting the heating temperature to be 350 ℃, and keeping the temperature for 60 min.
And closing an oxygen valve, opening an argon valve, ensuring the vacuum degree to be 0.4Pa, opening a magnetron sputtering power supply, setting magnetron sputtering current 4A, taking metal copper as a target material, depositing for 10 minutes to form a copper electrode layer, wherein the thickness of the copper electrode layer is 500nm, and the sheet resistance is 0.1 omega/□, thus obtaining the flexible energy storage film.
Tests prove that the thickness of the strontium titanate film in the obtained flexible energy storage film is 120nm, the minimum bending radius of the flexible energy storage film is 3mm, the grain size is 100nm, the dielectric constant is 300, the dielectric loss is 0.008, the breakdown field strength is 1800kV/cm, and the energy storage density is 30J/cm3The method can be applied to film capacitors.
Example 3:
as shown in FIG. 1, a rolled copper foil was used as a substrate, and the copper foil had a thickness of 12 μmRice with surface roughness of 0.4 μm, placing in vacuum chamber, and vacuumizing to 3 × 10-3Pa. The vacuum chamber is heated to 150 ℃, the heat preservation time is 10min, argon is filled, and the flow of the argon is 50 sccm. And (3) opening the Hall ion source, setting the voltage of the Hall ion source to be 1000v and the current to be 0.5A, and treating for 5min to enable the surface tension of the copper foil to reach 60 dynes.
Closing the gate valve until the vacuum degree is 0.2Pa, keeping the argon flow at 50sccm, starting a magnetron sputtering power supply to 120w, taking strontium titanate with the density of 98% as a target material, depositing for 1 minute, and forming a 60nm strontium titanate film prefabricated layer on the copper foil, wherein the grain size of the strontium titanate film prefabricated layer is 120nm, and the structure is compact.
And (3) closing the argon, filling oxygen with the flow rate of 120sccm, ensuring the vacuum degree to be 0.6Pa, setting the heating temperature to be 360 ℃, and keeping the temperature for 60 min.
And closing an oxygen valve, opening an argon valve, ensuring the vacuum degree to be 0.4Pa, opening a magnetron sputtering power supply, setting magnetron sputtering current 4A, taking metal copper as a target material, depositing for 10 minutes to form a copper electrode layer, wherein the thickness of the copper electrode layer is 1 mu m, and the sheet resistance is 0.05 omega/□, thus obtaining the flexible energy storage film.
Tests prove that the thickness of the strontium titanate film in the obtained flexible energy storage film is 50nm, the minimum bending radius of the flexible energy storage film is 2.5mm, the grain size is 140nm, the dielectric constant is 310, the dielectric loss is 0.008, the breakdown field strength is 2500kV/cm, and the energy storage density is 40J/cm3The method can be applied to film capacitors.
Example 4:
as shown in FIG. 1, a rolled copper foil as a substrate, which had a thickness of 12 μm and a surface roughness of 0.8 μm, was placed in a vacuum chamber and evacuated to a vacuum of 3X 10-3Pa. The vacuum chamber is heated to 200 ℃, the heat preservation time is 10min, argon is filled, and the flow of the argon is 50 sccm. And opening the Hall ion source, setting the voltage of the Hall ion source to be 1000v and the current to be 1A, and treating for 5min to enable the surface tension of the copper foil to reach 75 dynes.
Closing the gate valve until the vacuum degree is 0.2Pa, keeping the argon flow at 50sccm, starting a magnetron sputtering power supply to 50w, taking strontium titanate with the density of 96% as a target material, depositing for 2 minutes, and forming a 30nm strontium titanate film prefabricated layer on the copper foil, wherein the grain size of the strontium titanate film prefabricated layer is 10nm, and the structure is compact.
And (3) closing the argon, filling oxygen with the flow rate of 100sccm, ensuring the vacuum degree to be 0.6Pa, setting the heating temperature to be 400 ℃, and keeping the temperature for 60 min.
And closing an oxygen valve, opening an argon valve, ensuring the vacuum degree to be 0.4Pa, opening a magnetron sputtering power supply, setting magnetron sputtering current 4A, taking metal copper as a target material, depositing for 30 minutes to form a copper electrode layer, wherein the thickness of the copper electrode layer is 2 mu m, and the sheet resistance is 0.002m omega/□, thus obtaining the flexible energy storage film.
Tests prove that the thickness of the strontium titanate film in the obtained flexible energy storage film is 10nm, the minimum bending radius of the flexible energy storage film is 2mm, the grain size is 30nm, the dielectric constant is 280, the dielectric loss is 0.006, the breakdown field strength is 3000kV/cm, and the energy storage density is 55J/cm3The method can be applied to film capacitors.
Example 5:
as shown in FIG. 1, an electrolytic copper foil is used as a substrate, the copper foil has a thickness of 18 μm and a surface roughness of 0.5 μm, and the substrate is placed in a vacuum chamber and evacuated to a vacuum of 3X 10-3Pa. The vacuum chamber is heated to 250 ℃, the heat preservation time is 10min, argon is filled, and the flow of the argon is 30 sccm. And opening the Hall ion source, setting the voltage of the Hall ion source to be 1000v and the current to be 0.5A, and treating for 1min to enable the surface tension of the copper foil to reach 75 dynes.
Closing the gate valve until the vacuum degree is 0.5Pa, keeping the argon flow at 30sccm, starting a magnetron sputtering power supply to 200w, taking strontium titanate with the density of 98% as a target material, depositing for 5 minutes, and forming a strontium titanate film prefabricated layer with the thickness of 300nm on the copper foil, wherein the grain size of the strontium titanate film prefabricated layer is 450nm, and the structure is compact.
And (3) closing the argon, filling oxygen, ensuring that the vacuum degree is 0.3Pa, setting the heating temperature to 600 ℃, and keeping the temperature for 30min, wherein the oxygen flow is 70 sccm.
And closing an oxygen valve, opening an argon valve, ensuring the vacuum degree to be 0.4Pa, opening a magnetron sputtering power supply, setting magnetron sputtering current 4A, taking metal copper as a target material, depositing for 1 hour to form a copper electrode layer, wherein the thickness of the copper electrode layer is 3 mu m, and the sheet resistance is 0.001m omega/□, thus obtaining the flexible energy storage film.
Tests prove that the thickness of the strontium titanate film in the obtained flexible energy storage film is 240nm, the minimum bending radius of the flexible energy storage film is 10mm, the grain size is 500nm, the dielectric constant is 300, the dielectric loss is 0.008, the breakdown field strength is 1500kV/cm, and the energy storage density is 25J/cm3The method can be applied to film capacitors.
Example 6:
as shown in FIG. 1, an electrolytic copper foil is used as a substrate, the copper foil has a thickness of 18 μm and a surface roughness of 0.5 μm, and the substrate is placed in a vacuum chamber and evacuated to a vacuum of 3X 10-3Pa. The vacuum chamber is heated to 150 ℃, the heat preservation time is 10min, argon is filled, and the flow of the argon is 30 sccm. And opening the Hall ion source, setting the voltage of the Hall ion source to be 1000v and the current to be 0.5A, and treating for 1min to enable the surface tension of the copper foil to reach 65 dynes.
Closing the gate valve until the vacuum degree is 0.4Pa, keeping the argon flow at 30sccm, starting a magnetron sputtering power supply to 200w, taking strontium titanate with the density of 99% as a target material, depositing for 60 minutes, and forming a strontium titanate film prefabricated layer with the grain size of 3.5 microns on the copper foil, wherein the grain size of the strontium titanate film prefabricated layer is 450nm, and the structure is compact.
And (3) closing the argon, filling oxygen, ensuring the vacuum degree to be 1Pa with the oxygen flow of 150sccm, setting the heating temperature to be 600 ℃, and keeping the temperature for 30 min.
And closing an oxygen valve, opening an argon valve, ensuring the vacuum degree to be 0.4Pa, opening a magnetron sputtering power supply, setting magnetron sputtering current 4A, taking metal copper as a target material, depositing for 30 minutes to form a copper electrode layer, wherein the thickness of the copper electrode layer is 1.5 mu m, and the sheet resistance is 0.01m omega/□, thus obtaining the flexible energy storage film.
Tests prove that the thickness of the strontium titanate film in the obtained flexible energy storage film is 3 mu m, the minimum bending radius of the flexible energy storage film is 20mm, the grain size is 500nm, the dielectric constant is 300, the dielectric loss is 0.007, the breakdown field strength is 1000kV/cm, and the energy storage density is 12J/cm3The method can be applied to film capacitors.
Example 7:
as shown in FIG. 1, an electrolytic copper foil is used as a substrate, the copper foil has a thickness of 12 μm and a surface roughness of 0.5 μm, and the substrate is placed in a vacuum chamber and evacuated to a vacuum of 3X 10-3Pa. The vacuum chamber is heated to 150 ℃, the heat preservation time is 10min, argon is filled, and the flow of the argon is 30 sccm. And (3) opening the Hall ion source, setting the voltage of the Hall ion source to be 1000v and the current to be 0.5A, and treating for 6min to enable the surface tension of the copper foil to reach 70 dynes.
Closing the gate valve until the vacuum degree is 0.5Pa, keeping the argon flow at 30sccm, starting a magnetron sputtering power supply to 100w, taking strontium titanate with the density of 98% as a target material, depositing for 30 minutes, and forming a strontium titanate film prefabricated layer with the grain size of 2 mu m on the copper foil, wherein the grain size of the strontium titanate film prefabricated layer is 270nm, and the structure is compact.
And (3) closing the argon, filling oxygen with the flow rate of 120sccm, ensuring the vacuum degree to be 0.8Pa, setting the heating temperature to be 400 ℃, and keeping the temperature for 30 min.
And closing an oxygen valve, opening an argon valve, ensuring the vacuum degree to be 0.4Pa, opening a magnetron sputtering power supply, setting magnetron sputtering current 6A, taking metal copper as a target material, depositing for 10 minutes to form a copper electrode layer, wherein the thickness of the copper electrode layer is 800nm, and the sheet resistance is 0.05 omega/□, so as to obtain the flexible energy storage film.
Tests show that the thickness of the strontium titanate film in the obtained flexible energy storage film is 1.8 mu m, the minimum bending radius of the flexible energy storage film is 12mm, the grain size is 300nm, the dielectric constant is 310, the dielectric loss is 0.006, the breakdown field strength is 1500kV/cm, and the energy storage density is 25J/cm3The method can be applied to film capacitors.
Example 8:
as shown in FIG. 1, an electrolytic copper foil is used as a substrate, the copper foil has a thickness of 18 μm and a surface roughness of 0.5 μm, and the substrate is placed in a vacuum chamber and evacuated to a vacuum of 3X 10-3Pa. The vacuum chamber is heated to 150 ℃, the heat preservation time is 10min, argon is filled, and the flow of the argon is 30 sccm. And (3) opening the Hall ion source, setting the voltage of the Hall ion source to be 1000v and the current to be 0.5A, and treating for 1min to enable the surface tension of the copper foil to reach 60 dynes.
Closing the gate valve until the vacuum degree is 0.1Pa, keeping the argon flow at 30sccm, starting a magnetron sputtering power supply to 90w, taking strontium titanate with the density of 97% as a target material, depositing for 40 minutes, and forming a strontium titanate film prefabricated layer with the thickness of 900nm on the copper foil, wherein the grain size of the strontium titanate film prefabricated layer is 160nm, and the structure is compact.
And (3) closing the argon, filling oxygen with the flow rate of 90sccm, ensuring the vacuum degree to be 0.5Pa, setting the heating temperature to be 300 ℃, and keeping the temperature for 30 min.
And closing an oxygen valve, opening an argon valve, ensuring the vacuum degree to be 0.4Pa, opening a magnetron sputtering power supply, setting magnetron sputtering current 4A, taking metal copper as a target material, depositing for 10 minutes to form a copper electrode layer, wherein the thickness of the copper electrode layer is 100nm, and the sheet resistance is 0.5 omega/□, thus obtaining the flexible energy storage film.
Tests prove that the thickness of the strontium titanate film in the obtained flexible energy storage film is 800nm, the minimum bending radius of the flexible energy storage film is 10mm, the grain size is 200nm, the dielectric constant is 300, the dielectric loss is 0.008, the breakdown field strength is 1300kV/cm, and the energy storage density is 23J/cm3The method can be applied to film capacitors.
Example 9:
as shown in FIG. 1, an electrolytic copper foil is used as a substrate, the copper foil has a thickness of 12 μm and a surface roughness of 0.8 μm, and the substrate is placed in a vacuum chamber and evacuated to a vacuum pressure of 3X 10-3Pa. The vacuum chamber is heated to 200 ℃, the heat preservation time is 10min, argon is filled, and the flow of the argon is 30 sccm. And (3) opening the Hall ion source, setting the voltage of the Hall ion source to be 1000v and the current to be 0.5A, and treating for 1min to enable the surface tension of the copper foil to reach 70 dynes.
Closing the gate valve until the vacuum degree is 0.4Pa, keeping the argon flow at 120sccm, starting a magnetron sputtering power supply to 130w, taking strontium titanate with the density of 98% as a target material, depositing for 20 minutes, and forming a 560nm strontium titanate film prefabricated layer on the copper foil, wherein the grain size of the strontium titanate film prefabricated layer is 240nm, and the structure is compact.
And (3) closing the argon, filling oxygen with the flow rate of 50sccm, ensuring the vacuum degree to be 0.2Pa, setting the heating temperature to be 300 ℃, and keeping the temperature for 30 min.
And closing an oxygen valve, opening an argon valve, ensuring the vacuum degree to be 0.4Pa, opening a magnetron sputtering power supply, setting magnetron sputtering current 4A, taking metal copper as a target material, depositing for 10 minutes to form a copper electrode layer, wherein the thickness of the copper electrode layer is 500nm, and the sheet resistance is 0.1 omega/□, thus obtaining the flexible energy storage film.
Tests prove that the thickness of the strontium titanate film in the obtained flexible energy storage film is 500nm, the minimum bending radius of the flexible energy storage film is 6mm, the grain size is 200nm, the dielectric constant is 300, the dielectric loss is 0.006, the breakdown field strength is 1600kV/cm, and the energy storage density is 21J/cm3The method can be applied to film capacitors.
Example 10:
example 10 differs from example 1 only in that the substrate of example 10 is an aluminum foil, resulting in a flexible energy storage film as shown in (f) of fig. 2, which can be applied to a thin film capacitor. Tests prove that the thickness of the strontium titanate film in the obtained flexible energy storage film is 120nm, the minimum bending radius of the flexible energy storage film is 5mm, the grain size is 140nm, the dielectric constant is 300, the dielectric loss is 0.009, the breakdown field strength is 1500kV/cm, and the energy storage density is 25J/cm3The method can be applied to film capacitors.
Comparative example 1:
a strontium titanate thin film and a Pt electrode layer were sequentially formed on a silicon substrate by the magnetron sputtering method of example 1, using a rigid silicon substrate as a substrate, to obtain a strontium titanate energy storage thin film as shown in fig. 2 (e).
As can be seen from fig. 2, the strontium titanate ceramic energy storage thin film of comparative example 1 has no flexibility and large crystal grain size. The energy storage film of the embodiment 1 of the invention has flexibility, and the microstructure of the strontium titanate film is compact and uniform, and the grain size is small, so that the bending radius of the energy storage film is small and the energy storage density is excellent. The flexible energy storage film of example 10 has flexibility, but the crystal grain size is larger, and the bending radius and the energy storage performance of the flexible energy storage film are weaker than those of example 1.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (7)

1. A thin film capacitor, comprising a dielectric thin film and an electrode layer, wherein the dielectric thin film comprises a flexible metal substrate and a strontium titanate thin film formed on the flexible metal substrate, and the electrode layer is formed on the strontium titanate layer.
2. A film capacitor according to claim 1, wherein the minimum bend radius of the dielectric film is 2mm to 20 mm; and/or
The dielectric constant of the dielectric film is 280-310; and/or
The dielectric loss of the dielectric film is 0.003-0.05; and/or
The breakdown field strength of the dielectric film is 1000 kV/cm-3000 kV/cm; and/or
The energy storage density of the dielectric film is 12J/cm3～55J/cm3。
3. A thin film capacitor in accordance with claim 1, wherein the thickness of the strontium titanate thin film is 10nm to 2 μm, and the crystal grain size is 30nm to 500 nm.
4. A thin film capacitor according to claim 1, wherein the flexible metal substrate has a thickness of 12 to 18 μm; and/or
The surface roughness of the flexible metal substrate is 0.4-0.8 μm; and/or
The surface tension of the flexible metal substrate is more than or equal to 60 dynes; and/or
The flexible metal substrate includes a copper foil.
5. A thin film capacitor in accordance with claim 1, wherein the thickness of the electrode layer is 100nm to 3 μm.
6. A film capacitor as claimed in claim 1, wherein the sheet resistance of the electrode layer is 0.001m Ω/□ -0.5 Ω/□.
7. A thin film capacitor as claimed in claim 1, wherein the material of the electrode layer comprises at least one of copper, platinum, gold, silver, and aluminum.
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