CN112921288A - Preparation of high-energy-storage-density BaTiO3Ferroelectric thin film method, product and application thereof - Google Patents
Preparation of high-energy-storage-density BaTiO3Ferroelectric thin film method, product and application thereof Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 44
- 239000010409 thin film Substances 0.000 title claims abstract description 32
- 238000004146 energy storage Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000000151 deposition Methods 0.000 claims abstract description 90
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 66
- 239000000758 substrate Substances 0.000 claims abstract description 51
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 45
- 239000010408 film Substances 0.000 claims abstract description 39
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000004544 sputter deposition Methods 0.000 claims abstract description 29
- 230000008021 deposition Effects 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims description 23
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 22
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000013077 target material Substances 0.000 claims description 10
- 239000000919 ceramic Substances 0.000 claims description 9
- 239000004065 semiconductor Substances 0.000 claims description 9
- 239000011159 matrix material Substances 0.000 claims description 8
- 238000000861 blow drying Methods 0.000 claims description 7
- 229910052681 coesite Inorganic materials 0.000 claims description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000005086 pumping Methods 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052682 stishovite Inorganic materials 0.000 claims description 7
- 229910052905 tridymite Inorganic materials 0.000 claims description 7
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 6
- 239000003599 detergent Substances 0.000 claims description 6
- 241000877463 Lanio Species 0.000 claims description 5
- 229910052788 barium Inorganic materials 0.000 claims description 5
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000001771 vacuum deposition Methods 0.000 claims description 4
- 229910002340 LaNiO3 Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 5
- 230000005684 electric field Effects 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 241001479588 Packera glabella Species 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910002112 ferroelectric ceramic material Inorganic materials 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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- 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
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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 disclosure relates to the technical field of thin film material preparation, and particularly provides a method for preparing high-energy-storage-density BaTiO3A ferroelectric thin film method, a product and applications thereof. Preparation of high energy storage density BaTiO3The method of ferroelectric thin film comprises the steps of: treating a substrate, depositing a bottom electrode on the substrate, depositing a buffer layer on the bottom electrode, depositing a barium titanate dielectric layer on the buffer layer, depositing a top electrode on the barium titanate dielectric layer, wherein the substrate is treated on the substrateThe upper deposition bottom electrode is finished by adopting a radio frequency magnetron sputtering method, the sputtering atmosphere of the radio frequency magnetron sputtering method is pure Ar, and the air pressure is controlled to be 0.3 Pa. Solves the problems that the barium titanate film prepared by the in-situ preparation method at medium and low temperature in the prior art has poor performance and can not meet the application requirements.
Description
Technical Field
The disclosure relates to the technical field of thin film material preparation, and particularly provides a method for preparing high-energy-storage-density BaTiO3A ferroelectric thin film method, a product and applications thereof.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
With the continuous progress of technology, the demand of miniaturization and integration of modern semiconductor devices is higher and higher. The ferroelectric material, especially the ferroelectric film, is used as a source of an important functional device raw material in modern electronic industry, has good characteristics of ferroelectric, piezoelectric, pyroelectric and the like, has wide application prospect in the fields of microelectronics, optoelectronics, micro-electro-mechanical systems and the like, and is one of the leading edge and hot spot of current scientific research. Wherein the simple cubic perovskite ABO3The structural ferroelectric material has wide application potential in the electronic industry and the ceramic industry due to the characteristics of high dielectric constant, low dielectric loss, excellent ferroelectric and piezoelectric properties and the like.
Barium titanate (BaTiO)3BTO for short) is typically a simple cubic perovskite ABO3A structured ferroelectric material. As important features of the perovskite structure: A. the ions on the B site can be singly or compositely substituted by various ions with different electrovalence and radius (wherein the valence of A is +2 or +1, and the valence of B is +4 or + 5), so that various properties of the material can be adjusted in a large range, and different application requirements are further met.
In order to realize compatibility with a CMOS (complementary metal oxide semiconductor) process, the inventor provides a barium titanate film with a highly oriented c-axis and an in-situ preparation method thereof at a medium and low temperature in previous research.
Disclosure of Invention
Aiming at the problems that the barium titanate film prepared by the in-situ preparation method at medium and low temperature in the prior art has poor performance and can not meet the application requirements.
In one or some embodiments of the present disclosure, there is provided a method for preparing high energy storage density BaTiO3A method of ferroelectric thin film comprising the steps of: substrate processing, depositing a bottom electrode on a substrate, depositing a buffer layer on a bottom electrode, depositing a barium titanate dielectric layer on a buffer layer, depositing a barium titanate dielectric layer on a barium titanate dielectricAnd depositing a top electrode on the layer, wherein the deposition of the bottom electrode on the substrate is completed by adopting a radio frequency magnetron sputtering method, the sputtering atmosphere of the radio frequency magnetron sputtering method is pure Ar, and low-pressure sputtering is kept.
In one or some embodiments of the present disclosure, the above-mentioned preparation of high energy storage density BaTiO is provided3BaTiO prepared by ferroelectric film method3A ferroelectric thin film.
In one or some embodiments of the present disclosure, there is provided the above BaTiO3Use of a ferroelectric thin film in an electronic chip.
In one or some embodiments of the present disclosure, there is provided the above BaTiO3Use of a ferroelectric thin film in an integrated device.
One or some of the above technical solutions have the following advantages or beneficial effects:
(1) the BaTiO prepared in situ by adopting medium and low temperature is adopted in the present disclosure3The film is a nano columnar crystal, the deposition air pressure of the buffer layer is adjusted to be low on the basis of the prior art, and the deposition air pressure of the barium titanate film is adjusted to be high. Through electrical test, the obtained film has excellent ferroelectric property and energy storage property, and the residual polarization intensity is 10 mu C/cm2Saturation polarization 81. mu.C/cm2The breakdown field intensity is 8.1MV/cm, and the effective energy storage density is up to 221J/cm3The energy storage efficiency is 80%.
(2)BaTiO3Is a lead-free environment-friendly ferroelectric ceramic material with green environmental protection and simple element components.
(3) The preparation method is prepared under the medium-low temperature condition of 200-500 ℃, has wider temperature range of 350-500 ℃ and stronger operability compared with the prior art, and is more compatible with a CMOS-Si process.
(4) BaTiO prepared by magnetron sputtering method in the present disclosure3The film has the advantages of good compactness, strong substrate adhesion, high flatness, contribution to industrial popularization and the like.
(5) BaTiO prepared by the present disclosure3The film buffer layer is ABO3Perovskite materials of the type, preferably with BaTiO3Lattice matching and directing of BaTiO3The film grows into nano columnar crystals, and the orientation and the electrical property of the film are optimized.
(6) The present disclosure, after improving the parameters, greatly increases the maximum polarization and maximum applicable electric field as well as the cyclic energy storage density.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this disclosure, illustrate embodiments of the disclosure and, together with the description, serve to explain the disclosure and not to limit the disclosure.
FIG. 1 is a schematic view of the manufacturing method used in the example of the present invention.
FIG. 2 is a schematic diagram of a mask for preparing a top electrode used in an embodiment of the present invention, and the diameter of a yellow top electrode may be 200 μm to 1000 μm, where the yellow top electrode includes a 1-Si single crystal substrate, a 2-Pt/Ti bottom electrode, a 3-lanthanum nickelate buffer layer, a 4-barium titanate thin film, a 5-gold top electrode, and a 6-gold electrode for conducting the Pt/Ti bottom electrode and the gold top electrode.
FIG. 3 is a schematic structural diagram of a barium titanate thin film system prepared in the embodiment of the present invention.
FIG. 4 is a TEM (450 ℃ C. preparation) and XRD pattern of the barium titanate thin film prepared in the example of the present invention.
FIG. 5 is a single-sided hysteresis loop of a barium titanate thin film prepared in example 1 of the present invention (prepared at 350 ℃).
FIG. 6 shows a single-sided hysteresis loop of a barium titanate thin film prepared in example 2 of the present invention (prepared at 200 ℃).
FIG. 7 shows a single-sided hysteresis loop of a barium titanate thin film prepared in example 3 of the present invention (prepared at 500 ℃).
Detailed Description
The technical solutions in the embodiments of the present disclosure will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present disclosure, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the disclosure without making any creative effort, shall fall within the protection scope of the disclosure.
Aiming at the problems that the barium titanate film prepared by the in-situ preparation method at medium and low temperature in the prior art has poor performance and can not meet the application requirements.
In one or some embodiments of the present disclosure, there is provided a method for preparing high energy storage density BaTiO3A method of ferroelectric thin film comprising the steps of: the method comprises the following steps of substrate treatment, bottom electrode deposition on a substrate, buffer layer deposition on the bottom electrode, barium titanate dielectric layer deposition on the buffer layer, and top electrode deposition on the barium titanate dielectric layer, wherein the bottom electrode deposition on the substrate is completed by adopting a radio frequency magnetron sputtering method, the sputtering atmosphere of the radio frequency magnetron sputtering method is pure Ar, and low-pressure sputtering is kept.
Preferably, the air pressure of the deposition buffer layer is controlled to be lower than 0.3Pa and does not contain 0.3 Pa;
preferably, the pressure of the deposited barium titanate is controlled to be higher than 1.2Pa, and 1.2Pa is not contained. The magnetron sputtering prepared film has the following advantages: 1) high efficiency 2) high density 3) and strong substrate adhesion 4) good film flatness. The principle of preparing the film by the magnetron sputtering method is shown in figure 1: under the action of the electric field E, the electrons collide with argon atoms in the process of flying to the substrate, so that Ar is ionized+And a new electron is generated. Electrons are flown to the substrate, and Ar+The target material is impacted under the acceleration action of the high-voltage electric field. Atoms on the surface of the target material absorb Ar by absorption+The kinetic energy is separated from the lattice constraint, escapes from the surface of the target material, flies to the substrate and deposits on the substrate to form a film. The magnetron sputtering method can be used for preparing various thin film materials, such as metal films, ceramic films, polymer films, composite films and the like. There are many factors (such as gas flow, target power, temperature, coating atmosphere, etc.) that can affect the quality of magnetron sputtering films, so each process parameter should be well controlled in the coating practice process to improve the uniformity of the film and optimize its physical properties.
Preferably, the substrate treatment comprises the following steps: selecting semiconductor substrate Si or Si/SiO2As a matrix, ultrasonic cleaning is carried out by using an ultrasonic detergent to remove oily impurities, deionized water is used to remove the ultrasonic detergent, then inert gas is used for blow-drying, and finally the substrate is placed in a vacuum coating chamber for vacuumizing;
preferably, the ultrasonic detergent is acetone, alcohol or a mixture of the acetone and the alcohol, and further preferably is a mixture of the acetone and the alcohol;
preferably, the inert gas is nitrogen;
preferably, the step of vacuumizing the vacuum coating chamber comprises the following steps: vacuum pumping the back to 2 × 10-4Pa, heating to 300 ℃.
Preferably, the step of depositing the bottom electrode on the substrate comprises the steps of: depositing a bottom electrode layer on a substrate by adopting a conductive metal target Ti/Pt in a radio frequency or direct current magnetron sputtering mode at the temperature of the substrate treatment process;
preferably, the atmosphere at the time of deposition is Ar,
preferably, the flow rate of Ar gas is controlled at 39sccm,
preferably, the air pressure is controlled at 0.3Pa,
preferably, the target power is 55W,
preferably, the total film thickness of the bottom electrode is 150 nm.
Preferably, the step of depositing the buffer layer on the bottom electrode comprises the steps of: using LaNiO3The target material is used for depositing a buffer layer on the substrate in a radio frequency or direct current magnetron sputtering mode by keeping the temperature at 200-500 ℃;
preferably, the atmosphere during deposition is Ar and O2The mixed gas of (a) and (b),
preferably, the flow rate of Ar gas is controlled to be 60sccm and O2The flow rate was controlled at 15sccm,
preferably, the target power is 100W,
preferably, the total film thickness of the buffer layer is 100 nm;
preferably, the radio frequency or direct current magnetron sputtering temperature is 200-350 ℃. .
Preferably, the depositing of the barium titanate dielectric layer on the buffer layer comprises the steps of: using ceramic BaTiO3Target, and depositing BaTiO on the bottom electrode by radio frequency magnetron sputtering at 200-500 deg.C3A layer of a material selected from the group consisting of,
preferably, the sputtering atmosphere is Ar and O2The mixed gas of (a) and (b),
it is preferable thatThe flow rate of Ar is controlled to be 60sccm and O2The flow rate was controlled at 15sccm,
preferably, the air pressure is controlled to be 1.2Pa,
preferably, BaTiO3The sputtering power of the target was 100W,
preferably, the thickness is 160-3000 nm;
preferably, the temperature of the radio frequency magnetron sputtering is 200-350 ℃.
Preferably, the step of depositing the top electrode on the barium titanate dielectric layer comprises the steps of: depositing by adopting a metal target in a radio frequency or direct current magnetron sputtering mode at room temperature, wherein the sputtering atmosphere is air, and the target power density is 2-5W/cm2The diameter of the upper electrode is controlled to be 200-1000 μm.
Preferably, the method comprises the following steps:
(1) matrix treatment:
selecting semiconductor substrate Si or Si/SiO2Ultrasonic cleaning with acetone and alcohol to remove oily impurities on the surface, cleaning with deionized water, blow-drying with nitrogen, vacuum-pumping to 2 × 10-4Pa, heating to 300 ℃;
(2) depositing a bottom electrode on a substrate
Adopting a conductive metal target Ti/Pt, and depositing a bottom electrode layer on the substrate in a radio frequency or direct current magnetron sputtering mode at the temperature of the step (1), wherein the atmosphere during deposition is Ar, the flow rate of Ar is controlled at 39sccm, the air pressure is controlled at 0.3Pa, the target power is 55W, and the total film thickness of the bottom electrode is 150 nm;
(3) depositing a buffer layer on the bottom electrode
Adopts LaNiO with higher matching degree with tetragonal phase barium titanate3The target material is used for depositing a buffer layer on a substrate in a radio frequency or direct current magnetron sputtering mode by keeping the temperature at 200-500 ℃, and the atmosphere during deposition is Ar and O2The flow rate of Ar gas is controlled to be 60sccm and O2The flow is controlled to be 15sccm, the air pressure is controlled to be 0.3Pa, the target power is 100W, and the total film thickness of the buffer layer is 100 nm;
(4) depositing a barium titanate dielectric layer on the buffer layer
Using ceramic BaTiO3Target, and maintaining the temperature in the step (3) to deposit BaTiO on the bottom electrode in a radio frequency magnetron sputtering mode3Layer, sputtering atmosphere Ar and O2The flow rate of Ar gas is controlled to be 60sccm and O2The flow rate is controlled to be 15sccm, the air pressure is controlled to be 1.2Pa, and BaTiO3The sputtering power of the target is 100W, and the thickness is 160-3000 nm;
(5) depositing a top electrode on a barium titanate dielectric layer
Depositing by adopting a metal target in a radio frequency or direct current magnetron sputtering mode at room temperature, wherein the sputtering atmosphere is air, and the target power density is 2-5W/cm2The diameter of the upper electrode is controlled to be 200-1000 μm.
In one or some embodiments of the present disclosure, the above-mentioned preparation of high energy storage density BaTiO is provided3BaTiO prepared by ferroelectric film method3A ferroelectric thin film.
In one or some embodiments of the present disclosure, there is provided the above BaTiO3Use of a ferroelectric thin film in an electronic chip.
In one or some embodiments of the present disclosure, there is provided the above BaTiO3Use of a ferroelectric thin film in an integrated device.
Example 1
(1) Matrix treatment:
selecting semiconductor substrate Si or Si/SiO2Ultrasonic cleaning with acetone and alcohol to remove oily impurities on the surface, cleaning with deionized water, blow-drying with nitrogen, vacuum-pumping to 2 × 10-4Pa, heating to 300 ℃;
(2) depositing a bottom electrode on a substrate
And (2) adopting a conductive metal target Ti/Pt, and depositing a bottom electrode layer on the substrate in a radio frequency or direct current magnetron sputtering mode at the temperature of the step (1), wherein the atmosphere during deposition is Ar, the flow rate of Ar is controlled at 39sccm, the air pressure is controlled at 0.3Pa, the target power is 55W, and the total film thickness of the bottom electrode is 150 nm.
(3) Depositing a buffer layer on the bottom electrode
Adopts LaNiO with higher matching degree with tetragonal phase barium titanate3Target material, maintaining the temperature at 350 deg.C, and depositing buffer layer on the substrate by radio frequency or DC magnetron sputtering under Ar and O atmosphere2The flow rate of Ar gas is controlled to be 60sccm and O2The flow rate was controlled at 15sccm, the gas pressure was controlled at 0.24Pa, the target power was 100W, and the total buffer layer thickness was 100 nm.
(4) Depositing a barium titanate dielectric layer on the buffer layer
Using ceramic BaTiO3Target, and maintaining the temperature in the step (3) to deposit BaTiO on the bottom electrode in a radio frequency magnetron sputtering mode3Layer, sputtering atmosphere Ar and O2The flow rate of Ar gas is controlled to be 60sccm and O2The flow rate is controlled to be 15sccm, the air pressure is controlled to be 1.7Pa, and BaTiO3The sputtering power of the target is 100W, and the thickness is 160-3000 nm.
(5) Depositing a top electrode on a barium titanate dielectric layer
Depositing by adopting a metal target in a radio frequency or direct current magnetron sputtering mode at room temperature, wherein the sputtering atmosphere is air, and the target power density is 2-5W/cm2The diameter of the upper electrode is controlled to be 200-1000 μm.
Through the electrical performance test, the ferroelectric loop is shown in fig. 5, and it can be seen from fig. 5 that the ferroelectric thin film obtained in this embodiment has excellent energy storage performance.
Example 2
(1) Matrix treatment:
selecting semiconductor substrate Si or Si/SiO2Ultrasonic cleaning with acetone and alcohol to remove oily impurities on the surface, cleaning with deionized water, blow-drying with nitrogen, vacuum-pumping to 2 × 10-4Pa, heating to 300 ℃;
(2) depositing a bottom electrode on a substrate
And (2) adopting a conductive metal target Ti/Pt, and depositing a bottom electrode layer on the substrate in a radio frequency or direct current magnetron sputtering mode at the temperature of the step (1), wherein the atmosphere during deposition is Ar, the flow rate of Ar is controlled at 39sccm, the air pressure is controlled at 0.3Pa, the target power is 55W, and the total film thickness of the bottom electrode is 150 nm.
(3) Depositing a buffer layer on the bottom electrode
Adopts LaNiO with higher matching degree with tetragonal phase barium titanate3Target material, maintaining the temperature at 200 ℃ and depositing a buffer layer on the substrate in a radio frequency or direct current magnetron sputtering mode, wherein the atmosphere during deposition is Ar and O2The flow rate of Ar gas is controlled to be 60sccm and O2The flow rate was controlled at 15sccm, the gas pressure was controlled at 0.18Pa, the target power was 100W, and the total buffer layer thickness was 100 nm.
(4) Depositing a barium titanate dielectric layer on the buffer layer
Using ceramic BaTiO3Target, and maintaining the temperature in the step (3) to deposit BaTiO on the bottom electrode in a radio frequency magnetron sputtering mode3Layer, sputtering atmosphere Ar and O2The flow rate of Ar gas is controlled to be 60sccm and O2The flow rate is controlled to be 15sccm, the air pressure is controlled to be 1.6Pa, and BaTiO3The sputtering power of the target is 100W, and the thickness is 160-3000 nm.
(5) Depositing a top electrode on a barium titanate dielectric layer
Depositing by adopting a metal target in a radio frequency or direct current magnetron sputtering mode at room temperature, wherein the sputtering atmosphere is air, and the target power density is 2-5W/cm2The diameter of the upper electrode is controlled to be 200-1000 μm.
Example 3
(1) Matrix treatment:
selecting semiconductor substrate Si or Si/SiO2Ultrasonic cleaning with acetone and alcohol to remove oily impurities on the surface, cleaning with deionized water, blow-drying with nitrogen, vacuum-pumping to 2 × 10-4Pa, heating to 300 ℃;
(2) depositing a bottom electrode on a substrate
And (2) adopting a conductive metal target Ti/Pt, and depositing a bottom electrode layer on the substrate in a radio frequency or direct current magnetron sputtering mode at the temperature of the step (1), wherein the atmosphere during deposition is Ar, the flow rate of Ar is controlled at 39sccm, the air pressure is controlled at 0.3Pa, the target power is 55W, and the total film thickness of the bottom electrode is 150 nm.
(3) Depositing a buffer layer on the bottom electrode
Adopts LaNiO with higher matching degree with tetragonal phase barium titanate3Target material, keeping the temperature at 500 ℃ and depositing a buffer layer on the substrate in a radio frequency or direct current magnetron sputtering mode, wherein the atmosphere during deposition is Ar and O2The flow rate of Ar gas is controlled to be 60sccm and O2The flow rate was controlled at 15sccm, the gas pressure was controlled at 0.2Pa, the target power was 100W, and the total buffer layer thickness was 100 nm.
(4) Depositing a barium titanate dielectric layer on the buffer layer
Using ceramic BaTiO3Target, and maintaining the temperature in the step (3) to deposit BaTiO on the bottom electrode in a radio frequency magnetron sputtering mode3Layer, sputtering atmosphere Ar and O2The flow rate of Ar gas is controlled to be 60sccm and O2The flow rate is controlled to be 15sccm, the air pressure is controlled to be 1.5Pa, and BaTiO3The sputtering power of the target is 100W, and the thickness is 160-3000 nm.
(5) Depositing a top electrode on a barium titanate dielectric layer
Depositing by adopting a metal target in a radio frequency or direct current magnetron sputtering mode at room temperature, wherein the sputtering atmosphere is air, and the target power density is 2-5W/cm2The diameter of the upper electrode is controlled to be 200-1000 μm.
BaTiO prepared in examples 1 to 33The film is analyzed by XRD and TEM tests respectively, the structure of the film is a nano columnar crystal, and as can be seen from figure 4, the structure of the film prepared by the method is relatively complete at various temperatures.
The disclosure of the present invention is not limited to the specific embodiments, but rather to the specific embodiments, the disclosure is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. Preparation of high-energy-storage-density BaTiO3A method of making a ferroelectric thin film, comprising the steps of: substrate processing, bottom electrode deposition on substrate, bottom electrode deposition on bottom electrodeThe method comprises the following steps of (1) depositing a buffer layer, depositing a barium titanate dielectric layer on the buffer layer, and depositing a top electrode on the barium titanate dielectric layer, wherein the buffer layer deposition and the barium titanate deposition are completed by adopting a radio frequency magnetron sputtering method, the sputtering atmosphere of the radio frequency magnetron sputtering method is pure Ar, low-pressure sputtering is kept, and a barium titanate film is kept in high-pressure sputtering;
preferably, the air pressure of the deposition buffer layer is controlled to be lower than 0.3Pa and does not contain 0.3 Pa;
preferably, the pressure of the deposited barium titanate is controlled to be higher than 1.2Pa, and 1.2Pa is not contained.
2. The method for preparing high energy storage density nano columnar crystal BaTiO as claimed in claim 13A method of ferroelectric thin film, characterized in that the matrix treatment comprises the steps of: selecting semiconductor substrate Si or Si/SiO2As a matrix, ultrasonic cleaning is carried out by using an ultrasonic detergent to remove oily impurities, deionized water is used to remove the ultrasonic detergent, then inert gas is used for blow-drying, and finally the substrate is placed in a vacuum coating chamber for vacuumizing;
preferably, the ultrasonic detergent is acetone, alcohol or a mixture of the acetone and the alcohol, and further preferably is a mixture of the acetone and the alcohol;
preferably, the inert gas is nitrogen;
preferably, the step of vacuumizing the vacuum coating chamber comprises the following steps: vacuum pumping the back to 2 × 10-4Pa, heating to 300 ℃.
3. Preparation of high energy storage density BaTiO according to claim 13A method of depositing a ferroelectric thin film on a substrate, comprising the steps of: depositing a bottom electrode layer on a substrate by adopting a conductive metal target Ti/Pt in a radio frequency or direct current magnetron sputtering mode at the temperature of the substrate treatment process;
preferably, the atmosphere at the time of deposition is Ar,
preferably, the flow rate of Ar gas is controlled at 39sccm,
preferably, the air pressure is controlled at 0.3Pa,
preferably, the target power is 55W,
preferably, the total film thickness of the bottom electrode is 150 nm.
4. Preparation of high energy storage density BaTiO according to claim 13A method of forming a ferroelectric thin film, wherein depositing a buffer layer on a bottom electrode comprises the steps of: using LaNiO3The target material is used for depositing a buffer layer on the substrate in a radio frequency or direct current magnetron sputtering mode by keeping the temperature at 200-500 ℃;
preferably, the atmosphere during deposition is Ar and O2The mixed gas of (a) and (b),
preferably, the flow rate of Ar gas is controlled to be 60sccm and O2The flow rate was controlled at 15sccm,
preferably, the target power is 100W,
preferably, the total film thickness of the buffer layer is 100 nm;
preferably, the radio frequency or direct current magnetron sputtering temperature is 200-350 ℃.
5. The method for preparing high energy storage density nano columnar crystal BaTiO as claimed in claim 13A method of depositing a barium titanate dielectric layer on a buffer layer, comprising the steps of: using ceramic BaTiO3Target, and depositing BaTiO on the bottom electrode by radio frequency magnetron sputtering at 200-500 deg.C3A layer of a material selected from the group consisting of,
preferably, the sputtering atmosphere is Ar and O2The mixed gas of (a) and (b),
preferably, the flow rate of Ar gas is controlled to be 60sccm and O2The flow rate was controlled at 15sccm,
preferably, BaTiO3The sputtering power of the target was 100W,
preferably, the thickness is 160-3000 nm;
preferably, the temperature of the radio frequency magnetron sputtering is 200-350 ℃.
6. Preparation of high energy storage density BaTiO according to claim 13A method of depositing a ferroelectric thin film, wherein depositing a top electrode on a barium titanate dielectric layer comprises the steps of: using a metal target and performing magnetron sputtering at room temperature by radio frequency or direct currentDeposition, wherein the sputtering atmosphere is air, and the target power density is 2-5W/cm2The diameter of the upper electrode is controlled to be 200-1000 μm.
7. Preparation of high energy storage density BaTiO according to claim 13A method of forming a ferroelectric thin film, comprising the steps of:
(1) matrix treatment:
selecting semiconductor substrate Si or Si/SiO2Ultrasonic cleaning with acetone and alcohol to remove oily impurities on the surface, cleaning with deionized water, blow-drying with nitrogen, vacuum-pumping to 2 × 10-4Pa, heating to 300 ℃;
(2) depositing a bottom electrode on a substrate
Adopting a conductive metal target Ti/Pt, and depositing a bottom electrode layer on the substrate in a radio frequency or direct current magnetron sputtering mode at the temperature of the step (1), wherein the atmosphere during deposition is Ar, the flow rate of Ar is controlled at 39sccm, the air pressure is controlled at 0.3Pa, the target power is 55W, and the total film thickness of the bottom electrode is 150 nm;
(3) depositing a buffer layer on the bottom electrode
Adopts LaNiO with higher matching degree with tetragonal phase barium titanate3The target material is used for depositing a buffer layer on a substrate in a radio frequency or direct current magnetron sputtering mode by keeping the temperature at 200-500 ℃, and the atmosphere during deposition is Ar and O2The flow rate of Ar gas is controlled to be 60sccm and O2Controlling the flow at 15sccm, controlling the air pressure at less than 0.3Pa, controlling the target power at 100W, and controlling the total film thickness of the buffer layer at 100 nm;
(4) depositing a barium titanate dielectric layer on the buffer layer
Using ceramic BaTiO3Target, and maintaining the temperature in the step (3) to deposit BaTiO on the bottom electrode in a radio frequency magnetron sputtering mode3Layer, sputtering atmosphere Ar and O2The flow rate of Ar gas is controlled to be 60sccm and O2The flow rate is controlled to be 15sccm, the air pressure is controlled to be higher than 1.2Pa, and BaTiO3The sputtering power of the target is 100W, and the thickness is 160-3000 nm;
(5) a top electrode is deposited on the barium titanate dielectric layer.
Depositing by adopting a metal target in a radio frequency or direct current magnetron sputtering mode at room temperature, wherein the sputtering atmosphere is air, and the target power density is 2-5W/cm2The diameter of the upper electrode is controlled to be 200-1000 μm.
8. Preparation of high energy storage density BaTiO according to any one of claims 1 to 73BaTiO prepared by ferroelectric film method3A ferroelectric thin film.
9. BaTiO of claim 83Use of a ferroelectric thin film in an electronic chip.
10. BaTiO of claim 83Use of a ferroelectric thin film in an integrated device.
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