CN108531867B - Preparation method of flexible BTS/BZT/BTS multilayer thin film varactor - Google Patents

Preparation method of flexible BTS/BZT/BTS multilayer thin film varactor Download PDF

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CN108531867B
CN108531867B CN201810267139.0A CN201810267139A CN108531867B CN 108531867 B CN108531867 B CN 108531867B CN 201810267139 A CN201810267139 A CN 201810267139A CN 108531867 B CN108531867 B CN 108531867B
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CN108531867A (en
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于仕辉
刘荣闯
赵乐
李玲霞
孙永涛
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Tianjin University
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/04—Coating on selected surface areas, e.g. using masks
    • C23C14/042—Coating on selected surface areas, e.g. using masks using masks
    • 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
    • C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
    • 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

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Abstract

A method for preparing flexible BTS/BZT/BTS multilayer film varactor comprises firstly softening copper foilSexual substrate and Sb-doped SnO2Namely, the ATO target material is arranged on a target head of a pulse laser deposition system; pumping the background vacuum degree of the pulse laser deposition system to 3.0 x 10‑ 3Depositing to obtain an ATO thin film layer with the thickness of 50-1000 nm below Pa; and respectively loading BTS (base transceiver station) and BZT targets on a target head of a pulse laser deposition system, depositing to obtain 100-500 nm BTS, BZT and BTS thin film layers, then taking out the product, and preparing metal electrodes on the surfaces of the BTS thin film and the bottom electrode ATO layer to realize the integral preparation of the flexible BTS/BZT/BTS multilayer thin film varactor. The dielectric tuning rate of the invention is more than or equal to 50% @100kHz, the dielectric loss is less than or equal to 0.01, when the flexible curvature radius is 5.0mm, the performance change rate is less than or equal to 10%, the device has excellent performance, and the invention is suitable for being applied in flexible electronic technology.

Description

Preparation method of flexible BTS/BZT/BTS multilayer thin film varactor
Technical Field
The invention belongs to a ceramic composition characterized by components, and particularly relates to a preparation method of a flexible BTS/BZT/BTS multilayer thin film varactor.
Background
Flexible electronic technology is one of the most exciting and promising electronic technologies today as a new electronic technology revolution, and is receiving wide attention from both academia and industry. In recent years, developed countries have made major research plans for flexible electronics, such as the us FDCASU plan, the seventh framework plan of the european union, the japanese TRADIM plan, and the like. The department of science and technology in China also ranks flexible electronics as an important field of science and technology development. Flexible electronics have a wide range of applications due to their unique flexibility/ductility, portability, and efficient manufacturing processes. The method can be particularly applied to the information field such as flexible electronic displays, flexible folding mobile phones, flexible radio frequency/microwave circuits and the like; energy fields such as flexible solar cells, lithium ion batteries, etc.; health care such as artificial organs, "human networking" projects; the wearable intelligent equipment is used for aerospace, deep sea exploration and the like; the military state defense flexible electronic technology can realize the functions of intelligent skin, individual communication and invisibility, and improve the maneuverability and the concealment of battlefield battles.
Varactor asThe more and more the flexibility of the device, which is an important component of flexible electronic technology, is attracting attention, and the more and more the flexibility is required. BaZr0.2Ti0.8O3The (BZT) film is the dielectric tunable oxide film material which is most concerned at present, but the dielectric loss of the BZT film is higher (more than or equal to 0.01), so that the practical application is limited. BaSn0.15Ti0.85O3The (BTS) films have high dielectric tuning rates and lower dielectric losses. Therefore, the invention prepares the flexible BTS/BZT/BTS multilayer film varactor with excellent performance by compounding the BTS and the BZT film so as to meet the application requirement of the flexible electronic technology.
Disclosure of Invention
The invention aims to overcome the defect of dielectric tuning performance in the prior art, and provides a preparation method of a flexible BTS/BZT/BTS multilayer thin film varactor with excellent performance by using a pulse laser deposition technology.
The invention is realized by the following technical scheme.
A preparation method of a flexible BTS/BZT/BTS multilayer thin film varactor comprises the following steps:
(1) cleaning the surface of the copper foil, and putting the cleaned surface of the copper foil on a sample table in a cavity of a pulse laser deposition system to be used as a flexible substrate;
(2) sb-doped SnO2Namely, the ATO target material is arranged on a target head of a pulse laser deposition system; the distance between the target and the substrate is 40-90 mm;
the mass percentage content of Sb doped is more than 0 and less than or equal to 30 percent;
(3) pumping the background vacuum degree of the pulse laser deposition system to 3.0 x 10-3Introducing oxygen which is more than 0 and less than or equal to 50Pa as growth gas below Pa, and depositing at the substrate temperature of 200-700 ℃ to obtain an ATO thin film layer with the thickness of 50-1000 nm;
(4) taking out the substrate, covering the surface of the ATO layer by using a mask plate, reserving the position of a bottom electrode, and then placing the substrate on a sample table of a pulse laser deposition system;
(5) and respectively loading the BTS target and the BZT target on a target head of a pulse laser deposition system.
(6) Vacuum pumping the background of the pulsed laser deposition system to 1.0 × 10-3Pa or less, heating the substrate to 400-700 deg.C, and using 0-50 Pa O2As a growth gas, depositing to obtain a BTS thin film layer, wherein the thickness of the BTS thin film is 100-500 nm; then using 0-50 Pa O2As a growth gas, depositing to obtain a BZT thin film layer with the thickness of 100nm-500 nm; finally, O with the pressure of 0-50 Pa is used2As a growth gas, depositing to obtain a BTS thin film layer, wherein the thickness of the BTS thin film is 100-500 nm;
(7) and taking out a sample, and preparing a metal electrode on the surfaces of the BTS film and the bottom electrode ATO layer by using a mask plate to realize the integral preparation of the flexible BTS/BZT/BTS multilayer film varactor.
The thickness of the copper foil in the step (1) is 1 micron-1 mm, the purity is more than or equal to 98 percent, and the surface roughness is less than or equal to 300 nanometers.
The Sb doping content in the step (2) is 3-20% by mass.
The target material in the step (2) or the step (5) is a product which is prepared by a conventional preparation method or is sold on the market at will.
The thickness of the ATO, BTS, BZT or BTS thin film layer in the step (3) or the step (6) is controlled by adjusting the preparation process parameters or the deposition time.
The flexible BTS/BZT/BTS multilayer film varactor prepared by the pulsed laser deposition technology has the dielectric tuning rate of more than or equal to 50% @100kHz, the dielectric loss of less than or equal to 0.01, the performance change rate of less than or equal to 10% when the flexible curvature radius is 5.0mm, and the device has excellent performance and is suitable for being applied to the flexible electronic technology.
Drawings
Figure 1 is a graph of the tuning performance of the flexible BTS/BZT/BTS multilayer thin film varactor of example 1.
Detailed Description
The present invention is further illustrated below with reference to specific examples, which are intended to be illustrative only and not to limit the scope of the invention.
Example 1
(1) And cleaning the surface of the copper foil with the purity of 99%, the thickness of 100um and the surface roughness of 50nm, and putting the copper foil on a sample table in a cavity of a pulse laser deposition system to be used as a flexible substrate.
(2) SnO doped with 12 at% Sb2The target material is arranged on a target head of the pulse laser deposition system, and the distance between the target material and the substrate is 50 mm.
(3) Pumping the background vacuum degree of the pulse laser deposition system to 3.0 x 10-4Pa, using 2Pa oxygen as deposition gas, and depositing at the substrate temperature of 600 ℃ to obtain an ATO thin film layer with the thickness of 200 nm.
(4) And taking out the substrate, covering the surface of the ATO layer by using a mask plate, reserving the position of the bottom electrode, and then putting the substrate on a sample table in a pulse laser deposition system.
(5) Respectively loading BTS and BZT target materials prepared by solid-phase sintering method on the target head of a pulse laser deposition system, wherein the used raw material SnO2、BaCO3、TiO2And ZrO2The purity of the product is more than 99 percent.
(6) Vacuum pumping the background of the pulsed laser deposition system to 3.0 × 10-4Pa, and then heating the substrate to 700 ℃; using 15Pa oxygen as growth gas, and depositing to obtain a 150-nanometer-thick BTS thin film layer; then, using 15Pa oxygen as a growth gas, and depositing to obtain a 150-nanometer-thickness BZT thin film layer; and finally, using oxygen of 15Pa as growth gas to carry out deposition to obtain the BTS thin film layer with the thickness of 150 nanometers.
7. And taking out the product, preparing metal electrodes on the surfaces of the BTS thin film and the bottom electrode ATO by using the mask plate, realizing the preparation of the flexible BTS/BZT/BTS multilayer thin film varactor, and finally carrying out dielectric tuning and flexibility performance testing.
Fig. 1 reveals the tuning performance of the flexible BTS/BZT/BTS multilayer thin film varactor of example 1, from which it can be seen that the varactor has a tuning ratio of 61% and a dielectric loss of 0.0049. When the radius of curvature was 5.0mm, the tuning ratio was 58% and the dielectric loss was 0.0051.
Example 2
(1) Cleaning the surface of copper foil with the purity of 99%, the thickness of 100um and the surface roughness of 100nm, and putting the copper foil on a sample table in a cavity of a pulse laser deposition system to be used as a flexible substrate
(2) SnO doped with 12 at% Sb2The target material is arranged on a target head of the pulse laser deposition system, and the distance between the target material and the substrate is 80 mm.
(3) Pumping the background vacuum degree of the pulse laser deposition system to 9.0 x 10-4Pa, using 1Pa oxygen as deposition gas, and depositing at the substrate temperature of 700 ℃ to obtain an ATO thin film layer with the thickness of 300 nm.
(4) And taking out the substrate, covering the surface of the ATO layer by using a mask plate, reserving the position of the bottom electrode, and then putting the substrate on a sample table in a pulse laser deposition system.
(5) Respectively loading BTS and BZT target materials prepared by solid-phase sintering method on the target head of a pulse laser deposition system, wherein the used raw material SnO2、BaCO3、TiO2And ZrO2The purity of the product is more than 99 percent.
(6) Vacuum pumping the background of the pulsed laser deposition system to 8.0 × 10-4Pa, and then heating the substrate to 650 ℃; depositing to obtain a BTS thin film layer with the thickness of 100 nanometers by using oxygen with the pressure of 5Pa as growth gas; then, 5Pa oxygen is used as growth gas to deposit to obtain a 100-nanometer-thick BZT thin film layer; and finally, using 5Pa oxygen as a growth gas, and depositing to obtain a 100-nanometer-thick BTS thin film layer.
(7) And taking out the product, preparing metal electrodes on the surfaces of the BTS thin film and the bottom electrode ATO by using the mask plate, realizing the preparation of the flexible BTS/BZT/BTS multilayer thin film varactor, and finally carrying out dielectric tuning and flexibility performance testing.
The tuning ratio of the varactor of example 2 was 69% and the dielectric loss was 0.019. At a radius of curvature of 5.0mm, the tuning ratio was 67%, and the dielectric loss was 0.021.
Example 3
(1) And cleaning the surface of the copper foil with the purity of 99%, the thickness of 100um and the surface roughness of 50nm, and putting the copper foil on a sample table in a cavity of a pulse laser deposition system to be used as a flexible substrate.
(2) SnO doped with 12 at% Sb2The target material is arranged on a target head of a pulse laser deposition system, and the distance between the target material and the substrate50mm。
(3) Pumping the background vacuum degree of the pulse laser deposition system to 3.0 x 10-4Pa, using 2Pa oxygen as deposition gas, and depositing at the substrate temperature of 600 ℃ to obtain an ATO thin film layer with the thickness of 200 nm.
(4) And taking out the substrate, covering the surface of the ATO layer by using a mask plate, reserving the position of the bottom electrode, and then putting the substrate on a sample table in a pulse laser deposition system.
(5) Respectively loading BTS and BZT target materials prepared by solid-phase sintering method on the target head of a pulse laser deposition system, wherein the used raw material SnO2、BaCO3、TiO2And ZrO2The purity of the product is more than 99 percent.
(6) Vacuum pumping the background of the pulsed laser deposition system to 3.0 × 10-4Pa, and then heating the substrate to 700 ℃; using 50Pa oxygen as growth gas, and depositing to obtain a 200-nanometer-thick BTS thin film layer; then, 50Pa oxygen is used as growth gas to carry out deposition to obtain a 200-nanometer-thickness BZT thin film layer; finally, 50Pa oxygen is used as growth gas to carry out deposition to obtain a 200-nanometer-thick BTS thin film layer.
(7) And taking out the product, preparing metal electrodes on the surfaces of the BTS thin film and the bottom electrode ATO by using the mask plate, realizing the preparation of the flexible BTS/BZT/BTS multilayer thin film varactor, and finally carrying out dielectric tuning and flexibility performance testing.
The tuning ratio of the varactor of example 3 was 51% and the dielectric loss was 0.0047. When the radius of curvature was 5.0mm, the tuning ratio was 46% and the dielectric loss was 0.0052.
Example 4
(1) And cleaning the surface of the copper foil with the purity of 99%, the thickness of 100um and the surface roughness of 500nm, and putting the copper foil on a sample table in a cavity of a pulse laser deposition system to be used as a flexible substrate.
(2) SnO doped with 12 at% Sb2The target material is arranged on a target head of the pulse laser deposition system, and the distance between the target material and the substrate is 50 mm.
(3) Pumping the background vacuum degree of the pulse laser deposition system to 1.0 x 10-4Pa, using oxygen at 8Pa as deposition gas, substrateThe temperature is 700 ℃, and the ATO film layer with the thickness of 500nm is obtained by deposition.
(4) And taking out the substrate, covering the surface of the ATO layer by using a mask plate, reserving the position of the bottom electrode, and then putting the substrate on a sample table in a pulse laser deposition system.
(5) Respectively loading BTS and BZT target materials prepared by solid-phase sintering method on the target head of a pulse laser deposition system, wherein the used raw material SnO2、BaCO3、TiO2And ZrO2The purity of the product is more than 99 percent.
(6) Vacuum pumping the background of the pulsed laser deposition system to 3.0 × 10-4Pa, and then heating the substrate to 700 ℃; using 15Pa oxygen as growth gas, and depositing to obtain a 400-nanometer-thick BTS thin film layer; then, using oxygen of 20Pa as growth gas, and depositing to obtain a BZT thin film layer with the thickness of 400 nanometers; and finally, using oxygen of 20Pa as growth gas to deposit to obtain a BTS thin film layer with the thickness of 400 nanometers.
(7) And taking out the product, preparing metal electrodes on the surfaces of the BTS thin film and the bottom electrode ATO by using the mask plate, realizing the preparation of the flexible BTS/BZT/BTS multilayer thin film varactor, and finally carrying out dielectric tuning and flexibility performance testing.
The tuning ratio of the varactor of example 4 was 53% and the dielectric loss was 0.0071. At a radius of curvature of 5.0mm, the tuning ratio was 46% and the dielectric loss was 0.0078.
Example 5
(1) And cleaning the surface of the copper foil with the purity of 99%, the thickness of 100um and the surface roughness of 500nm, and putting the copper foil on a sample table in a cavity of a pulse laser deposition system to be used as a flexible substrate.
(2) SnO2The target material is arranged on a target head of the pulse laser deposition system, and the distance between the target material and the substrate is 50 mm.
(3) Pumping the background vacuum degree of the pulse laser deposition system to 1.0 x 10-4Pa, depositing under vacuum with the substrate temperature of 700 ℃ to obtain an ATO film layer with the thickness of 500 nm.
(4) And taking out the substrate, covering the surface of the ATO layer by using a mask plate, reserving the position of the bottom electrode, and then putting the substrate on a sample table in a pulse laser deposition system.
(5) Respectively loading BTS and BZT target materials prepared by solid-phase sintering method on the target head of a pulse laser deposition system, wherein the used raw material SnO2、BaCO3、TiO2And ZrO2The purity of the product is more than 99 percent.
(6) Vacuum pumping the background of the pulsed laser deposition system to 3.0 × 10-4Pa, and then heating the substrate to 700 ℃; depositing under vacuum to obtain a BTS thin film layer with the thickness of 400 nanometers; then depositing under vacuum to obtain a BZT thin film layer with the thickness of 400 nanometers; and finally depositing under vacuum to obtain a BTS thin film layer with the thickness of 400 nanometers.
(7) And taking out the product, preparing metal electrodes on the surfaces of the BTS thin film and the bottom electrode ATO by using the mask plate, realizing the preparation of the flexible BTS/BZT/BTS multilayer thin film varactor, and finally carrying out dielectric tuning and flexibility performance testing.
The tuning ratio of the varactor of example 5 was 59% and the dielectric loss was 0.01. At a radius of curvature of 5.0mm, the tuning ratio was 56%, and the dielectric loss was 0.011.

Claims (5)

1. A preparation method of a flexible BTS/BZT/BTS multilayer thin film varactor comprises the following steps:
(1) cleaning the surface of the copper foil, and putting the cleaned surface of the copper foil on a sample table in a cavity of a pulse laser deposition system to be used as a flexible substrate;
(2) sb-doped SnO2Namely, the ATO target material is arranged on a target head of a pulse laser deposition system; the distance between the target and the substrate is 40-90 mm;
the mass percentage content of Sb doping is more than 0 and less than or equal to 30 percent;
(3) pumping the background vacuum degree of the pulse laser deposition system to 3.0 x 10-3Introducing oxygen which is more than 0 and less than or equal to 50Pa as growth gas below Pa, and depositing at the substrate temperature of 200-700 ℃ to obtain an ATO thin film layer with the thickness of 50-1000 nm;
(4) taking out the substrate, covering the surface of the ATO layer by using a mask plate, reserving the position of a bottom electrode, and then placing the substrate on a sample table of a pulse laser deposition system;
(5) respectively loading BTS (base transceiver station) and BZT target materials onto a target head of a pulsed laser deposition system;
(6) vacuum pumping the background of the pulsed laser deposition system to 1.0 × 10-3Pa or less, heating the substrate to 400-700 deg.C, and using 0-50 Pa O2As a growth gas, depositing to obtain a BTS thin film layer, wherein the thickness of the BTS thin film is 100-500 nm; then using 0-50 Pa O2As a growth gas, depositing to obtain a BZT thin film layer with the thickness of 100nm-500 nm; finally, O with the pressure of 0-50 Pa is used2As a growth gas, depositing to obtain a BTS thin film layer, wherein the thickness of the BTS thin film is 100-500 nm;
(7) and taking out a sample, and preparing a metal electrode on the surfaces of the BTS film and the bottom electrode ATO layer by using a mask plate to realize the integral preparation of the flexible BTS/BZT/BTS multilayer film varactor.
2. The method for preparing the flexible BTS/BZT/BTS multilayer thin film varactor as claimed in claim 1, wherein the thickness of the copper foil in the step (1) is 1 micron to 1 mm, the purity is not less than 98%, and the surface roughness is not more than 300 nm.
3. The method for preparing the flexible BTS/BZT/BTS multilayer thin film varactor as claimed in claim 1, wherein the Sb doping content in the step (2) is 3-20% by mass.
4. The method for preparing a flexible BTS/BZT/BTS multilayer thin film varactor as claimed in claim 1, wherein the target material of the step (2) or the step (5) is a product which is made by a conventional preparation method or is commercially available.
5. The method of claim 1, wherein the ATO of step (3) and the thickness of the BTS, BZT and BTS thin film layers of step (6) are controlled by adjusting fabrication process parameters or deposition time.
CN201810267139.0A 2018-03-28 2018-03-28 Preparation method of flexible BTS/BZT/BTS multilayer thin film varactor Expired - Fee Related CN108531867B (en)

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