CN102260073A - Zinc-oxide-based low-voltage voltage-sensitive ceramic thin film material and preparation method thereof - Google Patents
Zinc-oxide-based low-voltage voltage-sensitive ceramic thin film material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to zinc oxide voltage-sensitive ceramics and specifically relates to a zinc-oxide-based low-voltage voltage-sensitive ceramic thin film material and a preparation method thereof. The thin film has a thickness of 1-3 mu m. The preparation method comprises the following steps: proportioning the following materials in percentage by mol: 95-98% of ZnO used as a main material, and 0.1-1.0% of Bi2O3, 0.1-1.0% of Sb2O3, 0.1-1.0% of Co2O3, 0.1-1.0% of Cr2O3 and 0.1-1.0% of MnO2 which are used as voltage-sensitive functional additives; carrying out ball milling, drying, granulating, pressing into a biscuit, and sintering into a sputtering target; and preparing the zinc-oxide-based low-voltage voltage-sensitive ceramic thin film material by a magnetron sputtering method. The voltage-sensitive voltage of the obtained thin film material is 2.03-4.84 V, the non-linear coefficient is 15.42-19.67, and the leakage current density is 0.24-0.83 mu A/mm<2>. The zinc-oxide-based low-voltage voltage-sensitive thin film material provided by the invention can be used for inhibiting transient high voltage and absorbing surge electric energy in integrated circuits.
Description
Technical field
The present invention relates to zinc oxide pressure-sensitive ceramic, specifically Zinc oxide-base low voltage varistor ceramics thin-film material and preparation method.
Background technology
Zinc oxide is a kind of important functional material and novel II-VI family semiconductor material with wide forbidden band; it have 3.37eV under the room temperature direct band gap and the 60meV exciton bind energy; good electromechanical coupling and lower electronics induce defective; has a broad-band gap as a kind of; low-k; high chemical stability and excellent piezoelectricity; the functional materials of photoelectric characteristic is widely used in a lot of fields; the epitaxial growth temperature of ZnO film is lower; help reducing equipment cost; suppress the solid phase external diffusion; improve film quality; doping also easy to implement; ZnO varistor is a kind of electronic component that is widely used in various circuit overcurrent protections; and the ZnO film of C axle orientation has significant photoelectricity and piezoelectric effect, often is used to device for non-linear optical; luminescent device and piezoelectric transducer spare.
The preparation method of zinc oxide-based ceramic film is more, mainly contains molecular beam epitaxy (MBE), metal organic vapor phase epitaxy (MOCVD), sol-gel method (Sol-gel), magnetron sputtering method etc.
Molecular beam epitaxy is the extension film-forming method that a kind of new development is got up; it also is a kind of special technique for vacuum coating; it is under UHV condition; the molecular beam of film composition element directly is sprayed onto substrate surface; thereby form the technology of epitaxial film; the ZnO film MBE of growing high-quality mainly contains laser-enhanced type and microwave enhanced two kinds; the general Sapphire Substrate that adopts; molecular beam epitaxy can be grown, and high C axle is orientated, high-quality ZnO film; but complex process, apparatus expensive, the speed of growth are slow, are unfavorable for large-scale production.
Metal organic vapor phase epitaxy is that the organometallic compound that a kind of utilization contains Zn is the Zn source, the cad technique of vaporization under certain temperature condition, decomposition and sedimentary vapor phase epitaxial growth film, the mocvd method quality of forming film is good, and can realize high-speed, big area, evenly, multi-disc one secondary growth, meet the industrialized development requirement, the shortcoming of mocvd method is a raw material unstable chemcial property, poisonous and cost an arm and a leg, and tail gas needs Special Equipment to handle.
Sol-gel method is to adopt to lift or organosol that lacquering technique will contain zincum salts evenly is applied on the substrate to produce the technology of ZnO film, and this technology realizes the preparation to the ZnO film of multi-element doping easily.Yet its quality of forming film is not so good, occurs crackle easily.
Magnetron sputtering method is research and most widely used technology, and magnetron sputtering has the following advantages: the particle energy that (1) sputters is tens electron-volts, and energy is big, film/basic good bonding strength, and film forming is fine and close; (2) can realize the sputtering sedimentation of large-area target; (3) can be used for refractory metal, alloy and compound film forming; (4) sputter rate height, substrate heats up little.
Domestic and international many scholars are doing a lot of work aspect the preparation ZnO pressure-sensitive film, and main achievement is as follows: Y. Suzuoki etc. utilizes radio frequency sputtering method to deposit ZnO/Bi on glass substrate
2O
3Bilayer film, thickness 1 μ m/0.3 μ m, pressure sensitive voltage be less than 10V, and have bigger nonlinear factor; N. Horio etc. utilizes radio frequency sputtering method to prepare ZnO/Pr
6O
11Double-deck pressure-sensitive film, thickness is 600nm/400nm, and pressure sensitive voltage is 20V, and nonlinear factor α value is 10; Jia Rui etc. utilize the Bi of sol-gel spray heating decomposition preparation
2O
3Etc. adulterated ZnO film, thickness is 3.25~8.41 μ m, and pressure sensitive voltage is 13.58~25.31V, and nonlinear factor α value is 7.99~22.38; Lu Hui etc. utilize direct current geseous discharge activation response evaporation coating technique, carrying out on the vacuum plating unit of the transformation of the way, is evaporation source with the pure metal zinc powder, heats substrate under the high vacuum background, feed the oxygen of certain atmospheric pressure value, and discharge ring added negative voltage, and the plasma body glow discharge that between evaporation source and substrate, produces oxygen, the zinc of evaporation is oxidized, on substrate, deposit ZnO film, film thickness is 0.3 μ m, and pressure sensitive voltage is 25V, and nonlinear factor α value is 9; Huang Yanqiu etc. utilize novel sol-gel method, with Bi
2O
3, Sb
2O
3Adulterated ZnO nano-powder is dispersed in and contains Zn (CH
3COO)
2, Bi (NO
3)
3And Sb
2O
3Colloidal sol in make precursor solution, adopt the method for spin coating to prepare the ZnO pressure-sensitive film, thickness is about 3 μ m, nonlinear factor α value is 6.2, pressure sensitive voltage is 5V, leakage current is 8 μ A; The novel sol-gel method of application such as Jiang Shenglin prepares the ZnO ceramic membrane, and its pressure sensitive voltage is lower than 5V, and nonlinear factor can reach 20, and leakage current density is less than 0.5 μ A/mm
2But the pressure sensitive voltage of the ZnO pressure-sensitive film that above-mentioned preparation method prepares is higher, and nonlinear factor is on the low side, is not suitable for requiring pressure sensitive voltage low as in the microelectronic industry technical requirements that nonlinear factor is high.
Summary of the invention
One of purpose of the present invention provides a kind of preparation method of Zinc oxide-base low voltage varistor ceramics thin-film material.
It is good that two of purpose of the present invention provides a kind of product performance, directly the Zinc oxide-base low-pressure pressure-sensitive ceramic material film of moulding on the Si sill.
To achieve these goals, the present invention is by the following technical solutions:
A kind of Zinc oxide-base low voltage varistor ceramics thin-film material, the thickness 1 μ m-3 μ m of film, it is characterized in that: described thin-film material comprises that by mole per-cent following component: ZnO95%~98% is a material of main part, Bi
2O
3, Sb
2O
3, Co
2O
3, Cr
2O
3And MnO
2Being pressure-sensitive functional additive, respectively is 0.1%~1.0%, and the pressure sensitive voltage of described thin-film material is 2.03~4.84V, and nonlinear factor is 15.42~19.67, and leakage current density is 0.24~0.83 μ A/mm
2
The preparation method of above-mentioned Zinc oxide-base low voltage varistor ceramics thin-film material is characterized in that:
1) utilize the conventional sintering legal system to be equipped with the zinc oxide-based ceramic target: to join according to following molar percentage component
Material, ZnO95%~98% is a material of main part, Bi
2O
3, Sb
2O
3, Co
2O
3, Cr
2O
3And MnO
2Being pressure-sensitive functional additive, respectively is 0.1%~1.0%; The ball milling after drying is pressed into biscuit after the granulation, sinter sputtering target material into.
2) utilize magnetron sputtering method to prepare Zinc oxide-base low voltage varistor ceramics thin-film material: substrate material is selected single face for use
The Si(111 of polishing) substrate, after the cleaning, good seal is stand-by; Cleaned substrate is put into metal spraying equipment,
Vacuumize the back at Si(111) polished surface of substrate spraying 5~10min, the preparation bottom electrode; What experiment was adopted spatters
The mode of penetrating is a rf magnetron sputtering, and sputter gas is a high purity argon, and argon flow amount is 30sccm, coating chamber
The base vacuum degree reaches 10
-5Pa, operating air pressure are 1.5~3.5Pa, and target-Ji spacing is 90mm, with Si(111)
The spraying of substrate faces up and is clamped on the pallet as substrate, and substrate does not heat, and sputtering time is 0.5~2h,
Sputtering power is 200~300W, and annealing temperature is 800 ℃~900 ℃, and annealing time is 0.5~2h, will move back
Film behind the fire is covered with aluminium foil, puts into metal spraying equipment, vacuumizes back spraying 5~10min, the preparation top
The utmost point promptly gets Zinc oxide-base low voltage varistor ceramics thin-film material.
The preparation method of above-mentioned Zinc oxide-base low voltage varistor ceramics thin-film material is characterized in that: the metal spraying area of upper current conducting cap is about 10mm
2
The preparation method of above-mentioned Zinc oxide-base low voltage varistor ceramics thin-film material, it is characterized in that: adopt agate ball, stainless cylinder of steel, dehydrated alcohol is a ball-milling medium, agate ball: the batching powder: the mass ratio of dehydrated alcohol is 2.5:1:1, wet-milling 4~7h in planetary high-energy ball mill, rotating speed are 200~300rpm; The slurry that ball milling is good becomes dry powder at 70 ℃ of insulation 24 h; After adding massfraction in the dry powder and be 2% the PVA aqueous solution, suppress, make powder become base with 60~80MPa pressure; Base substrate is put into the Si-Mo rod high-temperature electric resistance furnace, speed with 5 ℃/min rises to 500 ℃~600 ℃ from room temperature earlier, be incubated 120min in the air atmosphere, the back rises to 850 ℃~950 ℃ of sintering temperatures with the speed of 5 ℃/min, be incubated 120min in the air atmosphere, cool to room temperature with the furnace, promptly get sputtering target material.
The preparation method of above-mentioned Zinc oxide-base low voltage varistor ceramics thin-film material, it is characterized in that: Si(111) cleaning step of substrate is as follows: substrate is put into deionized water, ultrasonic cleaning 5~10min, twice; Ultrasonic cleaning 5~10min in acetone, twice; Ultrasonic cleaning 5~10min in dehydrated alcohol, twice; The substrate that cleans up is put into the beaker that fills dehydrated alcohol, and good seal is stand-by.
The present invention is by adjusting the rational proportion of pressure-sensitive functional additive, zinc oxide-based ceramic film in conjunction with preparation method's preparation, the Zinc oxide-base low voltage varistor ceramics thin-film material that it obtains at 800 ℃~900 ℃ annealing 0.5h~2h, pressure sensitive voltage is 2.03~4.84V, nonlinear factor is 15.42~19.67, and leakage current density is 0.24~0.83 μ A/mm
2, Zinc oxide-base low voltage varistor ceramics thin-film material of the present invention can be used for suppressing in the unicircuit instantaneous pressure, absorbs the surge electric energy.
Embodiment
EXAMPLE l
1) utilize the conventional sintering legal system to be equipped with the zinc oxide-based ceramic target: to prepare burden ZnO96.2%, Bi according to following molar percentage component
2O
31.0%, Sb
2O
31.0%, Co
2O
30.8%, Cr
2O
30.5%, MnO
20.5%; Adopt agate ball, stainless cylinder of steel, dehydrated alcohol is a ball-milling medium, agate ball: the batching powder: the mass ratio of dehydrated alcohol is 2.5:1:1, and wet-milling 7h in planetary high-energy ball mill, rotating speed are 250rpm; The slurry that ball milling is good becomes dry powder at 70 ℃ of insulation 24 h; After adding massfraction in the dry powder and be 2% the PVA aqueous solution,, make powder become base with the compacting of 60MPa pressure; Base substrate is put into the Si-Mo rod high-temperature electric resistance furnace, speed with 5 ℃/min rises to 600 ℃ from room temperature earlier, be incubated 120min in the air atmosphere, the back rises to 950 ℃ of sintering temperatures with the speed of 5 ℃/min, be incubated 120min in the air atmosphere, cool to room temperature with the furnace, promptly get the sputtering target material of φ 50 mm * 3mm.
2) utilize magnetron sputtering method to prepare Zinc oxide-base low voltage varistor ceramics thin-film material: substrate material is selected the Si(111 of single-sided polishing for use) substrate, its cleaning step is as follows: substrate is put into deionized water, ultrasonic cleaning 5~10min, twice; Ultrasonic cleaning 5~10min in acetone, twice; Ultrasonic cleaning 5~10min in dehydrated alcohol, twice; The substrate that cleans up is put into the beaker that fills dehydrated alcohol, and good seal is stand-by; Cleaned substrate is put into metal spraying equipment, vacuumize back spraying 5~10min, the preparation bottom electrode, it is rf magnetron sputtering that the sputter mode is adopted in experiment, sputtering target material is of a size of φ 50 mm * 3mm, sputter gas is high purity argon (Ar purity is 99.999%), and argon flow amount is 30sccm, and coating chamber base vacuum degree reaches 10
-5Pa, operating air pressure are 3.5Pa, and target-Ji spacing is 90mm, with Si(111) spraying of substrate faces up and is clamped on the pallet as substrate, substrate does not heat, and sputtering time is 2h, sputtering power 250W, annealing temperature is 800 ℃, annealing time is 1h, and the film after the annealing is partly covered with aluminium foil, puts into metal spraying equipment, vacuumize back spraying 5~10min, the preparation upper current conducting cap.
The Zinc oxide-base low voltage varistor ceramics film of present embodiment made is through performance test, and nonlinear factor is 19.67, and pressure sensitive voltage is 4.84V, and leakage current density is 0.24 μ A/mm
2
Embodiment 2
1) utilize the conventional sintering legal system to be equipped with the zinc oxide-based ceramic target: to prepare burden ZnO96.4%, Bi according to following molar percentage component
2O
30.8%, Sb
2O
31.0%, Co
2O
30.8%, Cr
2O
30.5%, MnO
20.5%; Adopt agate ball, stainless cylinder of steel, dehydrated alcohol is a ball-milling medium, agate ball: the batching powder: the mass ratio of dehydrated alcohol is 2.5:1:1, and wet-milling 6h in planetary high-energy ball mill, rotating speed are 200rpm; The slurry that ball milling is good becomes dry powder at 70 ℃ of insulation 24 h; After adding massfraction in the dry powder and be 2% the PVA aqueous solution,, make powder become base with the compacting of 70MPa pressure; Base substrate is put into the Si-Mo rod high-temperature electric resistance furnace, speed with 5 ℃/min rises to 500 ℃ from room temperature earlier, be incubated 120min in the air atmosphere, the back rises to 900 ℃ of sintering temperatures with the speed of 5 ℃/min, be incubated 120min in the air atmosphere, cool to room temperature with the furnace, promptly get the sputtering target material of φ 50 mm * 3mm.
2) utilize magnetron sputtering method to prepare Zinc oxide-base low voltage varistor ceramics thin-film material: substrate material is selected the Si(111 of single-sided polishing for use) substrate, its cleaning step is as follows: substrate is put into deionized water, ultrasonic cleaning 5~10min, twice; Ultrasonic cleaning 5~10min in acetone, twice; Ultrasonic cleaning 5~10min in dehydrated alcohol, twice; The substrate that cleans up is put into the beaker that fills dehydrated alcohol, and good seal is stand-by; Cleaned substrate is put into metal spraying equipment, vacuumize back spraying 5~10min, the preparation bottom electrode, it is rf magnetron sputtering that the sputter mode is adopted in experiment, sputtering target material is of a size of φ 50 mm * 3mm, sputter gas is high purity argon (Ar purity is 99.999%), and argon flow amount is 30sccm, and coating chamber base vacuum degree reaches 10
-5Pa, operating air pressure are 2.5Pa, and target-Ji spacing is 90mm, with Si(111) spraying of substrate faces up and is clamped on the pallet as substrate, substrate does not heat, and sputtering time is 1.5h, sputtering power 300W, annealing temperature is 840 ℃, annealing time is 1h, and the film after the annealing is partly covered with aluminium foil, puts into metal spraying equipment, vacuumize back spraying 5~10min, the preparation upper current conducting cap.
The Zinc oxide-base low voltage varistor ceramics film of present embodiment made is through performance test, and nonlinear factor is 17.34, and pressure sensitive voltage is 3.96V, and leakage current density is 0.47 μ A/mm
2
Embodiment 3
1) utilize the conventional sintering legal system to be equipped with the zinc oxide-based ceramic target: to prepare burden ZnO96.8%, Bi according to following molar percentage component
2O
30.7%, Sb
2O
31.0%, Co
2O
30.5%, Cr
2O
30.5%, MnO
20.5%; Adopt agate ball, stainless cylinder of steel, dehydrated alcohol is a ball-milling medium, agate ball: the batching powder: the mass ratio of dehydrated alcohol is 2.5:1:1, and wet-milling 4h in planetary high-energy ball mill, rotating speed are 300rpm; The slurry that ball milling is good becomes dry powder at 70 ℃ of insulation 24 h; After adding massfraction in the dry powder and be 2% the PVA aqueous solution,, make powder become base with the compacting of 65MPa pressure; Base substrate is put into the Si-Mo rod high-temperature electric resistance furnace, speed with 5 ℃/min rises to 500 ℃ from room temperature earlier, be incubated 120min in the air atmosphere, the back rises to 850 ℃ of sintering temperatures with the speed of 5 ℃/min, be incubated 120min in the air atmosphere, cool to room temperature with the furnace, promptly get the sputtering target material of φ 50 mm * 3mm.
2) utilize magnetron sputtering method to prepare Zinc oxide-base low voltage varistor ceramics thin-film material: substrate material is selected the Si(111 of single-sided polishing for use) substrate, its cleaning step is as follows: substrate is put into deionized water, ultrasonic cleaning 5~10min, twice; Ultrasonic cleaning 5~10min in acetone, twice; Ultrasonic cleaning 5~10min in dehydrated alcohol, twice; The substrate that cleans up is put into the beaker that fills dehydrated alcohol, and good seal is stand-by; Cleaned substrate is put into metal spraying equipment, vacuumize back spraying 5~10min, the preparation bottom electrode, it is rf magnetron sputtering that the sputter mode is adopted in experiment, sputtering target material is of a size of φ 50 mm * 3mm, sputter gas is high purity argon (Ar purity is 99.999%), and argon flow amount is 30sccm, and coating chamber base vacuum degree reaches 10
-5Pa, operating air pressure are 2.0Pa, and target-Ji spacing is 90mm, with Si(111) spraying of substrate faces up and is clamped on the pallet as substrate, substrate does not heat, and sputtering time is 1h, sputtering power 300W, annealing temperature is 860 ℃, annealing time is 1.5h, and the film after the annealing is partly covered with aluminium foil, puts into metal spraying equipment, vacuumize back spraying 5~10min, the preparation upper current conducting cap.
The Zinc oxide-base low voltage varistor ceramics film of present embodiment made is through performance test, and nonlinear factor is 15.42, and pressure sensitive voltage is 2.03V, and leakage current density is 0.83 μ A/mm
2
Claims (5)
1. Zinc oxide-base low voltage varistor ceramics thin-film material, the thickness 1 μ m-3 μ m of film, it is characterized in that: described thin-film material comprises that by mole per-cent following component: ZnO95%~98% is a material of main part, Bi
2O
3, Sb
2O
3, Co
2O
3, Cr
2O
3And MnO
2Being pressure-sensitive functional additive, respectively is 0.1%~1.0%, and the pressure sensitive voltage of described thin-film material is 2.03~4.84V, and nonlinear factor is 15.42~19.67, and leakage current density is 0.24~0.83 μ A/mm
2
2. the preparation method of a kind of Zinc oxide-base low voltage varistor ceramics thin-film material as claimed in claim 1 is characterized in that:
1) utilize the conventional sintering legal system to be equipped with the zinc oxide-based ceramic target:
Prepare burden according to following molar percentage component, ZnO95%~98% is a material of main part, Bi
2O
3, Sb
2O
3, Co
2O
3, Cr
2O
3And MnO
2Being pressure-sensitive functional additive, respectively is 0.1%~1.0%; The ball milling after drying is pressed into biscuit after the granulation, sinter sputtering target material into;
2) utilize magnetron sputtering method to prepare Zinc oxide-base low voltage varistor ceramics thin-film material:
Substrate material is selected the Si(111 of single-sided polishing for use) substrate, after the cleaning, good seal is stand-by; Cleaned substrate is put into metal spraying equipment, vacuumizes the back at Si(111) polished surface of substrate spraying 5~10min, the preparation bottom electrode; What experiment was adopted spatters
The mode of penetrating is a rf magnetron sputtering, and sputter gas is a high purity argon, and argon flow amount is 30sccm, and coating chamber base vacuum degree reaches 10
-5Pa, operating air pressure are 1.5~3.5Pa, and target-Ji spacing is 90mm, with Si(111) spraying of substrate faces up and is clamped on the pallet as substrate, and substrate does not heat, and sputtering time is 0.5~2h, sputtering power is 200~300W, annealing temperature is 800 ℃~900 ℃, and annealing time is 0.5~2h, and the film after the annealing is covered with aluminium foil, put into metal spraying equipment, vacuumize back spraying 5~10min, the preparation upper current conducting cap promptly gets Zinc oxide-base low voltage varistor ceramics thin-film material.
3. the preparation method of a kind of Zinc oxide-base low voltage varistor ceramics thin-film material as claimed in claim 2 is characterized in that: the metal spraying area of upper current conducting cap is about 10mm
2
4. the preparation method of a kind of Zinc oxide-base low voltage varistor ceramics thin-film material as claimed in claim 2, it is characterized in that: adopt agate ball, stainless cylinder of steel, dehydrated alcohol is a ball-milling medium, agate ball: the batching powder: the mass ratio of dehydrated alcohol is 2.5:1:1, wet-milling 4~7h in planetary high-energy ball mill, rotating speed are 200~300rpm; The slurry that ball milling is good becomes dry powder at 70 ℃ of insulation 24 h; After adding massfraction in the dry powder and be 2% the PVA aqueous solution, suppress, make powder become base with 60~80MPa pressure; Base substrate is put into the Si-Mo rod high-temperature electric resistance furnace, speed with 5 ℃/min rises to 500 ℃~600 ℃ from room temperature earlier, be incubated 120min in the air atmosphere, the back rises to 850 ℃~950 ℃ of sintering temperatures with the speed of 5 ℃/min, be incubated 120min in the air atmosphere, cool to room temperature with the furnace, promptly get sputtering target material.
5. the preparation method of a kind of Zinc oxide-base low voltage varistor ceramics thin-film material as claimed in claim 2, it is characterized in that: Si(111) cleaning step of substrate is as follows: substrate is put into deionized water, ultrasonic cleaning 5~10min, twice; Ultrasonic cleaning 5~10min in acetone, twice; Ultrasonic cleaning 5~10min in dehydrated alcohol, twice; The substrate that cleans up is put into the beaker that fills dehydrated alcohol, and good seal is stand-by.
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CN105777107A (en) * | 2016-03-17 | 2016-07-20 | 江苏新浦电子科技有限公司 | Ceramic target for preparing conducting glass by aid of magnetron sputtering method |
CN108409306A (en) * | 2018-03-22 | 2018-08-17 | 华南理工大学 | A kind of Zinc oxide pressure-sensitive ceramic material and preparation method thereof |
CN108409306B (en) * | 2018-03-22 | 2020-10-13 | 华南理工大学 | Zinc oxide pressure-sensitive ceramic material and preparation method thereof |
CN108624853A (en) * | 2018-05-11 | 2018-10-09 | 辽宁科技大学 | A kind of iron tailings devitrified glass film and the preparation method and application thereof |
CN109988997A (en) * | 2019-03-21 | 2019-07-09 | 淮阴工学院 | Thermosensitive film and its preparation method and application |
CN114438464A (en) * | 2022-01-26 | 2022-05-06 | 中国科学院上海硅酸盐研究所 | Bi, Pr and V-free zinc oxide-based pressure-sensitive thin film material and preparation method thereof |
CN114438464B (en) * | 2022-01-26 | 2023-01-31 | 中国科学院上海硅酸盐研究所 | Bi, pr and V-free zinc oxide-based pressure-sensitive thin film material and preparation method thereof |
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