CN108428640B - Preparation method of device for testing electric heating effect of ferroelectric film - Google Patents
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- 238000012360 testing method Methods 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000005485 electric heating Methods 0.000 title description 5
- 239000010408 film Substances 0.000 claims abstract description 77
- 238000000034 method Methods 0.000 claims abstract description 51
- 230000008569 process Effects 0.000 claims abstract description 23
- 239000010409 thin film Substances 0.000 claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 10
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- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 10
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 10
- 229910020696 PbZrxTi1−xO3 Inorganic materials 0.000 claims abstract description 7
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- 238000001259 photo etching Methods 0.000 claims description 18
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
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Abstract
The invention discloses a preparation method of a device for testing the electrothermal effect of a ferroelectric film. The device obtained by the invention is provided with Si/Si3N4/SiO2/TiO2/LaNiO3(LNO)/PbZrxTi1‑xO3In the device, an electric field is respectively applied to the LNO and the Pt electrodes to polarize the PZT thin film, temperature change caused by polarization is represented by Pt resistance change on the surface of the PZT, and temperature change in the polarization process of the ferroelectric thin film is obtained by correcting the temperature of the change value of the Pt resistance, so that guarantee can be provided for researching the electrothermal effect of the ferroelectric thin film.
Description
Technical Field
The invention relates to a preparation method of a ferroelectric material, in particular to a preparation method of a device for testing the electrothermal effect of a ferroelectric film.
Background
The main working substance of the mechanical gas circulation refrigerator is freon, which causes serious pollution to the environment, so that the exploration and development of a new refrigerating technology without freon are important research subjects faced by the scientific and technological world. One possible approach is to find suitable ferroelectric materials to develop ferroelectric depolarizing refrigerators. Compared with the traditional refrigeration, the refrigerator made by the electric heating effect of the ferroelectric material has the advantages of simple structure, low cost, no pollution, high energy conversion rate and the like.
The principle of ferroelectric refrigeration is to utilize the inverse pyroelectric Effect-electrothermal Effect (i.e. the phenomenon that the temperature of a ferroelectric material changes when an external electric field is applied to the ferroelectric material under adiabatic conditions. If the reverse electric field is applied to the ferroelectric body to depolarize, the temperature of the ferroelectric body is lowered, which is called adiabatic depolarization refrigeration. The electrothermal effect of the salt was reported by Kobeko as early as the 30 s of the 20 th century, but not until the 60 s of the 20 th century, much more has been reported about the electrothermal effect of ferroelectric ceramics and single crystal materials. However, since a sufficiently large electric field cannot be applied to the ferroelectric material, a main approach to improve the electrothermal effect is to make the ferroelectric material thin.
In recent years, the research on the electrothermal effect of the ferroelectric film has a series of major breakthroughs. The journal of Science reports PbZr of Cambridge university, England0.95Ti0.05O3The research work of the film electrothermal effect shows that under the action of an external electric field, PbZr0.95Ti0.05O3The film produces a temperature change of up to 12 c around the ferroelectric-paraelectric phase transition temperature. In addition, another breakthrough in the study of giant electrothermal effect of ferroelectric thin film is in the field of organic ferroelectric polymers. Neese et al found that the organic ferroelectric polymer material achieved a change in electrothermal temperature as high as 12K around room temperature. However, these electrothermal effects (the amount of change in absolute temperature under adiabatic conditions) are calculated from a thermodynamic theory using a temperature-dependent rate-of-change curve of ferroelectric polarization. Therefore, the device for testing the electrothermal effect of the ferroelectric film is prepared, and not only is an experimental means for testing the electrothermal effect of the ferroelectric film provided, but also a foundation is provided for further researching the microscopic mechanism of the electrothermal effect of the ferroelectric film.
Disclosure of Invention
The invention aims to provide a preparation method of a device for testing the electrothermal effect of a ferroelectric film, and provides a foundation for researching the microscopic mechanism of the electrothermal effect of the ferroelectric film.
The technical scheme of the invention is as follows:
a method for preparing a device for testing the electrothermal effect of ferroelectric film, which has Si/Si3N4/SiO2/TiO2/LaNiO3(LNO)/PbZrxTi1-xO3The preparation method of the (PZT)/Pt heat-insulating micro-bridge structure comprises the following steps:
(1) sequentially preparing SiO on Si substrate2、Si3N4Film, buffer layer TiO2A film, a bottom electrode LNO film and a ferroelectric film; wherein the LNO film is prepared by a sol-gel method and annealed by a rapid annealing method;
(2) photoetching the surface of the ferroelectric film, and then etching the ferroelectric film to the LNO film layer through Ar ions to obtain a ferroelectric film pattern;
(3) photoetching the surfaces of the LNO film and the ferroelectric film, and then etching the surfaces to Si through Ar ions3N4A thin film layer for obtaining an LNO bottom electrode pattern;
(4) preparing SiO on the surface of the device obtained in the step (3) by adopting a chemical vapor deposition method2A dielectric film is obtained by the steps of photoetching and Ar ion etching to form the annular SiO2A dielectric film;
(5) SiO obtained in step (4) by lift-off method2Obtaining a Pt temperature sensor pattern, namely a pin part of a Pt upper electrode on the dielectric film, and preparing the Pt film by adopting a dual-ion beam sputtering method in the lift-off process;
(6) obtaining a curved Pt temperature sensor graph by adopting a lift-off method, wherein a Pt film is prepared by adopting a double-ion-beam sputtering method in the lift-off process;
(7) photoetching and corroding holes on the device obtained in the step (6), and finally preparing a microbridge to obtain the device for testing the electrothermal effect of the ferroelectric film.
Further, the substrate material Si is 100 oriented single crystal, SiO2The thickness of the film is 200-300 nm, Si3N4The thickness of the film is 100-200 nm, TiO2The thickness of the film is 30-60 nm, the thickness of the LNO is 120-200 nm, and the thickness of the PZT film is 300-500 nm.
Further, the photoetching process comprises the processes of gluing, prebaking, ultraviolet exposure, developing, washing and postbaking; wherein the rotating speed of the coating, namely spin-coating photoresist, is 3000-5000 revolutions per minute; the pre-drying temperature is 70-85 ℃, and the time is 10-30 minutes; the ultraviolet exposure time is 15-25 seconds; developing by using an AZ1500 developing solution for 1-2 minutes; the washing is carried out by adopting purified water with the resistance of 18.2 MOmega; the post-drying temperature is 90-120 ℃, and the time is 10-20 minutes.
Further, the ferroelectric film is a ferroelectric film PZT or BaTiO3A perovskite ferroelectric thin film; the ferroelectric thin film PZT is prepared by a sol-gel method, wherein a PZT precursor is prepared into a solution by taking ethylene glycol monomethyl ether or acetylacetone as a solvent.
Further, the annealing mode of the LNO is performed in three stages: the first stage is annealing at 200 ℃ for 240 s; the second stage is annealing at 380 ℃ for 240s, and the third stage is annealing at 650 ℃ for 240 s.
Further, when the bent Pt resistance temperature sensor is prepared by adopting a dual-ion beam sputtering method, the value of the Pt resistance at room temperature is 400-600 ohms.
Further, in order to ensure that the upper electrode Pt film and the lower electrode LNO film are not short-circuited, SiO needs to be prepared before the Pt pin is prepared2The preparation method of the dielectric film or the dielectric ring comprises the following steps: preparing SiO on the surface of the device obtained in the step (3) by adopting a chemical vapor deposition method2Dielectric film, and obtaining SiO by photoetching and Ar ion etching2And (5) a dielectric film pattern.
The invention has the beneficial effects that:
(1) the Pt temperature sensor is prepared on the surface of the ferroelectric film, and the temperature change of the ferroelectric film in the polarization process can be quickly and simply obtained.
(2) The invention prepares Si/Si3N4/SiO2/TiO2The device has a thermal insulation/piezoelectric transducer/Pt/LNO micro-bridge structure, wherein the obtained device takes LNO as a lower electrode, PZT as a ferroelectric film and a Pt film as an upper electrode and a temperature sensor at the same time; electric fields are respectively applied to the LNO electrode and the Pt electrode to polarize the PZT thin film, temperature change caused by polarization is represented by Pt resistance change on the surface of the PZT, temperature change in the polarization process of the ferroelectric thin film is obtained by correcting the temperature of the change value of the Pt resistance, and guarantee can be provided for researching the electric heating performance of the ferroelectric thin film.
Drawings
FIG. 1 is a block diagram of the process flow of the present invention.
Fig. 2 to 8 are top views of devices obtained in the steps of example 1.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the present invention is not limited thereto.
Example 1
The invention relates to a preparation method for testing an electrothermal effect device of a ferroelectric film, which comprises the following steps in sequence:
(1) cleaning Si substrate material to ensure the flatness of the surface, and sequentially preparing SiO on the Si wafer2(300nm)、Si3N4(200nm)、TiO2(60nm), LNO (120nm), and PZT (300nm), wherein the top view thereof is shown in FIG. 2, and 1 is a PZT thin film; SiO 22、Si3N4The film is prepared by Chemical Vapor Deposition (CVD) method, and TiO is used as a base material2LNO, PZT are prepared by a sol-gel method; the annealing mode of LNO is carried out in three stages: the first stage is annealing at 200 ℃ for 240 s; the second stage is annealing at 380 ℃ for 240s, and the third stage is annealing at 650 ℃ for 240 s;
(2) photoetching the surface of the PZT thin film, and then etching the surface of the PZT thin film to an LNO thin film through Ar ions to obtain a PZT thin film pattern; the top view is shown as 3, 2 is a PZT graph, and 3 is an LNO film displayed after Ar ion etching; the photoetching process comprises the processes of gluing, pre-baking, ultraviolet exposure, developing, washing and post-baking; wherein, the rotating speed of the coating, namely the spin coating of the photoresist, is 4000 revolutions per minute and is 20 seconds; the pre-drying temperature is 85 ℃, and the time is 10 minutes; the time of ultraviolet exposure is 17 seconds; developing by using an AZ1500 developing solution for 1 minute; the washing is carried out by adopting purified water with the resistance of 18.2 MOmega; the postbaking temperature was 120 ℃ and the time was 20 minutes. And (3) Ar ion etching process: background vacuum degree of 2 x 10-3Pa, working air pressure of 2 x 10-2Pa, ion beam energy of 500 eV;
(3) performing photoetching on the surfaces of the LNO and PZT films, wherein the photoetching process comprises the processes of gluing, prebaking, ultraviolet exposure, developing, washing and postbaking; wherein, the rotating speed of the coating, namely the spin coating of the photoresist, is 4000 revolutions per minute and is 20 seconds; the pre-drying temperature is 85 ℃, and the time is 10 minutes; the time of ultraviolet exposure is 15 seconds; developing by using an AZ1500 developing solution for 1 minute; the washing is carried out by adopting purified water with the resistance of 18.2 MOmega; the postbaking temperature was 120 ℃ and the time 15 minutes. Then etching to Si by Ar ion etching3N4And (5) film forming to obtain an LNO bottom electrode pattern. And (3) etching process: background vacuum degree: 2*10-3Pa working air pressure: 2*10- 2Pa, ion beam energy of 500 eV; the top view is shown as 4, and 3 is LNO bottom electrodeA pole pin (which is a part of the LNO film displayed after Ar ion etching and is therefore all numbered 3), and 4 is Si displayed after Ar ion etching3N4A film;
(4) preparing SiO on the surface of a device by adopting a chemical vapor deposition method2A dielectric film is obtained by the steps of photoetching and Ar ion etching to form the annular SiO2A dielectric film; the photoetching process comprises the following steps of gluing, prebaking, ultraviolet exposure, developing, washing and postbaking: wherein, the rotating speed of the coating, namely the spin coating of the photoresist, is 4000 revolutions per minute and is 20 seconds; the pre-drying temperature is 85 ℃, and the time is 10 minutes; the time of ultraviolet exposure is 15 seconds; developing by using an AZ1500 developing solution for 50 seconds; the washing is carried out by adopting purified water with the resistance of 18.2 MOmega; the postbaking temperature is 118 ℃ and the time is 18 minutes; and (3) Ar ion etching process: background vacuum degree: 2*10-3Pa working air pressure: 2*10-2Pa, ion beam energy of 500 eV; SiO in the form of a ring2The purpose of the dielectric film is to protect a Pt temperature sensor (Pt upper electrode) prepared subsequently from short circuit with the lower electrode LNO; the top view is shown in FIG. 5, where 5 is SiO in the shape of a ring2A dielectric film;
(5) obtaining a lead wire pattern of a temperature sensor (Pt upper electrode) by adopting a lift-off method, wherein Pt is prepared by adopting a double-ion beam sputtering method; the top view is shown in fig. 6, and 6 is a Pt top electrode lead pattern. The double-ion beam sputtering process comprises the following steps: background vacuum degree: 2*10-3Pa, working air pressure of 2 x 10-2Pa, firstly, cleaning the Pt target material for 1 minute by the auxiliary source, wherein the ion energy is 300eV during cleaning; then the main source sputters the Pt target material, the ion energy is 600eV, and the sputtering time is 10 minutes:
(6) obtaining a curved Pt temperature sensor graph by adopting a lift-off method, wherein Pt is prepared by adopting a double-ion beam sputtering method; the plan view is shown in fig. 7, and 7 is a curved Pt temperature sensor pattern; the double-ion beam sputtering process comprises the following steps: background vacuum degree: 2*10-3Pa, working air pressure of 2 x 10-2Pa, firstly, cleaning the Pt target material for 1 minute by the auxiliary source, wherein the ion energy is 300eV during cleaning; then the main source sputters the Pt target with ion energy of 600eV and sputtering time of 15 minutes:
(7) photoetching the surface of the device to obtain an etch hole pattern, wherein the top view of the etch hole pattern is shown as 8, and 8 is the etch hole pattern; the photoetching process comprises the following steps of gluing, prebaking, ultraviolet exposure, developing, washing and postbaking: wherein, the rotating speed of the coating, namely the spin coating of the photoresist, is 4000 revolutions per minute and is 20 seconds; the pre-drying temperature is 85 ℃, and the time is 10 minutes; the time of ultraviolet exposure is 15 seconds; developing by using an AZ1500 developing solution for 1 minute and 20 seconds; the washing is carried out by adopting purified water with the resistance of 18.2 MOmega; the postbaking temperature is 120 ℃, and the time is 20 minutes; and carrying out chemical solution corrosion to obtain a heat insulation microbridge structure, and completing the preparation of the device for testing the electric heating effect of the ferroelectric film.
Claims (6)
1. A method for preparing a device for testing the electrothermal effect of ferroelectric film, which has Si/SiO2/ Si3N4/TiO2/LaNiO3/PbZrxTi1-xO3The Pt heat-insulating micro-bridge structure is characterized in that the preparation method comprises the following steps:
(1) sequentially preparing SiO on Si substrate2、Si3N4Film, buffer layer TiO2Film, bottom electrode LNO film and ferroelectric film PbZrxTi1-xO3(ii) a The LNO film is prepared by a sol-gel method, and is annealed by a rapid annealing method, wherein the annealing is carried out in three stages: the first stage is annealing at 200 ℃ for 240 s; the second stage is annealing at 380 ℃ for 240s, and the third stage is annealing at 650 ℃ for 240 s;
(2) in a ferroelectric thin film of PbZrxTi1-xO3Photoetching the surface, and then etching the surface to an LNO film layer through Ar ions to obtain a ferroelectric film PbZrxTi1-xO3A graph;
(3) in LNO thin film and ferroelectric thin film PbZrxTi1-xO3Photoetching the surface, and then etching to Si by Ar ion3N4A thin film layer for obtaining an LNO bottom electrode pattern;
(4) preparing SiO on the surface of the device obtained in the step (3) by adopting a chemical vapor deposition method2A dielectric film formed by photolithography,Ar ion etching step to obtain annular SiO2A dielectric film;
(5) SiO obtained in step (4) by lift-off method2Obtaining a pin pattern of the Pt temperature sensor on the dielectric film, and preparing the Pt film by adopting a double-ion-beam sputtering method in the lift-off process;
(6) obtaining a curved Pt temperature sensor graph by adopting a lift-off method, wherein a Pt film is prepared by adopting a double-ion-beam sputtering method in the lift-off process;
(7) photoetching and corroding holes on the device obtained in the step (6), and finally preparing a microbridge to obtain the device for testing the electrothermal effect of the ferroelectric film.
2. The method of claim 1, wherein the substrate material Si is 100-oriented single crystal, SiO2The thickness of the film is 200-300 nm, Si3N4The thickness of the film is 100-200 nm, TiO2The thickness of the film is 30-60 nm, the thickness of the LNO is 120-200 nm, and the thickness of the PZT film is 100-500 nm.
3. The method of claim 1, wherein the photolithography process comprises a process of coating, pre-baking, uv exposure, developing, rinsing, and post-baking; wherein the rotating speed of the coating, namely spin-coating photoresist, is 3000-5000 revolutions per minute; the pre-drying temperature is 70-85 ℃, and the time is 10-30 minutes; the ultraviolet exposure time is 15-25 seconds; developing by using an AZ1500 developing solution for 1-2 minutes; the washing is carried out by adopting purified water with the resistance of 18.2 MOmega; the post-drying temperature is 90-120 ℃, and the time is 10-20 minutes.
4. The method of claim 1, wherein the ferroelectric thin film is PZT or BaTiO3A perovskite ferroelectric thin film; the ferroelectric thin film PZT is prepared by a sol-gel method, wherein a PZT precursor is prepared into a solution by taking ethylene glycol monomethyl ether or acetylacetone as a solvent.
5. The method of claim 1, wherein the curved Pt resistance temperature sensor is fabricated by dual ion beam sputtering, and the Pt resistance value is 400-600 ohm at room temperature.
6. The method of claim 1, wherein SiO is prepared before preparing Pt lead2The preparation method of the dielectric film or the dielectric ring comprises the following specific steps: firstly, preparing SiO on the surface of the device obtained in the step (3) by adopting a chemical vapor deposition method2Dielectric film, and then photoetching and Ar ion etching are carried out to obtain SiO2And (5) a dielectric film pattern.
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| US5293041A (en) * | 1991-11-04 | 1994-03-08 | Honeywell Inc. | Thin film pyroelectric imaging array |
| CN1419263A (en) * | 2002-12-17 | 2003-05-21 | 华中科技大学 | Method for preparing Si base ferroelectric thin/thick film type micro-thermo-insulation structure array |
| CN1452434A (en) * | 2003-05-01 | 2003-10-29 | 清华大学 | Microacoustic device based on clamped diaphragm structure and mfg. method thereof |
| CN1693858A (en) * | 2005-05-20 | 2005-11-09 | 中国科学院上海技术物理研究所 | Absorbed layer of room-temp. ferroelectric film infrared focal plane probe and preparation method |
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|---|---|---|---|---|
| US5293041A (en) * | 1991-11-04 | 1994-03-08 | Honeywell Inc. | Thin film pyroelectric imaging array |
| CN1419263A (en) * | 2002-12-17 | 2003-05-21 | 华中科技大学 | Method for preparing Si base ferroelectric thin/thick film type micro-thermo-insulation structure array |
| CN1452434A (en) * | 2003-05-01 | 2003-10-29 | 清华大学 | Microacoustic device based on clamped diaphragm structure and mfg. method thereof |
| CN1693858A (en) * | 2005-05-20 | 2005-11-09 | 中国科学院上海技术物理研究所 | Absorbed layer of room-temp. ferroelectric film infrared focal plane probe and preparation method |
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| Title |
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| 用SiO2气凝胶做隔热层的铁电薄膜红外探测器性能与铁电薄膜层厚度的关系;林铁等;《红外与毫米波学报》;20071031;第329-335页 * |
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