CN108428640A - A kind of preparation method of test ferroelectric thin film electrocaloric effect device - Google Patents
A kind of preparation method of test ferroelectric thin film electrocaloric effect device Download PDFInfo
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Abstract
The present invention discloses a kind of preparation method of test ferroelectric thin film electrocaloric effect device.Obtained device of the present invention has Si/Si3N4/SiO2/TiO2/LaNiO3(LNO)/PbZrxTi1‑xO3(PZT) micro-bridge structure of/Pt thermal insulation, using LNO as the lower electrode of ferroelectric thin film PZT, Pt is as top electrode and temperature sensor, in the devices, electric field, which is added in respectively on LNO and Pt electrodes, makes pzt thin film polarize, and the temperature change caused by polarizing then is showed by the Pt resistance variations on the surfaces PZT, by the changing value to Pt resistance into the correction of trip temperature, to obtain the variation of the temperature in ferroelectric thin film polarization process, so as to provide guarantee for the electrocaloric effect of research ferroelectric thin film.
Description
Technical field
The present invention relates to the preparation methods of ferroelectric material, and in particular to a kind of system of test ferroelectric thin film electrocaloric effect device
Preparation Method.
Background technology
The groundwork substance of mechanical gas cycle refrigeration machine is freon, has serious pollution to environment, therefore
The new refrigeration technologies without freon are explored and developed, are the great research topics that whole world scientific and technological circle are faced.It is a kind of feasible
Approach be to find suitable ferroelectric material, develop ferroelectricity and depolarize refrigerator.Compared with conventional refrigeration, ferroelectric material is utilized
Refrigerator made of electrocaloric effect has many advantages, such as that simple in structure, at low cost, pollution-free, energy conversion rate is high.
Ferroelectricity refrigeration principle is to utilize backheating release effect-electrocaloric effect (Electrocaloric Effect), that is, is existed
When applying external electric field to ferroelectric material under adiabatic condition, the phenomenon that temperature changes.If thermal insulation, which applies reversed electric field, makes iron
Electric body depolarising, then ferroelectricity temperature reduction, referred to as adiabatic depolarising are freezed.Early in the 1930s, Kobeko is just reported
The electrocaloric effect of sieve breath salt, but until in the 1960s, just having more in relation to ferroelectric ceramics and monocrystal material electric heating
The report of effect.However, since ferroelectric material can not add sufficiently large electric field, the main path of electrocaloric effect is improved
It is to make film of ferroelectric material.
The research of the electrocaloric effect of ferroelectric thin film has a series of important breakthrough in recent years.Science magazine rans
Univ cambridge uk is about PbZr0.95Ti0.05O3The research work of film electrocaloric effect, find under the action of external electric field,
PbZr0.95Ti0.05O3The temperature that film produces up to 12 DEG C near ferroelectric phase-paraelectric phase phase transition temperature changes.In addition,
Another breakthrough that the huge electrocaloric effect research of ferroelectric thin film obtains is then in organic ferroelectric polymers field.Neese et al. has found
Organic ferroelectric polymer material obtains near room temperature the variation of the electric heating temperature of up to 12K.However, these electrocaloric effects
(variable quantity of absolute temperature under adiabatic condition) utilizes iron electric polarization variation with temperature rate bent based on thermodynamic (al) theory
Line computation is found out.Therefore, the device for preparing test ferroelectric thin film electrocaloric effect provides not only test ferroelectric thin film electrocaloric effect
Laboratory facilities, also provide the foundation further to study the micromechanism of ferroelectric thin film electrocaloric effect.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of test ferroelectric thin film electrocaloric effect device, to study ferroelectricity
The micromechanism of film electrocaloric effect provides the foundation.
The technical scheme is that：
A kind of preparation method of test ferroelectric thin film electrocaloric effect device, the device have Si/Si3N4/SiO2/TiO2/
LaNiO3(LNO)/PbZrxTi1-xO3(PZT) micro-bridge structure of/Pt thermal insulation, preparation method include the following steps：
(1) it is sequentially prepared SiO on a si substrate2、Si3N4Film, buffer layer TiO2Film, hearth electrode LNO films and ferroelectricity
Film；Wherein LNO films are prepared using sol-gel method, and are annealed using Rapid Annealing Method；
(2) photoetching is carried out on ferroelectric thin film surface, then passes through Ar ion etchings to LNO film layers, obtains ferroelectric thin film
Figure；
(3) photoetching is carried out in LNO films and ferroelectric thin film surface, then passes through Ar ion etchings to Si3N4Film layer obtains
Obtain LNO hearth electrode figures；
(4) SiO is prepared on the device surface obtained by step (3) using chemical vapor deposition method2Deielectric-coating passes through light
It carves, Ar ion-etching steps, obtains the SiO of ring-shaped2Deielectric-coating；
(5) lift-off methods SiO obtained by step (4) is used2Pt temperature sensors figure, that is, Pt is obtained on deielectric-coating
The pin portions of top electrode, Pt films are prepared using double ion beam sputtered method during lift-off；
(6) lift-off methods is used to obtain the Pt temperature sensor figures of bending, Pt films during lift-off
It is prepared using double ion beam sputtered method；
(7) the photoetching etch pit on step (6) obtained device finally prepares microbridge, obtains test ferroelectric thin film electric heating effect
The device answered.
Further, wherein substrate material Si is 100 monocrystalline being orientated, SiO2The thickness of film is 200~300nm,
Si3N4The thickness of film is 100~200nm, TiO2The thickness of film is 30~60nm, and the thickness of LNO is 120~200nm, PZT
The thickness of film is 300~500nm.
Further, photoetching process includes for gluing, front baking, uv-exposure, development, flushing, dries process afterwards；Wherein, it applies
The rotating speed of glue, that is, spin coating photoresist is 3000~5000 revs/min；Pre-bake temperature is 70~85 DEG C, 10~30 minutes time；It is purple
The time of outer exposure is 15~25 seconds；It is 1~2 minute that development, which uses AZ1500 developing liquid developings, time,；Flushing use resistance for
The pure water of 18.2M Ω carries out；It is 90~120 DEG C to dry temperature afterwards, and the time is 10~20 minutes.
Further, ferroelectric thin is ferroelectric thin film PZT or BaTiO3Perovskite ferroelectric film；Ferroelectric thin film PZT is using molten
Prepared by glue-gel method, wherein PZT presomas are configured to solution using ethylene glycol monomethyl ether or acetylacetone,2,4-pentanedione as solvent.
Further, the annealing way of LNO is that three phases is divided to carry out：First stage is the 240s that anneals at 200 DEG C；Second
Stage is the 240s that anneals at 380 DEG C, and the phase III is the 240s that anneals at 650 DEG C.
Further, when preparing forniciform Pt resistance temperature sensor using double ion beam sputtered method, Pt at room temperature
The value of resistance is 400~600 ohm.
Further, it in order to ensure that top electrode Pt films and lower electrode LNO films be not short-circuit, is needed before preparing Pt pins
Prepare SiO2Deielectric-coating or dielectric ring, preparation method are：Using chemical vapor deposition method in step (3) obtained device surface
Prepare SiO2Deielectric-coating obtains SiO by photoetching and Ar ion etchings2Medium film pattern.
The beneficial effects of the present invention are：
(1) present invention prepares Pt temperature sensors on ferroelectric thin film surface, can quickly, simply obtain ferroelectric thin film in pole
Temperature change during change.
(2) present invention is prepared into Si/Si3N4/SiO2/TiO2The micro-bridge structure of/LNO/PZT/Pt thermal insulation, obtained device with
LNO is lower electrode, and PZT is ferroelectric thin film, and Pt films are used as top electrode and temperature sensor simultaneously；Electric field be added in respectively LNO and
Pzt thin film is set to polarize on Pt electrodes, the temperature change caused by polarizing then is showed by the Pt resistance variations on the surfaces PZT, by right
The correction of the changing value of Pt resistance into trip temperature to obtain temperature change in ferroelectric thin film polarization process can be to grind
The electric heating property for studying carefully ferroelectric thin film provides guarantee.
Description of the drawings
Fig. 1 is the process flow diagram of the present invention.
Fig. 2 to Fig. 8 is respectively the vertical view of 1 each step obtained device of embodiment.
Specific implementation mode
The present invention is described in further details with reference to specific embodiment, but the present invention is not limited thereto.
Embodiment 1
The present invention tests the preparation method of ferroelectric thin film electrocaloric effect device, and specific steps are followed successively by：
(1) Si substrate materials are cleaned up to the flatness for ensureing its surface, SiO is sequentially prepared in Si on pieces2
(300nm)、Si3N4(200nm)、TiO2(60nm), LNO (120nm), PZT (300nm), as indicated with 2,1 is thin for PZT for vertical view
Film；SiO2、Si3N4Film is prepared using chemical vapour deposition technique, TiO2, LNO, PZT are prepared using sol-gel method；LNO's
Annealing way is that three phases is divided to carry out：First stage anneals 240s at a temperature of being 200 DEG C；Second stage is to anneal at 380 DEG C
240s, phase III are the 240s that anneals at 650 DEG C；
(2) photoetching is carried out on pzt thin film surface, then passes through Ar ion etchings to LNO films, obtains pzt thin film figure；
As indicated at 3,2 be PZT figures, the 3 LNO films to be shown after Ar ion etchings to its vertical view；Photoetching process includes to apply
Glue, uv-exposure, development, flushing, dries process at front baking afterwards；Wherein, the rotating speed of gluing, that is, spin coating photoresist is 4000 revs/min,
Rotation 20 seconds；Pre-bake temperature is 85 DEG C, 10 minutes time；The time of uv-exposure is 17 seconds；Development uses AZ1500 developer solutions
Development, time are 1 minute；It rinses and resistance is used to be carried out for the pure water of 18.2M Ω；It is 120 DEG C to dry temperature afterwards, and the time is 20 points
Clock.The technique of Ar ion etchings：Background vacuum is 2*10-3Pa, operating air pressure 2*10-2Pa, ion beam energy 500eV；
(3) carry out photoetching on LNO and pzt thin film surface, photoetching process include for gluing, front baking, uv-exposure, development,
It rinses, dry process afterwards；Wherein, the rotating speed of gluing, that is, spin coating photoresist is 4000 revs/min, is rotated 20 seconds；Pre-bake temperature is 85
DEG C, 10 minutes time；The time of uv-exposure is 15 seconds；It is 1 minute that development, which uses AZ1500 developing liquid developings, time,；It rinses
Resistance is used to be carried out for the pure water of 18.2M Ω；It is 120 DEG C to dry temperature afterwards, and the time is 15 minutes.Then pass through Ar ion etchings
It is etched to Si3N4Film obtains LNO hearth electrode figures.The technique of etching：Background vacuum：2*10-3Pa operating air pressures：2*10- 2Pa, ion beam energy 500eV；As indicated at 4,3 be that (it is to show after Ar ion etchings to LNO hearth electrodes pin to its vertical view
A part for the LNO films come, therefore marked as 3), 4 Si to be shown after Ar ion etchings3N4Film；
(4) chemical vapor deposition method is used to prepare SiO in device surface2Deielectric-coating is walked by photoetching, Ar ion etchings
Suddenly, the SiO of ring-shaped is obtained2Deielectric-coating；Photoetching process includes for gluing, front baking, uv-exposure, development, flushing, dried afterwards
Journey：Wherein, the rotating speed of gluing, that is, spin coating photoresist is 4000 revs/min, is rotated 20 seconds；Pre-bake temperature is 85 DEG C, and the time 10 divides
Clock；The time of uv-exposure is 15 seconds；It is 50 seconds that development, which uses AZ1500 developing liquid developings, time,；Flushing use resistance for
The pure water of 18.2M Ω carries out；It is 118 DEG C to dry temperature afterwards, and the time is 18 minutes；Ar ion etch process：Background vacuum：2*
10-3Pa operating air pressures：2*10-2Pa, ion beam energy 500eV；The SiO of ring-shaped2The purpose of deielectric-coating is the follow-up system of protection
Standby Pt temperature sensors (Pt top electrodes) and lower electrode LNO be not short-circuit；As figure 5 illustrates, 5 be the SiO of ring-shaped to its vertical view2It is situated between
Plasma membrane；
(5) lift-off methods is used to obtain the lead figure of temperature sensor (Pt top electrodes), wherein Pt using it is double from
It is prepared by beamlet sputtering method；As indicated with 6,6 be Pt top electrode lead figures to its vertical view.Double ion beam sputtered technique is：Background
Vacuum degree：2*10-3Pa, operating air pressure 2*10-2Pa, first auxiliary source cleaning Pt targets 1 minute, ion energy is when cleaning
300eV；Then main source sputters Pt targets, ion energy 600eV, and sputtering time is 10 minutes：
(6) lift-off methods are used to obtain forniciform Pt temperature sensors figure, wherein Pt is splashed using double-ion beam
It is prepared by shooting method；As shown with 7,7 be forniciform Pt temperature sensors figure to its vertical view；Double ion beam sputtered technique is：This
Bottom vacuum degree：2*10-3Pa, operating air pressure 2*10-2Pa, first auxiliary source cleaning Pt targets 1 minute, ion energy is when cleaning
300eV；Then main source sputters Pt targets, ion energy 600eV, and sputtering time is 15 minutes：
(7) photoetching is carried out in device surface, obtains corrosion hole pattern, as depicted in figure 8,8 be corrosion hole pattern to vertical view；Light
Carving technology includes for gluing, front baking, uv-exposure, development, flushing, dries process afterwards：Wherein, the rotating speed of gluing, that is, spin coating photoresist
It is 4000 revs/min, rotates 20 seconds；Pre-bake temperature is 85 DEG C, 10 minutes time；The time of uv-exposure is 15 seconds；Development is adopted
With AZ1500 developing liquid developings, the time is 20 seconds 1 minute；It rinses and resistance is used to be carried out for the pure water of 18.2M Ω；After dry temperature
It it is 120 DEG C, the time is 20 minutes；Chemical solution corrosion is carried out, heat-insulated microbridge structure is obtained, completes test ferroelectric thin film electric heating effect
Answer the preparation of device.
Claims (7)
1. a kind of preparation method of test ferroelectric thin film electrocaloric effect device, the device have Si/Si3N4/SiO2/TiO2/
LaNiO3/PbZrxTi1-xO3The micro-bridge structure of/Pt thermal insulation, which is characterized in that preparation method includes the following steps：
(1) it is sequentially prepared SiO on a si substrate2、Si3N4Film, buffer layer TiO2Film, hearth electrode LNO films and ferroelectric thin film
PbZrxTi1-xO3；Wherein LNO films are prepared using sol-gel method, and are annealed using Rapid Annealing Method；
(2) in ferroelectric thin film PbZrxTi1-xO3Surface carries out photoetching, then passes through Ar ion etchings to LNO film layers, obtains iron
Conductive film PbZrxTi1-xO3Figure；
(3) in LNO films and ferroelectric thin film PbZrxTi1-xO3Surface carries out photoetching, then passes through Ar ion etchings to Si3N4Film
Layer obtains LNO hearth electrode figures；
(4) SiO is prepared on the device surface obtained by step (3) using chemical vapor deposition method2Deielectric-coating passes through photoetching, Ar
Ion-etching step obtains the SiO of ring-shaped2Deielectric-coating；
(5) lift-off methods SiO obtained by step (4) is used2The pin figure that Pt temperature sensors are obtained on deielectric-coating,
Pt films are prepared using double ion beam sputtered method during lift-off；
(6) lift-off methods are used to obtain the Pt temperature sensor figures of bending, Pt films use during lift-off
It is prepared by double ion beam sputtered method；
(7) the photoetching etch pit on step (6) obtained device finally prepares microbridge, obtains test ferroelectric thin film electrocaloric effect
Device.
2. the preparation method of test ferroelectric thin film electrocaloric effect device according to claim 1, which is characterized in that wherein serve as a contrast
Bottom material Si is 100 monocrystalline being orientated, SiO2The thickness of film is 200~300nm, Si3N4The thickness of film be 100~
200nm, TiO2The thickness of film is 30~60nm, and the thickness of LNO is 120~200nm, the thickness of pzt thin film is 100~
500nm。
3. the preparation method of test ferroelectric thin film electrocaloric effect device according to claim 1, which is characterized in that photoetching work
Skill includes for gluing, front baking, uv-exposure, development, flushing, dries process afterwards；Wherein, the rotating speed of gluing, that is, spin coating photoresist is
3000~5000 revs/min；Pre-bake temperature is 70~85 DEG C, 10~30 minutes time；The time of uv-exposure is 15~25 seconds；
It is 1~2 minute that development, which uses AZ1500 developing liquid developings, time,；It rinses and resistance is used to be carried out for the pure water of 18.2M Ω；Afterwards
It is 90~120 DEG C to dry temperature, and the time is 10~20 minutes.
4. the preparation method of test ferroelectric thin film electrocaloric effect device according to claim 1, which is characterized in that ferroelectric thin
Film is PZT or BaTiO3Perovskite ferroelectric film；Ferroelectric thin film PZT using sol-gel method prepare, wherein PZT presomas with
Ethylene glycol monomethyl ether or acetylacetone,2,4-pentanedione are that solvent is configured to solution.
5. the preparation method of test ferroelectric thin film electrocaloric effect device according to claim 1, which is characterized in that LNO's
Annealing way is that three phases is divided to carry out：First stage anneals 240s at a temperature of being 200 DEG C；Second stage is to anneal at 380 DEG C
240s, phase III are the 240s that anneals at 650 DEG C.
6. the preparation method of test ferroelectric thin film electrocaloric effect device according to claim 1, which is characterized in that using double
When ion beam sputtering method prepares forniciform Pt resistance temperature sensor, the value of Pt resistance is 400~600 ohm at room temperature.
7. the preparation method of test ferroelectric thin film electrocaloric effect device according to claim 1, which is characterized in that preparing
It needs to prepare SiO before Pt pins2Deielectric-coating or dielectric ring, preparation method are specially：Chemical vapor deposition method is used first
SiO is prepared in step (3) obtained device surface2Deielectric-coating obtains SiO then by photoetching and Ar ion etchings2Deielectric-coating figure
Shape.
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Cited By (1)
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| CN109913803A (en) * | 2019-03-19 | 2019-06-21 | 中国科学院兰州化学物理研究所 | A kind of preparation method patterning the hot component of resistance thin-film electro |
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