CN101777622A - LiNbO3/SiO2/diamond multilayer piezoelectric film and preparation method thereof - Google Patents

LiNbO3/SiO2/diamond multilayer piezoelectric film and preparation method thereof Download PDF

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CN101777622A
CN101777622A CN201010030152.8A CN201010030152A CN101777622A CN 101777622 A CN101777622 A CN 101777622A CN 201010030152 A CN201010030152 A CN 201010030152A CN 101777622 A CN101777622 A CN 101777622A
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diamond
diamond substrate
sio
amorphous sio
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CN101777622B (en
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王新昌
田四方
王俊喜
贾建峰
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Zhengzhou University
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Abstract

The invention relates to a LiNbO3/SiO2/diamond multilayer piezoelectric film and a preparation method thereof, efficiently solving the problems of the temperature stability of surface acoustic wave (SAW) devices and preparation of high c-axis orientated LiNbO3 thin film. The technical scheme of the invention is as follows: an amorphous SiO2 buffering layer is introduced between a diamond substrate and a LiNbO3 piezoelectric thin film. The preparation method comprises the following steps of: firstly, taking silicon as a target material on the diamond substrate, and depositing the amorphous SiO2 on the diamond substrate by a pulse laser deposition method to form an amorphous SiO2 buffering layer; secondly, heating the prepared amorphous SiO2/diamond substrate, taking the LiNbO3 as the target material, and depositing the LiNbO3 on the amorphous SiO2 buffering layer by the pulse lasers to form a composite piezoelectric thin film having the amorphous SiO2 buffering layer between the LiNbO3 piezoelectric thin film layer and the diamond substrate; and cooling down the layer to 18-25 DEG C after the LiNbO3 piezoelectric thin film layer is deposited. The invention has simple structure, advanced and scientific method and high temperature stability, and improves the working frequency of the SAW devices.

Description

LiNbO 3/ SiO 2/ diamond multilayer piezoelectric film and preparation method thereof
One, technical field
The present invention relates to piezoelectric film material, particularly a kind of LiNbO 3/ SiO 2/ diamond multilayer piezoelectric film and preparation method thereof.
Two, background technology
Along with the fast development of mobile communication technology, the frequency of utilization of surface acoustic wave (SAW) device improves constantly, and has developed into present GHz level from original M Hz level.As everyone knows, the raising of SAW device operating frequency is mainly passed through to shorten the interdigital electrode cycle or use high-sound-velocity material, yet for traditional surface acoustic wave material such as LiNbO 3, LiTaO 3Because surperficial velocity of wave is lower, the operating frequency that is issued to GHz in current process conditions is quite difficult, thereby the exploitation high-sound-velocity material becomes the technical bottleneck that improves SAW device operating frequency Deng materials such as monocrystal material or PZT series piezoelectric ceramic.
Diamond is as the fastest material of acoustic surface wave propagation in all substances, and acoustic wave propagation velocity is higher than more than the 10000m/s, is the ideal material of preparation high frequency SAW device.Yet because diamond itself does not have piezoelectricity, can't excite and receive surface acoustic wave, therefore need combine and form multi-layer film structure with piezoelectric membrane.LiNbO 3Because of its excellent piezoelectricity, electric light, acousto-optic and nonlinear optical properties, and be widely used in making in all kinds of fiber waveguides, optical switch and the SAW device.Compare LiNbO with ZnO with piezoelectrics such as AlN 3Have bigger electromechanical coupling factor, Theoretical Calculation shows c axle orientation LiNbO 3The acoustic surface wave propagation speed of/diamond multilayer structure is up to 12000m/s, electromechanical coupling factor can reach 9%[H.Nakahata, A.Hachigo, K.Higaki et al., IEEE Trans.Ultrason.Ferroelectr.Freq.Contr.42 (1995) 362.], so c axle orientation LiNbO 3/ diamond multilayer structural material has great application value and application prospect aspect broadband, the high frequency SAW device.
Yet because lattice mismatch is big between diamond and the lithium niobate, and diamond high temperature in oxygen atmosphere is easy to oxidation, thus on diamond the high c axle orientation of preparation LiNbO 3Film is difficulty very.In addition, LiNbO 3Because of having bigger temperature coefficient, will influence LiNbO 3Temperature stability and the quality and the result of use of/diamond multilayer membrane structure SAW device.H.K.Lam etc. are at diamond and LiNbO 3Introduce amorphous Al between the film 2O 3As resilient coating, adopt pulsed laser deposition technique to prepare the LiNbO of c axle orientation 3Piezoelectric membrane, but lithium phase [H.K.Lam, J.Y.Dai, H.L.W.Chan, Jpn.J.Appl.Phys.43 (2004) L706.] has appearred in the piezoelectric membrane significantly lacking.Application number be 200510014977.X patent disclosure a kind of LiNbO 3/ ZnO/ diamond multi-layered film structure surface acoustic wave device and preparation method thereof adopts radiofrequency magnetron sputtering technology growth c axle orientation LiNbO 3Piezoelectric membrane.Because LiNbO 3, ZnO, Al 2O 3With adamantine frequency-temperature coefficient TCF all less than zero (temperature coefficient of delay TCD is all greater than zero), thereby with ZnO, Al 2O 3For the temperature stability of the multi-layer film structure SAW device of resilient coating does not improve.
Three, summary of the invention
At above-mentioned situation, for overcoming the prior art defective, the present invention's purpose just provides a kind of LiNbO 3/ SiO 2/ diamond multilayer piezoelectric film and preparation method thereof, the temperature stability and the high c axle that can effectively solve the SAW device are orientated LiNbO 3Film preparation problem, the technical scheme of its solution are, at diamond substrate and LiNbO 3Introduce amorphous SiO between the piezoelectric membrane 2Resilient coating, its preparation method be, at first makes target with silicon (Si) on 200-400 ℃ diamond substrate, with pulsed laser deposition with amorphous SiO 2Be deposited on the diamond substrate, constitute amorphous SiO 2Resilient coating, amorphous SiO 2Buffer layer thickness is 0.05-0.6 μ m; Again with the amorphous SiO for preparing 2/ diamond substrate is warming up to 600-750 ℃, with LiNbO 3Be target, with pulse laser with LiNbO 3Be deposited on amorphous SiO 2On the resilient coating, LiNbO 3Deposit thickness is 0.2-3 μ m, constitutes LiNbO 3Amorphous SiO is arranged between piezoelectric thin film layer and the diamond substrate 2The composite piezoelectric film of resilient coating, SiO 2And LiNbO 3In pulsed laser deposition process, all need feed 99.99% high purity oxygen gas respectively, oxygen is pressed and is 15-70Pa, and laser single-pulse energy density is 3.0-4.5J/cm 2, the distance between target and the substrate is 3.5-6.0cm; LiNbO 3After the piezoelectric thin film layer deposition, in 99.99% high purity oxygen gas of 30-70Pa, be cooled to room temperature 18-25 ℃, the LiNbO of preparation 3Film is high c axle oriented film, and the present invention is simple in structure, method advanced person, science, and easily preparation when improving SAW device operating frequency, efficiently solves the temperature stability problem of SAW device, is the innovation on the piezoelectric membrane.
Four, description of drawings
Accompanying drawing is a structural representation of the present invention.
Five, embodiment
Below in conjunction with drawings and Examples the specific embodiment of the present invention is elaborated.
Provided by accompanying drawing, product of the present invention is at diamond substrate 1 and LiNbO 3Introduce amorphous SiO between the piezoelectric membrane 3 2 Resilient coating 2 constitutes, and its concrete preparation method is provided by following examples:
Embodiment one
1, diamond substrate (with preceding capable of washing clean) is put into pulsed laser deposition equipment vacuum chamber, be evacuated to 10 -3Pa, heated substrate to 300 ℃, (Si) makes target with silicon, and distance be 4.5cm between target and the diamond substrate, feeds 99.99% high purity oxygen gas, and oxygen is pressed and is 15Pa, usefulness pulse laser deposited amorphous SiO on diamond substrate 2Resilient coating, amorphous SiO 2Buffer layer thickness is 0.13 μ m;
2, will deposit amorphous SiO 2The diamond substrate of resilient coating is warming up to 680 ℃, feeds 99.99% high purity oxygen gas in deposition process, and oxygen is pressed and remained on 60Pa, and laser frequency is at 3Hz, with LiNbO 3Be target, distance is 3.5J/cm at 4cm with the single pulse energy metric density between target and the diamond substrate 2Laser at amorphous SiO 2Deposit thickness is the LiNbO of 0.45 μ m on the resilient coating 3Piezoelectric thin film layer;
3, LiNbO 3After piezoelectric thin film layer deposition finishes, depress in 99.99% high purity oxygen of 60Pa and to be cooled to 20 ℃, obtain the LiNbO of surfacing 3/ SiO 2/ diamond multilayer piezoelectric film, the LiNbO of preparation 3Film is high c axle oriented film, and its crystal grain dimension is 95nm, and surface average roughness is 14.3nm.
Embodiment two
1, diamond substrate (with preceding capable of washing clean) is put into pulsed laser deposition equipment vacuum chamber, be evacuated to 10 -3Pa, heating diamond substrate to 350 ℃ is made target with silicon, carries out SiO in the 99.99% high purity oxygen gas atmosphere of 15Pa 2Deposition, between target and the substrate distance at 5.7cm, be the amorphous SiO of 0.3 μ m with pulse laser deposit thickness on diamond substrate 2Resilient coating;
2, will deposit amorphous SiO 2The diamond substrate of resilient coating is warming up to 640 ℃, feeds 99.99% high purity oxygen gas in deposition process, and oxygen is pressed and remained on 40Pa, and laser frequency is at 3Hz, with LiNbO 3Make target, distance is 4J/cm at 4.5cm with the single pulse energy metric density between target and the diamond substrate 2Laser at amorphous SiO 2Deposit thickness is the LiNbO of 0.6 μ m on the resilient coating 3Piezoelectric thin film layer;
3, LiNbO 3After piezoelectric thin film layer deposition finishes, depress in 99.99% high purity oxygen of 40Pa and to be cooled to 25 ℃, obtain the LiNbO of surfacing 3/ SiO 2/ diamond multilayer piezoelectric film, the LiNbO of preparation 3Film is high c axle oriented film, and its crystal grain dimension is 105nm, and surface average roughness is 16.5nm.
To the above-mentioned product LiNbO for preparing3/SiO 2/ diamond multilayer piezoelectric film experiment showed, amorphous SiO after deliberation2Temperature coefficient to sandwich construction has compensating action, one of best means of at present multi-component oxide film growth of pulsed laser deposition technique conduct, compare with sputtering technology to have and can keep the advantages such as target and film composition be consistent, pulsed laser deposition technique is conducive to the c-axis oriented growth of film simultaneously. The present invention is at diamond and LiNbO3Introduce and LiNbO between the film3Amorphous SiO with opposite temperature coefficients2As cushion, adopt pulsed laser deposition to prepare c-axis orientation LiNbO3Piezoelectric membrane so both can suppress the high-temperature oxydation on diamond film surface in the oxygen atmosphere and improve diamond and LiNbO3Between bigger lattice mismatch issue, can improve by compensating action again simultaneously the temperature stability of multi-layer film structure. Therefore, the present invention compares with technology with current material, and the present invention has following outstanding advantage:
(1) employing and diamond and LiNbO3Amorphous SiO with opposite temperature coefficients2As cushion, but establishment diamond and LiNbO3Between bigger lattice mismatch and the problem of diamond surface high-temperature oxydation, obtain the c-axis orientation LiNbO of surfacing3Film, the while can be improved by compensating action again the temperature stability of multilayer piezoelectric film, and the temperature coefficient of this multilayer piezoelectric film can pass through amorphous SiO2Thickness compensate adjusting;
(2) this multilayer piezoelectric film can satisfy the application demand in high electromechanical coupling factor, high frequency, fields such as high-performance SAW (Surface Acoustic Wave) device that temperature stability is good.

Claims (4)

1. LiNbO 3/ SiO 2/ diamond multilayer piezoelectric film is characterized in that, at diamond substrate (1) and LiNbO 3Piezoelectric membrane has amorphous SiO between (3) 2Resilient coating (2).
2. LiNbO 3/ SiO 2The preparation method of/diamond multilayer piezoelectric film is characterized in that, at diamond substrate and LiNbO 3Introduce amorphous SiO between the piezoelectric membrane 2Resilient coating, its preparation method be, at first makes target with silicon on 200-400 ℃ diamond substrate, with pulsed laser deposition with amorphous SiO 2Be deposited on the diamond substrate, constitute amorphous SiO 2Resilient coating, amorphous SiO 2Buffer layer thickness is 0.05-0.6 μ m; Again with the amorphous SiO for preparing 2/ diamond substrate is warming up to 600-750 ℃, with LiNbO 3Be target, with pulse laser with LiNbO 3Be deposited on amorphous SiO 2On the resilient coating, LiNbO 3Deposit thickness is 0.2-3 μ m, constitutes LiNbO 3Amorphous SiO is arranged between piezoelectric thin film layer and the diamond substrate 2The composite piezoelectric film of resilient coating, SiO 2And LiNbO 3In pulsed laser deposition process, all need feed 99.99% high purity oxygen gas respectively, oxygen is pressed and is 15-70Pa, and laser single-pulse energy density is 3.0-4.5J/cm 2, the distance between target and the substrate is 3.5-6.0cm; LiNbO 3After the piezoelectric thin film layer deposition, in 99.99% high purity oxygen gas of 30-70Pa, be cooled to room temperature 18-25 ℃, the LiNbO of preparation 3Film is high c axle oriented film.
3. LiNbO according to claim 1 and 2 3/ SiO 2The preparation method of/diamond multilayer piezoelectric film is characterized in that, is realized by following steps:
(1), diamond substrate is put into pulsed laser deposition equipment vacuum chamber, be evacuated to 10 -3Pa, heated substrate to 300 ℃ is made target with silicon, and distance be 4.5cm between target and the diamond substrate, feeds 99.99% high purity oxygen gas, and oxygen is pressed and is 15Pa, usefulness pulse laser deposited amorphous SiO on diamond substrate 2Resilient coating, amorphous SiO 2Buffer layer thickness is 0.13 μ m;
(2), will deposit amorphous SiO 2The diamond substrate of resilient coating is warming up to 680 ℃, feeds 99.99% high purity oxygen gas in deposition process, and oxygen is pressed and remained on 60Pa, and laser frequency is at 3Hz, with LiNbO 3Be target, distance is 3.5J/cm at 4cm with the single pulse energy metric density between target and the diamond substrate 2Laser at amorphous SiO 2Deposit thickness is the LiNbO of 0.45 μ m on the resilient coating 3Piezoelectric thin film layer;
(3), LiNbO 3After piezoelectric thin film layer deposition finishes, depress in 99.99% high purity oxygen of 60Pa and to be cooled to 20 ℃, obtain the LiNbO of surfacing 3/ SiO 2/ diamond multilayer piezoelectric film, the LiNbO of preparation 3Film is high c axle oriented film.
4. LiNbO according to claim 1 and 2 3/ SiO 2The preparation method of/diamond multilayer piezoelectric film is characterized in that, is realized by following steps
(1), diamond substrate is put into pulsed laser deposition equipment vacuum chamber, be evacuated to 10 -3Pa, heating diamond substrate to 350 ℃ is made target with silicon, carries out SiO in the 99.99% high purity oxygen gas atmosphere of 15Pa 2Deposition, between target and the substrate distance at 5.7cm, be the amorphous SiO of 0.3 μ m with pulse laser deposit thickness on diamond substrate 2Resilient coating;
(2), will deposit amorphous SiO 2The diamond substrate of resilient coating is warming up to 640 ℃, feeds 99.99% high purity oxygen gas in deposition process, and oxygen is pressed and remained on 40Pa, and laser frequency is at 3Hz, with LiNbO 3Make target, distance is 4J/cm at 4.5cm with the single pulse energy metric density between target and the diamond substrate 2Laser at amorphous SiO 2Deposit thickness is the LiNbO of 0.6 μ m on the resilient coating 3Piezoelectric thin film layer;
(3), LiNbO 3After piezoelectric thin film layer deposition finishes, depress in 99.99% high purity oxygen of 40Pa and to be cooled to 25 ℃, obtain the LiNbO of surfacing 3/ SiO 2/ diamond multilayer piezoelectric film, the LiNbO of preparation 3Film is high c axle oriented film.
CN201010030152.8A 2010-01-12 2010-01-12 LiNbO3/SiO2/diamond multilayer piezoelectric film and preparation method thereof Expired - Fee Related CN101777622B (en)

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CN102820322A (en) * 2012-09-06 2012-12-12 电子科技大学 GaN-based enhancement device containing ferroelectric layer and preparation method
CN105321806A (en) * 2015-08-21 2016-02-10 济南晶正电子科技有限公司 Composite single crystal thin film and method for manufacturing composite single crystal thin film
CN106601997A (en) * 2016-11-24 2017-04-26 天津大学 Preparation method of adopting pulsed laser sputtering deposition of fishing net SiOx film on negative current collector material
CN113141165A (en) * 2020-01-17 2021-07-20 中芯集成电路(宁波)有限公司 Composite substrate and manufacturing method thereof, surface acoustic wave resonator and manufacturing method thereof

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CN1540043A (en) * 2003-10-28 2004-10-27 浙江大学 Method for preparing thin film of lithium niobate crystal orientated in direction of caxis
CN100468965C (en) * 2005-09-05 2009-03-11 天津理工大学 LiNbO3/ZnO/diamond multi-layered film structure surface acoustic wave device and its preparing method

Cited By (8)

* Cited by examiner, † Cited by third party
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CN102820322A (en) * 2012-09-06 2012-12-12 电子科技大学 GaN-based enhancement device containing ferroelectric layer and preparation method
CN102820322B (en) * 2012-09-06 2015-07-01 电子科技大学 GaN-based enhancement device containing ferroelectric layer and preparation method
CN105321806A (en) * 2015-08-21 2016-02-10 济南晶正电子科技有限公司 Composite single crystal thin film and method for manufacturing composite single crystal thin film
WO2017032199A1 (en) * 2015-08-21 2017-03-02 济南晶正电子科技有限公司 Composite single crystal thin film and method for manufacturing composite single crystal thin film
CN106601997A (en) * 2016-11-24 2017-04-26 天津大学 Preparation method of adopting pulsed laser sputtering deposition of fishing net SiOx film on negative current collector material
CN106601997B (en) * 2016-11-24 2019-08-20 天津大学 A kind of preparation method of the pulsed laser deposition fishing net shaped SiOx film on negative current collector material
CN113141165A (en) * 2020-01-17 2021-07-20 中芯集成电路(宁波)有限公司 Composite substrate and manufacturing method thereof, surface acoustic wave resonator and manufacturing method thereof
WO2021143409A1 (en) * 2020-01-17 2021-07-22 中芯集成电路(宁波)有限公司 Composite substrate and manufacturing method therefor, and surface acoustic wave resonator and manufacturing method therefor

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