CN102611405A - Zinc oxide piezoelectric film for SAW (Surface Acoustic Wave) device and manufacturing method thereof - Google Patents

Zinc oxide piezoelectric film for SAW (Surface Acoustic Wave) device and manufacturing method thereof Download PDF

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CN102611405A
CN102611405A CN2012100625070A CN201210062507A CN102611405A CN 102611405 A CN102611405 A CN 102611405A CN 2012100625070 A CN2012100625070 A CN 2012100625070A CN 201210062507 A CN201210062507 A CN 201210062507A CN 102611405 A CN102611405 A CN 102611405A
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film
silicon substrate
monocrystalline silicon
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zinc oxide
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陈希明
张倩
阴聚乾
朱宇清
李福龙
郭燕
孙连婕
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Tianjin University of Technology
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Abstract

The invention relates to a zinc oxide piezoelectric film for an SAW (Surface Acoustic Wave) device, which is of a zinc oxide/aluminum/diamond-like composite film structure. A manufacturing method comprises the following steps of: placing single crystal silicon wafer with the cleaned surface into a vacuum growth cavity of a pulse laser system, depositing the diamond-like/aluminum thin film with graphite and aluminum as a target material; and depositing a zinc oxide film on the surface of the Al film with the zinc oxide as the target material through a radio-frequency magnetron sputtering process. The invention has the advantages that: the manufacturing method is simple and feasible and has low cost; the prepared diamond-like film surface is smooth and flat so as to be capable of largely reducing sound wave loss in a transmission process, the deposited Al film largely improves the electromechanical coupling coefficients of the zinc oxide film, the crystallization degree of the zinc oxide film is high, c-axis orientation is high, and the zinc oxide/aluminum/diamond-like composite film structure can be used for manufacturing high-performance, high-frequency and high power devices.

Description

A kind of zno piezoelectric thin film that is used for SAW device and preparation method thereof
Technical field
The present invention relates to the SAW device technical field, particularly a kind of zno piezoelectric thin film that is used for SAW device and preparation method thereof.
Background technology
In recent years, mobile communication rapid development makes radio communication frequency bands become a limited and valuable natural resources.For GSM, the frequency band that is lower than 1GHz has been taken (first generation digital system); The frequency of second generation digital system is from 900MHz to 1.9GHz; In third generation digital system, the global roaming frequency range is 1.8~2.2GHz, and global position system (GPS) frequency is 1.575GHz; The applying frequency scope of the new satellite communication of Low Earth Orbit (LEO) is 1.6GHz~2.5GHz; Therefore, the applying frequency of present GSM is increasingly high, is badly in need of surface acoustic wave (SAW) filter of high frequency; And, move logical moving communicator and all require the try one's best miniaturization and have bigger power bearing ability of surface acoustic wave SAW filter.
For the SAW device of interdigital transducer/ZnO/Al/ DLC composite construction, under the prerequisite of existing manufacture craft level, the interdigital transducer width can not unconfined miniaturization.Thereby the selection high elastic modulus, low-density, the backing material of high heat conductance becomes and improves the thin-film sound surface wave device performance and the main path in life-span.Diamond has the highest consistency and elasticity modulus, high thermal conductivity and resistivity under the room temperature, the highest velocity of sound.But because the diamond film surface of preparation is more coarse usually, be unfavorable for the preparation of interdigital transducer, can cause the scattering of surface acoustic wave, the produce power loss increases and inserts loss, thereby has a strong impact on the performance of device.And the high stable chemical performance of diamond hardness, through machinery, means such as chemical polishing are handled very difficulty.Greatly limited the application of diamond device.Compare with diamond; DLC is a kind of metastable amorphous carbon, its structure, and physicochemical properties approach diamond; Possess a lot of and the similar excellent properties of diamond; High like hardness, modulus of elasticity is high, thermal conductivity is high, wear resistance and corrosion resistance is high, coefficient of friction is low, good insulation performance property and chemical stability, large-area preparation at room temperature, and have the scattering that very smooth surface can reduce surface acoustic wave.Therefore, (diamond-like carbon, DLC) film is the desirable backing material of the thin-film sound surface wave device of preparation high-frequency, high power, low insertion loss to DLC.Because DLC itself is not a piezoelectric, can't excite and accept surface wave, therefore need on DLC, deposit one deck piezoelectric membrane processes thin-film sound surface wave device.
Because zinc-oxide film has high electromechanical coupling factor and low-k, is a kind of desirable piezoelectric that is used for SAW device.Realize the application of zinc-oxide film in SAW device; Key is to prepare the ZnO piezoelectric film that high-quality, surfacing, crystal defect are few, have the high C-axis preferred orientation, with reduce as far as possible in the sonic propagation process scattering with improve electromechanical coupling factor (K2).Between zinc oxide and DLC substrate, add metal level, can effectively improve the electromechanical coupling factor of zinc-oxide film.Wherein, in the middle of all metals, the Al metal level can realize that the amplitude peak of the electromechanical coupling factor of zno piezoelectric thin film promotes.Simultaneously, add the Al metal level and can further reduce the scattering in the acoustic surface wave propagation process, effectively improve SAW propagating speed.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art; A kind of zno piezoelectric thin film that is used for SAW device and preparation method thereof is provided; The SAW device frequency of this piezoelectric membrane preparation is high and can bear high-powerly, can satisfy the requirement of high-frequency and/or high-power mobile communication, and its preparation method process conditions are convenient and easy; Help applying on a large scale, be of great practical significance.
Technical scheme of the present invention:
A kind of zno piezoelectric thin film that is used for SAW device is the zinc oxide/aluminium/DLC structure of composite membrane that on the monocrystalline silicon substrate substrate, prepares.
ZnO film crystal grain dimension is 40-60nm in the said composite membrane, and thickness is 0.1-0.2 μ m; Al film crystal grain dimension is 40-60nm, and thickness is 0.1-0.2 μ m; The crystal grain dimension of DLC film is 30-40nm, and thickness is 1 μ m.
A kind of said preparation method who is used for the zno piezoelectric thin film of SAW device, step is following:
1) clean is carried out on the monocrystalline silicon substrate surface, monocrystalline silicon substrate is put into acetone or alcohol utilizes the ultrasonic cleaning machine to carry out ultrasonic cleaning, cold wind dries up;
2) monocrystalline silicon substrate that surface clean is clean is put into the vacuum growth chamber of pulse laser system, with mechanical pump and molecular pump the vacuum growth chamber is vacuumized;
3) with graphite be target, regulate the distance of graphite target and monocrystalline silicon substrate, in vacuum chamber, feed the working gas argon gas, through the laser ablation graphite target, depositing diamond-like film on monocrystalline silicon substrate;
4) with aluminium be target, regulate the distance between aluminium target and the monocrystalline silicon substrate, in vacuum chamber, feed argon gas then, through laser ablation aluminium target, depositing Al film on DLC film;
5) after the depositing Al film is accomplished; Continuation feeds argon gas in vacuum chamber; Stop the aluminium target is ablated; After treating that monocrystalline silicon substrate naturally cools to room temperature, take out monocrystalline silicon substrate be placed on carry out 10 minutes in the alcohol ultrasonic cleaning to remove the impurity on monocrystalline silicon substrate surface, transfer to magnetic control sputtering system to monocrystalline silicon substrate then and be fixed on the substrate;
6) with zinc oxide be target, regulate the distance between zinc oxide target and the silicon chip, after adopting mechanical pump and molecular pump to take out sputtering chamber vacuumized, to the vacuum chamber aerating oxygen, employing rf magnetron sputtering technology is at Al film surface deposition one deck zinc-oxide film;
7) zinc-oxide film to preparation carries out 30 minutes annealing in process under 400 ℃ of temperature in sputtering chamber and under oxygen atmosphere;
8) close gas, treat to take out behind the sample cool to room temperature, can make zno piezoelectric thin film.
Said technological parameter at monocrystalline silicon substrate surface employing impulse laser deposition system depositing diamond-like film is: the pressure of working gas argon gas is 0.5-30Pa; The distance of graphite target and monocrystalline silicon substrate is 40-80mm, and the monocrystalline silicon substrate temperature is 25-500 ℃, and target and monocrystalline silicon substrate rotational velocity are 5-15 rev/min, and laser energy is 100-300mJ, and laser pulse is 1-10Hz.
Said technological parameter at DLC substrate surface employing impulse laser deposition system depositing Al film is: the volume flow of working gas argon gas is 20sccm; Operating pressure 1-30Pa; The distance of Al target and monocrystalline silicon substrate is 40-100mm, underlayer temperature 300-500 ℃, and 5-15 rev/min of substrate rotating platform rotating speed; Laser energy is 100-300mJ, and laser pulse is 1-10Hz.
Said rf magnetron sputtering technological parameter at Al film surface deposition zinc-oxide film is: the range 3cm between 20 rev/mins of substrate rotating platform rotating speeds, 400 ℃ of underlayer temperatures, sputtering power 150W, oxygen flow 20sccm, operating pressure 1.7Pa, sputtering target and the substrate, sedimentation time 1-2 hour.
Advantage of the present invention is: adopt impulse laser deposition system to realize the deposition of high velocity of sound DLC film and Al film simultaneously, adopt radiofrequency magnetron sputtering technology to realize the deposition of zinc-oxide film, preparation is simple, with low cost; Prepared DLC film smooth surface is smooth; Can reduce the loss of sound wave in transmission course greatly; The Al film of deposition has improved the electromechanical coupling factor of zinc-oxide film greatly, and zinc-oxide film degree of crystallinity is high, and c-axle orientation is high; This ZnO/Al/DLC complex thin film structure can be used for making high-performance, high frequency and high power device.
Embodiment
In order to make those skilled in the art person understand the present invention program better, the present invention is done further detailed description below in conjunction with embodiment.
Embodiment 1:
A kind of preparation method who is used for the zno piezoelectric thin film of SAW device, step is following:
1) monocrystalline silicon substrate Si (100) is put into acetone or alcohol utilizes the ultrasonic cleaning machine to carry out ultrasonic cleaning 15 minutes, cold wind dries up;
2) monocrystalline silicon substrate that surface clean is clean is put on the substrate table of vacuum growth chamber of excimer pulsed laser system that wavelength is 250nm, with mechanical pump and molecular pump the vacuum growth chamber is evacuated to the base vacuum degree and equals 3 * 10 -4Pa;
3) be target with graphite, in vacuum chamber, feed the working gas argon gas, the pressure of argon gas is 15Pa, and the distance of regulating graphite target and monocrystalline silicon substrate is 70mm; The monocrystalline silicon substrate temperature is 400 ℃, and the autobiography speed of target and monocrystalline silicon substrate is 10 rev/mins, laser energy 300mJ; Pulse frequency 5GHz, frequency of depositing are 6000 times, through the laser ablation graphite target; Depositing diamond-like film on monocrystalline silicon substrate, the crystal grain dimension of DLC film is 30nm, thickness is 1 μ m;
4) with aluminium be target, in vacuum chamber, feed argon gas then, flow is 20sccm, operating pressure 12Pa; The distance of regulating between aluminium target and the monocrystalline silicon substrate is 100mm, and the monocrystalline silicon substrate temperature is 400 ℃, and the autobiography speed of target and monocrystalline silicon substrate is 15 rev/mins, and laser energy is 200mJ; Pulse frequency is 5Hz, and frequency of depositing is 1000 times, through laser ablation aluminium target; Depositing Al film on DLC film, Al film crystal grain dimension is 40nm, thickness is 0.1 μ m;
5) after the depositing Al film is accomplished; Continuation feeds argon gas in vacuum chamber; Stop the aluminium target is ablated; After treating that monocrystalline silicon substrate naturally cools to room temperature, take out monocrystalline silicon substrate be placed on carry out 10 minutes in the alcohol ultrasonic cleaning to remove the impurity on monocrystalline silicon substrate surface, transfer to magnetic control sputtering system to monocrystalline silicon substrate then and be fixed on the substrate;
6) adopt mechanical pump and molecular pump to take out sputtering chamber vacuumized after, to the vacuum chamber aerating oxygen, flow is 20sccm, is target with zinc oxide; The distance of regulating between zinc oxide target and the silicon chip is 3cm, and substrate rotating platform rotating speed is 20 rev/mins, and 400 ℃ of underlayer temperatures, sputtering power are 150w; Gas pressure intensity 1.7Pa, sedimentation time 2h adopts rf magnetron sputtering technology; At Al film surface deposition one deck zinc-oxide film, ZnO film crystal grain dimension is 50nm, and thickness is 0.1 μ m;
7) in sputtering chamber and at the zinc-oxide film to preparation under the oxygen atmosphere of 80Pa, under 400 ℃ of temperature, carry out 30 minutes annealing in process;
8) close gas, treat to take out behind the sample cool to room temperature, can make zno piezoelectric thin film.
Embodiment 2:
A kind of preparation method who is used for the zno piezoelectric thin film of SAW device, step is following:
1) monocrystalline silicon substrate Si (100) is put into acetone or alcohol utilizes the ultrasonic cleaning machine to carry out ultrasonic cleaning 15 minutes, cold wind dries up;
2) monocrystalline silicon substrate that surface clean is clean is put on the substrate table of vacuum growth chamber of excimer pulsed laser system that wavelength is 250nm, with mechanical pump and molecular pump the vacuum growth chamber is evacuated to the base vacuum degree and equals 3 * 10 -4Pa;
3) be target with graphite, in vacuum chamber, feed the working gas argon gas, the pressure of argon gas is 25Pa, and the distance of regulating graphite target and monocrystalline silicon substrate is 65mm; The monocrystalline silicon substrate temperature is 400 ℃, and the autobiography speed of target and monocrystalline silicon substrate is 10 rev/mins, laser energy 300mJ; Pulse frequency 5GHz, frequency of depositing are 6000 times, through the laser ablation graphite target; Depositing diamond-like film on monocrystalline silicon substrate, the crystal grain dimension of DLC film is 30nm, thickness is 1 μ m;
4) with aluminium be target, in vacuum chamber, feed argon gas then, flow is 20sccm, operating pressure 12Pa; The distance of regulating between aluminium target and the monocrystalline silicon substrate is 100mm, and the monocrystalline silicon substrate temperature is 400 ℃, and the autobiography speed of target and monocrystalline silicon substrate is 15 rev/mins, and laser energy is 300mJ; Pulse frequency is 5Hz, and frequency of depositing is 1000 times, through laser ablation aluminium target; Depositing Al film on DLC film, Al film crystal grain dimension is 45nm, thickness is 0.1 μ m;
5) after the depositing Al film is accomplished; Continuation feeds argon gas in vacuum chamber; Stop the aluminium target is ablated; After treating that monocrystalline silicon substrate naturally cools to room temperature, take out monocrystalline silicon substrate be placed on carry out 10 minutes in the alcohol ultrasonic cleaning to remove the impurity on monocrystalline silicon substrate surface, transfer to magnetic control sputtering system to monocrystalline silicon substrate then and be fixed on the substrate;
6) adopt mechanical pump and molecular pump to take out sputtering chamber vacuumized after, to the vacuum chamber aerating oxygen, flow is 20sccm, is target with zinc oxide; The distance of regulating between zinc oxide target and the silicon chip is 3cm, and substrate rotating platform rotating speed is 20 rev/mins, and 400 ℃ of underlayer temperatures, sputtering power are 150w; Gas pressure intensity 1.7Pa, sedimentation time 2h adopts rf magnetron sputtering technology; At Al film surface deposition one deck zinc-oxide film, ZnO film crystal grain dimension is 50nm, and thickness is 0.1 μ m;
7) in sputtering chamber and at the zinc-oxide film to preparation under the oxygen atmosphere of 100Pa, under 400 ℃ of temperature, carry out 30 minutes annealing in process;
8) close gas, treat to take out behind the sample cool to room temperature, can make zno piezoelectric thin film.
On above-mentioned zno piezoelectric thin film, prepare interdigital transducer, promptly can be made into interdigital transducer/ZnO/Al/ DLC structure of composite membrane SAW device.Add Al film front and rear fork finger transducer/ZnO/ DLC structure of composite membrane SAW device changes of properties, as shown in the table:
Figure BDA0000142230950000051
Can find out: after adding the Al film and being the intermediate layer, interdigital transducer/ZnO/Al/ diamond-like carbon composite film structure is compared with interdigital transducer/ZnO/ diamond-like carbon composite film structure, and maximum electromechanical coupling factor has improved 75%, and phase velocity also is significantly improved.
In sum, compared with prior art, the invention provides a kind of piezoelectric membrane that is used for high-performance surface acoustic wave (SAW) device; SAW device frequency with its preparation is high; And can bear high-powerly, can satisfy the requirement of high-frequency and/or high-power mobile communication, in addition; The present invention also provides a kind of preparation method who is used for the piezoelectric membrane of high-performance surface acoustic wave (SAW) device; These preparation method's process conditions are convenient and easy, help applying on a large scale, are of great practical significance.
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; Can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.

Claims (6)

1. a zno piezoelectric thin film that is used for SAW device is characterized in that: be the zinc oxide/aluminium/DLC structure of composite membrane that on the monocrystalline silicon substrate substrate, prepares.
2. according to the said zno piezoelectric thin film that is used for SAW device of claim 1, it is characterized in that: ZnO film crystal grain dimension is 40-60nm in the said composite membrane, and thickness is 0.1-0.2 μ m; Al film crystal grain dimension is 40-60nm, and thickness is 0.1-0.2 μ m; The crystal grain dimension of DLC film is 30-40nm, and thickness is 1 μ m.
3. preparation method who is used for the zno piezoelectric thin film of SAW device according to claim 1 is characterized in that step is following:
1) clean is carried out on the monocrystalline silicon substrate surface, monocrystalline silicon substrate is put into acetone or alcohol utilizes the ultrasonic cleaning machine to carry out ultrasonic cleaning, cold wind dries up;
2) monocrystalline silicon substrate that surface clean is clean is put into the vacuum growth chamber of pulse laser system, with mechanical pump and molecular pump the vacuum growth chamber is vacuumized;
3) with graphite be target, regulate the distance of graphite target and monocrystalline silicon substrate, in vacuum chamber, feed the working gas argon gas, through the laser ablation graphite target, depositing diamond-like film on monocrystalline silicon substrate;
4) with aluminium be target, regulate the distance between aluminium target and the monocrystalline silicon substrate, in vacuum chamber, feed argon gas then, flow is 20sccm, through laser ablation aluminium target, and depositing Al film on DLC film;
5) after the depositing Al film is accomplished; Continuation feeds argon gas in vacuum chamber; Stop the aluminium target is ablated; After treating that monocrystalline silicon substrate naturally cools to room temperature, take out monocrystalline silicon substrate be placed on carry out 10 minutes in the alcohol ultrasonic cleaning to remove the impurity on monocrystalline silicon substrate surface, transfer to magnetic control sputtering system to monocrystalline silicon substrate then and be fixed on the substrate;
6) with zinc oxide be target, regulate the distance between zinc oxide target and the silicon chip, after adopting mechanical pump and molecular pump to take out sputtering chamber vacuumized, to the vacuum chamber aerating oxygen, employing rf magnetron sputtering technology is at Al film surface deposition one deck zinc-oxide film;
7) zinc-oxide film to preparation carries out 30 minutes annealing in process under 400 ℃ of temperature in sputtering chamber and under oxygen atmosphere;
8) close gas, treat to take out behind the sample cool to room temperature, can make zno piezoelectric thin film.
4. according to the said preparation method who is used for the zno piezoelectric thin film of SAW device of claim 3, it is characterized in that: said technological parameter at monocrystalline silicon substrate surface employing impulse laser deposition system depositing diamond-like film is: the pressure of working gas argon gas is 0.5-30Pa; The distance of graphite target and monocrystalline silicon substrate is 40-80mm, and the monocrystalline silicon substrate temperature is 25-500 ℃, and target and monocrystalline silicon substrate rotational velocity are 5-15 rev/min, and laser energy is 100-300mJ, and laser pulse is 1-10Hz.
5. according to the said preparation method who is used for the zno piezoelectric thin film of SAW device of claim 3; It is characterized in that: said technological parameter at DLC substrate surface employing impulse laser deposition system depositing Al film is: the volume flow of working gas argon gas is 20sccm; Operating pressure 1-30Pa; The distance of Al target and monocrystalline silicon substrate is 40-100mm, underlayer temperature 300-500 ℃, and 5-15 rev/min of substrate rotating platform rotating speed; Laser energy is 100-300mJ, and laser pulse is 1-10Hz.
6. according to the said preparation method who is used for the zno piezoelectric thin film of SAW device of claim 3, it is characterized in that: said rf magnetron sputtering technological parameter at Al film surface deposition zinc-oxide film is: the range 3cm between 20 rev/mins of substrate rotating platform rotating speeds, 400 ℃ of underlayer temperatures, sputtering power 150W, oxygen flow 20sccm, operating pressure 1.7Pa, sputtering target and the substrate, sedimentation time 1-2 hour.
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CN105468873A (en) * 2015-12-24 2016-04-06 中北大学 Silicon substrate optical waveguide laser surface smoothing simulation method
CN110670027A (en) * 2019-11-07 2020-01-10 清华大学 Surface acoustic wave device based on double-layer electrode high electromechanical coupling coefficient and preparation method thereof
CN112383288A (en) * 2020-11-16 2021-02-19 清华大学 Temperature-compensated packaging-free surface acoustic wave device and preparation method thereof
CN115216745A (en) * 2022-06-30 2022-10-21 中国工程物理研究院电子工程研究所 Piezoelectric thick film preparation method based on sequential physical deposition and industrial-grade piezoelectric thick film

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102778509A (en) * 2012-08-17 2012-11-14 天津理工大学 SAW (surface acoustic wave) gas sensor substrate
CN105420676A (en) * 2015-11-23 2016-03-23 安徽松泰包装材料有限公司 Film manufacturing process
CN105468873A (en) * 2015-12-24 2016-04-06 中北大学 Silicon substrate optical waveguide laser surface smoothing simulation method
CN105468873B (en) * 2015-12-24 2018-08-14 中北大学 The surface-smoothing emulation mode of silicon substrate laser optical waveguide
CN110670027A (en) * 2019-11-07 2020-01-10 清华大学 Surface acoustic wave device based on double-layer electrode high electromechanical coupling coefficient and preparation method thereof
CN112383288A (en) * 2020-11-16 2021-02-19 清华大学 Temperature-compensated packaging-free surface acoustic wave device and preparation method thereof
CN115216745A (en) * 2022-06-30 2022-10-21 中国工程物理研究院电子工程研究所 Piezoelectric thick film preparation method based on sequential physical deposition and industrial-grade piezoelectric thick film
CN115216745B (en) * 2022-06-30 2023-09-05 中国工程物理研究院电子工程研究所 Piezoelectric thick film preparation method based on sequential physical deposition and industrial-grade piezoelectric thick film

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