CN103952674B - The preparation method of the voltage-controlled varactor of a kind of zinc oxide - Google Patents

The preparation method of the voltage-controlled varactor of a kind of zinc oxide Download PDF

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Publication number
CN103952674B
CN103952674B CN201410139003.3A CN201410139003A CN103952674B CN 103952674 B CN103952674 B CN 103952674B CN 201410139003 A CN201410139003 A CN 201410139003A CN 103952674 B CN103952674 B CN 103952674B
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voltage
zno
preparation
zinc oxide
sputtering
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CN103952674A (en
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李玲霞
郑浩然
于仕辉
许丹
董和磊
金雨馨
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Tianjin University
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Tianjin University
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Abstract

The invention discloses the preparation method of the voltage-controlled varactor of a kind of zinc oxide, first by ZnO powder compression moulding, adopt solid sintering technology to fire ZnO target in 1100 DEG C; Cleaned up by Pt-Si substrate, utilize magnetron sputtered deposition technology, deposition obtains ZnO film, sputtering power 100 ~ 200W; 400 DEG C ~ 600 DEG C after annealing process in oxygen atmosphere stove again, annealing time 5 ~ 60min; Recycling mask prepares metal electrode, and utilizes hot vapour deposition method or sputtering method to prepare Au or Pt electrode.The tuning rate high (more than 70%) of ZnO of the present invention voltage-controlled film varactor, driving voltage low (being less than 80kV/cm), material is inexpensive, and technique is simple, electric property is excellent, has a good application prospect.

Description

The preparation method of the voltage-controlled varactor of a kind of zinc oxide
Technical field
The invention belongs to electronic information material and components and parts field, be specifically related to the preparation method of the voltage-controlled film varactor of a kind of novel oxidized zinc.
Background technology
Microwave dielectric material as new function electronic ceramics, because its application in microwave function device receives increasing concern.Compared with block materials, thin-film device operating voltage is low, fast response time, can with microstrip circuitry technology and semiconductor technology integrated.The future development of microwave electron system forward broadband, heavy body, volume miniaturization more, therefore day by day urgent to the demand of integrated, high performance microwave device.Its specific inductivity of dielectric material with adjustable regulates by extra electric field, utilize this characteristic can frequency, phase place, the amplitude of modulated microwave signal, make voltage-controlled microwave device, it is had broad application prospects in the military and civilian electronic systems such as mobile communication, statllite system, radar system.
ZnO material is easy to get, inexpensive, become one of thin-film material having potentiality to be exploited most, we take Pt-Si as substrate, adopt magnetron sputtering method deposition ZnO film, the tuning rate of the novel Zn O tunable thin film varactor obtained reaches more than 70%, driving voltage is low, and therefore, ZnO film has a good application prospect in micro-wave communication components and parts.
Summary of the invention
Object of the present invention, is adopt ZnO material that is inexpensive, that be easy to get, utilizes magnetron sputtered deposition technology, provide a kind of preparation method preparing the voltage-controlled film varactor of novel Zn O high tuning rate.
The present invention is achieved by following technical solution.
A preparation method for the voltage-controlled varactor of zinc oxide, has following steps:
(1) take ZnO powder, compression moulding, adopt solid sintering technology to fire ZnO target in 1100 DEG C;
(2) Pt-Si substrate is cleaned up, with N 2dry up and put in magnetron sputtering sample table;
(3) base vacuum of magnetic control sputtering system is evacuated to P<7.0 × 10 -6torr, then heats Pt-Si substrate to 300 ~ 700 DEG C;
(4) using high-purity argon gas and oxygen as sputter gas, Ar and O 2throughput ratio be 10:1 ~ 2:1, total gas flow rate is 100sccm, and sputtering pressure is 10mTorr, and sputtering power is 100 ~ 200W, carries out deposition and obtains ZnO film;
(5) after step (4) stops, when Pt-Si underlayer temperature is down to below 200 DEG C, take out goods, in oxygen atmosphere stove, carry out after annealing process, described annealing temperature is 400 DEG C ~ 600 DEG C, and annealing time is 5 ~ 60min;
(6) utilize mask to prepare metal electrode above the ZnO film after step (5) annealing, and utilize hot vapour deposition method or sputtering method to prepare Au or Pt electrode.
The purity of described step (1) ZnO powder is 99%.
The purity of described step (4) argon gas and oxygen is 99.99%.
The thickness that described step (4) obtains ZnO film is 150 ~ 500nm, controls film thickness by regulating sputtering power and depositing time.
Pressure≤the 0.1Mpa of oxygen is passed into, oxygen purity >=99% in described step (5) oxygen atmosphere stove.
The electrode of described step (6) is circular electrode, diameter≤0.3mm.
The tuning rate high (more than 70%) of ZnO of the present invention voltage-controlled film varactor, driving voltage low (being less than 80kV/cm), material is inexpensive, and preparation technology's flow process is simple, electric property is excellent, has a good application prospect.
The film tuning device of prior art adopts bismuth zinc niobate and strontium-barium titanate as medium layer usually, its tuning rate 50% ~ 60%, and driving electric field is all greater than 2MV/cm; The present invention adopts ZnO material, utilizes magnetron sputtered deposition technology, and the performance of the ZnO high tuning rate voltage-controlled film varactor provided is better than traditional dielectric tuning material.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph that embodiment 1 is prepared in the ZnO film goods on Pt-Si substrate;
Fig. 2 is electric capacity (electric field-tunable) collection of illustrative plates that embodiment 1 is prepared in the ZnO film goods on Pt-Si substrate.
Embodiment
Set forth the present invention further below in conjunction with specific embodiment, these embodiments are only not used in for illustration of the present invention and limit the scope of the invention.
Embodiment 1
(1) taking purity with electronic balance is 99%ZnO powder, makes type at the pressure of 30Mpa, then is placed in cabinet-type electric furnace and is progressively warming up to 1100 DEG C, and is incubated 6 hours, adopts solid sintering technology making ZnO target;
(2) Pt-Si substrate is cleaned up, with N 2dry up and put in magnetron sputtering sample table;
(3) base vacuum of magnetic control sputtering system is evacuated to 6.0 × 10 -6torr, then heated substrate to 450 DEG C;
(4) with high-purity (99.99%) Ar and O 2as sputter gas, the throughput ratio of argon gas and oxygen is 4:1; Total gas flow rate is 100sccm, and sputtering pressure is 10mTorr, and sputtering power is 150W, carries out deposition and obtains ZnO film, and depositing the film thickness obtained is 200nm, controls film thickness by adjusting process parameter or depositing time;
(5) when Pt-Si underlayer temperature is down to below 200 DEG C, the ZnO film obtained is inserted in atmosphere furnace and carries out after annealing process, pass into the O that purity is 99% 2, annealing gas pressure is 0.02Mpa, and annealing temperature is 550 DEG C, and annealing time is 10min;
(6) mask is utilized to prepare metal electrode above ZnO film after annealing, and the circular Au electrode that to utilize the method for sputtering to plate diameter be 0.2mm, the obtained voltage-controlled varactor of ZnO.
Fig. 1 is the electron scanning micrograph that embodiment 1 is prepared in the ZnO film goods on Pt-Si substrate, visible obtained ZnO film surfacing, uniform particles.
Fig. 2 is electric capacity (electric field-tunable) collection of illustrative plates that embodiment 1 is prepared in the ZnO film goods on Pt-Si substrate, and under the electric field of 65kV/cm, tuning rate is 86% as seen.
Embodiment 2
Embodiment 2 is substantially the same manner as Example 1, and difference is: the sputtering power of embodiment 2 step (4) is 100W, and annealing temperature is 400 DEG C.The tuning rate of the voltage-controlled film varactor of embodiment 2 is 72%, and driving electric field is 62kV/cm.
Sputtering power and the performance of annealing temperature to film have decisive influence.Sputtering time is coordinated mutually with sputtering power usually, by adjustment sputtering time, to ensure the film (sputtering power is different, and the sputter rate of film is different) preparing appointed thickness under different capacity.
Embodiment 3
Embodiment 3 is substantially the same manner as Example 1, and difference is: the sputtering power of embodiment 3 step (4) is 200W, and annealing temperature is 600 DEG C.The tuning rate of the voltage-controlled film varactor of embodiment 3 is 71%, and driving electric field is 63kV/cm.
Bound value and the interval value of each processing parameter of the present invention (sputtering power, temperature, time) can realize the present invention, are not illustrated one by one at this.

Claims (6)

1. a preparation method for the voltage-controlled varactor of zinc oxide, has following steps:
(1) take ZnO powder, compression moulding, adopt solid sintering technology to fire ZnO target in 1100 DEG C;
(2) Pt-Si substrate is cleaned up, with N 2dry up and put in magnetron sputtering sample table;
(3) base vacuum of magnetic control sputtering system is evacuated to P<7.0 × 10 -6torr, then heats Pt-Si substrate to 300 ~ 700 DEG C;
(4) using high-purity argon gas and oxygen as sputter gas, Ar and O 2throughput ratio be 10:1 ~ 2:1, total gas flow rate is 100sccm, and sputtering pressure is 10mTorr, and sputtering power is 100 ~ 200W, carries out deposition and obtains ZnO film;
(5) after step (4) stops, to be deposited when having the Pt-Si underlayer temperature of ZnO film to be down to below 200 DEG C, take out goods, it is carried out after annealing process in oxygen atmosphere stove, described annealing temperature is 400 DEG C ~ 600 DEG C, and annealing time is 5 ~ 60min;
(6) utilize mask above the ZnO film of the Pt-Si substrate after step (5) after annealing and adopt hot vapour deposition method or sputtering method to prepare Au or Pt electrode.
2. the preparation method of the voltage-controlled varactor of a kind of zinc oxide according to claim 1, is characterized in that, the purity of described step (1) ZnO powder is 99%.
3. the preparation method of the voltage-controlled varactor of a kind of zinc oxide according to claim 1, is characterized in that, the purity of described step (4) argon gas and oxygen is 99.99%.
4. the preparation method of the voltage-controlled varactor of a kind of zinc oxide according to claim 1, is characterized in that, the thickness that described step (4) obtains ZnO film is 150 ~ 500nm, controls film thickness by regulating sputtering power and depositing time.
5. the preparation method of the voltage-controlled varactor of a kind of zinc oxide according to claim 1, is characterized in that, passes into the pressure≤0.1Mpa of oxygen, oxygen purity >=99% in described step (5) oxygen atmosphere stove.
6. the preparation method of the voltage-controlled varactor of a kind of zinc oxide according to claim 1, is characterized in that, the electrode of described step (6) is circular electrode, diameter≤0.3mm.
CN201410139003.3A 2014-04-08 2014-04-08 The preparation method of the voltage-controlled varactor of a kind of zinc oxide Expired - Fee Related CN103952674B (en)

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CN108447789B (en) * 2018-03-28 2020-06-02 天津大学 Preparation method of flexible film varactor
CN110491687A (en) * 2019-08-14 2019-11-22 天津大学 A kind of preparation method of transparent Indium nickel film varactor

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CN103397303A (en) * 2013-07-31 2013-11-20 天津大学 Preparation method of voltage-controlled varactor made of transparent bismuth magnesium niobate thin films
CN103526171A (en) * 2013-10-21 2014-01-22 上海理工大学 Preparation method of aluminum-doped zinc oxide film with tunable preferred orientations

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WO2002007311A2 (en) * 2000-07-13 2002-01-24 Rutgers, The State University Integrated tunable surface acoustic wave technology and systems provided thereby

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CN101096594A (en) * 2007-06-25 2008-01-02 武汉科技学院 Zinc oxide film transmitting blue light and purple light under room temperature and preparation method thereof
CN103397303A (en) * 2013-07-31 2013-11-20 天津大学 Preparation method of voltage-controlled varactor made of transparent bismuth magnesium niobate thin films
CN103526171A (en) * 2013-10-21 2014-01-22 上海理工大学 Preparation method of aluminum-doped zinc oxide film with tunable preferred orientations

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