CN103526171A - Preparation method of aluminum-doped zinc oxide film with tunable preferred orientations - Google Patents
Preparation method of aluminum-doped zinc oxide film with tunable preferred orientations Download PDFInfo
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- CN103526171A CN103526171A CN201310497082.0A CN201310497082A CN103526171A CN 103526171 A CN103526171 A CN 103526171A CN 201310497082 A CN201310497082 A CN 201310497082A CN 103526171 A CN103526171 A CN 103526171A
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Abstract
The invention discloses a preparation method of an aluminum-doped zinc oxide film with tunable preferred orientations. The preparation method comprises the following steps: heating a quartz substrate to a certain temperature; pre-sputtering a target for a certain time with certain working gas and under a certain working pressure and vacuum degree, thus obtaining a pre-sputtered target; sputtering the pre-sputtered target on the quartz substrate rotating at a certain speed for a period of time through direct-current magnetic control and depositing so as to obtain a film; cooling the film to room temperature, thus obtaining the aluminum-doped zinc oxide film, wherein the certain time lasts for 8-10 minutes, the certain speed is 3-6 rotations per minute, and the period of time lasts for 5-25 minutes. Through the preparation method disclosed by the invention, controllable tuning or conversion with different preferred orientations of an axis a and an axis c is achieved when the AZO (aluminum-doped zinc oxide) film is prepared; meanwhile, the preparation method is also capable of preparing ZAO films with different growth orientations in different areas on the same substrate through certain shielding treatment, and developing the potential application value; the ZAO films, which are finally obtained, are excellent in performance and particularly has potential application value in fields of piezoelectric effect and the like.
Description
Technical field
The present invention is specifically related to the tunable Al-Doped ZnO film preparation method of a kind of preferred orientation.
Background technology
In recent years, zinc oxide (ZnO) nesa coating has obtained research very widely.Zinc-oxide film is with respect to ITO and SnO
2, there is low price, depositing temperature is relatively low and in atmosphere of hydrogen, there is the advantage such as stability better.As a kind of important optoelectronic information material, mix the good photoelectric characteristic of aluminium (AZO) zinc oxide transparent conducting film it is widely used in fields such as solar cell, liquid-crystal display, hot mirrors.
The preparation method of current AZO film has multiple, comprises sol-gel method, chemical Vapor deposition process, electron-beam vapor deposition method, pulsed laser deposition and magnetron sputtering method etc.But the AZO film that the whole bag of tricks of having reported prepares mostly is the growth of c-axis preferred orientation that is (002) face preferred orientation aspect crystalline structure, the preparation method of the AZO film that relevant a axle orientation that is (100) face preferred orientation are grown and property research abundant not enough.Utilize the conversion of the different preferred orientations of AZO film to set up certain contact with the theory of piezoelectric effect, probably obtain a kind of novel piezoelectric transducer.Therefore, along with for the going deep into of AZO thin film study, more fully obviously necessary for film different orientation growth pattern phase co-conversion and tuning preparation method and research.
Patent of invention (publication number: 101113533) introduced with low cost by the method for electrochemical deposition process making ZnO film, be easy to big area preparation, but can only prepare, there is single c-axle oriented zinc-oxide film, can not realize the tuning of the different preferred orientation growths of zinc-oxide film.
Summary of the invention
In order to address the above problem, the invention provides the tunable Al-Doped ZnO film preparation method of a kind of preferred orientation, can realize a axle (100) face and the tuning conversion of c-axis (002) face, obtain the tuning of the different preferred orientation growths of zinc-oxide film.
In order to achieve the above object, the present invention has adopted following technical scheme:
A tunable Al-Doped ZnO film preparation method, has such feature, comprises following steps: quartz substrate is heated to certain temperature; Under certain working gas, operating air pressure and vacuum tightness, target is carried out to the pre-sputtering of certain hour, obtain pre-sputtering target; By pre-sputtering target by direct magnetic control in the quartz substrate with given pace rotation sputter for some time to deposit and to obtain film; And by film cooling to room temperature, obtain Al-Doped ZnO film, wherein, certain hour is 8-10 minute, given pace is 3-6 rev/min, for some time is 5-25 minute.
Further, the tunable Al-Doped ZnO film preparation method of preferred orientation of the present invention, can also have such feature: above-mentioned certain temperature is 350 degrees Celsius.
Further, the tunable Al-Doped ZnO film preparation method of preferred orientation of the present invention, can also have such feature: above-mentioned target is the zinc-oxide ceramic target of the aluminum oxide that contains 2% massfraction.
Further, the tunable Al-Doped ZnO film preparation method of preferred orientation of the present invention, can also have such feature: above-mentioned working gas is that purity is 99.99% argon gas, and operating air pressure is 10
-2-10
-1handkerchief, vacuum tightness is greater than 5 * 10
-4.
Further, the tunable Al-Doped ZnO film preparation method of preferred orientation of the present invention, can also have such feature: above-mentioned certain hour is 10 minutes.
Further, the tunable Al-Doped ZnO film preparation method of preferred orientation of the present invention, can also have such feature: above-mentioned given pace is 4 revs/min.
Further, the tunable Al-Doped ZnO film preparation method of preferred orientation of the present invention, can also have such feature: above-mentioned for some time is 5 minutes, and above-mentioned Al-Doped ZnO film is the Al-Doped ZnO film of c-axis preferred orientation.
Further, the tunable Al-Doped ZnO film preparation method of preferred orientation of the present invention, can also have such feature: above-mentioned for some time is 25 minutes, and above-mentioned Al-Doped ZnO film is the Al-Doped ZnO film of a axle preferrel orientation.
In addition, the tunable Al-Doped ZnO film preparation method of preferred orientation of the present invention, can also have such feature: above-mentioned for some time is 15 minutes, above-mentioned Al-Doped ZnO film is for have the Al-Doped ZnO film of c-axis preferred orientation and a axle preferrel orientation simultaneously.
Effect and the effect of invention
According to the tunable Al-Doped ZnO film preparation method of the preferred orientation the present invention relates to, the controllable tuning or conversion of a axle preferred orientations different from c-axis while having realized preparation AZO film, and this preparation method can also process by certain covering the AZO film of preparing different growth orientation in different zones in same substrate, develops its potential using value.The AZO film finally obtaining has excellent performance, especially in fields such as piezoelectric effects, has potential using value.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the AZO film of a axle in embodiment, the growth of c-axis different orientation; And
Fig. 2 is the XRD diffracting spectrum of the AZO film prepared in embodiment.
Embodiment
Following examples are specifically addressed the present invention by reference to the accompanying drawings.
Base material can have influence on the preparation of Al-Doped ZnO film in this preparation method, so the substrate in this preparation method adopts quartz substrate.Reactive magnetron sputtering in the present invention is under the baking condition of 350 ℃, in vacuum chamber, to carry out substrate 1 is carried out.
A tunable Al-Doped ZnO film preparation method, comprises following steps:
The quartz substrate of cleaning after (as ultrasonic cleaning) is contained in substrate chuck, quartz substrate is heated to 350 ℃;
The zinc-oxide ceramic target of the aluminum oxide that employing contains 2% massfraction is target, and shifting board is placed between substrate chuck and target, and the argon gas that is 99.99% in purity is working gas, 10
-2-10
-1pa is that operating air pressure and vacuum tightness are greater than 5 * 10
-4working conditions under, open direct supply, the target of the speed rotation with 3-6 rev/min is carried out to the build-up of luminance pre-sputtering of 8-10min, obtain pre-sputtering target;
Open the rotation of substrate chuck, remove shifting board, by pre-sputtering target by direct magnetic control in substrate sputter 5-25min to deposit and to obtain film.Other details is identical with conventional magnetron sputtering, is not described in detail.
Film cooling, to room temperature, is obtained to Al-Doped ZnO film.
Processing parameter in above-mentioned scope and material are selected for a axle of film, the variation of c-axis growth orientation relative intensity has impact significantly.By adjusting the time of magnetron sputtering, can obtain thering is c-axis preferred orientation, there is a axle preferrel orientation or there is c-axis preferred orientation simultaneously and the Al-Doped ZnO film of a axle preferrel orientation.
Embodiment mono-
Fig. 1 is the schematic diagram of the AZO film of a axle in embodiment, the growth of c-axis different orientation.
Fig. 2 is the XRD diffracting spectrum of the AZO film prepared in embodiment.
The tunable Al-Doped ZnO film preparation method of preferred orientation in the present embodiment one, comprises following steps:
The quartz substrate of cleaning after (as ultrasonic cleaning) is contained in substrate chuck, quartz substrate is heated to 350 ℃;
The zinc-oxide ceramic target of the aluminum oxide that employing contains 2% massfraction is target, and shifting board is placed between substrate chuck and target, and the argon gas that is 99.99% in purity is working gas, 10
-2-10
-1pa is that operating air pressure and vacuum tightness are greater than 5 * 10
-4working conditions under, open direct supply, the target of the speed rotation with 4 revs/min is carried out to the build-up of luminance pre-sputtering of 10min, obtain pre-sputtering target;
Open the rotation of substrate chuck, remove shifting board, by pre-sputtering target by direct magnetic control in substrate sputter 25min to deposit and to obtain film.Other details is identical with conventional magnetron sputtering, is not described in detail.
Film cooling, to room temperature, is obtained having the Al-Doped ZnO film of a axle preferrel orientation, and as shown in S1 in Fig. 1 and Fig. 2, the Relative Peak that the S1 sample of XRD spectra demonstration is 100 is larger by force, shows that sample S1 has obvious a axle preferrel orientation.
The effect of embodiment mono-and effect
The tunable Al-Doped ZnO film preparation method of preferred orientation who relates to according to the present embodiment one, it is 25min by adjusting the magnetron sputtering time, has finally obtained having the Al-Doped ZnO film of a axle preferrel orientation.
Embodiment bis-
The tunable Al-Doped ZnO film preparation method of preferred orientation in the present embodiment two, comprises following steps:
The quartz substrate of cleaning after (as ultrasonic cleaning) is contained in substrate chuck, quartz substrate is heated to 350 ℃;
The zinc-oxide ceramic target of the aluminum oxide that employing contains 2% massfraction is target, and shifting board is placed between substrate chuck and target, and the argon gas that is 99.99% in purity is working gas, 10
-2-10
-1pa is that operating air pressure and vacuum tightness are greater than 5 * 10
-4working conditions under, open direct supply, the target of the speed rotation with 4 revs/min is carried out to the build-up of luminance pre-sputtering of 10min, obtain pre-sputtering target;
Open the rotation of substrate chuck, remove shifting board, by pre-sputtering target by direct magnetic control in substrate sputter 15min to deposit and to obtain film.Other details is identical with conventional magnetron sputtering, is not described in detail.
By film cooling to room temperature, obtain having the Al-Doped ZnO film of a axle and two kinds of preferred orientations of c-axis simultaneously, as shown in S2 in Fig. 1 and Fig. 2,100, S2 sample that XRD spectra shows and 002 's Relative Peak strong with the variation of having compared in embodiment 1, the peak of 100 weakens by force relatively and the peak of 002 is strong obviously improves, and shows that sample S1 has a axle and two kinds of different preferred orientations of c-axis simultaneously.
The effect of embodiment bis-and effect
The tunable Al-Doped ZnO film preparation method of preferred orientation who relates to according to the present embodiment two, it is 15min by adjusting the magnetron sputtering time, has finally obtained having the Al-Doped ZnO film of two kinds of preferred orientations of an a axle c-axis simultaneously.
Embodiment tri-
The tunable Al-Doped ZnO film preparation method of preferred orientation in the present embodiment three, comprises following steps:
The quartz substrate of cleaning after (as ultrasonic cleaning) is contained in substrate chuck, quartz substrate is heated to 350 ℃;
The zinc-oxide ceramic target of the aluminum oxide that employing contains 2% massfraction is target, and shifting board is placed between substrate chuck and target, and the argon gas that is 99.99% in purity is working gas, 10
-2-10
-1pa is that operating air pressure and vacuum tightness are greater than 5 * 10
-4working conditions under, open direct supply, the target of the speed rotation with 4 revs/min is carried out to the build-up of luminance pre-sputtering of 10min, obtain pre-sputtering target;
Open the rotation of substrate chuck, remove shifting board, by pre-sputtering target by direct magnetic control in substrate sputter 5min to deposit and to obtain film.Other details is identical with conventional magnetron sputtering, is not described in detail.
Film cooling, to room temperature, is obtained having the Al-Doped ZnO film of c-axis preferred orientation, and as shown in S3 in Fig. 1 and Fig. 2, the Relative Peak that the S3 sample of XRD spectra demonstration is 002 is larger by force, shows that sample S1 has obvious c-axis preferred orientation.
The effect of embodiment tri-and effect
The tunable Al-Doped ZnO film preparation method of preferred orientation who relates to according to the present embodiment three, it is 5min by adjusting the magnetron sputtering time, has finally obtained having the Al-Doped ZnO film of c-axis preferred orientation.
A axle (100) when this preparation method has realized preparation AZO film and the controllable tuning or conversion of the different preferred orientations of c-axis (002), and this preparation method can also process by certain covering the AZO film of preparing different growth orientation in different zones in same substrate, develops its potential using value.The AZO film finally obtaining has excellent performance, especially in fields such as piezoelectric effects, has potential using value.
Claims (9)
1. the tunable Al-Doped ZnO film preparation method of preferred orientation who prepares a axle preferrel orientation, the tunable Al-Doped ZnO film of c-axis preferred orientation, is characterized in that, comprises following steps:
Quartz substrate is heated to certain temperature;
Under certain working gas, operating air pressure and vacuum tightness, target is carried out to the pre-sputtering of certain hour, obtain pre-sputtering target;
By described pre-sputtering target by direct magnetic control in the described quartz substrate with given pace rotation sputter for some time to deposit and to obtain film; And
Described film cooling, to room temperature, is obtained to described Al-Doped ZnO film,
Wherein, described certain hour is 8-10 minute,
Described given pace is 3-6 rev/min,
Described for some time is 5-25 minute.
2. the tunable Al-Doped ZnO film preparation method of preferred orientation as claimed in claim 1, is characterized in that:
Wherein, described certain temperature is 350 degrees Celsius.
3. the tunable Al-Doped ZnO film preparation method of preferred orientation as claimed in claim 1, is characterized in that:
Wherein, described target is the zinc-oxide ceramic target of the aluminum oxide that contains 2% massfraction.
4. the tunable Al-Doped ZnO film preparation method of preferred orientation as claimed in claim 1, is characterized in that:
Wherein, described working gas is that purity is 99.99% argon gas,
Described operating air pressure is 10
-2-10
-1handkerchief,
Described vacuum tightness is greater than 5 * 10
-4.
5. the tunable Al-Doped ZnO film preparation method of preferred orientation as claimed in claim 1, is characterized in that:
Wherein, described certain hour is 10 minutes.
6. the tunable Al-Doped ZnO film preparation method of preferred orientation as claimed in claim 1, is characterized in that:
Wherein, described given pace is 4 revs/min.
7. the tunable Al-Doped ZnO film preparation method of preferred orientation as claimed in claim 1, is characterized in that:
Wherein, described for some time is 5 minutes, and described Al-Doped ZnO film is the Al-Doped ZnO film of described c-axis preferred orientation.
8. the tunable Al-Doped ZnO film preparation method of preferred orientation as claimed in claim 1, is characterized in that:
Wherein, described for some time is 25 minutes, and described Al-Doped ZnO film is the Al-Doped ZnO film of described a axle preferrel orientation.
9. the tunable Al-Doped ZnO film preparation method of preferred orientation as claimed in claim 1, is characterized in that:
Wherein, described for some time is 15 minutes, and described Al-Doped ZnO film is for have the Al-Doped ZnO film of described c-axis preferred orientation and described a axle preferrel orientation simultaneously.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103952674A (en) * | 2014-04-08 | 2014-07-30 | 天津大学 | Preparation method of zinc oxide voltage controlled varactor |
| CN112831768A (en) * | 2021-01-04 | 2021-05-25 | 南京佑天金属科技有限公司 | Preparation method and application of hafnium nitride film with high crystallization quality |
| CN116866731A (en) * | 2023-05-29 | 2023-10-10 | 武汉工程大学 | Liquid crystal microlens array imaging method, system, equipment and medium based on aluminum-doped zinc oxide |
Citations (1)
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| CN102453869A (en) * | 2010-10-28 | 2012-05-16 | 海洋王照明科技股份有限公司 | Preparation method and application of aluminum-doped zinc oxide conductive film |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102453869A (en) * | 2010-10-28 | 2012-05-16 | 海洋王照明科技股份有限公司 | Preparation method and application of aluminum-doped zinc oxide conductive film |
Non-Patent Citations (3)
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| BEOM-KI SHIN等: "Effect of deposition power on structural and electrical properties of Al-doped ZnO films using pulsed direct-current magnetron sputtering with single cylindrical target", 《MATERIALS SCIENCE IN SEMICONDUCTOR PROCESSING》, vol. 14, no. 1, 31 March 2011 (2011-03-31), XP028176753, DOI: 10.1016/j.mssp.2010.12.013 * |
| KANG HYON RI等: "The structural properties of Al doped ZnO films depending on the thickness and their effect on the electrical properties", 《APPLIED SURFACE SCIENCE》, vol. 258, no. 4, 1 December 2011 (2011-12-01) * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103952674A (en) * | 2014-04-08 | 2014-07-30 | 天津大学 | Preparation method of zinc oxide voltage controlled varactor |
| CN103952674B (en) * | 2014-04-08 | 2016-03-02 | 天津大学 | The preparation method of the voltage-controlled varactor of a kind of zinc oxide |
| CN112831768A (en) * | 2021-01-04 | 2021-05-25 | 南京佑天金属科技有限公司 | Preparation method and application of hafnium nitride film with high crystallization quality |
| CN116866731A (en) * | 2023-05-29 | 2023-10-10 | 武汉工程大学 | Liquid crystal microlens array imaging method, system, equipment and medium based on aluminum-doped zinc oxide |
| CN116866731B (en) * | 2023-05-29 | 2024-05-10 | 武汉工程大学 | Liquid crystal microlens array imaging method, system, equipment and medium based on aluminum-doped zinc oxide |
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