CN101845615A - Method for preparing single crystal transparent ZnO film by adopting RF (Radio Frequency) magnetron sputtering - Google Patents
Method for preparing single crystal transparent ZnO film by adopting RF (Radio Frequency) magnetron sputtering Download PDFInfo
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- CN101845615A CN101845615A CN201010186969A CN201010186969A CN101845615A CN 101845615 A CN101845615 A CN 101845615A CN 201010186969 A CN201010186969 A CN 201010186969A CN 201010186969 A CN201010186969 A CN 201010186969A CN 101845615 A CN101845615 A CN 101845615A
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Abstract
The invention relates to a preparation technology of a ZnO film with high crystallinity, comprising the main technological steps of firstly, preparing ZnO ceramic targets; secondly, washing a glass liner; and thirdly, preparing a ZnO film on the glass liner. In the invention, in the process of magnetron sputtering, the background vacuum degree in a sputtering cavity is 1.8*10<-4>Pa, the sputtering power is unified to be 150W, the distance between the targets and the liner is defined to be 10cm, the temperature of a substrate is 450-600 DEG C, the Ar to O2 ratio is 40:0-20:20 (sccm:sccm), and the sputtering air pressure is 1Pa. The prepared ZnO film has favorable transparency and excellent crystallinity, and a crystal particle has good c-axis oriented growth characteristics.
Description
Technical field
The invention belongs to technical field of electronic materials, particularly a kind of ZnO transparent film and preparation method thereof.
Background technology
ZnO is the compound semiconductor with hexagonal system wurtzite structure of a kind of II-VI family, and its band gap width can be up to 3.37eV.The ZnO material non-toxic, the prices of raw and semifnished materials are cheap, and chemical stability is good.ZnO film has the optical transmittance height simultaneously, growth temperature is low, capability of resistance to radiation is strong and electronics saturation drift velocity advantages of higher.
ZnO has wide application prospect in a lot of fields, especially at interdisciplinary fields such as photoelectronics, ZnO film can also be applied to surface acoustic wave device, solar cell, gas sensor, pressure-active element, ultraviolet detector, luminescent device etc. except being applied among the TFT as active layer.
The performance of ZnO film and applied research thereof are in some aspects as comparative maturity such as piezoelectric properties, and the research of others has also obtained important achievement.Will be still attach most importance to from present various countries scholar's relevant research research from now on the aspects such as development research of development research, pressure sensitive quality and the low-voltage piezoresistor of the development research of the photoelectric property of ZnO film and photoelectric device, gas sensor.Advanced photoelectric device is one of basis of a lot of modern industry developments, and ZnO film has some more superior photoelectric property, and therefore, aspect the preparation of some photoelectric device, ZnO film has its special advantages.Utilize the better transparency electrode of ZnO film exploitation electrical property, have very wide prospect at aspects such as luminous element, solar cell window material, optical waveguide material, emission low pressure flat-panel screens materials.
The method for preparing at present the ZnO transparent film has a variety of, such as radio frequency sputtering method, double ion beam sputtered sedimentation, chemical Vapor deposition process, molecular beam hydatogenesis, pulsed laser deposition, spray heating decomposition and sol-gel method etc., certainly the film of prepared in various methods structure with all can have in nature certain different.Magnetron sputtering technique because of have the sedimentation rate height, substrate temperature is low, the film forming adhesion is good, easy to control, can realize advantages such as big area molding, can become the research focus of ZnO film technology of preparing with IC planar device process compatible.Magnetron sputtering is the major technique that present transparent conductive film industrialization is produced, and also is that ZnO film is realized commercial gordian technique.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of ZnO film, this method can prepare the ZnO film of high-crystallinity.
The preparation single crystal ZnO is transparent among the present invention leads the process program that film adopts and is: at first, and preparation ZnO ceramic target; Then, clean glass substrate; At last, use the sputter membrane equipment on glass substrate, to prepare ZnO film.
The technical process of preparation solid ceramic ZnO sputtering target material is: the sintering of the pressed compact of 1. weighing → 2. ball milling → 3. oven dry → 4. granulation → 5. → 6.;
Concrete grammar is: take by weighing a certain amount of purity as required and be 99.9%～99.95% reference level ZnO powder, and subsequently with these ZnO powders ball milling 18～20 hours in ball mill, granulation then after the powder after the oven dry sieved, the used binding agent of granulation is PVA; Re-use sieve after powder and binding agent mixed.With hydropress the powder that mixes is pressed into the target body that diameter is 50～60mm then, the added pressure of pressed compact is 75～90Mpa, makes target consolidation more; Then the target that suppresses is put into sintering oven, at first pre-burning under 700～750 degrees centigrade high temperature is increased to sintering temperature 1100～1200 degrees centigrade then, continues sintering, makes target become porcelain; Allow its naturally cooling then; Obtaining thickness after polishing is the ZnO solid ceramic sputtering target material thin discs of 3.8mm～4mm.
The membrane equipment of Shi Yonging is a JPG450C3 type high vacuum multilayer film magnetic control sputtering system in the present invention.Wherein during sputter in the sputtering chamber base vacuum degree be 1.75 * 10
-4～1.8 * 10
-4Pa, sputtering power are 150～160W, and the distance between target and the substrate is decided to be 10cm, and the scope of substrate temperature is 450 ℃～600 ℃, and argon oxygen ratio is that (sccm: sccm), sputtering pressure was 1Pa in 40: 0～20: 20.
Useful result of the present invention is: the ZnO film of the process program preparation among the present invention has the C axle preferrel orientation of height, has successfully realized the preparation of single crystal ZnO transparent film.
Embodiment
To be described in further detail the present invention by present embodiment below.
Embodiment one
(1) preparation ZnO ceramic target
Take by weighing 100g purity and be 99.95% reference level ZnO powder, with these ZnO powders ball milling 20 hours in ball mill, earlier with granulation then after the 60 purpose sieve, the used binding agent of granulation is PVA with the powder after the oven dry subsequently; Re-use 40 purpose sieve after powder and binding agent mixed.With hydropress the powder that mixes is pressed into the target body that diameter is 60mm then, the added pressure of pressed compact is 80MPa; Then the target that suppresses is put into sintering oven, at first pre-burning 2 hours under 750 degrees centigrade high temperature is increased to sintering temperature 1100 degrees centigrade then, continues sintering 2 hours, allows its naturally cooling then; Obtaining diameter after polishing is 60 ± 0.04mm, and thickness is the ZnO solid ceramic sputtering target material thin discs of 3.8mm～4mm.
(2) clean glass substrate;
(3) on glass substrate, prepare ZnO film.
Use JPG450C3 type high vacuum multilayer film magnetic control sputtering system on glass substrate, to prepare ZnO film; Wherein during sputter in the sputtering chamber base vacuum degree be 1.8 * 10
-4Pa, sputtering power are 150W, and the distance between target and the substrate is 10cm, and substrate temperature is 450 ℃, and argon oxygen ratio is that (sccm: sccm), sputtering pressure was 1Pa, and sputtering time is 30 minutes in 35: 5.
Embodiment two
(1) preparation ZnO ceramic target
Take by weighing 100g purity and be 99.9% reference level ZnO powder, subsequently with these ZnO powders ball milling 18 hours in ball mill, granulation then after the powder after the oven dry sieved, the used binding agent of granulation is PVA; Re-use sieve after powder and binding agent mixed.With hydropress the powder that mixes is pressed into the target body that diameter is 50mm then, the added pressure of pressed compact is 75MPa; Then the target that suppresses is put into sintering oven, at first pre-burning 2.5 hours under 700 degrees centigrade high temperature is increased to sintering temperature 1200 degrees centigrade then, continues sintering 2 hours, allows its naturally cooling then; Obtaining thickness after polishing is the ZnO solid ceramic sputtering target material thin discs of 3.8mm～4mm.
(2) clean glass substrate;
(3) on glass substrate, prepare ZnO film.
Use JPG450C3 type high vacuum multilayer film magnetic control sputtering system on glass substrate, to prepare ZnO film; Wherein during sputter in the sputtering chamber base vacuum degree be 1.75 * 10-4Pa, sputtering power is 155W, the distance between target and the substrate is 8cm, substrate temperature is 500 ℃, argon oxygen ratio is that (sccm: sccm), sputtering pressure was 1Pa, and sputtering time is 30 minutes in 30: 10.
Embodiment three
(1) preparation ZnO ceramic target;
Take by weighing 100g purity and be 99.92% reference level ZnO powder, subsequently with these ZnO powders ball milling 19 hours in ball mill, granulation then after the powder after the oven dry sieved, the used binding agent of granulation is PVA; Re-use sieve after powder and binding agent mixed.With hydropress the powder that mixes is pressed into the target body that diameter is 60mm then, the added pressure of pressed compact is 90MPa; Then the target that suppresses is put into sintering oven, at first pre-burning 2 hours under 750 degrees centigrade high temperature is increased to sintering temperature 1100 degrees centigrade then, continues sintering 2 hours, allows its naturally cooling then; Obtaining thickness after polishing is the ZnO solid ceramic sputtering target material thin discs of 3.8mm～4mm.
(2) clean glass substrate;
(3) on glass substrate, prepare ZnO film.
Wherein during sputter in the sputtering chamber base vacuum degree be 1.8 * 10-4Pa, sputtering power is 160W, the distance between target and the substrate is 12cm, substrate temperature is 600 ℃, argon oxygen ratio is that (sccm: sccm), sputtering pressure was 1Pa, and sputtering time is 30 minutes in 20: 20.
The above is a concrete case study on implementation of the present invention, but the present invention is not limited to the disclosed content of above-mentioned example; Related parameter can adjust by practical situation in the disclosed scope of content of the present invention.
Claims (5)
1.RF magnetron sputtering prepares the method for single crystal transparent ZnO film, it is characterized in that, at first, preparation ZnO ceramic target; Then, clean glass substrate; At last, use the sputter membrane equipment on glass substrate, to prepare ZnO film; The manufacture craft flow process of described preparation ZnO ceramic target is:
1. the sintering of the pressed compact of weighing → 2. ball milling → 3. oven dry → 4. granulation → 5. → 6.,
Concrete grammar is: take by weighing a certain amount of purity as required and be 99.9%～99.95% reference level ZnO powder, and subsequently with these ZnO powders ball milling 18～20 hours in ball mill, granulation then after the powder after the oven dry sieved, the used binding agent of granulation is PVA; Re-use sieve after powder and binding agent mixed.With hydropress the powder that mixes is pressed into the target body that diameter is 50～60mm then, the added pressure of pressed compact is 75～90MPa; Then the target that suppresses is put into sintering oven, at first pre-burning under 700～750 degrees centigrade high temperature is increased to sintering temperature 1100～1200 degrees centigrade then, continues sintering, allows its naturally cooling then; Obtaining thickness after polishing is the ZnO solid ceramic sputtering target material thin discs of 3.8mm～4mm.
2. RF magnetron sputtering as claimed in claim 1 prepares the method for single crystal transparent ZnO film, and described use sputter membrane equipment prepares ZnO film on glass substrate, it is characterized in that, membrane equipment is a JPG450C3 type high vacuum multilayer film magnetic control sputtering system; Wherein during sputter in the sputtering chamber base vacuum degree be 1.8 * 10
-4Pa, the sputtering power unification is decided to be 150W, and the distance between target and the substrate is decided to be 8～12cm, and the scope of substrate temperature is 450 ℃～600 ℃, and argon oxygen ratio is that (sccm: sccm), sputtering pressure was 1Pa in 40: 0～20: 20.
3. RF magnetron sputtering as claimed in claim 2 prepares the method for single crystal transparent ZnO film, it is characterized in that, described JPG450C3 type high vacuum multilayer film magnetic control sputtering system when sputter in the sputtering chamber base vacuum degree be 1.75 * 10
-4～1.8 * 10
-4Pa, sputtering power are 150～160W.
4. the method for preparing single crystal transparent ZnO film as claim 2 or 3 described RF magnetron sputterings, it is characterized in that, distance between target and the substrate is decided to be 8～12cm, the scope of substrate temperature is 450 ℃～600 ℃, argon oxygen ratio is that (sccm: sccm), sputtering pressure was 1Pa in 40: 0～20: 20.
5. RF magnetron sputtering as claimed in claim 2 prepares the method for single crystal transparent ZnO film, it is characterized in that, the sputtering time that uses the sputter membrane equipment to prepare ZnO film on glass substrate is 30 minutes.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102280529A (en) * | 2011-08-05 | 2011-12-14 | 保定天威集团有限公司 | Transparent conductive film with high Haze value and preparation method thereof |
| CN102351428A (en) * | 2011-06-23 | 2012-02-15 | 江苏宇天港玻新材料有限公司 | Production technology applying ceramic target to magnetron sputtering coated glass |
| CN103091692A (en) * | 2013-01-10 | 2013-05-08 | 同济大学 | Impedance type nickel film heatmeter based on laser etching method and manufacturing method thereof |
| CN103124805A (en) * | 2011-06-08 | 2013-05-29 | 株式会社半导体能源研究所 | Sputtering target, method for manufacturing sputtering target, and method for forming thin film |
| CN103724008A (en) * | 2013-12-13 | 2014-04-16 | 西北稀有金属材料研究院 | Pure zinc oxide ceramic sputtering target material and preparation method thereof |
| CN105869807A (en) * | 2016-05-03 | 2016-08-17 | 中国地质大学（北京） | Preparation method of zinc oxide-bismuth oxide thin film varistor |
| CN110208369A (en) * | 2019-06-19 | 2019-09-06 | 西南交通大学 | Multi-functional sound surface wave sensor and its preparation method and application |
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| US10889888B2 (en) | 2011-06-08 | 2021-01-12 | Semiconductor Energy Laboratory Co., Ltd. | Sputtering target, method for manufacturing sputtering target, and method for forming thin film |
| US11959165B2 (en) | 2011-06-08 | 2024-04-16 | Semiconductor Energy Laboratory Co., Ltd. | Semiconductor device comprising oxide semiconductor film |
| CN103124805A (en) * | 2011-06-08 | 2013-05-29 | 株式会社半导体能源研究所 | Sputtering target, method for manufacturing sputtering target, and method for forming thin film |
| CN103290371A (en) * | 2011-06-08 | 2013-09-11 | 株式会社半导体能源研究所 | Sputtering target, method for manufacturing sputtering target, and method for forming thin film |
| US11066739B2 (en) | 2011-06-08 | 2021-07-20 | Semiconductor Energy Laboratory Co., Ltd. | Sputtering target, method for manufacturing sputtering target, and method for forming thin film |
| US8889477B2 (en) | 2011-06-08 | 2014-11-18 | Semiconductor Energy Laboratory Co., Ltd. | Method for forming thin film utilizing sputtering target |
| CN103290371B (en) * | 2011-06-08 | 2015-02-25 | 株式会社半导体能源研究所 | Sputtering target, method for manufacturing sputtering target, and method for forming thin film |
| US9382611B2 (en) | 2011-06-08 | 2016-07-05 | Semiconductor Energy Laboratory Co., Ltd. | Sputtering target, method for manufacturing sputtering target, and method for forming thin film |
| CN102351428A (en) * | 2011-06-23 | 2012-02-15 | 江苏宇天港玻新材料有限公司 | Production technology applying ceramic target to magnetron sputtering coated glass |
| CN102280529A (en) * | 2011-08-05 | 2011-12-14 | 保定天威集团有限公司 | Transparent conductive film with high Haze value and preparation method thereof |
| CN103091692B (en) * | 2013-01-10 | 2015-08-19 | 同济大学 | Based on the impedance type nickel film calorimeter and preparation method thereof of laser etching method |
| CN103091692A (en) * | 2013-01-10 | 2013-05-08 | 同济大学 | Impedance type nickel film heatmeter based on laser etching method and manufacturing method thereof |
| CN103724008A (en) * | 2013-12-13 | 2014-04-16 | 西北稀有金属材料研究院 | Pure zinc oxide ceramic sputtering target material and preparation method thereof |
| CN105869807A (en) * | 2016-05-03 | 2016-08-17 | 中国地质大学（北京） | Preparation method of zinc oxide-bismuth oxide thin film varistor |
| CN110208369A (en) * | 2019-06-19 | 2019-09-06 | 西南交通大学 | Multi-functional sound surface wave sensor and its preparation method and application |
| CN110208369B (en) * | 2019-06-19 | 2020-08-14 | 西南交通大学 | Multifunctional surface acoustic wave sensor and preparation method and application thereof |
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Effective date of registration: 20110411 Address after: 523718 Tian Xin Industrial Zone, Tangxia Town, Dongguan, Guangdong Applicant after: Guangdong Zhicheng Champoin Group Co., Ltd. Co-applicant after: Huazhong University of Science and Technology Address before: 523718 Tian Xin Industrial Zone, Tangxia Town, Dongguan, Guangdong Applicant before: Guangdong Zhicheng Champoin Group Co., Ltd. |
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