CN101337773A - Method for preparing ITO film with high conductivity - Google Patents
Method for preparing ITO film with high conductivity Download PDFInfo
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- CN101337773A CN101337773A CNA2008100633992A CN200810063399A CN101337773A CN 101337773 A CN101337773 A CN 101337773A CN A2008100633992 A CNA2008100633992 A CN A2008100633992A CN 200810063399 A CN200810063399 A CN 200810063399A CN 101337773 A CN101337773 A CN 101337773A
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- ito film
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Abstract
The invention relates to a preparation method for a film, and aims to provide a preparation method for an ITO film with high conductive performance. The preparation method comprises the following steps: firstly, dissolving the inorganic salt predecessor of tin in ethanol, dissolving the inorganic salt predecessor of indium in acetylacetone, and controlling the ratio of the molar mass of the tin and the indium to be 1:10, stirring and refluxing the two solutions after being mixed for 3 hours at the 60 to 65 DEG C, and obtaining uniform and transparent light yellow sol rubber; secondly, taking quartz glass as a basal body, abstracting and plating the sol rubber, controlling the abstracting speed to be 200 mm/min; then carrying out the pre-heating treatment to a sol rubber film for 10 minutes at the 100 DEG C, later carrying out the annealing treatment for 1 hours at 550 DEG C, and obtaining a layer of ITO film; repeating the steps, and obtaining a multilayer ITO film; and thirdly, placing the ITO film under an ultraviolet light source for processing for 1 to 10 minutes through ultraviolet irradiation, and finally obtaining the ITO film with high conductive performance.
Description
Technical field
The present invention relates to a kind of preparation method of film, particularly a kind of preparation method with high conduction performance ITO film.
Background technology
Tin-doped indium oxide (Indium Tin Oxide claim ITO) transparent conductive film, as a kind of n type degeneracy semiconductor, with the transmittance in its excellent conducting performance, the higher visible-range, with matrix binding ability and good chemical stability preferably, more and more receive publicity, comprised in a lot of fields that the plane shows that aspects such as (liquid-crystal display LCD, display of organic electroluminescence OLED), solar cell, transmitter, functional glass are used widely.
At present, the preparation method of ITO film is a lot, comprise magnetron sputtering method, chemical meteorology deposition method, spray pyrolysis, anion electroplating method, vacuum vapor deposition method, ion beam sputtering and sol-gel method etc., with wherein the development the most sophisticated magnetron sputtering method compare, sol-gel method has that processing unit is simple, easy control of process conditions, production cost is lower and be easy to outstanding advantage such as big area industrialization production, and therefore preparing the ITO film with sol-gel method has been subjected to extensive concern both domestic and external.
As a kind of transparent conductive film material, the ITO film conductivity can quality directly determined the height of its using value, therefore the side of preparing hinders littler, the better ITO film of electroconductibility and prepares the ITO film for sol-gel method and be of great immediate significance under lower cost.
Summary of the invention
The objective of the invention is to propose a kind of preparation method with high conduction performance ITO film.The present invention prepares on the basis of ITO film in common sol-gel method, increased the processing sequence of one simple possible, promptly handled the ITO film, the resistance of film side is obviously reduced with UV-irradiation, improved the conductivity of film, the transmittance of film remains unchanged substantially simultaneously.
To achieve these goals, the present invention has adopted following concrete technological step:
(1) the inorganic salt precursor with tin is dissolved in ethanol, and the inorganic salt precursor of indium is dissolved in methyl ethyl diketone, and the ratio of the molar mass of control tin and indium is 1: 10; Two kinds of solution are mixed the back 60～65 ℃ of following stirring and refluxing 3 hours, obtain the faint yellow colloidal sol of transparent and homogeneous;
(2) be matrix with the silica glass, above-mentioned colloidal sol is lifted plated film, pull rate is 200mm/min; Again with dissolved glue film 100 ℃ of following thermal pretreatment 10 minutes, 550 ℃ of following anneal 1 hour, obtain 1 layer ITO film afterwards; Repeat above step, obtain multiwalled ITO film;
(3) aforementioned multiwalled ITO film is placed under the ultraviolet source through UV-irradiation and handled 1～10 minute, obtain having the ITO film of high conduction performance.
As a kind of improvement, the inorganic salt precursor of described tin is a tin chloride, and its chemical formula is SnCl
45H
2O.
As a kind of improvement, the inorganic salt precursor of described indium is an indium nitrate, and its chemical formula is In (NO)
34.5H
2O.
As a kind of improvement, used ultraviolet source is the conventional portable ultraviolet source, and irradiation power is 15～2000W.
The beneficial effect that the present invention had is:
The present invention handles by the UV-irradiation of simple possible, make side's resistance of the ITO film of sol-gel method preparation reduce 20%～50%, but the transmittance of film does not reduce, thereby under the prerequisite that does not influence the film light transmission, improved the conductivity of film, reached with low cost and obtain high performance purpose.
Description of drawings
Fig. 1 is 5 layers the AFM surface topography map of ITO film before UV-irradiation is handled 5min;
Fig. 2 is 5 layers the AFM surface topography map of ITO film after UV-irradiation is handled 5min;
Fig. 3 is the cross section line profile figure of 5 layers the AFM surface topography map correspondence of ITO film before UV-irradiation is handled 5min;
Fig. 4 is the cross section line profile figure of 5 layers the AFM surface topography map correspondence of ITO film after UV-irradiation is handled 5min;
Fig. 5 is 5 layers the AFM surface topography map of ITO film before UV-irradiation is handled 10min;
Fig. 6 is 5 layers the AFM surface topography map of ITO film after UV-irradiation is handled 10min;
Fig. 7 is the cross section line profile figure of 5 layers the AFM surface topography map correspondence of ITO film before UV-irradiation is handled 10min;
Fig. 8 is the cross section line profile figure of 5 layers the AFM surface topography map correspondence of ITO film after UV-irradiation is handled 10min;
Fig. 9 is 5 layers the XRD spectra of ITO film before and after UV-irradiation is handled 4min;
Figure 10 is 10 layers the XRD spectra of ITO film before and after UV-irradiation is handled 4min;
Figure 11 is before 5 layers ITO film UV-irradiation is handled and the XRD spectra of different time;
Figure 12 is that 10 groups of ITO films are at the square resistive graphic representation of different UV-irradiation under the treatment time;
Figure 13 is that the different ITO film of the number of plies is handled the variation histogram that hinders below the 4min in UV-irradiation;
Figure 14 is the different ITO film of the number of plies is handled transmittance under the 4min in UV-irradiation a change curve;
Figure 15 is 5 layers the transmittance change curve of ITO film under the different time radiation treatment.
Embodiment
Take by weighing 2.5gIn (NO)
34.5H
2O is dissolved in the 10ml methyl ethyl diketone, will be dissolved in the SnCl of micro-raw spirit
45H
2O mixes (tin indium molar ratio was by 1: 10) with it, at 60-65 ℃ of stirring and refluxing 3h, obtain ITO colloidal sol.Lift as matrix with silica glass then, pull rate is 200mm/min, and dissolved glue film is earlier at 100 ℃ of following thermal pretreatment 10min, put into 500 ℃ of heating of retort furnace again, take out naturally cooling behind the 1h rapidly, repeat above flow process (lifting-preheating-annealing), obtain multiwalled ITO film.Gained ITO film is placed on the radiation treatment of carrying out UV-light under the portable ultraviolet source of UV2000W, and the irradiation time of various sample does not wait from 1min to 10min.
Fig. 1 to Fig. 4 is the AFM surface topography map and the corresponding cross section line profile figure of 5 layers of ITO film, and wherein Fig. 1,3 is that Fig. 2,4 is behind the radiation treatment 5min before the radiation treatment.Both more as can be seen, after UV-irradiation was handled 5min, the grain-size on the surface of film obviously increased, and rootmean-square (RMS) surfaceness reduces to some extent, was reduced to 0.915nm by 1.342nm.Fig. 5 to Fig. 8 is the AFM surface topography map and the corresponding cross section line profile figure of 5 layers of ITO film, wherein Fig. 5,7 is before the radiation treatment, Fig. 6,8 is behind the radiation treatment 10min, equally after UV-irradiation is handled 10min, grain-size obviously increases, but rootmean-square (RMS) surfaceness does not have considerable change.Fig. 9 is 5 layers the XRD spectra of ITO film before and after UV-irradiation is handled 4min, and as can be seen from the figure UV-irradiation is handled the polycrystalline structure in cube ferrimanganic ore deposit that does not change film, but diffraction peak is strengthened, and has improved the degree of crystallinity of film greatly.Figure 10 is 10 layers the XRD spectra of ITO film before and after UV-irradiation is handled 4min, and same UV-irradiation is handled the degree of crystallinity that does not change the crystalline structure of film but improved film.Figure 11 is before 5 layers ITO film UV-irradiation is handled and the XRD spectra of different time (2.5min, 5min, 7.5min, 10min), the UV-irradiation that can draw different time from figure is handled the degree of crystallinity that has all improved film, but the difference of irradiation time is little to the influence of degree of crystallinity.Figure 12 is that the different ITO film of 10 prescriptions resistance is at the square resistive graphic representation of different UV-irradiation under the treatment time, as can be seen from the figure the UV-irradiation of different time is handled the side's resistance that all makes film certain reducing, but reduce degree and certain variation is arranged with the difference of irradiation time, when the time is 4min, reduce the degree maximum.Figure 13 is the variation histogram that the ITO film of number of plies difference (4 layers-10 layers) hinders below UV-irradiation is handled 4min, and UV-irradiation is handled the side that makes number of plies different I TO film and hindered all to have significantly and reduce as seen from the figure.Figure 14 is the change curve of ITO film transmittance under UV-irradiation processing 4min of number of plies difference (2,4,8 layers), and as seen from the figure, the radiation treatment of UV-light does not have influence substantially to the transmittance of ITO film.Figure 15 is 5 layers the transmittance change curve of ITO film after different time (2.5min, 5min, 7.5min) radiation treatment, and the variation of UV-irradiation time does not change the transmittance of ITO film equally.
At last, it is also to be noted that what more than enumerate only is specific embodiments of the invention.Obviously, the invention is not restricted to above examples of implementation, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (4)
1, a kind of preparation method with high conduction performance ITO film is characterized in that, may further comprise the steps:
(1) the inorganic salt precursor with tin is dissolved in ethanol, and the inorganic salt precursor of indium is dissolved in methyl ethyl diketone, and the ratio of the molar mass of control tin and indium is 1: 10; Two kinds of solution are mixed the back 60～65 ℃ of following stirring and refluxing 3 hours, obtain the faint yellow colloidal sol of transparent and homogeneous;
(2) be matrix with the silica glass, above-mentioned colloidal sol is lifted plated film, pull rate is 200mm/min; Again with dissolved glue film 100 ℃ of following thermal pretreatment 10 minutes, 550 ℃ of following anneal 1 hour, obtain 1 layer ITO film afterwards; Repeat above step, obtain multiwalled ITO film;
(3) aforementioned multiwalled ITO film is placed under the ultraviolet source through UV-irradiation and handled 1～10 minute, obtain having the ITO film of high conduction performance.
According to the described preparation method with high conduction performance ITO film of claim 1, it is characterized in that 2, the inorganic salt precursor of described tin is a tin chloride, its chemical formula is SnCl
45H
2O.
According to the described preparation method with high conduction performance ITO film of claim 1, it is characterized in that 3, the inorganic salt precursor of described indium is an indium nitrate, its chemical formula is In (NO)
34.5H
2O.
According to the described preparation method with high conduction performance ITO film of claim 1, it is characterized in that 4, used ultraviolet source is the conventional portable ultraviolet source, irradiation power is 15～2000W.
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| CN2008100633992A CN101337773B (en) | 2008-08-14 | 2008-08-14 | Method for preparing ITO film with high conductivity |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101949091A (en) * | 2010-07-30 | 2011-01-19 | 东华大学 | Preparation method of ITO/polyester composite conductive fabric through sol-gel method |
| CN101950043A (en) * | 2010-08-19 | 2011-01-19 | 浙江理工大学 | ITO film loaded silica optical fiber and preparation method thereof |
| CN102298478A (en) * | 2011-10-11 | 2011-12-28 | 南京华显高科有限公司 | Preparation method for electrode protecting film of capacitive touch screen |
| CN102339905A (en) * | 2011-10-24 | 2012-02-01 | 通用光伏能源(烟台)有限公司 | Method for manufacturing transparent conductive oxide film glass by using LPCVD (low pressure chemical vapor deposition) technology and taking inorganic salt as precursor |
| CN103922609A (en) * | 2014-03-27 | 2014-07-16 | 浙江大学 | Preparation method and product of colloid ITO nanocrystal film |
| CN104037279A (en) * | 2014-07-01 | 2014-09-10 | 厦门市三安光电科技有限公司 | Method for manufacturing light emitting diode (LED) with current blocking layer |
| CN105776889A (en) * | 2016-03-26 | 2016-07-20 | 上海大学 | Method for enhancing transparency and conductivity of conducting glass |
| CN105992408A (en) * | 2015-02-11 | 2016-10-05 | 佛山市顺德区美的电热电器制造有限公司 | Manufacturing method of electrothermal film layer, the electrothermal film layer, electric heating disc and cooking utensil |
| CN107992234A (en) * | 2017-12-29 | 2018-05-04 | 东莞北斗同创智能科技有限公司 | A kind of intelligence wearing touch-screen and its semi-transparent ito film layer manufacturing method thereof |
| CN108962436A (en) * | 2018-07-06 | 2018-12-07 | 无锡众创未来科技应用有限公司 | The method for manufacturing transparent conductive film |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1299326C (en) * | 2004-07-30 | 2007-02-07 | 西安理工大学 | Tin-doped indium oxide film and making process of fine pattern |
-
2008
- 2008-08-14 CN CN2008100633992A patent/CN101337773B/en not_active Expired - Fee Related
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101949091B (en) * | 2010-07-30 | 2011-12-14 | 东华大学 | Preparation method of ITO/polyester composite conductive fabric through sol-gel method |
| CN101949091A (en) * | 2010-07-30 | 2011-01-19 | 东华大学 | Preparation method of ITO/polyester composite conductive fabric through sol-gel method |
| CN101950043B (en) * | 2010-08-19 | 2014-08-27 | 浙江理工大学 | ITO film loaded silica optical fiber and preparation method thereof |
| CN101950043A (en) * | 2010-08-19 | 2011-01-19 | 浙江理工大学 | ITO film loaded silica optical fiber and preparation method thereof |
| CN102298478A (en) * | 2011-10-11 | 2011-12-28 | 南京华显高科有限公司 | Preparation method for electrode protecting film of capacitive touch screen |
| CN102339905A (en) * | 2011-10-24 | 2012-02-01 | 通用光伏能源(烟台)有限公司 | Method for manufacturing transparent conductive oxide film glass by using LPCVD (low pressure chemical vapor deposition) technology and taking inorganic salt as precursor |
| CN103922609A (en) * | 2014-03-27 | 2014-07-16 | 浙江大学 | Preparation method and product of colloid ITO nanocrystal film |
| CN104037279A (en) * | 2014-07-01 | 2014-09-10 | 厦门市三安光电科技有限公司 | Method for manufacturing light emitting diode (LED) with current blocking layer |
| CN105992408A (en) * | 2015-02-11 | 2016-10-05 | 佛山市顺德区美的电热电器制造有限公司 | Manufacturing method of electrothermal film layer, the electrothermal film layer, electric heating disc and cooking utensil |
| CN105992408B (en) * | 2015-02-11 | 2020-03-10 | 佛山市顺德区美的电热电器制造有限公司 | Manufacturing method of electric heating film layer, electric heating disc and cooking utensil |
| CN105776889A (en) * | 2016-03-26 | 2016-07-20 | 上海大学 | Method for enhancing transparency and conductivity of conducting glass |
| CN105776889B (en) * | 2016-03-26 | 2019-02-01 | 上海大学 | A method of enhancing electro-conductive glass permeability and electric conductivity |
| CN107992234A (en) * | 2017-12-29 | 2018-05-04 | 东莞北斗同创智能科技有限公司 | A kind of intelligence wearing touch-screen and its semi-transparent ito film layer manufacturing method thereof |
| CN108962436A (en) * | 2018-07-06 | 2018-12-07 | 无锡众创未来科技应用有限公司 | The method for manufacturing transparent conductive film |
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|---|---|
| CN101337773B (en) | 2010-12-08 |
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Effective date of registration: 20190508 Address after: 310000 Room 814, Building 5, Poly Tiandi Center, Hangzhou Economic and Technological Development Zone, Zhejiang Province Patentee after: Hangzhou Xinzhi Investment Management Co., Ltd. Address before: 310018 No. 5, No. 2 Street, Xiasha Higher Education Park, Hangzhou City, Zhejiang Province Patentee before: Zhejiang Sci-Tech University |
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