CN113106405A - Method for reducing infrared absorption rate of ITO film - Google Patents
Method for reducing infrared absorption rate of ITO film Download PDFInfo
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- CN113106405A CN113106405A CN202110290390.0A CN202110290390A CN113106405A CN 113106405 A CN113106405 A CN 113106405A CN 202110290390 A CN202110290390 A CN 202110290390A CN 113106405 A CN113106405 A CN 113106405A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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Abstract
The invention provides a method for reducing the infrared absorptivity of an ITO film, which comprises the following steps: a substrate cleaning step: using transparent high-quality float glass as a substrate, and cleaning the substrate by using acetone in an ultrasonic environment; the ITO film preparation step: depositing an ITO film, setting the rotating speed and sputtering power of a target material, and obtaining the ITO film after a set time; and (3) annealing treatment: and (3) carrying out rapid thermal annealing treatment on the prepared ITO film by using a rapid thermal treatment furnace, and annealing to obtain the final ITO film. The invention realizes the preparation of the ITO film with low infrared absorption and high transmissivity, and the resistivity of the film is lower. And the subsequent treatment process of the invention is simple and stable.
Description
Technical Field
The invention relates to the field of films for silicon optical communication, in particular to a method for reducing the infrared absorption rate of an ITO film.
Background
In a silicon optical communication system, active devices such as photodetectors and modulators need to use electrodes in order for the devices to operate properly. The commonly used electrode material is metal electrode such as Ti/TiN/Al, Al/Ti/Au, W/Cu, etc. However, the metal electrode has strong infrared absorption to light in the infrared communication band, which results in large propagation loss of light in the waveguide, thereby reducing the responsivity of the detector. The ITO film has the characteristics of high light transmittance and low resistance through process optimization, can be used as a detector electrode, and well solves the problem of high infrared absorption of a metal electrode.
Linfeng et al (patent number: 201310306744.1) completely clean and polish the transparent film substrate, select a proper magnetron sputtering condition to deposit an ITO film, and finally anneal for 15-25 minutes in an environment of 90-150 ℃ to obtain the ITO conductive film with high light transmittance and low resistivity applied to the field of mobile communication touch screens. Wangwonjun et al (patent number: 201310737480.5) move the ITO film to make a nano-corrugated structure by the distance of the focal point of picosecond laser from the ITO film by 2-3mm, thereby improving the infrared band light transmittance of the film solar cell. Honrui gold et al (patent number: 201611121607.0) bombard the surface of Cu/ITO composite film by electron beam irradiation under certain vacuum degree and certain power to modify it, and cool to obtain the composite film with enhanced near infrared transmission.
The first method is mainly applied to the field of touch screens, the resistivity of the film is still high, and the first method is not suitable for silicon optical communication; the preparation processes of the nanometer corrugated structure and the Cu/ITO composite film of the last two methods are complex.
In order to reduce the infrared absorptivity and the resistivity of the ITO film and improve the light transmittance of the ITO film, annealing treatment is carried out on the ITO film subjected to magnetron sputtering under specific conditions in an air atmosphere to obtain the ITO film with high transmittance and low resistivity. The method has simple follow-up treatment on the ITO film and good stability, and can be well applied to the germanium-silicon photoelectric detector within the 1510-1630nm wave band range as a low infrared absorption electrode.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for reducing the infrared absorptivity of an ITO film.
The method for reducing the infrared absorptivity of the ITO film provided by the invention comprises the following steps:
a substrate cleaning step: using transparent high-quality float glass as a substrate, and cleaning the substrate by using acetone in an ultrasonic environment;
the ITO film preparation step: depositing an ITO film, setting the rotating speed and sputtering power of a target material, and obtaining the ITO film after a set time;
and (3) annealing treatment: and (3) carrying out rapid thermal annealing treatment on the prepared ITO film by using a rapid thermal treatment furnace, and annealing to obtain the final ITO film.
Preferably, a Denton magnetron sputtering device is used for depositing the ITO film.
Preferably, in the step of preparing the ITO film, the rotating speed of the target is 3.6rpm, and the sputtering power is 200W.
Preferably, in the step of preparing the ITO film, the ITO film with the thickness of 300nm is obtained after 583 s.
Preferably, the method further comprises the step of testing the optical performance: the film was tested for absorbance (A), transmittance (T), and reflectance (R) using a Lamda950 ultraviolet-visible near infrared spectrophotometer, with the experimental set-up measuring range being 400-1800 nm.
Preferably, the method further comprises the following electrical performance testing steps: and carrying out I-V test on the ITO film by using a semiconductor parameter tester.
Preferably, the semiconductor parametric tester comprises an agent BA1500 device.
Preferably, the rapid thermal processing furnace includes an RTP-CT150M apparatus.
Preferably, in the annealing treatment step, the annealing temperature is 300-500 ℃, and the annealing time is 5 minutes.
Preferably, in the annealing treatment step, the annealing atmosphere is air.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention realizes the preparation of the ITO film with low infrared absorption and high transmissivity, and the resistivity of the film is lower.
2. The subsequent treatment process of the invention is simple and stable.
3. The ITO thin film obtained by the process has the infrared absorptivity reduced to below 10 percent, the light transmittance improved to above 80 percent and the resistivity of 9.35 x 10 within the wavelength range of 1510-1630nm-6Omega · m, can replace the traditional metal electrode to be used in active devices such as detectors, modulators and the like, and reduce the infrared absorption brought by the metal electrode.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a flow chart of the steps of the present invention.
FIGS. 2-7 are graphs of the optical properties of films after unannealed and different annealing temperature treatments.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be obvious to those skilled in the art that various changes and modifications can be made without departing from the spirit of the invention. All falling within the scope of the present invention.
As shown In FIGS. 1 to 7, the present invention provides a method for reducing the infrared absorption rate of an ITO thin film, In element of a metal phase In the ITO thin film reacts with oxygen In the air during an air atmosphere annealing process to form In an oxidized state2O3Resulting in a reduced carrier concentration in the ITO. According to the delude model, a decrease in carrier concentration red-shifts the absorption wavelength of light. As the annealing temperature is increased, the carrier concentration is gradually reduced, and the absorption of the 1510-1630nm wave band is gradually reduced. On the other hand, the resistivity increases with decreasing carrier concentration, so the choice of temperature requires a compromise between absorption and resistivity. The annealing temperature is determined by a series of experiments below.
Step S1: and (3) cleaning the substrate, namely cleaning the substrate by using transparent high-quality float glass as a substrate and using acetone in an ultrasonic environment to ensure the cleanness of the surface of the substrate.
Step S2: preparing an ITO film: and depositing the ITO film by using a Denton magnetron sputtering device, wherein the rotating speed of a target is 3.6rpm, the sputtering power is 200W, and obtaining the ITO film with the thickness of 300nm after 583 s.
Step S3: annealing treatment: and (3) carrying out rapid thermal annealing treatment on the prepared ITO film by using a rapid thermal treatment furnace (Premtec RTP-CT150M), wherein the annealing temperature is 300-500 ℃, the annealing time is 5 minutes, and the annealing atmosphere is air. And annealing to obtain the final ITO film.
Step S4: and (3) testing optical performance: the film was tested for absorbance (a), transmittance (T), and reflectance (R) using a Lamda950 uv-vis nir spectrophotometer. The measurement range of the experimental setup was 400-1800 nm. The results of the thin film tests obtained under the different annealing conditions are shown in fig. 2-7. The absorbance and transmittance at 1550nm are shown in Table 1.
Step S5: and (3) testing electrical properties: I-V testing was performed on the ITO film using a semiconductor parameter tester (active BA1500) to obtain film resistivities at different annealing temperatures as shown in Table 2.
TABLE 1 absorption and transmittance of ITO thin films at different annealing temperatures
TABLE 2 resistivity of ITO films at different annealing temperatures
Example 1:
according to a first embodiment of the present invention, there is provided the steps of:
(1) and (3) cleaning the substrate, namely cleaning the substrate by using transparent high-quality float glass as a substrate and using acetone in an ultrasonic environment to ensure the cleanness of the surface of the substrate.
(2) Preparing an ITO film: and depositing the ITO film by using a Denton multi-target magnetron sputtering device, wherein the target rotating speed is 3.6rpm, the sputtering power is 200W, and obtaining the ITO film with the thickness of 300nm after 583 s.
(3) Annealing treatment: the prepared ITO film was subjected to rapid thermal annealing using a rapid thermal processing furnace (Premtec RTP-CT150M) at 300 ℃ for 5 minutes in an atmosphere of air. And annealing to obtain the final ITO film.
(4) And (3) testing optical performance: the film was tested for absorbance (a), transmittance (T), and reflectance (R) using a Lamda950 uv-vis nir spectrophotometer. The measurement range of the experimental setup was 400-1800 nm. The results of the thin film tests obtained under the different annealing conditions are shown in figure 3.
(5) And (3) testing electrical properties: the ITO film was subjected to I-V test using a semiconductor parameter tester (active BA1500) to obtain film resistivity as shown in Table 2.
Example 2:
the procedure was carried out in the same manner as in example 1 except for the following differences.
And (3) carrying out rapid thermal annealing treatment on the ITO film prepared in the step (2) by using a rapid thermal treatment furnace (Premtec RTP-CT150M), wherein the annealing temperature is 350 ℃, the annealing time is 5 minutes, and the annealing atmosphere is air. And annealing to obtain the final ITO film.
The obtained results are different from the optical properties of the ITO thin film in example 1, and the obtained results are shown in FIG. 4; the resistivity of the obtained films was shown in Table 2, depending on the resistance characteristics.
Example 3:
the procedure was carried out in the same manner as in example 1 except for the following differences.
And (3) carrying out rapid thermal annealing treatment on the ITO film prepared in the step (2) by using a rapid thermal treatment furnace (Premtec RTP-CT150M), wherein the annealing temperature is 400 ℃, the annealing time is 5 minutes, and the annealing atmosphere is air. And annealing to obtain the final ITO film.
The obtained results are different from the optical properties of the ITO thin film in example 1, and the obtained results are shown in FIG. 5; the resistivity of the obtained films was shown in Table 2, depending on the resistance characteristics.
Example 4:
the procedure was carried out in the same manner as in example 1 except for the following differences.
And (3) carrying out rapid thermal annealing treatment on the ITO film prepared in the step (2) by using a rapid thermal treatment furnace (Premtec RTP-CT150M), wherein the annealing temperature is 450 ℃, the annealing time is 5 minutes, and the annealing atmosphere is air. And annealing to obtain the final ITO film.
The obtained results were different from the optical properties of the ITO thin film of example 1, and the obtained results are shown in FIG. 6; the resistivity of the obtained films was shown in Table 2, depending on the resistance characteristics.
Example 5:
the procedure was carried out in the same manner as in example 1 except for the following differences.
And (3) carrying out rapid thermal annealing treatment on the ITO film prepared in the step (2) by using a rapid thermal treatment furnace (Premtec RTP-CT150M), wherein the annealing temperature is 500 ℃, the annealing time is 5 minutes, and the annealing atmosphere is air. And annealing to obtain the final ITO film.
The results obtained were different from the optical properties of the ITO thin film of example 1, and the results are shown in FIG. 7; the resistivity of the obtained films was shown in Table 2, depending on the resistance characteristics.
Annealing at 450 deg.C for 5 min in air atmosphere to obtain ITO film with infrared absorption rate reduced to below 10%, light transmittance increased to above 80%, and resistivity of 9.35 x 10-6Omega · m, can replace the traditional metal electrode to be used in active devices such as detectors, modulators and the like, and reduce the infrared absorption brought by the metal electrode.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The embodiments and features of the embodiments of the present application may be combined with each other arbitrarily without conflict.
Claims (10)
1. A method for reducing the infrared absorptivity of an ITO film is characterized by comprising the following steps:
a substrate cleaning step: using transparent float glass as a substrate, and cleaning the substrate by using acetone in an ultrasonic environment;
the ITO film preparation step: depositing an ITO film, setting the rotating speed and sputtering power of a target material, and obtaining the ITO film after a set time;
and (3) annealing treatment: and (3) carrying out rapid thermal annealing treatment on the prepared ITO film by using a rapid thermal treatment furnace, and annealing to obtain the final ITO film.
2. The method for reducing the infrared absorptivity of the ITO film according to claim 1, wherein the ITO film is deposited by a Denton magnetron sputtering device.
3. The method for reducing the infrared absorptivity of the ITO film according to claim 1, wherein in the ITO film preparing step, the target rotating speed is 3.6rpm, and the sputtering power is 200W.
4. The method for reducing the infrared absorptivity of the ITO thin film according to claim 1, wherein in the ITO thin film preparing step, the ITO thin film with the thickness of 300nm is obtained after 583 seconds.
5. The method for reducing the infrared absorptivity of the ITO thin film according to claim 1, further comprising the step of testing the optical properties of: the absorption rate, the transmission rate and the reflectivity of the film are tested by using a Lamda950 ultraviolet-visible near infrared spectrophotometer, and the measurement range of the experimental setting is 400-1800 nm.
6. The method for reducing the infrared absorptivity of the ITO film according to claim 1, further comprising the step of testing the electrical properties of: and carrying out I-V test on the ITO film by using a semiconductor parameter tester.
7. The method for reducing the infrared absorptivity of the ITO thin film according to claim 6, wherein the semiconductor parameter tester comprises an Agient BA1500 device.
8. The method for reducing the infrared absorptivity of the ITO film according to claim 1, wherein the rapid thermal processing furnace comprises an RTP-CT150M equipment.
9. The method of claim 1, wherein the annealing step comprises an annealing temperature of 300-500 ℃ for 5 minutes.
10. The method for reducing the infrared absorptivity of the ITO thin film according to claim 1, wherein in the annealing treatment step, the annealing atmosphere is air.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104593739A (en) * | 2014-12-25 | 2015-05-06 | 庞凤梅 | Radio-frequency magnetron sputtering process for improving properties of ITO (indium tin oxide) films and ITO film |
| CN105951046A (en) * | 2016-05-19 | 2016-09-21 | 昆明理工大学 | Preparation method of ITO thin film |
| CN106521415A (en) * | 2016-10-27 | 2017-03-22 | 中山大学 | Modified transparent conductive indium oxide film annealing method |
| TW201738181A (en) * | 2015-12-24 | 2017-11-01 | 日本電氣硝子股份有限公司 | Transparent conductive film, substrate provided with transparent conductive film, and method for producing substrate provided with transparent conductive film |
| CN111733388A (en) * | 2019-03-25 | 2020-10-02 | 东莞新科技术研究开发有限公司 | Preparation method of ITO film |
-
2021
- 2021-03-18 CN CN202110290390.0A patent/CN113106405A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104593739A (en) * | 2014-12-25 | 2015-05-06 | 庞凤梅 | Radio-frequency magnetron sputtering process for improving properties of ITO (indium tin oxide) films and ITO film |
| TW201738181A (en) * | 2015-12-24 | 2017-11-01 | 日本電氣硝子股份有限公司 | Transparent conductive film, substrate provided with transparent conductive film, and method for producing substrate provided with transparent conductive film |
| CN105951046A (en) * | 2016-05-19 | 2016-09-21 | 昆明理工大学 | Preparation method of ITO thin film |
| CN106521415A (en) * | 2016-10-27 | 2017-03-22 | 中山大学 | Modified transparent conductive indium oxide film annealing method |
| CN111733388A (en) * | 2019-03-25 | 2020-10-02 | 东莞新科技术研究开发有限公司 | Preparation method of ITO film |
Non-Patent Citations (2)
| Title |
|---|
| 刘峰: "射频磁控溅射制备ITO薄膜及其透明导电性能的研究", 《中国优秀硕士学位论文全文数据库（工程科技Ⅰ辑）》 * |
| 王德苗等: "真空和大气退火对ITO膜特性的影响", 《浙江大学学报》 * |
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Application publication date: 20210713 |