CN103031517A - ITO (indium tin oxide) film and manufacturing method thereof - Google Patents
ITO (indium tin oxide) film and manufacturing method thereof Download PDFInfo
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- CN103031517A CN103031517A CN2011103020412A CN201110302041A CN103031517A CN 103031517 A CN103031517 A CN 103031517A CN 2011103020412 A CN2011103020412 A CN 2011103020412A CN 201110302041 A CN201110302041 A CN 201110302041A CN 103031517 A CN103031517 A CN 103031517A
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Abstract
The invention relates to an ITO (indium tin oxide) film and a manufacturing method thereof. The ITO film comprises an ITO main body layer and an ITO covering layer arranged on the main body layer, wherein the atomic ratio value of O/(In+Sn) in the covering layer is less than that of O/(In+Sn) in the main body layer, and the thickness of the covering layer is between 50 angstroms and 200 angstroms. The invention further provides a manufacturing method of the ITO film. The method comprises the following steps of: (A) depositing one ITO main body layer under an environment with oxygen gas and argon gas; and (B) depositing one ITO covering layer on the ITO main body layer under an environment with argon gas and hydrogen gas, thereby manufacturing the ITO film. The covering layer of the ITO film provided by the invention can provide an electrical property stabilizing effect, and can be used for avoiding the influence of an annealing process on the electrical property of the film, so as to form the ITO film with excellent light transmittance and electrical conductivity.
Description
Technical field
The present invention relates to a kind ofly comprise the tectal indium tin oxides film of low oxygen content tin indium oxide, and the making method of this indium tin oxides film.
Background technology
Tin indium oxide (Indium Tin Oxide, ITO) is a kind of at Indium sesquioxide (In
2O
3) an amount of stannic oxide (SnO of middle interpolation
2) formed semiconductor material.Because the indium tin oxide films of crystalline form can possess excellent electroconductibility, light transmission and low reflection characteristic simultaneously, be widely used in recent years the fields such as flat-panel screens, touch panel, solar cell or various optical coatings, become a kind of transparent electrode material indispensable in the opto-electronics.
Yet, in case after the indium tin oxide films crystallization, just be difficult for carrying out again etch process.Therefore, usually can be first at the indium tin oxide films of the noncrystalline kenel of substrate deposition, etch predetermined electrode pattern with suitable etching solution after, again film is carried out anneal, use forming the crystalline form indium tin oxide films that possesses electroconductibility and light transmission.
Comprise in order to the method for making indium tin oxide films at present: sol-gel method, spray pyrolysis, physical vaporous deposition or chemical Vapor deposition process etc.Wherein, physical vaporous deposition is the method that is most commonly used to be coated with indium tin oxides film.Generally be under the normal temperature state, carry out sputter-deposited with tin indium oxide target material, for reaching better resistance and penetration coefficient, usually pass into a small amount of oxygen.When indium tin oxides film is deposited on substrate through behind the wet etching process, can carry out high-temperature annealing process in atmosphere, at this moment, indium tin oxides film can be constantly oxidized, carrier concentration reduction, resistivity in the film are improved, and then the conductive characteristic of deteriorated indium tin oxide films.
The problem that faces for overcoming prior art, the present invention develops a kind of indium tin oxide films with tectum protection, to avoid film constantly oxidized detrimentally affect that is caused in annealing process.
Summary of the invention
Main purpose of the present invention provides a kind of indium tin oxides film; it comprises one deck in order to protect the tin indium oxide tectum of body layer; can avoid the indium tin oxides film detrimentally affect that continuous oxidation causes in annealing process, promote by this photoelectric characteristic of indium tin oxides film.
For reaching above-mentioned purpose, the invention provides a kind of indium tin oxides film, comprising: the tin indium oxide body layer; And be arranged at tin indium oxide tectum on this body layer; Wherein, in this tin indium oxide tectum Sauerstoffatom to the atomic ratio (atomic ratio of oxygen to sum of Indium and tin) (O/ (In+Sn)) of the indium tin atom atomic ratio less than O/ (In+Sn) in this tin indium oxide body layer.
In indium tin oxides film of the present invention, Sauerstoffatom accounts for the ratio (that is, body layer and tectal oxygen level) of phosphide atom and tin atom sum for affecting the key factor of tin indium oxide membrane property in body layer and the tectum.In this specification sheets, " O/ (In+Sn) " represention oxygen atom represents body layer or tectal oxygen level in the indium tin oxides film for the ratio of phosphide atom and tin atom sum with this.
In indium tin oxides film of the present invention, effect in order to ensure the electrical quality of tin indium oxide tectum stabilizing films, the atomic ratio that is preferably O/ (In+Sn) in the tin indium oxide tectum is controlled in below 1.25, and better is that atomic ratio with O/ (In+Sn) in the tin indium oxide tectum is controlled between 1.19 and 1.24.In addition, the oxygen level of tin indium oxide body layer also is the key factor that affects the film characteristics of indium tin oxides film.When the oxygen level of tin indium oxide body layer is too high, can improve the resistivity of indium tin oxides film; Cross when low when the oxygen level of tin indium oxide body layer, then can reduce the light transmission of indium tin oxides film.Therefore, in order to ensure resistivity and the light transmission of indium tin oxides film, the atomic ratio that is preferably O/ (In+Sn) in the tin indium oxide body layer is controlled between 1.3 to 1.45.
In indium tin oxides film of the present invention, the tin indium oxide tectum can affect the transmittance of film.Therefore, in order to ensure the light transmission of indium tin oxides film, being preferably the tectal gauge control of tin indium oxide is between 50 to 200 dusts.
Another object of the present invention is that a kind of making method of indium tin oxides film is being provided, can not need increase extra processing step, directly in same sputter cavity, finish the making that comprises body layer and tectal indium tin oxides film with a sputtering process, use forming the indium tin oxides film with good stability and photoelectric characteristic.
For reaching above-mentioned purpose, the invention provides a kind of making method of indium tin oxides film, it comprises the following steps: (A), at oxygen and ar gas environment deposit one tin indium oxide body layer; And (B), under argon gas and hydrogen environment, on the tin indium oxide body layer deposition one tin indium oxide tectum, to make above-mentioned indium tin oxides film; Wherein, step (A) and step (B) are to finish the making of indium tin oxides film in same sputter cavity with sputtering process.
In the making method of indium tin oxides film of the present invention; because the method mainly is to finish the making of two kinds of different film films with one-time process at same sputter cavity; by adjusting body layer and tectal oxygen level, make the indium tin oxide films with tectum protection.In this making method, the parameter setting of sputtering process can change along with the difference of sputtering machine table or target, and therefore, this sputtering process parameter also need not to be confined to a certain specific scope.
Therefore, sputtering machine table and target that the present invention is corresponding different, can control respectively the filming parameter of two-stage process, directly in same sputter cavity, comprise body layer and tectal indium tin oxides film with a sputtering process formation, under the prerequisite that does not improve process complexity, the indium tin oxides film that makes stability more and not destroyed by annealing process.
In addition, indium tin oxides film of the present invention can be controlled in suitable scope with body layer and tectal oxygen level, to promote the electrical quality of indium tin oxides film, makes it possess lower resistivity and higher resistance uniformity coefficient; And with body layer and tectal gauge control in suitable scope, to guarantee the light transmission of indium tin oxides film, use the indium tin oxides film that formation is not destroyed by annealing process.
Description of drawings
Fig. 1 is the diagrammatic cross-section of indium tin oxides film of the present invention.
Fig. 2 is the sheet resistance value of the embodiment of the invention 1 to embodiment 3 and comparative example 1 and the graphic representation of sheet resistance unevenness.
Fig. 3 is that the tectal thickness of tin indium oxide is to the graphic representation of sheet resistance value and sheet resistance unevenness.
Fig. 4 be in the tin indium oxide tectum of different thickness optical wavelength to the graphic representation of the transmittance of indium tin oxides film.
The primary clustering nomenclature:
1 indium tin oxides film, 11 tin indium oxide body layers, 12 tin indium oxide tectums
Embodiment
Indium tin oxides film of the present invention can be controlled in suitable scope with body layer and tectal oxygen level, below by the analysis of resistivity and resistance uniformity coefficient, knows quite well body layer and tectal oxygen level to the impact of the electrical quality of indium tin oxides film.
Below, will further by following each embodiment content of the present invention be described, but what should understand is that these embodiment are only in order to the usefulness of explanation, and should not be regarded as the restriction of the present invention on implementing.
Embodiment 1
At first, place a substrate and a sputtered target material in the sputter cavity, both are at a distance of 10 centimeters.Afterwards, passing into oxygen and the flow that flow is 0.4sccm is the argon gas of 50sccm, with 0.5W/cm
2Electric power, operating pressure is maintained under the 2.5mtorr, deposit thickness is
Tin indium oxide body layer 11, as shown in Figure 1.
Then, in same sputter cavity, adjust the filming parameter of instrument, under identical operating pressure and electric power, passing into hydrogen and the flow that flow is 10sccm is the argon gas of 40sccm, forms thickness and be on tin indium oxide body layer 11
Tin indium oxide tectum 12, as shown in Figure 1.
Accordingly, the present invention need not increase extra processing step, can be directly in same sputter cavity with a sputtering process, finish the deposition of two kinds of different film films.By adjusting different filming parameters, form tin indium oxide body layer 11 and the tin indium oxide tectum 12 of two kinds of different film oxygen level, use forming the indium tin oxides film 1 with 12 protections of tin indium oxide tectum.
Measure respectively the oxygen level of tin indium oxide body layer 11 and tin indium oxide tectum 12 with x-ray photoelectron power spectrum (X-ray photoelectron spectroscopy, XPS).Wherein, the atomic ratio of the O/ of tin indium oxide body layer 11 (In+Sn) is 1.33; And the atomic ratio of the O/ of tin indium oxide tectum 12 (In+Sn) is 1.24.
After indium tin oxides film is made, in 245 ℃ atmospheric environment, carry out annealing process, namely finish the making of indium tin oxide films of the present invention.
Described as embodiment 1, embodiment 2 shows greatly identical method and makes the indium tin oxides film that comprises tin indium oxide tectum and tin indium oxide body layer.
The present embodiment difference from Example 1 is, makes the tectal filming parameter of tin indium oxide and be that to pass into hydrogen and the flow that flow is 15sccm be the argon gas of 35sccm, and the atomic ratio that forms O/ (In+Sn) is 1.22 tin indium oxide tectum.
Described as embodiment 1, embodiment 3 shows greatly identical method and makes the indium tin oxides film that comprises tin indium oxide tectum and tin indium oxide body layer.
The present embodiment difference from Example 1 is, makes the tectal filming parameter of tin indium oxide and be that to pass into hydrogen and the flow that flow is 20sccm be the argon gas of 30sccm, and the atomic ratio that forms O/ (In+Sn) is 1.19 tin indium oxide tectum.
Comparative example 1
Comparative example 1 is to make the tin indium oxide body layer with the method as embodiment 1, but does not have to protect the tin indium oxide tectum of body layer on this body layer, and directly the parameter with body layer deposits
Indium tin oxide films.
" the tin indium oxide tectum is on the impact of the photoelectric characteristic of indium tin oxides film "
Test case 1: sheet resistance value and sheet resistance unevenness
In test case 1, be the sample of inquiring into embodiment 1 to embodiment 3 and comparative example 1, before not passing through annealing process and after the annealed technique, the tectal existence of tin indium oxide is on the impact of sheet resistance value and the sheet resistance unevenness of indium tin oxides film.Wherein, the tectal oxygen level of the filming parameter of each sample and tin indium oxide is with the test of x-ray photoelectron power spectrum, and its result is as shown in table 1.
Table 1: the tectal filming parameter of the tin indium oxide of each sample and oxygen level value in the test case 1
Embodiment 1 | |
|
Comparative example 1 | |
Argon flow amount | 40sccm | 35sccm | 30sccm | - |
Hydrogen flowing quantity | 10sccm | 15sccm | 20sccm | - |
Tectal O/ (In+Sn) | 1.24 | 1.22 | 1.19 | 1.33 |
Embodiment 1 to embodiment 3 indium tin oxides film compared to comparative example 1, after annealed technique, its sheet resistance value and sheet resistance unevenness are to measure by four-point probe, and the result wherein has lower sheet resistance value and lower sheet resistance unevenness as shown in Figure 2.
Experimental result shows; because embodiment 1 to embodiment 3 has the tin indium oxide tectum and protects its body layer; can avoid annealing process to continue the detrimentally affect that oxidation causes to indium tin oxides film, thereby can access the indium tin oxides film that resistivity is lower and uniformity coefficient is better.
Otherwise, because be tradition, the indium tin oxides film of comparative example 1 do not have a film of tin indium oxide tectum protection, so that film is easy in annealing process is constantly oxidized, and the indium tin oxides film that the formation sheet resistivity is higher and the sheet resistance uniformity coefficient is relatively poor.
Test case 2: cover thickness is on the impact of sheet resistance value and sheet resistance unevenness
In test case 2, be to inquire into not through before the annealing process and after the annealed technique, the tectal thickness of tin indium oxide is on the impact of sheet resistance value and the sheet resistance unevenness of indium tin oxides film.It is obtained that this sample is that the filming parameter by embodiment 2 changes the different sputter time.When the sputter time was respectively 100 seconds, 200 seconds and 300 seconds, the tectal thickness of prepared tin indium oxide was about respectively
And
Wherein, the sample of this test case is sheet resistance value and the sheet resistance unevenness that measures sample by four-point probe.Along with the growth of sputter time, can make thicker tin indium oxide tectum.As shown in Figure 3, after the annealed processing, when the tectal thickness of tin indium oxide greater than
To can not cause significant impact to the sheet resistance value, and can significantly promote the homogeneity of sheet resistance.Yet, when the tectal thickness of tin indium oxide is thicker, for promoting the inhomogeneity help of sheet resistance value more obvious, can reduce the unevenness of sheet resistance value, promote the electrical quality of indium tin oxides film.
Test case 3: cover thickness is on the impact of transmittance
In test case 3, be to inquire into the tectal thickness of tin indium oxide to the impact of the transmittance of indium tin oxides film.It is obtained that this sample is that the filming parameter by embodiment 2 changes the different sputter time.When the sputter time was respectively 200 seconds, 400 seconds and 600 seconds, the tectal thickness of prepared tin indium oxide was about respectively
And
Wherein, the sample of this test case is sheet resistance value and the sheet resistance unevenness that measures sample by four-point probe.Along with the growth of sputter time, can make respectively thickness and be
And
The tin indium oxide tectum.As shown in Figure 4, do not have the tectal indium tin oxides film of tin indium oxide and can have higher transmittance, along with the tectal thickness of tin indium oxide is thicker, can significantly reduce the transmittance of indium tin oxides film, therefore, be preferably with the tectal gauge control of tin indium oxide in
In, to guarantee the transmittance of indium tin oxides film.
When the tectal thickness of tin indium oxide is
The time, be under 300 to 900 nanometers in wavelength, still can keep its transmittance and reach more than 90%.Experimental result shows, as long as the tectal thickness of tin indium oxide maintains the transmittance that still can guarantee indium tin oxides film in certain scope.
In sum, the present invention can form the indium tin oxides film with tectum and body layer by simple sputtering process, this indium tin oxides film is by the protection of tectum, can avoid indium tin oxides film to be subject to the destruction of annealing process, make still to be possessed lower resistivity and higher resistance uniformity coefficient after the annealed technique of indium tin oxides film; Simultaneously, tectal gauge control can be guaranteed its light transmission in suitable scope, use to make not being subjected to annealing process to destroy the indium tin oxides film that possesses again the good light electrical characteristic.
Claims (6)
1. indium tin oxides film comprises:
One tin indium oxide body layer; And
One tin indium oxide tectum, it is to be arranged on the described tin indium oxide body layer;
Wherein, in the described tin indium oxide tectum Sauerstoffatom to the atomic ratio O/ (In+Sn) of the indium tin atom atomic ratio less than O/ (In+Sn) in the described tin indium oxide body layer.
2. indium tin oxides film as claimed in claim 1, wherein, the atomic ratio of O/ (In+Sn) is less than 1.25 in the described tin indium oxide tectum.
3. indium tin oxides film as claimed in claim 2, wherein, the atomic ratio of O/ (In+Sn) is between 1.19 to 1.24 in the described tin indium oxide tectum.
4. indium tin oxides film as claimed in claim 1, wherein, the atomic ratio of O/ (In+Sn) is between 1.3 to 1.45 in the described tin indium oxide body layer.
5. indium tin oxides film as claimed in claim 1, wherein, the tectal thickness of described tin indium oxide is between 50 to 200 dusts.
6. the making method of an indium tin oxides film comprises the following steps:
(A) at oxygen and ar gas environment deposit one tin indium oxide body layer; And
(B) under argon gas and hydrogen environment, deposition one tin indium oxide tectum is a kind of such as each described indium tin oxides film of claim 1-5 to make on described tin indium oxide body layer.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105839064A (en) * | 2016-04-19 | 2016-08-10 | 宜昌南玻显示器件有限公司 | Preparation method of amorphous indium tin oxide thin film |
CN115537813A (en) * | 2022-10-11 | 2022-12-30 | 兰州空间技术物理研究所 | Preparation method of antistatic composite atomic oxygen protective coating for space |
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DE3309955A1 (en) * | 1983-03-19 | 1984-09-20 | Licentia Patent-Verwaltungs-Gmbh, 6000 Frankfurt | Process for producing In Sn oxide layers |
JPS61195509A (en) * | 1985-02-25 | 1986-08-29 | ダイセル化学工業株式会社 | Manufacture of transparent conductive film |
JPH0364450A (en) * | 1989-07-31 | 1991-03-19 | Kyocera Corp | Formation of transparent conductive film |
US20030035906A1 (en) * | 2001-05-09 | 2003-02-20 | Hassan Memarian | Transparent conductive stratiform coating of indium tin oxide |
EP1316626A2 (en) * | 2001-12-03 | 2003-06-04 | Konica Corporation | Transparent conductive layer forming method, transparent conductive layer formed by the method, and material comprising the layer |
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2011
- 2011-10-09 CN CN2011103020412A patent/CN103031517A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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DE3309955A1 (en) * | 1983-03-19 | 1984-09-20 | Licentia Patent-Verwaltungs-Gmbh, 6000 Frankfurt | Process for producing In Sn oxide layers |
JPS61195509A (en) * | 1985-02-25 | 1986-08-29 | ダイセル化学工業株式会社 | Manufacture of transparent conductive film |
JPH0364450A (en) * | 1989-07-31 | 1991-03-19 | Kyocera Corp | Formation of transparent conductive film |
US20030035906A1 (en) * | 2001-05-09 | 2003-02-20 | Hassan Memarian | Transparent conductive stratiform coating of indium tin oxide |
EP1316626A2 (en) * | 2001-12-03 | 2003-06-04 | Konica Corporation | Transparent conductive layer forming method, transparent conductive layer formed by the method, and material comprising the layer |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105839064A (en) * | 2016-04-19 | 2016-08-10 | 宜昌南玻显示器件有限公司 | Preparation method of amorphous indium tin oxide thin film |
CN115537813A (en) * | 2022-10-11 | 2022-12-30 | 兰州空间技术物理研究所 | Preparation method of antistatic composite atomic oxygen protective coating for space |
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Application publication date: 20130410 |