CN113025988A - Indium tin oxide film heat treatment and evaluation method thereof - Google Patents
Indium tin oxide film heat treatment and evaluation method thereof Download PDFInfo
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- CN113025988A CN113025988A CN202110215926.2A CN202110215926A CN113025988A CN 113025988 A CN113025988 A CN 113025988A CN 202110215926 A CN202110215926 A CN 202110215926A CN 113025988 A CN113025988 A CN 113025988A
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 30
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000011156 evaluation Methods 0.000 title description 5
- 238000002834 transmittance Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 20
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000001301 oxygen Substances 0.000 claims abstract description 17
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 8
- 239000010408 film Substances 0.000 claims description 58
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 7
- 239000010409 thin film Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 abstract description 4
- 238000004458 analytical method Methods 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 description 10
- 239000011521 glass Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- 230000008859 change Effects 0.000 description 6
- 238000000137 annealing Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000007669 thermal treatment Methods 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- 206010021143 Hypoxia Diseases 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- DALUDRGQOYMVLD-UHFFFAOYSA-N iron manganese Chemical compound [Mn].[Fe] DALUDRGQOYMVLD-UHFFFAOYSA-N 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002186 photoelectron spectrum Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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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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- 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
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F30/00—Computer-aided design [CAD]
- G06F30/20—Design optimisation, verification or simulation
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- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F2119/00—Details relating to the type or aim of the analysis or the optimisation
- G06F2119/08—Thermal analysis or thermal optimisation
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- Chemical Kinetics & Catalysis (AREA)
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- Computer Hardware Design (AREA)
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Abstract
The invention provides a heat treatment method of an indium tin oxide film, which directly carries out heat treatment on the indium tin oxide film by using a vacuum tube type high-temperature sintering furnace, and has simple operation and small experimental error. The inventor objectively and comprehensively evaluates the light transmittance and the thermal stability of the indium tin oxide film after heat treatment, and specifically detects the light transmittance of the indium tin oxide film under low-temperature heat treatment by using an ultraviolet-visible-near infrared spectrophotometer to find that the light transmittance of the indium tin oxide film after heat treatment is basically stable at low temperature. Then, further fitting analysis was performed by XPS measurement, by OⅡ/OⅠThe area ratio of the peaks gives a substantially constant number of oxygen vacancies, thus demonstrating that the indium tin oxide film is lowThe conclusion that the light transmittance is basically stable at the temperature provides an idea for researching the photoelectric property of the indium tin oxide film.
Description
Technical Field
The invention belongs to the technical field of film heat treatment, relates to a heat treatment method of an indium tin oxide film, and particularly relates to heat treatment of the indium tin oxide film and an evaluation method thereof.
Background
Indium Tin Oxide (ITO) film material is a heavily doped and highly degenerated n-type semiconductor material with wider energy gap and complex cubic iron manganese (In) type2O3Structure, [100 ]]Polycrystalline with the direction being the most apparently oriented structure). The ITO film not only has excellent photoelectric properties such as low resistivity (1 x 10-4 omega cm), high visible light transmittance (not less than 90%), high infrared reflectivity (not less than 70%), high ultraviolet absorptivity (not less than 85%), but also has high hardness, wear resistance, chemical corrosion resistance and good processing performance. Therefore, since the industrial production in the century, it has been widely used in the technical fields of LED chips, solar cells, Thin Film Transistors (TFTs), electrochromic windows, flat panel displays, and antistatic coatings, and plays an important role. With the rapid rise of the semiconductor LED lighting industry, LED chips with high brightness and high stability are receiving more and more attention.
The ITO film has a conductive mechanism of Sn4+Replacing oxygen vacancies, Sn4+Substitution of In2O3Among them, the chemical states of Sn and In greatly affect the photoelectric properties of the ITO thin film. In the crystal lattice3+An electron donor band may be provided, Sn in a higher valence state may increase carrier concentration, conductivity of the ITO film may be increased, and oxygen vacancies may provide two hole conduction. Therefore, when the film thickness is constant, the degree of oxidation of indium and tin and the number of oxygen vacancies affect the transmittance and resistivity of the ITO filmThe main factors of (1). Transparent conductive films can be prepared by a variety of methods, such as direct current and radio frequency magnetron sputtering, electron beam evaporation, sol-gel, reactive thermal evaporation, spray pyrolysis, chemical vapor deposition, pulsed laser deposition, and the like. The parameter conditions in the preparation process have a decisive influence on the photoelectric properties of the ITO film. However, the heat treatment also has a very important influence on the transmittance and the photoelectric properties of the ITO film, and especially plays a decisive role in the change of the transmittance of the ITO film.
Disclosure of Invention
In the prior art, a rapid annealing furnace, a returned alloy furnace, a closed annealing furnace, an MOCVD (metal organic chemical vapor deposition), an MBE (moving bed) and an Sk-3-3-12 annealing system are generally used for carrying out the ITO film heat treatment, but the devices have high cost, harsh temperature and pressure conditions and large test errors. Therefore, an object of the present invention is to provide a thermal treatment method for an ITO thin film, which is low in cost, simple in operation, and small in test error, so as to solve the above problems.
Based on the above, the invention provides a heat treatment method of indium tin oxide film, comprising,
preparing an ITO film by adopting a magnetron sputtering method;
rare gas is taken as carrier gas, the temperature rising and reducing speed is controlled, and the ITO film is subjected to heat treatment in a vacuum tube type high-temperature sintering furnace;
and controlling the cooling rate to obtain the ITO film after heat treatment.
The invention adopts the magnetron sputtering method In the prior art to prepare the ITO film, and concretely adopts magnetron sputtering equipment to plate the ITO film, and the target material is indium tin oxide, wherein In2O3SnO content of 90%2The content is 10%. In addition, the invention selects a common glass sheet as a substrate when preparing the ITO film, so as to be convenient for a transmittance test and a contrast test.
Further, the invention uses a vacuum tube type high-temperature sintering furnace to carry out heat treatment on the ITO film.
Further, the carrier gas is selected from helium, nitrogen and argon.
Further, the introduction rate of the carrier gas is 200 sccm.
Further, the heating rate of the vacuum tube type high-temperature sintering furnace is 15 ℃/min.
Further, the cooling rate of the vacuum tube type high-temperature sintering furnace is 1.5 ℃/min.
The invention also provides an evaluation method of the ITO film prepared by the indium tin oxide film heat treatment method, and particularly relates to evaluation of the thermal stability of the ITO film through the light transmittance and oxygen vacancy change of the film.
Compared with the prior art, the invention has the following beneficial effects or advantages:
the prior art has expensive used equipment, harsh working temperature and pressure conditions, higher cost and larger error of experimental results. The invention directly carries out heat treatment on the ITO film by using the vacuum tube type high-temperature sintering furnace, and has simple operation and small experimental error. The inventor objectively and comprehensively evaluates the light transmittance and the thermal stability of the ITO film after heat treatment, and specifically detects the light transmittance of the ITO film under low-temperature heat treatment by using an ultraviolet-visible-near infrared spectrophotometer to find that the light transmittance of the ITO film after heat treatment is basically stable at low temperature. Then, further fitting analysis was performed by XPS measurement, by OⅡ/OⅠThe number of oxygen vacancies is basically constant according to the area ratio of the peaks, so that the conclusion that the light transmittance of the ITO film is basically stable at low temperature is proved, and a thought is provided for researching the photoelectric property of the ITO film.
Drawings
FIG. 1 is a graph showing the change in light transmittance of an ITO film at 661 nm.
FIG. 2 is a graph of low temperature transmittance of an ITO film.
FIG. 3 is a chemical state diagram of oxygen element of an untreated ITO film.
FIG. 4 is a chemical state diagram of oxygen element of an ITO film heat-treated at a low temperature of 100 ℃.
FIG. 5 is a chemical state diagram of oxygen element of the ITO film heat-treated at a low temperature of 250 ℃.
FIG. 6 is a graph showing the change in oxygen vacancy of the ITO film.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings, but the present invention is not limited to the following embodiments.
(1) Thermal treatment of ITO film
The invention uses JGP-350C magnetron sputtering equipment to prepare an ITO film, a substrate is common glass (the size is 10 multiplied by 20mm), a target is indium tin oxide (In which2O3SnO content of 90%2Content 10%), and the size of the obtained ITO film was 20X 20 mm.
The prepared ITO film is placed into a vacuum tube of a vacuum tube type high-temperature sintering furnace, high-purity argon is introduced at the rate of 200sccm, and four medium and low temperature treatment areas of 100 ℃, 200 ℃ and 250 ℃ and a high temperature treatment area of 300-800 ℃ are respectively arranged for testing. When each treatment is tested, the heating rate is set to be 15 ℃/min, the temperature is kept for 20min after the corresponding temperature is reached, then the temperature is reduced to 100 ℃ at the cooling rate of 1.5 ℃/min, and finally the ITO film after heat treatment is obtained after natural cooling to the room temperature.
(2) ITO film transmittance test
And (3) carrying out transmittance tests at different temperatures by using an Agilent Cary 5000 ultraviolet-visible-near infrared spectrophotometer, taking the transmission curve of the uncoated glass as a reference in the experiment, then placing the coated glass on a sample test frame for scanning, and comparing the transmission curve with the transmission curve of the uncoated glass to obtain the transmittance curve of the ITO film. Wherein, the parameters of the scanning coated glass are the same as the parameters of the scanning reference glass and are as follows: the width of the slit is 1nm, the wavelength scanning range is 300-800 nm, and the response time is 1 min. The results are shown in fig. 1 and fig. 2, and the results show that the transmittance of pure glass in the medium and low temperature regions is reduced and the film is almost flat, which shows that the ITO film has better thermal stability during low temperature heat treatment.
(3) XPS test analysis of ITO film
XPS test is carried out by adopting an American PHZ.Quantum 2000X-ray photoelectron spectrometer, an Al target is selected, an excitation source h upsilon is 1486.69eV, and the vacuum degree of an analysis chamber is superior to 5 multiplied by 10-7Pa, the chemical composition of the surface of the ITO thin film and the chemical state of O element at different temperatures (low temperature) were analyzed by selecting 23.5eV, and the results are shown in fig. 3 to 6.
ITO is obtained through analysisThe change in the number of oxygen vacancies in the film is the primary cause of the light transmittance. As shown in FIGS. 3, 4 and 5, the X photoelectron spectrum of the O element was measured and fitted to a Gaussian function to obtain OI、OII、OIIIHas a binding energy of 529.5 + -0.5 eV, 530.5 + -0.5 eV, 532.00 + -0.5 eV, respectively, wherein O isIRepresents lattice oxygen, OIIOxygen representing an anoxic zone; o isIIIRepresenting foreign organic oxygen or SiO2And O, andII/OIthe method is used for analyzing the oxygen deficiency condition of the ITO film and can reflect the number of oxygen vacancies. O isII/OIThe change of (A) is substantially constant from 0.191 which is not annealed to 0.421 at 100 ℃ to 0.313 at 200 ℃ to 0.43 at 250 ℃ as shown in FIG. 6, and O passes throughII/OIThe constancy of the ratio of (a) demonstrates the substantial constancy of the number of oxygen vacancies, and thus the stability of the ITO thin film under low-temperature heat treatment.
As described above, the present invention can be preferably implemented, and the above-mentioned embodiments only describe the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various changes and modifications of the technical solution of the present invention made by those skilled in the art without departing from the design spirit of the present invention shall fall within the protection scope defined by the present invention.
Claims (8)
1. A heat treatment method of indium tin oxide film is characterized in that the method comprises the following steps,
preparing an ITO film by adopting a magnetron sputtering method;
rare gas is taken as carrier gas, the temperature rising rate is controlled, and the ITO film is subjected to heat treatment in a vacuum tube type high-temperature sintering furnace;
and controlling the cooling rate to obtain the ITO film after heat treatment.
2. The method of claim 1, wherein the carrier gas is selected from helium, nitrogen, and argon.
3. The method according to claim 1, wherein the carrier gas is introduced at a rate of 200 sccm.
4. The method of claim 1, wherein the temperature increase rate is 15 ℃/min.
5. The method of claim 1, wherein the temperature reduction rate is 1.5 ℃/min.
6. The method for heat treatment of indium tin oxide film according to claim 1, wherein In is In the ITO film prepared by magnetron sputtering2O3SnO content of 90%2The content is 10%.
7. A method for evaluating an ITO thin film produced by the heat-treating method for an indium tin oxide thin film according to any one of claims 1 to 6.
8. The method according to claim 7, wherein the thermal stability of the ITO film is evaluated by changes in film transmittance and oxygen vacancy.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114242849A (en) * | 2021-11-25 | 2022-03-25 | 福建兆元光电有限公司 | ITO annealing method for improving LED brightness |
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2021
- 2021-02-26 CN CN202110215926.2A patent/CN113025988A/en active Pending
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| CN1334570A (en) * | 2000-07-25 | 2002-02-06 | 日本板硝子株式会社 | Base plate with transparent electric conductive film and method for mfg. same and touch screen using said base plate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114242849A (en) * | 2021-11-25 | 2022-03-25 | 福建兆元光电有限公司 | ITO annealing method for improving LED brightness |
| CN114242849B (en) * | 2021-11-25 | 2023-06-16 | 福建兆元光电有限公司 | ITO annealing method for improving brightness of LED |
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