Film layer structure, preparation method thereof and photoelectric device

By using indium oxide doped titanium oxide tantalum cerium oxide film as an intermediate transition layer or protective layer in optoelectronic devices, the problems of poor adhesion of silver films and high-temperature water vapor erosion in optoelectronic devices are solved, and the attachment of metal films is significantly improved Focus and durability.

CN119491198APending Publication Date: 2025-02-21FIRST RARE MATERIALS CO LTD
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Patent Information

Application Number
CN202411727419.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-28
Publication Date
2025-02-21

AI Technical Summary

Technical Problem

Silver films are prone to mold release in optoelectronic devices and migrate and agglomerate in high temperature and water vapor environments, reducing their performance.

Method used

The film layer structure is prepared between the substrate and the metal film by magnetron sputtering technology using indium oxide doped titanium oxide cerium oxide film as the intermediate transition layer or protective layer.

Benefits of technology

The surface energy matching of the metal film and the substrate is improved, the internal stress caused by the difference in thermal expansion coefficient and lattice constant is alleviated, the adhesion of the metal film is enhanced, and the metal film is effectively protected from high temperature and water vapor erosion.

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Abstract

The invention discloses a film layer structure, a preparation method thereof and a photoelectric device, and relates to the technical field of magnetron sputtering coating. The film layer structure comprises an indium oxide doped titanium oxide, tantalum oxide and cerium oxide film arranged between the metal film and the substrate and capable of effectively enhancing the adhesive force between the metal film and the substrate, and further comprises an indium oxide doped titanium oxide, tantalum oxide and cerium oxide film arranged on the surface of the metal film and capable of effectively protecting the metal film from being eroded by high temperature and water vapor. The film layer structure provided by the invention is suitable for being prepared by a magnetron sputtering method.
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Description

Technical Field

[0001] The invention relates to the technical field of magnetron sputtering coating, and in particular to a film layer structure and a preparation method thereof, and a photoelectric device. Background Art

[0002] Silver film has the advantages of low resistivity and high reflectivity, and is widely used in optoelectronic devices such as Low-E glass and OLED devices. Low-E glass uses silver film to selectively reflect infrared and ultraviolet rays, and OLED devices use silver film as an anode to increase display brightness.

[0003] However, in these applications, silver films directly sputtered onto substrates such as glass are prone to demolding, and silver atoms migrate and agglomerate when heated or in a water vapor environment, thereby reducing the performance of the silver film. Summary of the invention

[0004] The embodiments of the present invention provide a film layer structure and a preparation method thereof, and an optoelectronic device, which are intended to enhance the adhesion of a metal film on a substrate in the optoelectronic device and protect the metal film from high temperature and water vapor.

[0005] The method for preparing the film structure provided by the present invention comprises:

[0006] A first film layer is sequentially prepared on a substrate, and a second film layer is sequentially prepared on the first film layer; among the first film layer and the second film layer, one film layer is made of a metal film, and the other film layer is made of an indium oxide-doped titanium oxide, tantalum oxide, and cerium oxide thin film.

[0007] Optionally, the first film layer is an indium oxide-doped titanium oxide, tantalum oxide, cerium oxide thin film, and the material of the second film layer is a metal film. After the step of preparing the second film layer on the first film layer, the method further includes:

[0008] A third film layer is prepared on the second film layer; the material of the third film layer is an indium oxide-doped titanium oxide, tantalum oxide, cerium oxide thin film.

[0009] Optionally, the metal film is a silver film.

[0010] Optionally, the indium oxide doped titanium oxide tantalum oxide cerium oxide thin film is prepared by magnetron sputtering indium oxide doped titanium oxide tantalum oxide cerium oxide target, comprising the following steps:

[0011] S1, installing indium oxide doped titanium oxide, tantalum oxide, cerium oxide targets on a magnetron sputtering system;

[0012] S2, placing the substrate or the substrate prepared with the metal film into the waiting chamber, and evacuating the sputtering chamber;

[0013] S3, introducing argon gas into the sputtering chamber, adjusting the gas pressure, setting the target spacing and sputtering power, and turning on the power supply for pre-sputtering;

[0014] S4, placing the substrate in the waiting chamber into the sputtering chamber, introducing a mixed gas of argon, hydrogen and oxygen into the sputtering chamber, adjusting the gas pressure, setting the target distance and sputtering power, and turning on the power to deposit indium oxide-doped titanium oxide, tantalum oxide, cerium oxide thin films.

[0015] Optionally, in step S4, the mixed gas includes a first mixed gas consisting of 2% hydrogen and 98% argon, and a second mixed gas consisting of 10% oxygen and 90% argon;

[0016] The flow ratio of the first mixed gas to the second mixed gas is 80:20 to 90:10;

[0017] The steps of adjusting the gas pressure are specifically as follows: adjusting the gas pressure in the sputtering chamber to 2.5 mtorr-5.2 mtorr;

[0018] The specific steps of setting the target spacing and sputtering power are: setting the target spacing to 45mm-100mm and the sputtering power to 810W-1430W.

[0019] Optionally, the component ratio of the indium oxide doped titanium oxide, tantalum oxide, and cerium oxide target is indium oxide: titanium oxide: tantalum oxide: cerium oxide = 98.57wt%: 0.63wt%: 0.51wt%: 0.28wt%.

[0020] Optionally, the silver film is prepared by magnetron sputtering a silver target, comprising the following steps:

[0021] S5, installing silver target on magnetron sputtering system;

[0022] S6, placing the substrate or the substrate prepared with the indium oxide-doped titanium oxide, tantalum oxide, cerium oxide thin film into the waiting chamber, and evacuating the sputtering chamber;

[0023] S7, introducing argon gas into the sputtering chamber, adjusting the gas pressure, setting the target spacing and sputtering power, and turning on the power supply for pre-sputtering;

[0024] S8, placing the substrate in the waiting chamber into the sputtering chamber, introducing argon gas into the sputtering chamber, adjusting the gas pressure, setting the target spacing and sputtering power, and turning on the power to deposit the silver film.

[0025] Optionally, in step S8, the step of adjusting the gas pressure is specifically: adjusting the gas pressure in the sputtering chamber to 1.2 mtorr-5.7 mtorr;

[0026] The specific steps of setting the target spacing and sputtering power are: setting the target spacing to 45mm-100mm and the sputtering power to 810-1430W.

[0027] Optionally, the thickness of the indium oxide-doped titanium oxide-tantalum oxide-cerium oxide film is 10-30 nm, and the thickness of the silver film is 50-100 nm.

[0028] The present invention provides a film layer structure formed by the above-mentioned method for preparing the film layer structure.

[0029] The present invention also provides a photoelectric device, comprising:

[0030] substrate;

[0031] A film layer structure is arranged on the surface of the glass substrate, and the film layer structure includes a first film layer arranged on the substrate and a second film layer arranged on the first film layer; among the first film layer and the second film layer, one of the film layers is made of a metal film, and the other film layer is made of an indium oxide-doped titanium oxide, tantalum oxide, and cerium oxide thin film.

[0032] Optionally, the material of the first film layer is an indium oxide-doped titanium oxide, tantalum oxide, cerium oxide thin film, the material of the second film layer is a metal film, and the film layer structure further includes:

[0033] A third film layer is disposed on the second film layer, and the material of the third film layer is an indium oxide-doped titanium oxide, tantalum oxide, cerium oxide thin film.

[0034] The present invention has the following beneficial effects:

[0035] In the film structure provided by the present invention, the indium oxide-doped titanium oxide, tantalum oxide, cerium oxide thin film has good electrical conductivity and high transmittance in the visible light range, does not affect the photoelectric performance of metal films such as silver films in photoelectric devices, and can be arranged between the metal film and the substrate as an intermediate transition layer, or arranged on the surface of the metal film as a protective layer, to achieve the following beneficial effects:

[0036] 1. Indium oxide doped titanium oxide, tantalum oxide, cerium oxide thin film as an intermediate transition layer can improve the surface energy matching between metal films such as silver films and substrates, and at the same time alleviate the internal stress between the substrate and the metal film due to differences in thermal expansion coefficient, lattice constant, etc., enhance the adhesion of the metal film on the substrate surface, and avoid demolding;

[0037] 2. Indium oxide doped with titanium oxide, tantalum oxide, and cerium oxide thin films as the surface protection layer of the metal film can prevent the water vapor in the environment from directly corroding the metal film; and tantalum oxide is beneficial to improving the crystallinity of the film, and cerium oxide is beneficial to lattice contraction and enhancing the condensed state of indium oxide, thereby inhibiting the agglomeration and migration of metal atoms in the metal film, such as inhibiting the agglomeration and migration of silver atoms in the silver film, and further protecting the metal film from high temperature and water vapor erosion;

[0038] 3. Indium oxide doped titanium oxide, tantalum oxide, and cerium oxide films can be prepared by magnetron sputtering. Tantalum oxide can improve the crystallinity of the film, and the radius of cerium ions is larger than that of indium ions, which is beneficial to lattice contraction and improves target density, and is further beneficial to magnetron sputtering for coating, thereby improving the quality and deposition rate of the film. BRIEF DESCRIPTION OF THE DRAWINGS

[0039] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.

[0040] Figure 1 It is a structural schematic diagram of the membrane structure proposed by the present invention;

[0041] Figure 2 Surface morphology of Example 1 of the present invention and Comparative Example 1 after adhesion test;

[0042] Figure 3 This is the surface morphology of Example 1 of the present invention before and after the double 85 test;

[0043] Figure 4 This is the surface morphology of comparative example 2 of the present invention before and after the double 85 test.

[0044] Description of reference numerals:

[0045] 1. Substrate; 2. First film layer; 3. Second film layer; 4. Third film layer. DETAILED DESCRIPTION

[0046] In order to make the purpose, features and advantages of the present invention more obvious and easy to understand, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the embodiments described below are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0047] The terms "first", "second", "third", "fourth", etc. (if any) in the specification and drawings of the present application are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequence. It should be understood that the data used in this way can be interchanged where appropriate, so that the embodiments of the present application described herein can be implemented in an order other than those illustrated or described herein, for example. In addition, the terms "including" and "having" and any of their variations are intended to cover non-exclusive inclusions, for example, a process, method, system, product or device that includes a series of steps or units is not necessarily limited to those steps or units that are clearly listed, but may include other steps or units that are not clearly listed or inherent to these processes, methods, products or devices.

[0048] In optoelectronic devices such as Low-E glass and OLED devices, silver film is widely used due to its advantages of low resistivity and high reflectivity; however, in these applications, silver film is prone to demolding when directly sputtered on substrates such as glass, and silver atoms will migrate and agglomerate in heating and water vapor environments, thereby reducing the performance of the silver film.

[0049] In addition, metal films such as gold, copper, aluminum, and nickel, which are commonly used in optoelectronic devices, also have poor adhesion to substrates such as glass and are corroded in high temperature and water vapor environments, which leads to mold release and performance deterioration.

[0050] The inventors of this application have discovered through intensive research that indium oxide-doped titanium oxide, tantalum oxide, cerium oxide thin films have good electrical conductivity and high transmittance in the visible light range, do not affect the photoelectric properties of metal films such as silver films in optoelectronic devices, and can be arranged between the metal film and the substrate as an intermediate transition layer to enhance the adhesion of the metal film on the substrate, or be arranged on the surface of the metal film as a protective layer to protect the metal film from high temperature and water vapor erosion.

[0051] Based on this, the present invention proposes a film layer structure and a preparation method thereof.

[0052] like Figure 1 As shown, in one embodiment, the method for preparing the film structure provided by the present invention includes:

[0053] Providing a substrate 1;

[0054] A first film layer 2 is prepared on the substrate, and a second film layer 3 is prepared on the first film layer 2 in sequence; one of the first film layer 2 and the second film layer 3 is made of a metal film, and the other is made of an indium oxide-doped titanium oxide, tantalum oxide, cerium oxide film.

[0055] In this embodiment, the substrate includes a glass substrate, a ceramic substrate, a semiconductor substrate, a metal substrate, a plastic substrate and a composite material substrate, etc.; in some cases, the surface energies of the metal film and the glass substrate do not match, and the metal film has poor adhesion on the glass substrate; in some cases, the metal film has poor adhesion on the ceramic substrate; in some cases, the metal film has poor adhesion on the semiconductor substrate; in some cases, the metal film has poor adhesion on substrates of other metal materials; in some cases, the metal film has poor adhesion on a plastic substrate; in other cases, the metal film has poor adhesion on a composite material substrate composed of two or more different materials.

[0056] In this embodiment, based on the specific adhesion between the metal film and the substrate, the metal film can be a metal material commonly used in optoelectronic devices such as silver, gold, copper, aluminum, nickel, or an alloy material based on metals such as silver, gold, copper, aluminum, nickel, etc.; the metal film has a low resistivity, or a high reflectivity, or both a low resistivity and a high reflectivity.

[0057] In this embodiment, the optoelectronic devices may be some pure optical devices such as Low-E glass, reflective lenses, etc., and the metal film is mainly used as a reflective film layer. For example, Low-E glass can use silver film to selectively reflect infrared or ultraviolet rays, and microscopes, telescopes and laser equipment can use silver film to achieve reflection and focusing; the optoelectronic devices may also be some electronic devices such as touch screens, electronic sensors, diodes, semiconductor switching elements, etc., and the metal film is mainly used as a conductive film layer; the optoelectronic devices may also be some devices that need to utilize both the conductivity and reflective properties of the metal film, for example, OLED devices can use silver film as an anode to increase the display brightness, and solar cells can use silver film as a back electrode to improve the photoelectric conversion efficiency of solar cells, etc.

[0058] In one embodiment, the optoelectronic device is Low-E glass, and the film structure on the glass surface of the Low-E glass includes a silver film and an indium oxide-doped titanium oxide, tantalum oxide, cerium oxide thin film. The titanium oxide in the indium oxide-doped titanium oxide, tantalum oxide, cerium oxide thin film has a strong blocking effect on ultraviolet rays.

[0059] The indium oxide-doped titanium oxide, tantalum oxide, and cerium oxide thin films proposed in this embodiment can be disposed between the metal film and the substrate as an intermediate transition layer, or can be disposed on the surface of the metal film as a protective layer.

[0060] Scenario 1

[0061] The first film layer 2 is an indium oxide-doped titanium oxide, tantalum oxide, and cerium oxide thin film, and the second film layer 3 is a metal film.

[0062] The indium oxide doped titanium oxide, tantalum oxide, cerium oxide thin film is arranged between the metal film and the substrate as an intermediate transition layer, which can improve the surface energy matching between the metal film such as silver film and the substrate, and at the same time alleviate the internal stress between the substrate and the metal film caused by the differences in thermal expansion coefficient, lattice constant, etc., enhance the adhesion of the metal film on the substrate surface, and avoid demolding.

[0063] Scenario 2

[0064] The first film layer 2 is a metal film, and the second film layer 3 is an indium oxide-doped titanium oxide, tantalum oxide, and cerium oxide thin film.

[0065] Indium oxide doped titanium oxide, tantalum oxide, and cerium oxide thin films are arranged on the surface of the metal film as a protective layer to prevent the water vapor in the environment from directly corroding the metal film; and tantalum oxide is beneficial to improving the crystallinity of the film, and the radius of cerium ions is larger than that of indium ions, so cerium oxide is beneficial to lattice contraction and enhances the condensed state of the original indium oxide, thereby inhibiting the agglomeration and migration of metal atoms in the metal film (such as silver atoms in the silver film), and further protecting the metal film from high temperature and water vapor erosion.

[0066] Scenario 3

[0067] After the step of preparing the second film layer 3 on the first film layer 2, it also includes: preparing the third film layer 4 on the second film layer 3; the materials of the first film layer 2 and the third film layer 4 are both indium oxide doped titanium oxide tantalum oxide cerium oxide thin films, and the material of the second film layer 3 is a metal film.

[0068] The first film layer 2 is used to enhance the adhesion of the metal film on the surface of the substrate, and the third film layer 4 is used to protect the metal film from high temperature and water vapor erosion.

[0069] In the film layer structure proposed in the embodiment of the present invention, the indium oxide-doped titanium oxide, tantalum oxide, cerium oxide thin film can be prepared on a substrate by magnetron sputtering, electron beam evaporation, pulsed laser deposition, ion beam sputtering, and the like.

[0070] Among them, indium oxide doped titanium oxide, tantalum oxide, cerium oxide thin films are particularly suitable for preparation by magnetron sputtering.

[0071] Specifically, in the material system of indium oxide doped with titanium oxide, tantalum oxide and cerium oxide, tantalum oxide is beneficial to improving the crystallinity of the film, and the radius of the cerium ion is larger than that of the indium ion, which is beneficial to the lattice contraction and the increase of the target density. The higher density target is beneficial to increasing the deposition rate, as well as improving the density and uniformity of the film. It can withstand higher sputtering power and longer sputtering time during sputtering, and the sputtering process is more stable.

[0072] In some embodiments, magnetron sputtering to prepare an indium oxide-doped titanium oxide, tantalum oxide, cerium oxide thin film comprises the following steps:

[0073] S1, installing indium oxide-doped titanium oxide, tantalum oxide, cerium oxide target on the magnetron sputtering system.

[0074] In a preferred embodiment, the component ratio of indium oxide doped titanium oxide, tantalum oxide and cerium oxide target is indium oxide (In2O3): titanium oxide (TiO2): tantalum oxide (Ta2O5): cerium oxide (CeO2) = 98.57wt%: 0.63wt%: 0.51wt%: 0.28wt%.

[0075] S2, placing the substrate or the substrate prepared with the metal film into the waiting chamber, and evacuating the sputtering chamber.

[0076] In a preferred embodiment, the sputtering chamber is evacuated to .

[0077] S3, introduce argon gas into the sputtering chamber, adjust the gas pressure, set the target distance and sputtering power, and turn on the power to perform pre-sputtering.

[0078] In a preferred embodiment, the gas pressure is adjusted to 2.5 mtorr-5.2 mtorr.

[0079] In a preferred embodiment, the target spacing is set to 45 mm-100 mm, the sputtering power of the pre-sputtering is set to 810 W-1430 W, and the pre-sputtering time is set to 5 min-20 min.

[0080] S4, placing the substrate in the waiting chamber into the sputtering chamber, introducing a mixed gas of argon, hydrogen and oxygen into the sputtering chamber, adjusting the gas pressure, setting the target distance and sputtering power, and turning on the power to deposit indium oxide-doped titanium oxide, tantalum oxide, cerium oxide thin films.

[0081] In a preferred embodiment, the mixed gas includes a first mixed gas composed of 2% hydrogen and 98% argon, and a second mixed gas composed of 10% oxygen and 90% argon, and the flow ratio of the first mixed gas and the second mixed gas is 80:20 to 90:10. The electrical properties of the thin film prepared by using the mixed gas composed of hydrogen, oxygen and argon as the working gas are better; the gas pressure is adjusted to 2.5mtorr-5.2mtorr.

[0082] In a preferred embodiment, the target spacing is set to 45 mm-100 mm, the sputtering power is set to 810 W-1430 W, the deposition time is set to 5-28 s, and the thickness of the deposited indium oxide-doped titanium oxide, tantalum oxide, cerium oxide film is set to 10-30 nm.

[0083] Based on the above-mentioned embodiment of magnetron sputtering indium oxide doped titanium oxide tantalum oxide cerium oxide thin film, the present invention further proposes the following specific embodiments using silver film as the metal film in the film layer structure.

[0084] It should be noted that the following specific embodiments are only partial embodiments of the present invention, which are used to verify the beneficial effects of the film layer structure proposed in the present invention, and are not limitations of the present invention; those skilled in the art can select metal films of other materials according to actual needs, or adjust the magnetron sputtering parameters according to specific circumstances to obtain more embodiments, but these embodiments do not depart from the spirit and scope of the embodiments of the present invention.

[0085] Example 1

[0086] The glass substrate is ultrasonically cleaned with deionized water, acetone, and ethanol in sequence, and then blown dry with nitrogen gas, and the treated glass substrate is placed in a waiting chamber.

[0087] Sputtering the first film layer

[0088] An indium oxide-doped titanium oxide, tantalum oxide, and cerium oxide target is installed on a magnetron sputtering system, and the target component ratio is indium oxide (In2O3): titanium oxide (TiO2): tantalum oxide (Ta2O5): cerium oxide (CeO2) = 98.57wt%: 0.63wt%: 0.51wt%: 0.28wt%.

[0089] The sputtering chamber was evacuated to 5.5 × 10 -6 Torr.

[0090] Argon gas was introduced into the sputtering chamber, and the gas pressure controller was adjusted to keep the vacuum degree of the chamber at 3 mtorr.

[0091] The target spacing was set to 90 mm, the power was set to 1000 W, and the power was turned on for pre-sputtering for 10 minutes.

[0092] Place the glass substrate in the waiting chamber into the sputtering chamber, and introduce a mixed gas consisting of Ar, H2, and O2 into the sputtering chamber; Ar and H2 use Ar-H2 mixed gas bottles with an Ar-H2 ratio of 98:2, and Ar and O2 use Ar-O2 mixed gas bottles with an Ar-O2 ratio of 90:10; the gas flow ratio of Ar-H2 and Ar-O2 is 80:15, the gas pressure is adjusted to 3mtorr, and the target spacing is set to 90mm.

[0093] Turn on the power, set the sputtering power to 1000W, start depositing the first film layer, the deposition time is 5s, and the thickness of the sputtered first film layer is 10-30nm.

[0094] Sputtering the second film layer

[0095] A pure silver target with a purity of 4N is installed on the magnetron sputtering system.

[0096] The sample with the first film layer deposited thereon is placed in the waiting chamber.

[0097] Evacuate the sputtering chamber to ; Optionally, evacuate the sputtering chamber to .

[0098] Argon gas is introduced into the sputtering chamber, and the gas pressure controller is adjusted to make the vacuum degree of the sputtering chamber within 1.2 mtorr-5.7 mtorr; optionally, the gas pressure controller is adjusted to make the vacuum degree of the sputtering chamber within 3.5 mtorr.

[0099] The target spacing is set to 45mm-100mm, the power is set to 810W-1430W, and the power is turned on for pre-sputtering for 5min-20min; optionally, the target spacing is set to 90mm, the power is set to 900W, and the power is turned on for pre-sputtering for 20min.

[0100] Place the glass substrate in the waiting chamber into the sputtering chamber, introduce argon gas into the sputtering chamber, adjust the gas pressure controller to make the vacuum degree of the sputtering chamber at 1.2mtorr-5.7mtorr, set the target spacing to 45mm-100mm, turn on the power, set the sputtering power to 810W-1430W, start depositing the second film layer, and the deposition time is 20s-36s; optionally, adjust the gas pressure controller to make the vacuum degree of the sputtering chamber at 3.5mtorr, set the target spacing to 90mm, turn on the power, set the power to 900W, start depositing the thin film, and the deposition time is 20s.

[0101] The thickness of the sputtered second film layer is 50-100 nm.

[0102] Sputtering the third film layer

[0103] An indium oxide-doped titanium oxide, tantalum oxide, and cerium oxide target material is installed on a magnetron sputtering system, and the component ratio of the target material is the same as that of the target material used for sputtering the first film layer.

[0104] The sputtering chamber is evacuated to .

[0105] Argon gas was introduced into the sputtering chamber, and the gas pressure controller was adjusted to keep the vacuum degree of the sputtering chamber at 3 mtorr.

[0106] The target spacing was set to 90 mm, the power was set to 1000 W, and the power was turned on for pre-sputtering for 10 minutes.

[0107] The sample with the first and second film layers sputtered in the waiting chamber is placed in the sputtering chamber, and a mixed gas composed of Ar, H2, and O2 is introduced into the sputtering chamber, wherein the composition and gas flow ratio of Ar-H2 and Ar-O2 are consistent with those of sputtering the first film layer. The gas pressure is adjusted to 3mtorr, the target spacing is 90mm, the power is turned on, the sputtering power is set to 1000W, and the thin film deposition is started for 5s.

[0108] The thickness of the sputtered third film layer is 10-30nm.

[0109] The total thickness of the film structure consisting of the first film layer, the second film layer and the third film layer prepared on the glass substrate in this embodiment is .

[0110] Comparative Example 1

[0111] Compared with Example 1, the difference is that there is no first film layer, and the preparation methods of the second film layer and the third film layer refer to Example 1.

[0112] Comparative Example 2

[0113] Compared with Example 1, the difference is that there is no third film layer, and the preparation method of the first film layer and the second film layer refers to that of Example 1.

[0114] The samples prepared in Example 1 and Comparative Example 1 were subjected to an adhesion test, specifically: the film layer structure of the sample was cut into 6×6 squares, a total of 36 squares of 1 mm×1 mm, and then the film layer structure was adhered with tape, and the number of squares adhered by the tape was calculated.

[0115] like Figure 2 As shown, Figure 2 The middle left picture shows the surface morphology of the sample of Example 1 after the adhesion test. Figure 2 The middle right picture shows the surface morphology of the sample of comparative example 1 after the adhesion test; after several adhesion test processes, no squares of embodiment 1 fell off, while all 36 squares of comparative example 1 fell off.

[0116] It can be seen that the first film layer, i.e., the indium oxide-doped titanium oxide, tantalum oxide, cerium oxide film layer disposed between the glass substrate and the silver film, greatly enhances the adhesion of the silver film on the glass substrate and has a significant effect in improving the demolding problem of the silver film.

[0117] The samples prepared in Example 1 and Comparative Example 2 were subjected to a double 85 test (i.e., a long-term test was conducted under constant temperature and humidity conditions of 85°C and 85% relative humidity to simulate the working state of the samples in a high temperature and high humidity environment, and the test duration was selected to be 100 hours).

[0118] like Figure 3 As shown, Figure 3 The left picture in the middle shows the surface morphology of the sample of Example 1 before constant temperature and humidity, and the right picture shows the surface morphology of the sample of Example 1 after constant temperature and humidity. It can be seen that after the double 85 test, the sample of Example 1 still maintains a complete surface morphology, and basically no discoloration, deformation, fogging, demolding and other phenomena occur, and the silver film can still be used normally.

[0119] like Figure 4 As shown, Figure 4The middle left picture shows the surface morphology of the sample of Comparative Example 2 before constant temperature and humidity, and the right picture shows the surface morphology of the sample of Comparative Example 2 after constant temperature and humidity. It can be seen that after the double 85 test, the surface of the sample of Comparative Example 2 has already shown serious deformation and demolding, and the silver film is difficult to continue to use.

[0120] It can be seen that the third film layer, i.e., the indium oxide-doped titanium oxide, tantalum oxide, cerium oxide film layer disposed on the surface of the silver film, effectively avoids the corrosion of the silver film by high temperature and water vapor environment, inhibits the migration and agglomeration of silver atoms, and has a significant protective effect on the silver film.

[0121] In a specific embodiment of the present invention, a silver film is used as the metal film in the film layer structure, and a film layer structure with indium oxide-doped titanium oxide, tantalum oxide, and cerium oxide thin films as intermediate transition layers and protective layers is prepared on a glass substrate by a magnetron sputtering method. The intermediate transition layer has a significant effect on improving the demolding problem of the silver film on the glass substrate, and the protective layer has a significant protective effect on the silver film.

[0122] Since various metal films in optoelectronic devices also widely have the same or similar problems as silver films, namely, poor adhesion between metal films and substrates such as glass and corrosion in high temperature and water vapor environments, those skilled in the art can understand that the film layer structure of the indium oxide-doped titanium oxide, tantalum oxide, and cerium oxide thin film proposed in the embodiment of the present invention as an intermediate transition layer and a protective layer can effectively improve the adhesion of the metal film on the substrate and protect the metal film to avoid corrosion of the metal film by high temperature and water vapor environments.

[0123] The present invention further provides a photoelectric device, comprising a substrate, and a film layer structure provided by the above-mentioned embodiment and disposed on a surface of the substrate.

[0124] The optoelectronic device can be some pure optical devices such as Low-E glass, reflective lenses, etc., in which the metal film is mainly used as a reflective film layer; it can also be some electronic devices such as touch screens, electronic sensors, diodes, semiconductor switching elements, etc., in which the metal film is mainly used as a conductive film layer; it can also be some devices that need to utilize both the conductivity and reflective properties of the metal film, for example, the metal film in an OLED device can be used as an anode, the metal film in a solar cell can be used as a back electrode, etc.; the beneficial effects that can be achieved by the aforementioned film layer structure and preparation method embodiments can also be achieved by the optoelectronic device, and will not be repeated here.

[0125] The embodiments described above are only used to illustrate the technical solutions of the present application, rather than to limit them. Although the present application has been described in detail with reference to the aforementioned embodiments, a person skilled in the art should understand that the technical solutions described in the aforementioned embodiments may still be modified, or some of the technical features may be replaced by equivalents. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the embodiments of the present application.

Claims

1. A method for preparing a film structure, characterized in that: include: A first film layer is sequentially prepared on a substrate, and a second film layer is sequentially prepared on the first film layer; among the first film layer and the second film layer, one film layer is made of a metal film, and the other film layer is made of an indium oxide-doped titanium oxide, tantalum oxide, and cerium oxide thin film.

2. The method for preparing a film structure according to claim 1, characterized in that: The material of the first film layer is an indium oxide-doped titanium oxide, tantalum oxide, and cerium oxide thin film, and the material of the second film layer is a metal film. After the step of preparing the second film layer on the first film layer, the method further includes: A third film layer is prepared on the second film layer; the material of the third film layer is an indium oxide-doped titanium oxide, tantalum oxide, cerium oxide thin film.

3. The method for preparing a film structure according to claim 1 or 2, characterized in that: The metal film is a silver film.

4. The method for preparing a film structure according to claim 1 or 2, characterized in that: The indium oxide doped titanium oxide, tantalum oxide, cerium oxide thin film is prepared by magnetron sputtering indium oxide doped titanium oxide, tantalum oxide, cerium oxide target material, comprising the following steps: S1, installing indium oxide doped titanium oxide, tantalum oxide, cerium oxide targets on a magnetron sputtering system; S2, placing the substrate or the substrate prepared with the metal film into the waiting chamber, and evacuating the sputtering chamber; S3, introducing argon gas into the sputtering chamber, adjusting the gas pressure, setting the target spacing and sputtering power, and turning on the power supply for pre-sputtering; S4, placing the substrate in the waiting chamber into the sputtering chamber, introducing a mixed gas of argon, hydrogen and oxygen into the sputtering chamber, adjusting the gas pressure, setting the target distance and sputtering power, and turning on the power to deposit indium oxide-doped titanium oxide, tantalum oxide, cerium oxide thin films.

5. The method for preparing a film structure according to claim 4, characterized in that: In step S4, the mixed gas includes a first mixed gas consisting of 2% hydrogen and 98% argon, and a second mixed gas consisting of 10% oxygen and 90% argon; The flow ratio of the first mixed gas to the second mixed gas is 80:20 to 90:10; The steps of adjusting the gas pressure are specifically as follows: adjusting the gas pressure in the sputtering chamber to 2.5 mtorr-5.2 mtorr; The specific steps of setting the target spacing and sputtering power are: setting the target spacing to 45mm-100mm and the sputtering power to 810W-1430W.

6. The method for preparing a film structure according to claim 4, characterized in that: The component ratio of the indium oxide doped titanium oxide, tantalum oxide and cerium oxide target material is indium oxide: titanium oxide: tantalum oxide: cerium oxide = 98.57wt%: 0.63wt%: 0.51wt%: 0.28wt%.

7. The method for preparing a film structure according to claim 3, characterized in that: The silver film is prepared by magnetron sputtering a silver target, comprising the following steps: S5, installing silver target on magnetron sputtering system; S6, placing the substrate or the substrate prepared with the indium oxide-doped titanium oxide, tantalum oxide, cerium oxide thin film into the waiting chamber, and evacuating the sputtering chamber; S7, introducing argon gas into the sputtering chamber, adjusting the gas pressure, setting the target spacing and sputtering power, and turning on the power supply for pre-sputtering; S8, place the substrate in the waiting chamber into the sputtering chamber, introduce argon gas into the sputtering chamber, adjust the gas pressure in the sputtering chamber to 1.2mtorr-5.7mtorr, set the target spacing to 45mm-100mm, the sputtering power to 810-1430W, and turn on the power to deposit the silver film.

8. A film layer structure formed by the method for preparing a film layer structure according to any one of claims 1 to 7.

9. A photoelectric device, characterized in that: include: substrate; A film layer structure is arranged on the surface of the substrate, and the film layer structure includes a first film layer arranged on the substrate and a second film layer arranged on the first film layer; among the first film layer and the second film layer, one of the film layers is made of a metal film, and the other film layer is made of an indium oxide-doped titanium oxide, tantalum oxide, and cerium oxide thin film.

10. The optoelectronic device according to claim 9, characterized in that: The material of the first film layer is an indium oxide-doped titanium oxide, tantalum oxide, and cerium oxide thin film, the material of the second film layer is a metal film, and the film layer structure further includes: A third film layer is disposed on the second film layer, and the material of the third film layer is an indium oxide-doped titanium oxide, tantalum oxide, cerium oxide thin film.

Citation Information

Patent Citations

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