Photoluminescent thin film and its preparation method
By combining sol-gel method and rapid thermal annealing, a terbium-doped tin oxide film is prepared under an inert atmosphere, solving the problem of insufficient photoluminescence performance of SnO2 films, and achieving high-efficiency photoluminescence performance in the visible light band. It is suitable for silicon-based light sources, LED light sources, and display devices.
Patent Information
- Application Number
- CN202110972565.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2021-08-24
- Publication Date
- 2025-08-05
- Estimated Expiration
- 2041-08-24
AI Technical Summary
It is difficult to prepare SnO2 films with high efficiency photoluminescence properties, especially in the visible and near-infrared bands, with insufficient transmittance and luminescence properties.
A terbium-doped tin oxide film is prepared under an inert atmosphere by combining sol-gel method and rapid thermal annealing. Defects are formed in the film by rapid heating and annealing treatment, and rapidly cooling is reduced in the inert gas atmosphere to maintain these defects, resulting in poor crystal field symmetry, thereby increasing the probability of terbium ion transition.
The prepared terbium-doped tin oxide film shows significant photoluminescence performance and improved luminescence intensity in the visible light band, and is suitable for silicon-based light sources, LED light sources and display devices.
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Figure CN115896758B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of luminescent materials, and in particular to a photoluminescent film and a preparation method thereof. Background Art
[0002] SnO2 is a wide-bandgap semiconductor with a bandgap of 3.6 eV. It features high carrier mobility, low phonon energy, and high transmittance in the visible and near-infrared bands. Currently, high-quality SnO2 thin films can be produced through vacuum vapor deposition. Doping SnO2 with Sb or F significantly increases the electron concentration, making it an excellent conductive material. However, the preparation of photoluminescent materials with luminescence properties and the improvement of their luminescence performance remain pressing technical challenges. Summary of the Invention
[0003] The technical problem to be solved by the present invention is to provide a photoluminescent film and a preparation method thereof, which can improve the luminescent properties of the photoluminescent film and enhance its photoluminescent properties.
[0004] To solve the above technical problems, the present invention provides a technical solution, namely, a method for preparing a photoluminescent film, comprising the following steps: spin-coating a mixed solution of a tin salt and a terbium salt on a substrate and heating the mixed solution on a heating table to obtain a thin film based on the substrate; placing the thin film based on the substrate in a rapid thermal annealing device and annealing the thin film in an inert gas atmosphere to obtain a terbium-doped tin oxide thin film based on the substrate, wherein the terbium-doped tin oxide thin film is a photoluminescent film.
[0005] The temperature of the annealing treatment is higher than the temperature of heating on the heating stage.
[0006] The inert gas includes nitrogen, argon or helium.
[0007] Wherein, in the inert gas atmosphere, the flow rate of the inert gas is 0.1-10 L / min.
[0008] Wherein, the solvent of the mixed solution of tin salt and terbium salt is ethanol.
[0009] Wherein, the molar volume ratio of the tin salt to the solvent is 1 mmol:(7.5-113.6) ml.
[0010] The annealing treatment is performed at a temperature of 100-1300° C. in an inert gas atmosphere, and the annealing treatment time is 1-100 seconds.
[0011] The heating temperature on the heating table is 10-250°C.
[0012] The molar ratio of the tin salt to the terbium salt is 100:(0.06-29).
[0013] The terbium salt includes one or more of terbium chloride hexahydrate, terbium nitrate, terbium sulfate, and terbium carbonate; the tin salt includes one or more of stannous chloride dihydrate, stannous sulfate, and stannous nitrate.
[0014] The substrate includes a semiconductor substrate, and the semiconductor substrate includes a crystalline silicon substrate, a germanium substrate, a gallium arsenide substrate, and a gallium nitride substrate.
[0015] The present invention also includes a second technical solution, a photoluminescent film prepared by the above-mentioned method for preparing a photoluminescent film, the photoluminescent film comprising a terbium-doped tin oxide film, and the photoluminescent film photoluminescent in the visible light band.
[0016] Among them, the terbium-doped tin oxide film photoluminescently emits light in the 500nm, 550nm, 590nm and 630nm bands.
[0017] Beneficial effects of the present invention:
[0018] (1) The method for preparing a photoluminescent film of the present invention adopts a combination of a sol-gel method and a rapid thermal treatment method, and anneals a terbium-doped tin oxide film with photoluminescent properties in an inert atmosphere. The terbium-doped tin oxide film prepared by the present invention using a rapid thermal annealing device, on the one hand, is further annealed by the film based on the substrate by rapid heating, and a large number of defects are formed in the film by heating in a short time; on the other hand, since the inert gas is an oxygen-deficient gas, annealing in an inert atmosphere will also form a large number of oxygen vacancy defects in the film. The terbium-doped tin oxide film is obtained by rapid cooling. During the rapid cooling process, these defects cannot be repaired, resulting in a deterioration of the crystal field symmetry, resulting in an increase in the probability of terbium ion transition, so that the obtained terbium-doped tin oxide film has a stronger luminescence intensity than the sample annealed in an air atmosphere, and can be widely used in silicon-based light sources, LED light sources, display devices and other fields.
[0019] (2) The preparation method of the terbium-doped tin oxide thin film of the present invention has cheap and easily available raw materials, a simple synthesis process with low cost, a short reaction cycle, no pollution to the environment, and a low thermal budget. BRIEF DESCRIPTION OF THE DRAWINGS
[0020] Figure 1 1 is a photoluminescence image of the terbium-doped tin oxide thin film prepared in Example 1 of the present invention and the comparative example.
[0021] Figure 2 1 is the XRD pattern of the terbium-doped tin oxide thin films prepared in Example 1 of the present invention and the comparative example.
[0022] Figure 3 1 is a scanning electron microscope image of the terbium-doped tin oxide thin film prepared in Example 1 of the present invention and the comparative example. DETAILED DESCRIPTION
[0023] An embodiment of the present invention provides a method for preparing a photoluminescent film, comprising the following steps: spin-coating a mixed solution of a tin salt and a terbium salt on a substrate, and heating the solution on a heating table to obtain a thin film based on the substrate; and placing the thin film based on the substrate in a rapid thermal annealing device and annealing the thin film in an inert gas atmosphere to obtain a terbium-doped tin oxide thin film based on the substrate, wherein the terbium-doped tin oxide thin film is a photoluminescent film.
[0024] The present invention combines a sol-gel method with a rapid thermal process to prepare photoluminescent terbium-doped tin oxide thin films under an inert gas atmosphere. This method utilizes readily available, inexpensive raw materials, a simple and low-cost synthesis process, a short reaction cycle, and is environmentally friendly. It also offers a low thermal budget and exhibits enhanced photoluminescence compared to samples annealed in air.
[0025] The embodiment of the present invention uses a rapid thermal annealing device to prepare a terbium-doped tin oxide thin film. The substrate-based thin film is further annealed by rapidly heating. On the one hand, the short-term heating causes a large number of defects in the thin film; on the other hand, since the inert gas is an oxygen-deficient gas, annealing in a nitrogen atmosphere will also form a large number of oxygen vacancy defects in the thin film. The terbium-doped tin oxide thin film is obtained by rapid cooling. During the rapid cooling process, these defects cannot be repaired, resulting in a deterioration of the crystal field symmetry, which increases the probability of terbium ion transitions, resulting in a terbium-doped tin oxide thin film with a strong luminescence intensity. Tb 3+ Absorbs visible light, of which green light is emitted from 5 D4→ 7 F J Transition, higher energy level blue light comes from 5 D3→ 7 F J transition, but this transition is easy to pass through Tb( 5 D3)+Tb( 7 F6)→Tb( 5 D4)+Tb( 7 F6) cross-relaxation process and quenching occurs. The embodiment of the present invention can improve Tb 3+ of 5 D4→ 7 F J Transition and 5 D3→ 7 F J The quenching caused by the transition is eliminated, and a terbium-doped tin oxide film with strong luminescence intensity is obtained. The terbium-doped tin oxide film prepared in the embodiment of the present invention can be widely used in the fields of silicon-based light sources, LED light sources, display devices, etc.
[0026] The embodiment of the present invention increases the lattice defects of the terbium-doped tin oxide film by annealing in an inert gas atmosphere, which is greater than that of the terbium-doped tin oxide film prepared by annealing in an air atmosphere. As a result, the photoluminescence performance of the terbium-doped tin oxide film prepared by the embodiment of the present invention is greater than that of the terbium-doped tin oxide film prepared by annealing in an air atmosphere.
[0027] In an embodiment of the present invention, a rapid thermal annealing device is used in an inert gas atmosphere for annealing, wherein the rapid thermal annealing temperature rise rate is 200°C / s; the temperature drop rate is 100-200°C / s; and the nitrogen flow rate is 1-10 L / min. In an embodiment of the present invention, the annealing atmosphere is an inert gas atmosphere.
[0028] In the embodiment of the present invention, the temperature of the annealing treatment is higher than the temperature of heating on the heating table, so that a relatively pure terbium-doped tin oxide thin film can be obtained through further annealing treatment.
[0029] In an embodiment of the present invention, the inert gas includes nitrogen, argon or helium.
[0030] Among them, nitrogen is preferably used as the inert gas.
[0031] Wherein, in the inert gas atmosphere, the flow rate of the inert gas is 0.1-10 L / min.
[0032] The annealing treatment is performed at a temperature of 100-1300° C. in an inert gas atmosphere, and the annealing treatment time is 1-100 seconds.
[0033] The heating temperature on the heating table is 10-250°C.
[0034] In the embodiments of the present invention, the terbium salt includes one or more of terbium chloride hexahydrate, terbium nitrate, terbium sulfate, and terbium carbonate; and the tin salt includes one or more of stannous chloride dihydrate, stannous sulfate, and stannous nitrate. In the embodiments of the present invention, a terbium-doped tin oxide thin film can be prepared using the above raw materials.
[0035] In the embodiment of the present invention, the molar ratio of tin salt to terbium salt is 100:(0.06-29). By controlling the ratio of tin salt to terbium salt and the amount of terbium doped, the prepared terbium-doped tin oxide film has a strong photoluminescence intensity.
[0036] In an embodiment of the present invention, the molar volume ratio of the tin salt to the solvent is 1 mmol:(7.5-113.6) ml. By controlling the amount of the solvent, the concentration of the mixed solution is controlled, thereby controlling the uniformity and thickness of the film.
[0037] In the embodiment of the present invention, the solvent includes ethanol. Tin salt and terbium salt are soluble in ethanol, and ethanol is volatile, which can shorten the preparation time of the terbium stannate chlorate thin film product.
[0038] In an embodiment of the present invention, the substrate comprises a semiconductor substrate. Specifically, the semiconductor substrate comprises a crystalline silicon substrate, a germanium substrate, a gallium arsenide substrate, or a gallium nitride substrate. The terbium stannate chlorate thin film based on the semiconductor substrate can be applied to fields such as silicon-based light sources, LED light sources, and integrated circuits.
[0039] The present invention also includes a second technical solution, comprising a photoluminescent film produced by the above-described method for producing a photoluminescent film. The photoluminescent film comprises a terbium-doped tin oxide film, and the photoluminescent film emits light in the visible light band. The photoluminescent film of this embodiment of the present invention can be applied to fields such as silicon-based light sources, LED light sources, display devices, and integrated circuits. This embodiment of the present invention improves the photoluminescent properties of the terbium-doped tin oxide film by combining a sol-gel method and a rapid thermal process under an inert gas atmosphere, thereby increasing the photoluminescent intensity in the visible light band.
[0040] In embodiments of the present invention, terbium-doped tin oxide emits photoluminescence in the 500nm, 550nm, 590nm, and 630nm wavelength bands. In these embodiments, the 500nm wavelength emits bluish-indigo light, the 550nm wavelength emits green light, the 590nm wavelength emits yellow light, and the 630nm wavelength emits red light. The green light has the highest intensity.
[0041] The following specific examples are used to further illustrate the method described in the present invention, but it is not intended that the present invention is limited to these examples.
[0042] Example 1:
[0043] A method for preparing a photoluminescent film, comprising the following steps:
[0044] Step 1: dissolving 0.4516 g (2 mmol) of stannous chloride dihydrate and 0.0216 g (0.058 mmol) of terbium chloride hexahydrate in 15 ml of anhydrous ethanol and stirring at room temperature until completely dissolved to form solution A, wherein the molar ratio of stannous chloride dihydrate to terbium chloride hexahydrate is 100:29; and the molar volume ratio of stannous chloride dihydrate to ethanol is 1 mmol:7.5 mL.
[0045] Step 2: Take 40 μl of solution A and prepare a film on a silicon substrate by spin coating. Spin coat 3 layers and heat on a heating table at 150° C. to obtain a thin film based on a silicon substrate.
[0046] Step three, the thin film based on the silicon substrate obtained in step two is annealed at 1000°C for 1s in a nitrogen atmosphere with a rapid thermal annealing device (RTP) and a nitrogen flow rate of 1.5 L / min, thereby obtaining a terbium-doped tin oxide thin film based on the substrate; wherein the terbium-doped tin oxide thin film is a photoluminescent film that photoluminesces in the visible band.
[0047] like Figure 1 As shown, Figure 1 The spectrum of N2 in the nitrogen atmosphere is the photoluminescence spectrum of the terbium-doped tin oxide film prepared in the embodiment of the present invention, and the spectrum of air is the photoluminescence spectrum of the terbium-doped tin oxide film prepared in the air atmosphere in the comparative example. It can be seen from the figure that the photoluminescence intensity of the sample annealed in the nitrogen atmosphere is 3 times higher than that of the sample annealed in the air.
[0048] The embodiment of the present invention combines a sol-gel method with a rapid thermal process to prepare a terbium-doped tin oxide thin film in a nitrogen atmosphere. The prepared terbium-doped tin oxide thin film has better photoluminescence performance than the sample annealed in air. The embodiment of the present invention uses a rapid thermal annealing device to prepare the terbium-doped tin oxide thin film. On the one hand, the rapid heating further anneals the thin film based on the substrate, and the short heating time causes a large number of defects to form in the film. On the other hand, because nitrogen is an oxygen-deficient gas, annealing in a nitrogen atmosphere also forms a large number of oxygen vacancy defects in the film. The terbium-doped tin oxide thin film is obtained by rapid cooling. During the rapid cooling process, these defects cannot be repaired, resulting in a deterioration of the crystal field symmetry, which increases the probability of terbium ion transitions, resulting in the obtained terbium-doped tin oxide thin film having a strong luminescence intensity.
[0049] Figure 2 As shown, Figure 1 The spectrum of N2 in the air is the XRD spectrum of the terbium-doped tin oxide film prepared in the embodiment of the present invention, and the spectrum of air is the XRD spectrum of the terbium-doped tin oxide film prepared by annealing in an air atmosphere in the comparative example. Figure 2 It can be seen that the diffraction peaks of the terbium-doped tin oxide film prepared in the embodiment of the present invention at the (110), (101) and (211) crystal planes correspond to the characteristic peaks of the tin oxide phase. The terbium content in the embodiment of the present invention is relatively small and is not shown in the XRD spectrum, indicating that a crystalline terbium-doped tin oxide film is formed. The terbium-doped tin oxide film in the embodiment of the present invention is a crystalline terbium-doped tin oxide film.
[0050] Figure 3 (a) is a scanning electron microscope image of a terbium-doped tin oxide thin film prepared by annealing in air atmosphere in the comparative example. Figure 3 (b) is a scanning electron microscope image of a terbium-doped tin oxide film prepared in an embodiment of the present invention. Figure 3It can be seen that the terbium-doped tin oxide film prepared in the embodiment of the present invention has better dispersibility, while the terbium-doped tin oxide film prepared in the comparative example has a certain degree of cohesion. The particle size of the particles in the terbium-doped tin oxide film prepared in the embodiment of the present invention is larger than that in the terbium-doped tin oxide film prepared in the comparative example.
[0051] Comparative Example
[0052] A method for preparing a photoluminescent film, comprising the following steps:
[0053] Step 1: dissolving 0.4516 g (2 mmol) of stannous chloride dihydrate and 0.0216 g (0.058 mmol) of terbium chloride hexahydrate in 15 ml of anhydrous ethanol and stirring at room temperature until completely dissolved to form solution A, wherein the molar ratio of stannous chloride dihydrate to terbium chloride hexahydrate is 100:29; and the molar volume ratio of stannous chloride dihydrate to ethanol is 1 mmol:7.5 mL.
[0054] Step 2: Take 40 μl of solution A and prepare a film on a silicon substrate by spin coating. Spin coat 3 layers and heat on a heating table at 150° C. to obtain a thin film based on a silicon substrate.
[0055] Step three, the thin film based on the silicon substrate obtained in step two is annealed at 1000°C for 1s in an air atmosphere with a nitrogen flow rate of 1.5L / min using a rapid thermal annealing device (RTP), thereby obtaining a terbium-doped tin oxide thin film based on the substrate; wherein the terbium-doped tin oxide thin film is a photoluminescent film that photoluminesces in the visible band.
[0056] Example 2:
[0057] A method for preparing a photoluminescent film, comprising the following steps:
[0058] Step 1: dissolve 0.4516 g of stannous chloride dihydrate and 0.0216 g of terbium chloride hexahydrate in 15 ml of anhydrous ethanol, and stir at room temperature until completely dissolved to form solution A.
[0059] Step 2: Take 40 μl of solution A and prepare a film on a silicon substrate by spin coating. Spin coat 3 layers and heat on a heating table at 150° C. to obtain a thin film based on a silicon substrate.
[0060] Step three, the thin film based on the silicon substrate obtained in step two is subjected to rapid thermal annealing equipment (RTP) in an argon atmosphere at 1000°C for 1s with an argon flow rate of 1.5L / min to obtain a terbium-doped tin oxide thin film based on the substrate; wherein the terbium-doped tin oxide thin film is a photoluminescent film that photoluminesces in the visible band.
[0061] The performance of the terbium-doped tin oxide film prepared in the embodiment of the present invention is similar to that in the embodiment.
[0062] Example 3:
[0063] A method for preparing a photoluminescent film, comprising the following steps:
[0064] Step 1: dissolve 0.4516 g of stannous chloride dihydrate and 0.0216 g of terbium chloride hexahydrate in 15 ml of anhydrous ethanol, and stir at room temperature until completely dissolved to form solution A.
[0065] Step 2: Take 40 μl of solution A and prepare a film on a silicon substrate by spin coating. Spin coat 3 layers and heat on a heating table at 150° C. to obtain a thin film based on a silicon substrate.
[0066] Step three, the thin film based on the silicon substrate obtained in step two is subjected to rapid thermal annealing equipment (RTP) in a helium atmosphere at 1000°C for 1s with a helium flow rate of 1.5L / min to obtain a terbium-doped tin oxide thin film based on the substrate; wherein the terbium-doped tin oxide thin film is a photoluminescent film that photoluminesces in the visible band.
[0067] The performance of the terbium-doped tin oxide film prepared in the embodiment of the present invention is similar to that in the embodiment.
[0068] Example 4
[0069] A method for preparing a photoluminescent film, comprising the following steps:
[0070] Step 1: dissolve 0.4516 g of stannous chloride dihydrate and 0.0216 g of terbium chloride hexahydrate in 15 ml of anhydrous ethanol, and stir at room temperature until completely dissolved to form solution A.
[0071] Step 2: Take 40 μl of solution A and prepare a film on a silicon substrate by spin coating. Spin coat 3 layers and heat on a heating table at 10° C. for 2 h to obtain a thin film based on a silicon substrate.
[0072] Step three, the thin film based on the silicon substrate obtained in step two is subjected to rapid thermal annealing equipment (RTP) in a nitrogen atmosphere at 100°C for 1s with a nitrogen flow rate of 0.1L / min to obtain a terbium-doped tin oxide thin film based on the substrate; wherein the terbium-doped tin oxide thin film is a photoluminescent film that photoluminesces in the visible band.
[0073] The performance of the terbium-doped tin oxide film prepared in the embodiment of the present invention is similar to that in the embodiment.
[0074] Example 5
[0075] A method for preparing a photoluminescent film, comprising the following steps:
[0076] Step 1: dissolve 0.4516 g of stannous chloride dihydrate and 0.0216 g of terbium chloride hexahydrate in 15 ml of anhydrous ethanol, and stir at room temperature until completely dissolved to form solution A.
[0077] Step 2: Take 40 μl of solution A and prepare a film on a silicon substrate by spin coating. Spin coat 3 layers and heat on a heating table at 250° C. for 2 h to obtain a thin film based on a silicon substrate.
[0078] Step three, the thin film based on the silicon substrate obtained in step two is subjected to rapid thermal annealing equipment (RTP) at 900°C for 100s in a nitrogen atmosphere with a nitrogen flow rate of 10L / min to obtain a terbium-doped tin oxide thin film based on the substrate; wherein the terbium-doped tin oxide thin film is a photoluminescent film that photoluminesces in the visible band.
[0079] The performance of the terbium-doped tin oxide film prepared in the embodiment of the present invention is similar to that in the embodiment.
[0080] Example 6
[0081] A method for preparing a photoluminescent film, comprising the following steps:
[0082] Step 1: dissolve 0.4516 g of stannous chloride dihydrate and 0.0216 g of terbium chloride hexahydrate in 15 ml of anhydrous ethanol, and stir at room temperature until completely dissolved to form solution A.
[0083] Step 2: Take 40 μl of solution A and prepare a film on a silicon substrate by spin coating. Spin coat 3 layers and heat on a heating table at 250° C. for 24 hours to obtain a thin film based on a silicon substrate.
[0084] Step three, the thin film based on the silicon substrate obtained in step two is annealed at 1300°C for 40s in a nitrogen atmosphere using a rapid thermal annealing device (RTP), with a nitrogen flow rate of 5 L / min, a heating rate of 200°C / s, and a cooling rate of 200°C / s, to obtain a terbium-doped tin oxide thin film based on the substrate; wherein the terbium-doped tin oxide thin film is a photoluminescent thin film that photoluminesces in the visible band.
[0085] The performance of the terbium-doped tin oxide film prepared in the embodiment of the present invention is similar to that in the embodiment.
[0086] Example 7
[0087] A method for preparing a photoluminescent film, comprising the following steps:
[0088] Step 1: Dissolve 0.4516 g (2 mmol) of stannous chloride dihydrate and 0.0036 g (0.001 mmol) of terbium chloride hexahydrate in 15 ml of anhydrous ethanol and stir at room temperature until completely dissolved to form solution A. The molar ratio of stannous chloride dihydrate to terbium chloride hexahydrate is 100:0.5; and the molar volume ratio of stannous chloride dihydrate to ethanol is 1 mmol:7.5 mL.
[0089] Step 2: Take 40 μl of solution A and prepare a film on a silicon substrate by spin coating. Spin coat 10 layers and heat on a heating table at 250° C. for 12 hours to obtain a thin film based on a silicon substrate.
[0090] Step three, the thin film based on the silicon substrate obtained in step two is annealed at 1200°C for 40s in a nitrogen atmosphere using a rapid thermal annealing device (RTP), with a nitrogen flow rate of 0.5 L / min, a heating rate of 200°C / s, and a cooling rate of 300°C / s, thereby obtaining a terbium-doped tin oxide thin film based on the substrate; wherein the terbium-doped tin oxide thin film is a photoluminescent thin film that photoluminesces in the visible band.
[0091] The performance of the terbium-doped tin oxide film prepared in the embodiment of the present invention is similar to that in the embodiment.
[0092] Example 8
[0093] A method for preparing a photoluminescent film comprises the following steps:
[0094] Step 1: dissolve 0.5 g of stannous nitrate 20-hydrate and 0.00572 g of terbium nitrate in 20 ml of anhydrous ethanol, and stir at room temperature until completely dissolved to form a mixed solution A.
[0095] Step 2: Take solution A and prepare a film on a germanium substrate by spin coating. Spin coat 6 layers and heat on a heating table at 200° C. for 20 minutes to obtain a thin film based on a germanium substrate.
[0096] Step three, the thin film based on the silicon substrate obtained in step two is annealed at 600°C for 30s in a nitrogen atmosphere using a rapid thermal annealing device (RTP), with a nitrogen flow rate of 1 L / min, a heating rate of 100°C / s, and a cooling rate of 100°C / s, to obtain a terbium-doped tin oxide thin film based on the substrate; wherein the terbium-doped tin oxide thin film is a photoluminescent thin film that photoluminesces in the visible band.
[0097] The performance of the terbium-doped tin oxide film prepared in the embodiment of the present invention is similar to that in the embodiment.
[0098] Obviously, the above embodiments are merely illustrative examples for clarity of explanation and are not intended to limit the implementation methods. Those skilled in the art will recognize that any modifications, equivalent substitutions, or improvements based on the above description and within the methods and principles of the present invention are intended to be within the scope of protection of the present invention. It is not necessary and impossible to enumerate all implementation methods here. Obvious variations or modifications arising therefrom remain within the scope of protection of the present invention.
Claims
1. A method for preparing a photoluminescent film, characterized in that: The following steps are involved: Spin-coating a mixed solution of tin salt and terbium salt on a substrate and heating it on a heating table to obtain a thin film based on the substrate; placing the substrate-based thin film in a rapid thermal annealing device and performing annealing treatment in an inert gas atmosphere to obtain a substrate-based terbium-doped tin oxide thin film, wherein the terbium-doped tin oxide thin film is a photoluminescent thin film; The rapid thermal annealing equipment is used to perform annealing treatment in an inert gas atmosphere, wherein the rapid thermal annealing temperature rise rate is 200°C / s; the temperature drop rate is 100-200°C / s; and the nitrogen flow rate is 1-10 L / min.
2. The method for preparing a photoluminescent film according to claim 1, wherein: The temperature of the annealing treatment is higher than the temperature of heating on the heating stage.
3. The method for preparing a photoluminescent film according to claim 1, wherein: Inert gases include nitrogen, argon, or helium.
4. The method for preparing a photoluminescent film according to claim 1, wherein: In the inert gas atmosphere, the flow rate of the inert gas is 0.1-10 L / min.
5. The method for preparing a photoluminescent film according to claim 1, wherein: The solvent of the mixed solution of tin salt and terbium salt is ethanol.
6. The method for preparing a photoluminescent film according to claim 1, wherein: The temperature of the annealing treatment in the inert gas atmosphere is 100-1300° C., and the time of the annealing treatment is 1-100 seconds.
7. The method for preparing a photoluminescent film according to claim 1, wherein: The heating temperature on the heating table is 10-250°C.
8. The method for preparing a photoluminescent film according to claim 1, wherein: The molar ratio of the tin salt to the terbium salt is 100:(0.06-29).
9. A photoluminescent film, characterized in that: The photoluminescent film is prepared by the preparation method of any one of claims 1 to 8, wherein the photoluminescent film comprises a terbium-doped tin oxide film, and the photoluminescent film photoluminescently emits light in the visible light band.
10. The photoluminescent film according to claim 9, characterized in that The terbium-doped tin oxide thin film photoluminescently emits light at wavelengths of 500 nm, 550 nm, 590 nm and 630 nm.
Citation Information
Patent Citations
Terbium-doped gadolinium oxide green light luminescent film and preparation method thereof
CN101560680A
Method of fabricating a terbium-doped electroluminescence device via metal organic deposition processes
US20080026494A1