Tin terbium chlorate and a method for preparing the same

Abstract

The application relates to the field of luminescent materials, in particular to a terbium stannum chlorate and a preparation method thereof. The preparation method of the terbium stannum chlorate comprises the following steps: taking stannous chloride dihydrate and a terbium salt as precursors, dissolving the precursors in a solvent at room temperature to form a solution A; performing spin coating on a substrate to form a film, and heating to obtain a terbium stannum chlorate film based on the substrate. The method has the advantages of simple preparation process, low requirement on equipment, high controllability, less heat budget in the preparation process, and excellent photoluminescence performance of the product.

Description

Technical Field

[0001] This invention relates to the field of luminescent materials, specifically to a terbium tin chloride and its preparation method. Background Technology

[0002] SnO2 is a wide-bandgap semiconductor with a bandgap of 3.6 eV. It exhibits high carrier mobility, low phonon energy, and high transmittance in the visible and near-infrared bands. Doping with Sb or F can significantly increase the electron concentration in SnO2, making it an excellent conductive material. As a commercially available transparent conductive material, the preparation process of SnO2 is currently very mature, and high-quality thin films can be obtained through vacuum phase deposition. SnO2 has high solid solubility of rare earth elements (up to ~10 mol%), and its oxygen-rich environment is conducive to the optical transition of rare earth ions. Developing and preparing materials with photoluminescence properties is an urgent research topic. Summary of the Invention

[0003] The primary technical problem to be solved by this invention is to provide a terbium tin chloride with simple process, low cost, short reaction cycle, and strong photoluminescence performance, and its preparation method.

[0004] To solve the above-mentioned technical problems, this application provides a technical solution as follows: a method for preparing terbium stanchlorate, comprising: using stannous chloride dihydrate and terbium salt as precursors, dissolving them in a solvent at room temperature to form solution A; spin-coating solution A onto a substrate to form a film, heating it to obtain a terbium stanchlorate thin film based on the substrate.

[0005] The heating temperature is 10-250℃.

[0006] The terbium salt is terbium chloride hexahydrate.

[0007] The mass ratio of stannous chloride dihydrate to terbium chloride hexahydrate is (0.1-1):(0.0001-0.1).

[0008] The solvent includes ethanol.

[0009] The mass-to-volume ratio of stannous chloride dihydrate, terbium chloride hexahydrate, and ethanol is (0.1-1)g:(0.0001-0.1)g:(0.5-50)ml.

[0010] The substrate includes a silicon substrate, a germanium substrate, a gallium arsenide substrate, or a gallium nitride substrate.

[0011] The number of spin coating layers ranges from 1 to 10.

[0012] This application also includes a second technical solution: a terbium stanchlorate, prepared by the above-mentioned terbium stanchlorate preparation method, the terbium stanchlorate comprising a terbium stanchlorate thin film, the terbium stanchlorate thin film exhibiting visible-wavelength photoluminescence.

[0013] Among them, the terbium stanchlorate thin film has a luminescence intensity of 3.8 × 10⁻⁶ at 550 nm. 3 .

[0014] The beneficial effects of this invention are:

[0015] (1) The present invention provides a method for preparing terbium stanchlorate, which combines sol-gel method and heat treatment on a heating stage to prepare terbium stanchlorate thin film. No expensive instruments or equipment are required; terbium stanchlorate thin film can be obtained through reasonable process control, and terbium stanchlorate exhibits strong photoluminescence properties in the visible wavelength range. It can be applied in fields such as silicon-based light sources, LED light sources, integrated circuits, and display devices.

[0016] (2) The method for preparing terbium tin chloride of the present invention uses inexpensive and readily available raw materials, has a simple synthesis process, high controllability, low cost, short reaction cycle, and no environmental pollution. The terbium tin chloride thin film material prepared by this method has strong photoluminescence properties.

[0017] (3) The method for preparing terbium tin chloride of the present invention has a low reaction temperature and a small heat budget, which can reduce energy consumption. Attached Figure Description

[0018] Figure 1 This is a photoluminescence pattern of the terbium tin chloride thin film prepared in Example 1 of this application.

[0019] Figure 2 This is a scanning electron microscope image of the terbium tin chloride thin film prepared in Example 1 of this application.

[0020] Figure 3 This is another scanning electron microscope image of the terbium tin chloride thin film prepared in Example 1 of this application.

[0021] Figure 4 This is an EDS image of the terbium tin chloride thin film prepared in Example 1 of this application. Detailed Implementation

[0022] The following specific embodiments are used to further illustrate the methods described in this invention, but it is not intended that this invention is limited to these embodiments.

[0023] This application provides a method for preparing terbium stanchlorate, comprising: using stannous chloride dihydrate and terbium salt as precursors, dissolving them in a solvent at room temperature to form solution A; spin-coating solution A onto a substrate to form a film, heating to obtain a substrate-based terbium stanchlorate thin film.

[0024] The preparation method of terbium stanchlorate in this application embodiment is simple. A sol is formed at room temperature, which is then spin-coated to form a gel. A terbium stanchlorate thin film is obtained by heating. This method is simple, uses low-cost raw materials, has a short preparation cycle, produces highly uniform thin films, and is environmentally friendly. The terbium stanchlorate prepared in this application embodiment exhibits strong photoluminescence properties in the visible light band and can be used in light sources, such as silicon-based light sources, LED light sources, and display devices.

[0025] In this embodiment, the heating temperature is 10-250℃. This application can prepare terbium stanchlorate thin films through low-temperature heating, requiring a low thermal budget, and the prepared terbium stanchlorate thin films exhibit photoluminescence properties. In this embodiment, the heating temperature can be 25℃, 50℃, 60℃, 80℃, 100℃, 120℃, 150℃, 180℃, 210℃, or 250℃, etc.

[0026] In this embodiment, the terbium salt includes terbium chloride hexahydrate. The use of terbium chloride hexahydrate as the terbium salt in this embodiment results in a high purity of the prepared terbium stanchlorate. In other embodiments, the terbium salt may also include terbium nitrate, etc.

[0027] In this embodiment, the mass ratio of stannous chloride dihydrate to terbium chloride hexahydrate is (0.1-1):(0.0001-0.1). In this embodiment, by controlling the mass ratio of stannous chloride dihydrate to terbium chloride hexahydrate, the photoluminescence performance of the prepared terbium stanchlorate thin film is optimized.

[0028] In this embodiment, the solvent includes ethanol. Stannous chloride dihydrate and terbium chloride hexahydrate are soluble in ethanol, and ethanol is volatile, which can reduce the preparation time of the terbium stanchlorate thin film product. In other embodiments, the solvent may also be a mixture of water and ethanol.

[0029] In this embodiment, the mass-to-volume ratio of stannous chloride dihydrate, terbium chloride hexahydrate, and ethanol is (0.1-1) g:(0.0001-0.1) g:(0.5-50) ml. By reasonably controlling the mass-to-volume ratio of stannous chloride dihydrate, terbium chloride hexahydrate, and ethanol, this embodiment ensures that stannous chloride dihydrate and terbium chloride hexahydrate are completely dispersed in ethanol, and terbium stannate can be prepared.

[0030] In this embodiment, the substrate is a silicon substrate. In other embodiments, the substrate may also be a germanium substrate, a gallium arsenide substrate, or a gallium nitride substrate. This can improve the photoluminescence performance of the substrate, enabling the formation of a terbium stanchlorate thin film based on a silicon substrate, which can be applied to silicon-based light sources, LED light sources, and integrated circuits.

[0031] In this embodiment, the number of spin-coated layers is 1-10. Specifically, the number of spin-coated layers can be 1, 2, 3, 5, 6, 8, or 10 layers. By spin-coating different numbers of layers of solution A, the thickness of the prepared film can be set as needed, and the photoluminescence performance is optimal at this thickness. In this embodiment, the thickness of the terbium stanchlorate film is 1-100 nm.

[0032] This application also includes a second technical solution: a terbium stanchlorate, prepared by the above-described method for preparing terbium stanchlorate, comprising a terbium stanchlorate thin film, the terbium stanchlorate thin film exhibiting visible-wave photoluminescence. The terbium stanchlorate thin film of this application embodiment can be applied to silicon-based light sources, LED light sources, display devices, integrated circuits, and other fields.

[0033] In this embodiment, the terbium stanchlorate thin film exhibits a luminescence intensity of 3.8 × 10⁻⁶ in the 550 nm wavelength band. 3 The terbium stanchlorate implemented in this application has extremely strong photoluminescence properties.

[0034] To facilitate understanding of the technical solution of this application, the following specific embodiments are provided.

[0035] Example 1:

[0036] A method for preparing terbium tin chloride, comprising the following steps:

[0037] Step 1: Dissolve 0.4516g of stannous chloride dihydrate and 0.0216g of terbium chloride hexahydrate in 15ml of anhydrous ethanol in sequence, and stir at room temperature until completely dissolved to form mixed solution A;

[0038] Step 2: Take 40 μl of solution A and spin-coat it onto a silicon substrate to form a film. Spin-coat 3 layers and heat it on a 150°C heating stage to obtain a terbium tin chloride thin film based on a silicon substrate.

[0039] like Figure 1 The image shown is a photoluminescence pattern of the terbium tin chloride thin film fabricated in this embodiment. Figure 1 As can be seen, the prepared terbium stanchlorate thin film exhibits strong photoluminescence properties in the visible band; at 550 nm, the luminescence intensity is 3.8 × 10⁻⁶. 3 At 490 nm, the luminescence intensity is 1.8 × 10⁻⁶. 3 At 590 nm, the luminescence intensity is 1.45 × 10⁻⁶. 3 In the 628nm wavelength band, the luminescence intensity is 1.2 × 10⁻⁶. 3 .like Figure 2 and Figure 3The image shown is a scanning electron microscope image of the terbium stanchlorate thin film prepared according to an embodiment of this application. It can be seen from the image that the prepared terbium stanchlorate thin film is highly dense and uniformly distributed, with the terbium stanchlorate particles having a particle size between 100 nm and 800 nm. Figure 4 As shown in the figure, the EDS diagram of the product prepared in the embodiment of this application shows that the prepared product contains elements oxygen, tin, chlorine and terbium, indicating that the product prepared in the embodiment of this application is terbium tin chlorate.

[0040] Example 2:

[0041] The difference between this embodiment and Embodiment 1 is that the amount of terbium chloride hexahydrate in step one is changed to 0.0036g, as detailed below:

[0042] Methods for preparing terbium tin chloride include:

[0043] Step 1: Dissolve 0.4516g of stannous chloride dihydrate and 0.0036g of terbium chloride hexahydrate in 15ml of anhydrous ethanol, and stir at room temperature until completely dissolved to form mixed solution A;

[0044] Step 2: Take 40 μl of solution A and spin-coat it onto a silicon substrate to form a film. Spin-coat 3 layers and heat it on a 150°C heating stage for 10 minutes to obtain a terbium tin chloride thin film based on a silicon substrate.

[0045] In this embodiment, a terbium stanchlorate thin film can be formed on a silicon substrate. The morphology and properties of the terbium stanchlorate thin film are the same as or similar to those in Example 1. This embodiment of the application achieves shorter preparation time and lower temperature for the terbium stanchlorate thin film, requiring less thermal preheating.

[0046] Example 3:

[0047] The difference between this embodiment and Embodiment 1 is that the amount of ethanol in step one is changed to 20 ml, as detailed below:

[0048] Methods for preparing terbium tin chloride include:

[0049] Step 1: Dissolve 0.4516g of stannous chloride dihydrate and 0.0216g of terbium chloride hexahydrate in 20ml of anhydrous ethanol, and stir at room temperature until completely dissolved to form mixed solution A;

[0050] Step 2: Take 40 μl of solution A and spin-coat it onto a silicon substrate to form a film. Spin-coat 3 layers and heat it on a 150°C heating stage to obtain a terbium tin chloride thin film based on a silicon substrate.

[0051] Example 4:

[0052] The difference between this embodiment and Embodiment 1 is that the temperature of the heating table in step two is changed to 50°C. Everything else is the same as in Embodiment 1, as detailed below:

[0053] Methods for preparing terbium tin chloride include:

[0054] Step 1: Dissolve 0.4516g of stannous chloride dihydrate and 0.0216g of terbium chloride hexahydrate in 15ml of anhydrous ethanol in sequence, and stir at room temperature until completely dissolved to form mixed solution A;

[0055] Step 2: Take 40 μl of solution A and spin-coat it onto a silicon substrate to form a film. Spin-coat 3 layers and heat it on a 50°C heating stage to obtain a terbium tin chloride thin film based on a silicon substrate.

[0056] Example 5:

[0057] The difference between this embodiment and Embodiment 1 is that the temperature of the heating table in step two is changed to 60°C. Everything else is the same as in Embodiment 1, as detailed below:

[0058] Methods for preparing terbium tin chloride include:

[0059] Step 1: Dissolve 0.4516g of stannous chloride dihydrate and 0.0216g of terbium chloride hexahydrate in 15ml of anhydrous ethanol in sequence, and stir at room temperature until completely dissolved to form mixed solution A;

[0060] Step 2: Take 40 μl of solution A and spin-coat it onto a silicon substrate to form a film. Spin-coat 3 layers and heat it on a 60°C heating stage to obtain a terbium tin chloride thin film based on a silicon substrate.

[0061] Example 6:

[0062] The difference between this embodiment and Embodiment 1 is that the temperature of the heating table in step two is changed to 70°C. Everything else is the same as in Embodiment 1, as detailed below:

[0063] Methods for preparing terbium tin chloride include:

[0064] Step 1: Dissolve 0.4516g of stannous chloride dihydrate and 0.0216g of terbium chloride hexahydrate in 15ml of anhydrous ethanol in sequence, and stir at room temperature until completely dissolved to form mixed solution A;

[0065] Step 2: Take 40 μl of solution A and spin-coat it onto a silicon substrate to form a film. Spin-coat 3 layers and heat it on a 70°C heating stage to obtain a terbium tin chloride thin film based on a silicon substrate.

[0066] Example 7:

[0067] The difference between this embodiment and Embodiment 1 is that the temperature of the heating table in step two is changed to 80°C. Everything else is the same as in Embodiment 1, as detailed below:

[0068] Methods for preparing terbium tin chloride include:

[0069] Step 1: Dissolve 0.4516g of stannous chloride dihydrate and 0.0216g of terbium chloride hexahydrate in 15ml of anhydrous ethanol in sequence, and stir at room temperature until completely dissolved to form mixed solution A;

[0070] Step 2: Take 40 μl of solution A and spin-coat it onto a silicon substrate to form a film. Spin-coat 3 layers and heat it on an 80°C heating stage to obtain a terbium tin chloride thin film based on a silicon substrate.

[0071] Example 8:

[0072] The difference between this embodiment and Embodiment 1 is that the temperature of the heating table in step two is changed to 90°C. Everything else is the same as in Embodiment 1, as detailed below:

[0073] Methods for preparing terbium tin chloride include:

[0074] Step 1: Dissolve 0.4516g of stannous chloride dihydrate and 0.0216g of terbium chloride hexahydrate in 15ml of anhydrous ethanol in sequence, and stir at room temperature until completely dissolved to form mixed solution A;

[0075] Step 2: Take 40 μl of solution A and spin-coat it onto a silicon substrate to form a film. Spin-coat 3 layers and heat it on a 90°C heating stage to obtain a terbium tin chloride thin film based on a silicon substrate.

[0076] Example 9:

[0077] The difference between this embodiment and Embodiment 1 is that the temperature of the heating table in step two is changed to 100°C. Everything else is the same as in Embodiment 1, as detailed below:

[0078] Methods for preparing terbium tin chloride include:

[0079] Step 1: Dissolve 0.4516g of stannous chloride dihydrate and 0.0216g of terbium chloride hexahydrate in 15ml of anhydrous ethanol in sequence, and stir at room temperature until completely dissolved to form mixed solution A;

[0080] Step 2: Take 40 μl of solution A and spin-coat it onto a silicon substrate to form a film. Spin-coat 3 layers and heat it on a 100°C heating stage to obtain a terbium tin chloride thin film based on a silicon substrate.

[0081] Example 10:

[0082] Methods for preparing terbium tin chloride include:

[0083] Step 1: Dissolve 0.4516g of stannous chloride dihydrate and 0.0216g of terbium chloride hexahydrate in 15ml of anhydrous ethanol in sequence, and stir at room temperature until completely dissolved to form mixed solution A;

[0084] Step 2: Take 40 μl of solution A and spin-coat it onto a silicon substrate to form a film. Spin-coat 3 layers and heat it on a 250°C heating stage for 20 min to obtain a terbium tin chloride thin film based on a silicon substrate.

[0085] Example 11:

[0086] Methods for preparing terbium tin chloride include:

[0087] Step 1: Dissolve 0.4516g of stannous chloride dihydrate and 0.0216g of terbium chloride hexahydrate in 15ml of anhydrous ethanol in sequence, and stir at room temperature until completely dissolved to form mixed solution A;

[0088] Step 2: Take 40 μl of solution A and spin-coat it onto a silicon substrate to form a film. Spin-coat 3 layers and heat it on a 10°C heating stage for 2 hours to obtain a terbium tin chloride thin film based on a silicon substrate.

[0089] Example 12:

[0090] Methods for preparing terbium tin chloride include:

[0091] Step 1: Dissolve 0.4516g of stannous chloride dihydrate and 0.0216g of terbium chloride hexahydrate in 15ml of anhydrous ethanol in sequence, and stir at room temperature until completely dissolved to form mixed solution A;

[0092] Step 2: Take 40 μl of solution A and spin-coat it onto a silicon substrate to form a film. Spin-coat 3 layers and heat it on a 10°C heating stage for 2 hours to obtain a terbium tin chloride thin film based on a silicon substrate.

[0093] Example 13:

[0094] Methods for preparing terbium tin chloride include:

[0095] Step 1: Dissolve 0.1g of stannous chloride dihydrate and 0.0001g of terbium chloride hexahydrate in 0.5ml of anhydrous ethanol, stir at room temperature until completely dissolved, and stir for 2 minutes to form mixed solution A;

[0096] Step 2: Take the above solution A and prepare a film on the germanium substrate by spin coating. Spin coat one layer and heat it on a 50°C heating stage for 1 hour to obtain a terbium tin chloride thin film based on the germanium substrate.

[0097] Example 14:

[0098] Methods for preparing terbium tin chloride include:

[0099] Step 1: Dissolve 1g of stannous chloride dihydrate and 0.1g of terbium chloride hexahydrate in 50ml of anhydrous ethanol, and stir at room temperature until completely dissolved to form mixed solution A;

[0100] Step 2: Take the above solution A and prepare a film on a gallium arsenide substrate by spin coating. Spin coat 10 layers and heat on an 80°C heating stage for 0.5 h to obtain a terbium stanchlorate thin film based on a gallium arsenide substrate.

[0101] Example 15:

[0102] Methods for preparing terbium tin chloride include:

[0103] Step 1: Dissolve 1g of stannous chloride dihydrate and 0.0001g of terbium chloride hexahydrate in 10ml of anhydrous ethanol, and stir at room temperature until completely dissolved to form mixed solution A;

[0104] Step 2: Take the above solution A and spin-coat it onto a gallium nitride substrate to form a film. Spin-coat 6 layers and heat it on an 80°C heating stage for 0.5 hours to obtain a terbium stanchlorate thin film based on a gallium nitride substrate.

[0105] Example 16:

[0106] Methods for preparing terbium tin chloride include:

[0107] Step 1: Dissolve 0.1g of stannous chloride dihydrate and 0.1g of terbium chloride hexahydrate in 50ml of anhydrous ethanol, and stir at room temperature until completely dissolved to form mixed solution A;

[0108] Step 2: Take the above solution A and prepare a film on a gallium nitride substrate by spin coating. Spin coat 8 layers and heat on an 80°C heating stage for 0.2 h to obtain a terbium stanchlorate thin film based on a gallium nitride substrate.

[0109] Although embodiments of the present invention have been disclosed above, they are not limited to the applications listed in the specification and embodiments. It can be applied to various fields suitable for the invention. Other modifications can be readily made by those skilled in the art. Therefore, without departing from the general concept defined by the claims and their equivalents, the invention is not limited to the specific details and examples shown and described herein.

Claims

1. A method for preparing terbium tin chloride, characterized in that, include: Using stannous chloride dihydrate and terbium salt as precursors, the solutions are dissolved in solvents at room temperature to form solution A; Solution A is spin-coated onto a substrate to form a film, and then heated to obtain a terbium stanchlorate thin film based on the substrate; the heating temperature is 50-250℃; the terbium salt is terbium chloride hexahydrate; the mass ratio of stannous chloride dihydrate to terbium chloride hexahydrate is (0.1-1):(0.0001-0.1); the solvent includes ethanol; the mass-volume ratio of stannous chloride dihydrate, terbium chloride hexahydrate, and ethanol is (0.1-1)g:(0.0001-0.1)g:(0.5-50)mL.

2. The method for preparing terbium tin chloride according to claim 1, characterized in that, The substrate includes a silicon substrate, a germanium substrate, a gallium arsenide substrate, or a gallium nitride substrate.

3. The method for preparing terbium tin chloride according to claim 1, characterized in that, The spin coating has 1-10 layers.

4. A terbium tin chloride, characterized in that, The terbium stannate is prepared by the method of any one of claims 1-3, wherein the terbium stannate comprises a terbium stannate thin film, and the terbium stannate thin film exhibits visible-wavelength photoluminescence.

5. The terbium tin chloride according to claim 4, characterized in that, The terbium stanchlorate thin film exhibits a luminescence intensity of 3.8 × 10⁻⁶ at 550 nm. 3 .

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