A light-emitting element of silicon-based rare earth doped light-emitting material and a preparation method thereof

Abstract

The present invention belongs to the field of rare earth doped luminescent materials, and discloses a light-emitting element of a silicon-based rare earth doped luminescent material and a preparation method thereof, the preparation method comprising the following steps: S1. Processing a silicon source and a carbon source into powder and mixing them evenly, dropping a binder and then forming, placing the powder in a resistance furnace under a vacuum environment for heating reaction, and obtaining a porous silicon carbide substrate; S2. Doping scattering particles in the silicon carbide substrate described in S1 by ion implantation, and placing the silicon carbide substrate in a high-temperature tubular diffusion furnace for annealing, and obtaining a doped silicon carbide substrate; S3. Arranging luminescent nanoparticles in the holes of the doped silicon carbide substrate described in S2 by deposition, and depositing a binding layer on the surface, and obtaining a silicon-based rare earth doped light-emitting element. The silicon-based rare earth doped light-emitting element prepared by the method has high optical efficiency and compatibility, and has high stability and low energy consumption.

Description

Technical Field

[0001] The present invention relates to the technical field of rare earth doped luminescent materials, and in particular to a luminescent element of silicon-based rare earth doped luminescent materials and a preparation method thereof. Background Art

[0002] As light displays are increasingly used in people's daily lives, the requirements for them will continue to increase. At the current stage, more and more people have shown great interest in photoluminescent devices for modern displays.

[0003] Silicon-based rare earth light-emitting elements are a new type of fluorescent device that achieves its fluorescent properties by introducing rare earth elements into the silicon matrix. They are used in many fields such as optical communications, lasers, sensors, etc.

[0004] Since silicon is the main semiconductor raw material, rare earth doping can make it have fluorescent properties, which has important application value in optoelectronics and other fields. However, the optical efficiency and compatibility of existing rare earth doped light-emitting elements are low, and the stability and low energy consumption are relatively poor. It is necessary to prepare rare earth doped light-emitting elements with better performance through better preparation methods. Summary of the invention

[0005] In view of the shortcomings of the prior art, the purpose of the present invention is to provide a light-emitting element of a silicon-based rare earth doped light-emitting material and a method for preparing the same. The silicon-based rare earth doped light-emitting element prepared by this method has high optical efficiency and compatibility, and not only has high stability and low energy consumption.

[0006] To achieve the above object, the present invention provides the following technical solutions:

[0007] A method for preparing a light-emitting element of a silicon-based rare earth doped light-emitting material comprises the following steps:

[0008] S1. Preparation of substrate: Processing a silicon source and a carbon source with a mass ratio of 1.5:1 into powder and mixing them evenly, adding a binder and then forming, placing in a resistance furnace under a vacuum environment for heating reaction, and obtaining a porous silicon carbide substrate;

[0009] S2. Substrate doping: doping the scattering particles in the silicon carbide substrate described in S1 by ion implantation, and placing it in a high-temperature tubular diffusion furnace for annealing to obtain a doped silicon carbide substrate;

[0010] S3. Pretreatment: Depositing luminescent nanoparticles with a particle size of 2-5 nanometers densely on the surface of the doped silicon carbide substrate to form a dense characteristic layer;

[0011] S4. Synthetic light-emitting element: The light-emitting nanoparticles with a particle size of 10-20 nanometers are arranged in the holes of the pretreated doped silicon carbide substrate in S3 by deposition, and a restraining layer is deposited on the surface of the characteristic layer to obtain a silicon-based rare earth doped light-emitting element;

[0012] The scattering particles are one of erbium silicate, gadolinium silicate, thulium silicate and neodymium silicate;

[0013] The luminescent nanoparticles are one or more of quantum dots and quantum rods, and are coated with silicon carbide.

[0014] Preferably, in S1, the silicon source is one or more of silicon dioxide, silicon metal or tetraethyl orthosilicate.

[0015] Preferably, in S1, the carbon source is one or more of carbon nanotubes, graphite blocks or graphene.

[0016] Preferably, in S1, the binder is a mixture of carbon black and silicate adhesive, which are mixed in a mass ratio of 1:1.

[0017] Preferably, in S1, the heating temperature of the resistance furnace is 2000-2200°C, and the heating time is 3-5h.

[0018] Preferably, in S2, the specific steps of the annealing operation are: placing the doped silicon carbide substrate in a high-temperature tubular diffusion furnace at 800-1000° C., annealing for 1.5-5 hours, and continuously introducing nitrogen into the furnace.

[0019] Preferably, in S4, the binding layer is composed of a uniform mixture of one of erbium nitride, gadolinium nitride, thulium nitride and neodymium nitride and silicon carbide in a ratio of 1:2, and the nitride used is consistent with the rare earth element contained in the scattering particles.

[0020] A light-emitting element of a silicon-based rare earth doped light-emitting material is prepared based on a preparation method of a light-emitting element of a silicon-based rare earth doped light-emitting material.

[0021] Compared with the prior art, the present invention has the following beneficial effects:

[0022] The present invention reduces the lattice mismatch between the substrate and the rare earth metal elements by doping the rare earth metal elements into the silicon substrate, so as to effectively avoid the generation of defects in the light-emitting element during use. It improves the efficiency of the silicon-based rare earth doped light-emitting element and also increases its service life. The excitation and emission properties of the rare earth metal elements are improved by annealing treatment, which helps to activate the rare earth elements and improve their optical efficiency.

[0023] The present invention forms a hole structure by pretreating and synthesizing a silicon substrate, and deposits and encapsulates luminescent nanoparticles in the holes of the silicon substrate, thereby improving the luminescent characteristics of the luminescent element and its stability to temperature, humidity and special environments, and increasing its compatibility in use.

[0024] The present invention adopts an integrated silicon carbide structure to enhance the integrity and hardness of the silicon-based rare earth light-emitting element structure, and forms a stack of rare earth elements in a porous base structure through ion implantation, which can emit its fluorescence more efficiently after activation, and effectively control the doping concentration on the base to prevent its spontaneous radiation quenching or failure to induce obvious fluorescence, so as to exhibit its optimal optical performance and reduce its required energy consumption. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 The present invention is a process flow chart for preparing the silicon-based rare earth doped light-emitting element. DETAILED DESCRIPTION

[0026] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments 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.

[0027] See also Figure 1 , the present invention provides:

[0028] Example 1

[0029] A method for preparing a light-emitting element of a silicon-based rare earth doped light-emitting material:

[0030] S1. Process a silicon source and a carbon source in a mass ratio of 1.5:1 into powder and mix them evenly, add a binder composed of 1:1 carbon black and silicate adhesive, and then form them, place them in a resistance furnace under a vacuum environment and heat them at 2000°C for 3 hours to obtain a porous silicon carbide substrate. In this embodiment, silicon dioxide is used as the silicon source and nanocarbon tubes are used as the carbon source.

[0031] S2. Erbium silicate is doped into the silicon carbide substrate described in S1 by ion implantation, and then the substrate is placed in a high-temperature tubular diffusion furnace at 800° C. for annealing for 5 hours, and nitrogen is continuously introduced into the furnace to obtain a doped silicon carbide substrate.

[0032] S3. The luminescent nanoparticles with a particle size of 5 nanometers are densely deposited on the surface of the doped silicon carbide substrate to form a dense characteristic layer;

[0033] S4. The luminescent nanoparticles with a particle size of 20 nanometers are arranged in the holes of the pretreated doped silicon carbide substrate described in S3 by deposition, and a binding layer is deposited on the surface with silicon carbide mixed with erbium nitride to obtain a silicon-based rare earth doped light-emitting element.

[0034] Example 2

[0035] A method for preparing a light-emitting element of a silicon-based rare earth doped light-emitting material:

[0036] S1. Process a silicon source and a carbon source in a mass ratio of 1.5:1 into powder and mix them evenly, add a binder composed of 1:1 carbon black and silicate adhesive, and then form them, place them in a resistance furnace under a vacuum environment and heat them at 2100°C for 4 hours to obtain a porous silicon carbide substrate. In this embodiment, the silicon source is silicon metal and the carbon source is graphite block.

[0037] S2. Thulium silicate is doped into the silicon carbide substrate described in S1 by ion implantation, and then the substrate is placed in a high-temperature tubular diffusion furnace at 900° C. for annealing for 3.5 hours, and nitrogen is continuously introduced into the furnace to obtain a doped silicon carbide substrate.

[0038] S3. The luminescent nanoparticles with a particle size of 2 nanometers are closely deposited on the surface of the doped silicon carbide substrate to form a dense characteristic layer;

[0039] S4. The luminescent nanoparticles with a particle size of 10 nanometers are arranged in the holes of the pretreated doped silicon carbide substrate described in S3 by deposition, and a binding layer is deposited on the surface with silicon carbide mixed with thulium nitride to obtain a silicon-based rare earth doped light-emitting element.

[0040] Example 3

[0041] A method for preparing a light-emitting element of a silicon-based rare earth doped light-emitting material:

[0042] S1. Process a silicon source and a carbon source in a mass ratio of 1.5:1 into powder and mix them evenly, add a binder composed of 1:1 carbon black and silicate adhesive, and then form them, place them in a resistance furnace under a vacuum environment and heat them at 2200°C for 5 hours to obtain a porous silicon carbide substrate. In this embodiment, the silicon source is tetraethyl orthosilicate and the carbon source is graphene.

[0043] S2. Neodymium silicate is doped into the silicon carbide substrate described in S1 by ion implantation, and then the substrate is placed in a high-temperature tubular diffusion furnace at 1000° C. for annealing for 2 h, and nitrogen is continuously introduced into the furnace to obtain a doped silicon carbide substrate.

[0044] S3. The luminescent nanoparticles with a particle size of 5 nanometers are densely deposited on the surface of the doped silicon carbide substrate to form a dense characteristic layer;

[0045] S4. The luminescent nanoparticles with a particle size of 10 nanometers are arranged in the holes of the pretreated doped silicon carbide substrate described in S3 by deposition, and a binding layer is deposited on the surface with silicon carbide mixed with neodymium nitride to obtain a silicon-based rare earth doped light-emitting element.

[0046] Example 4

[0047] A method for preparing a light-emitting element of a silicon-based rare earth doped light-emitting material:

[0048] S1. Process a silicon source and a carbon source in a mass ratio of 1.5:1 into powder and mix them evenly, add a binder composed of 1:1 carbon black and silicate adhesive, and then form them, place them in a resistance furnace under a vacuum environment and heat them at 2200°C for 5 hours to obtain a porous silicon carbide substrate. In this embodiment, the silicon source is tetraethyl orthosilicate and the carbon source is nanocarbon tubes.

[0049] S2. doping gadolinium silicate into the silicon carbide substrate described in S1 by ion implantation, placing it in a high-temperature tubular diffusion furnace at 1000° C., annealing for 4 hours, and continuously introducing nitrogen into the furnace to obtain a doped silicon carbide substrate.

[0050] S3. The luminescent nanoparticles with a particle size of 2 nanometers are closely deposited on the surface of the doped silicon carbide substrate to form a dense characteristic layer;

[0051] S4. The luminescent nanoparticles with a particle size of 20 nanometers are arranged in the holes of the pretreated doped silicon carbide substrate described in S3 by deposition, and a binding layer is deposited on the surface with silicon carbide mixed with gadolinium carbon nitride to obtain a silicon-based rare earth doped light-emitting element.

[0052] Comparative Example:

[0053] Comparative Example 1

[0054] There are the following differences between Comparative Example 1 and Example 1. The only difference is that in Comparative Example 1, the substrate doping operation described in Example 1 is omitted, thereby canceling the "annealing" step. Other components, amounts and preparation processes are the same as those in Example 1.

[0055] Comparative Example 2

[0056] Comparative Example 2 differs from Example 1 in that the pretreatment of the doped silicon carbide substrate described in Example 1 is omitted in Comparative Example 2, and other components, amounts and preparation processes are the same as those in Example 1.

[0057] Comparative Example 3

[0058] There are the following differences between Comparative Example 3 and Example 1, the only difference is that in Comparative Example 3, the substrate preparation process described in Example 1 is simplified, thereby eliminating the formation of a porous substrate and preparing a silicon carbide substrate without pores. The remaining components, amounts and preparation processes are the same as those in Example 1.

[0059] The relevant performance tests of the silicon-based rare earth doped light-emitting elements prepared in the above embodiments and comparative examples are as follows:

[0060] The above-mentioned Examples 1-4 and Comparative Examples 1-3 were tested for spectral performance, optical efficiency, electrical performance, and stability life.

[0061] Optical efficiency: Optical efficiency refers to the ratio of the luminous flux emitted by a light source to the power consumed, and the unit is lumen / watt. Different light sources emit the same luminous flux, and the less power they consume, the higher the luminous efficiency.

[0062] Electrical properties: Electrical properties are the focus of many material studies. Common test parameters include resistivity, square resistance, carrier concentration, carrier mobility, etc. Common test methods include four-probe method, van der Waersburg method, and Hall effect.

[0063] Stability life test: When the operating voltage is 3.6V, the power is continuously turned on to accelerate aging, and how long the light-emitting element can continue to work in a high temperature and high humidity environment and in a normal environment.

[0064] The test results are shown in the following table:

[0065]

[0066] The test results in the table show:

[0067] The relevant physical and chemical data of the present embodiment 1 and comparative examples 1-3 show that the present invention can reduce the lattice mismatch between the substrate and the rare earth metal elements, thereby effectively avoiding the defects of the light-emitting element during use. Through the research of this project, the performance of silicon-based rare earth ion doped light-emitting devices is effectively improved, and the service life of the devices is extended. At the same time, after heat treatment, the excitation luminescence properties of rare earth metals are further improved, thereby promoting the activation and luminescence of rare earth ions. It can be seen from the relevant data of Example 1 and Comparative Example 3 that by pretreating and synthesizing the silicon substrate, and depositing and encapsulating fluorescent nanoparticles in the pores of the silicon substrate, the luminescence performance and temperature resistance and special environment resistance of the device can be improved, while enhancing its compatibility for use.

[0068] Although the embodiments of the present invention have been disclosed as above, they are not limited to the applications listed in the specification and the implementation modes. They can be fully applied to various fields suitable for the present invention. For those skilled in the art, additional modifications can be easily implemented. Therefore, without departing from the general concept defined by the claims and the scope of equivalents, the present invention is not limited to specific details.

Claims

1. A method for preparing a light-emitting element of a silicon-based rare earth doped light-emitting material, characterized in that: The following steps are involved: S1. Preparation of substrate: Processing a silicon source and a carbon source with a mass ratio of 1.5:1 into powder and mixing them evenly, adding a binder and then forming, placing in a resistance furnace under a vacuum environment for heating reaction, and obtaining a porous silicon carbide substrate; S2. Substrate doping: doping the scattering particles in the silicon carbide substrate described in S1 by ion implantation, and placing it in a high-temperature tubular diffusion furnace for annealing to obtain a doped silicon carbide substrate; S3. Pretreatment: Depositing luminescent nanoparticles with a particle size of 2-5 nanometers densely on the surface of the doped silicon carbide substrate to form a dense characteristic layer; S4. Synthetic light-emitting element: The light-emitting nanoparticles with a particle size of 10-20 nanometers are arranged in the holes of the pretreated doped silicon carbide substrate in S3 by deposition, and a restraining layer is deposited on the surface of the characteristic layer to obtain a silicon-based rare earth doped light-emitting element; The scattering particles are one of erbium silicate, gadolinium silicate, thulium silicate and neodymium silicate; The luminescent nanoparticles are one or more of quantum dots and quantum rods, and are coated with silicon carbide.

2. The method for preparing a light-emitting element of a silicon-based rare earth doped light-emitting material according to claim 1, characterized in that: In S1, the silicon source is one or more of silicon dioxide, silicon metal or tetraethyl orthosilicate.

3. The method for preparing a light-emitting element of a silicon-based rare earth doped light-emitting material according to claim 1, characterized in that: In S1, the carbon source is one or more of carbon nanotubes, graphite blocks or graphene.

4. The method for preparing a light-emitting element of a silicon-based rare earth doped light-emitting material according to claim 1, characterized in that: In S1, the binder is a mixture of carbon black and silicate adhesive, which are mixed in a mass ratio of 1:

1.

5. The method for preparing a light-emitting element of a silicon-based rare earth doped light-emitting material according to claim 1, characterized in that: In S1, the resistance furnace heating temperature is 2000-2200°C, and the heating time is 3-5h.

6. The method for preparing a light-emitting element of a silicon-based rare earth doped light-emitting material according to claim 1, characterized in that: In S2, the specific steps of the annealing operation are: placing the doped silicon carbide substrate in a high-temperature tubular diffusion furnace at 800-1000° C., annealing for 1.5-5 hours, and continuously introducing nitrogen into the furnace.

7. The method for preparing a light-emitting element of a silicon-based rare earth doped light-emitting material according to claim 1, characterized in that: In S4, the binding layer is composed of a uniform mixture of one of erbium nitride, gadolinium nitride, thulium nitride and neodymium nitride mixed with silicon carbide in a ratio of 1:2, and the nitride used is consistent with the rare earth element contained in the scattering particles.

8. A light-emitting element of a silicon-based rare earth doped light-emitting material, characterized in that: The light-emitting element is prepared based on the method for preparing a light-emitting element of a silicon-based rare earth-doped light-emitting material according to any one of claims 1 to 7.

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