Preparation method of Dy < 3 + >-doped black talc-based high-performance luminescent glass

Abstract

The invention discloses a preparation method of Dy < 3 + > doped black talc-based high-performance luminescent glass. The luminescent glass comprises the following chemical components in percentage by weight: 80wt% of black talc, 20wt% of Na2O and 1-4wt% of Dy2O3. The preparation method comprises the following steps: weighing the three raw materials according to the mass ratio, uniformly mixing in a ceramic mortar, putting into an Al2O3 crucible, putting into a high-temperature muffle furnace, carrying out high-temperature melting at the melting temperature of 1600 DEG C, and keeping the temperature for 2 hours. Pouring the glass melt on a preheated stainless steel mold, placing the mold in a low-temperature muffle furnace for annealing treatment at the annealing temperature of 680 DEG C, and keeping the temperature for 10 hours; and cooling the annealing furnace to room temperature to obtain the black talc-based luminescent glass. The optimum excitation wavelength of the prepared luminescent glass is 350nm, the main emission peaks are blue light (the peak wavelength is 483nm) and yellow light (the peak wavelength is 576nm), and the luminescent glass emits white light under the irradiation of ultraviolet light. The luminescent glass has the advantages of simple preparation method, low equipment requirement, short production period, strong practicability and the like, and can be widely applied to the fields of decoration, counterfeiting prevention, illumination and the like.

Description

Technical Field

[0001] The invention belongs to the field of inorganic luminescent glass materials, relates to the high-value utilization of black talc, and specifically relates to a Dy 3+ Preparation method of high-performance luminescent glass based on doped black talc. Background Art

[0002] In recent years, inorganic luminescent glass has been widely reported. On the one hand, this is due to the melting preparation process of glass materials, which allows rare earth ions to be evenly dispersed in the network structure of glass, thereby obtaining a uniform and good luminous effect; on the other hand, compared with phosphors, glass has better thermal and chemical stability and lower light loss, which can effectively solve the problems of LED device service life and lighting quality decline, and become an effective substitute for phosphors for the new generation of LEDs.

[0003] The main chemical components of black talc in Guangfeng District, Shangrao City, Jiangxi Province are silicon dioxide / magnesium oxide (SiO2 / MgO), and there are also a small amount of alkali / alkaline earth metal oxides (K2O / CaO), which have the potential to prepare silicate glass. In view of this, the present application uses black talc as a matrix to prepare a luminescent glass material. The optical properties of Dy2O3-doped black talc-based luminescent glass were studied by fluorescence spectrometer. The main emission peaks are blue light (peak wavelength 483nm) and yellow light (peak wavelength 576nm). White light is emitted under ultraviolet light. It is an inorganic luminescent glass material with potential application value and is expected to be used in the field of luminescent materials for LEDs. Summary of the invention

[0004] The purpose of the present invention is to provide a black talc-based luminescent glass material. The luminescent glass is a type of high-performance concentrated green light luminescent material, and is expected to be applied in the field of luminescent glass materials for LEDs.

[0005] Another object of the present invention is to provide a Dy 3+ The preparation method of doped black talc-based luminescent glass solves the problem of low-value utilization of black talc in Guangfeng District, Shangrao City.

[0006] The Dy 3+ The method for preparing the high-performance luminescent glass doped with black talc specifically comprises the following steps:

[0007] (1) Mix black talc, Na2O and Dy2O3 in a ceramic mortar according to a pre-designed mass ratio, and put them into an Al2O3 crucible to obtain a batch material. The mass percentage of each component is: black talc (80%), Na2O (20%), Dy2O3 (1-4%);

[0008] (2) placing the batch material in a high-temperature muffle furnace and melting it at 1600° C. for 2 hours to obtain a uniform glass melt;

[0009] (3) The glass melt is poured onto a preheated stainless steel mold and placed in a low-temperature muffle furnace for annealing at 680° C. for 10 hours to release the stress in the melt. The annealing furnace is cooled to room temperature to obtain a black talc-based luminescent glass product. BRIEF DESCRIPTION OF THE DRAWINGS

[0010] (1) Figure 1 Dy prepared in the present invention 3+ XRD spectrum of high-performance luminescent glass based on doped black talc;

[0011] (2) Figure 2 Dy prepared in the present invention 3+ Actual picture of doped black talc-based high-performance luminescent glass under UV light / natural light;

[0012] (3) Figure 3 Dy prepared in the present invention 3+ Fluorescence excitation and emission spectra of high-performance luminescent glass based on doped black talc;

[0013] (4) Figure 4 Dy prepared in the present invention 3+ The fluorescence emission intensity of high-performance luminescent glass based on doped black talc varies with Dy 3+ Doping concentration variation diagram;

[0014] (5) Figure 5 Dy prepared in the present invention 3+ Fluorescence lifetime spectrum of high-performance luminescent glass based on doped black talc and its relationship with Dy 3+ Doping concentration variation diagram. DETAILED DESCRIPTION

[0015] The present invention is further described below with reference to the embodiments, but the protection scope of the present invention should not be limited thereto.

[0016] A kind of Dy 3+ The method for preparing high-performance luminescent glass based on doped black talc comprises the following steps:

[0017] (1) Mix black talc, Na2O and Dy2O3 in a ceramic mortar according to a pre-designed raw material mass ratio, and put them into an Al2O3 crucible to obtain a batch material. The mass percentage of each component is: black talc (80%), Na2O (20%), Dy2O3 (1-4%);

[0018] (2) placing the batch material in a high-temperature muffle furnace and melting it at 1600° C. for 2 hours to obtain a uniform glass melt;

[0019] (3) The glass melt is poured onto a preheated stainless steel mold and placed in a low-temperature muffle furnace for annealing at 680° C. for 10 hours to release the stress in the melt. The annealing furnace is cooled to room temperature to obtain a black talc-based luminescent glass product.

[0020] Example 1

[0021] The three raw materials of black talc, Na2O and Dy2O3 are mixed evenly in a ceramic mortar according to the pre-designed raw material mass ratio, and loaded into an Al2O3 crucible to obtain a batch material. The mass percentage of each component is: black talc (80%), Na2O (20%), and Dy2O3 (1%). The batch material is placed in a high-temperature muffle furnace and melted at 1600°C for 2 hours to obtain a uniform glass melt. The glass melt is poured onto a preheated stainless steel mold and placed in a low-temperature muffle furnace for annealing at 680°C for 10 hours to release the stress in the melt. The annealing furnace is cooled to room temperature to obtain a black talc-based luminescent glass product, the relative value of which is 87.7% of the fluorescence intensity, and the value of the fluorescence lifetime is 0.958ms. The Dy prepared in this embodiment 3+ The photoexcitation and emission spectra of ion-doped black talc-based luminescent glass products are shown in the attached Figure 2 The excitation spectrum contains multiple excitation peaks at 324, 350, 364, and 387 nm. This is due to the fact that Dy 3+ Ionic 6 H 15 / 2 Ground state to 6 P 3 / 2 , 9 P 7 / 2 , 4 P 5 / 2 ,and 4 I 13 / 2 The strong excitation band in the wavelength range of 300 to 400 nm indicates that Dy 3+ The ion-doped black talc-based luminescent glass can be effectively excited by near-ultraviolet light. Under the excitation of ultraviolet light with an optimal wavelength of 350nm, the emission spectrum contains three narrow emission bands at 483, 576 and 673nm, corresponding to Dy 3+ Ionic 4 F 9 / 2 - 6 H 15 / 2 (blue emission), 6 H 13 / 2 (yellow emission) and 6 H 11 / 2 (red emission) transition, the luminescent color is in the warm white light region, and can be used to prepare lighting or display devices using near-ultraviolet light as the excitation light source.

[0022] Example 2

[0023] The three raw materials of black talc, Na2O and Dy2O3 are mixed uniformly in a ceramic mortar according to the pre-designed raw material mass ratio, and loaded into an Al2O3 crucible to obtain a batch material. The mass percentage of each component is: black talc (80%), Na2O (20%), and Dy2O3 (2%). The batch material is placed in a high-temperature muffle furnace and melted at a temperature of 1600°C for 2 hours to obtain a uniform glass melt. The glass melt is poured onto a preheated stainless steel mold and placed in a low-temperature muffle furnace for annealing at 680°C for 10 hours to release the stress in the melt. The annealing furnace is cooled to room temperature to obtain a black talc-based luminescent glass product, the relative value of the integrated intensity of its fluorescence emission is 100% and the value of the fluorescence lifetime is 0.858ms.

[0024] Example 3

[0025] The three raw materials of black talc, Na2O and Dy2O3 are mixed uniformly in a ceramic mortar according to the pre-designed raw material mass ratio, and loaded into an Al2O3 crucible to obtain a batch material. The mass percentage of each component is: black talc (80%), Na2O (20%), and Dy2O3 (3%). The batch material is placed in a high-temperature muffle furnace and melted at a temperature of 1600°C for 2 hours to obtain a uniform glass melt. The glass melt is poured onto a preheated stainless steel mold and placed in a low-temperature muffle furnace for annealing treatment at 680°C for 10 hours to release the stress in the melt. The annealing furnace is cooled to room temperature to obtain a black talc-based luminescent glass product, the relative value of the integrated intensity of its fluorescence emission is 95.1%, and the value of the fluorescence lifetime is 0.801ms.

[0026] Example 4

[0027] The three raw materials of black talc, Na2O and Dy2O3 are mixed uniformly in a ceramic mortar according to the pre-designed raw material mass ratio, and loaded into an Al2O3 crucible to obtain a batch material. The mass percentage of each component is: black talc (80%), Na2O (20%), and Dy2O3 (4%). The batch material is placed in a high-temperature muffle furnace and melted at a temperature of 1600°C for 2 hours to obtain a uniform glass melt. The glass melt is poured onto a preheated stainless steel mold and placed in a low-temperature muffle furnace for annealing treatment at 680°C for 10 hours to release the stress in the melt. The annealing furnace is cooled to room temperature to obtain a black talc-based luminescent glass product, the relative value of the integrated intensity of its fluorescence emission is 83.6%, and the value of the fluorescence lifetime is 0.759ms.

[0028] Table 1 Dy prepared in Examples 1-4 3+Fluorescence emission integrated relative intensity and fluorescence lifetime data of high performance luminescent glass based on doped black talc

[0029]

Claims

1. A Dy 3+ A method for preparing high-performance luminescent glass based on doped black talc, characterized in that: The steps are as follows: (1) Mix black talc, Na2O and Dy2O3 in a ceramic mortar according to a pre-designed mass ratio, and put them into an Al2O3 crucible to obtain a batch material. The mass percentage of each component is: black talc (80%), Na2O (20%), Dy2O3 (1-4%); (2) placing the batch material in a high-temperature muffle furnace and melting it at 1600° C. for 2 hours to obtain a uniform glass melt; (3) The glass melt is poured onto a preheated stainless steel mold and placed in a low-temperature muffle furnace for annealing at 680° C. for 10 hours to release the stress in the melt. The annealing furnace is cooled to room temperature to obtain a black talc-based luminescent glass product.

2. A Dy according to claim 1 3+ A method for preparing high-performance luminescent glass based on doped black talc, characterized in that: The raw materials include black talc, Na2O and Dy2O3.

3. A Dy according to claim 2 3+ A method for preparing high-performance luminescent glass based on doped black talc, characterized in that: The melting temperature is 1600℃ / 2h.

4. A Dy according to claim 2 3+ A method for preparing high-performance luminescent glass based on doped black talc, characterized in that: The annealing system is 680℃ / 10h.

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