Sm < 3 + >-doped black talc-based luminescent glass and preparation method thereof

Abstract

The invention discloses Sm < 3 + >-doped black talc-based luminescent glass and a preparation method thereof, the main raw material is selected from a specific mineral resource black talc in Guangfeng District of Shangjiao City, Jiangxi Province, and the luminescent glass is characterized by comprising the following chemical components: 90wt% of black talc, 10wt% of Na2O and 0.5-4wt% of Sm < 3 + >. The three raw materials are weighed according to the proportion, are uniformly mixed, and are melted in a high-temperature muffle furnace at 1600 DEG C for 2 hours to obtain a glass melt. The glass melt is placed in a muffle furnace at 680 DEG C for 2 h of annealing treatment, and after the glass melt is cooled to the room temperature, the Sm < 3 + > doped black talc-based luminescent glass is obtained. The prepared luminescent glass has three obvious emission peaks at 564 nm, 600 nm and 647 nm under excitation of near ultraviolet light with the wavelength of 403 nm, the strongest emission peak is located at 600 nm, the emission spectrum is mainly orange red light, the luminescent glass can be applied to white light LED devices, the preparation method is simple, and industrial production is facilitated.

Description

Technical Field

[0001] The present invention belongs to the field of inorganic photoelectric materials, and specifically relates to a Sm 3+ Doped black talc-based luminescent glass and preparation method thereof. Background Art

[0002] In recent years, inorganic luminescent glass has been widely reported in inorganic optoelectronic materials. On the one hand, the special melting preparation process of glass provides good conditions for the uniform dispersion of rare earth ions in the glass structure; on the other hand, the thermal / chemical stability and light loss of inorganic luminescent glass are more obvious than those of phosphors. Therefore, inorganic luminescent glass effectively solves the problems of reduced service life and lighting quality of LED phosphor devices, and has attracted widespread attention from researchers at home and abroad.

[0003] The black talc in Guangfeng District, Shangrao City, Jiangxi Province mainly includes SiO 2 MgO, K 2 O and CaO are small amounts of chemical components. From the perspective of chemical composition, black talc has the potential to synthesize silicate glass. Therefore, this application uses black talc as the main raw material and dopes a small amount of Sm 3+ , synthesized inorganic luminescent glass material. The fluorescence emission spectrum of this material is in the orange-red light region 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 realize the high value utilization of black talc and provide a Sm 3+ A method for preparing black talc-doped luminescent glass.

[0005] The Sm 3+ The doped black talc-based luminescent glass and the preparation method thereof specifically comprise the following steps:

[0006] (1) 90 wt% black talc, 10 wt% Na 2 O and 0.5-4wt% Sm 2 O 3 Mix well in a ceramic mortar to obtain a batch material;

[0007] (2) Pour the batch material into Al 2 O 3 The crucible was placed in a high-temperature muffle furnace and melted at 1600°C for 2 hours to obtain a uniform glass melt;

[0008] (3) The glass melt is poured onto a preheated stainless steel mold and placed in a muffle furnace at 680°C for annealing for 10 hours. The annealing furnace is cooled to room temperature to obtain Sm 3+ Doped black talc-based luminescent glass. BRIEF DESCRIPTION OF THE DRAWINGS

[0009] Figure 1 0.5wt% Sm 3+ XRD pattern of doped black talc-based luminescent glass;

[0010] Figure 2 2.5wt% Sm 3+ Actual picture of doped black talc-based luminescent glass under UV light / natural light;

[0011] Figure 3 The different contents of Sm in the present invention 3+ Fluorescence excitation and emission spectra of doped black talc-based luminescent glass;

[0012] Figure 4 The different contents of Sm in the present invention 3+ Fluorescence emission intensity spectrum of doped black talc-based luminescent glass;

[0013] Figure 5 The different contents of Sm in the present invention 3+ Fluorescence lifetime spectrum of doped black talc-based luminescent glass. DETAILED DESCRIPTION

[0014] 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.

[0015] A Sm 3+ Doped black talc-based luminescent glass and preparation method thereof, the steps are as follows:

[0016] (1) 90 wt% black talc, 10 wt% Na 2 O and 0.5-4wt% Sm 2 O 3 Mix well in a ceramic mortar to obtain a batch material;

[0017] (2) Pour the batch material into Al 2 O 3 The crucible was placed in a high-temperature muffle furnace and melted at 1600°C for 2 hours to obtain a uniform glass melt;

[0018] (3) The glass melt is poured onto a preheated stainless steel mold and placed in a muffle furnace at 680°C for annealing for 10 hours. The annealing furnace is cooled to room temperature to obtain Sm 3+ Doped black talc-based luminescent glass.

[0019] Example 1

[0020] 90wt% black talc, 10wt% Na 2 O and 0.5wt% Sm 2 O3 Mix well in a ceramic mortar to obtain a batch material. Pour the batch material into Al 2 O 3 The crucible was placed in a high-temperature muffle furnace and melted at 1600°C for 2 hours to obtain a glass melt. The glass melt was poured onto a preheated stainless steel mold and placed in a low-temperature muffle furnace at 680°C for annealing for 10 hours. The annealing furnace was cooled to room temperature to obtain a black talc-based luminescent glass product, the relative value of the integrated intensity of the fluorescence emission was 82.1%, and the value of the fluorescence lifetime was 2.465ms. Figure 2 Characteristic absorption peaks can be observed at 344nm, 361nm, 373nm and 403nm in the excitation spectrum, which are attributed to Sm 3+ from 6 H 5 / 2 To 4 H 9 / 2 , 4 D 3 / 2 , 4 D 1 / 2 and 4 F 7 / 2 The transition of Sm 3+ At 403nm 6 H 5 / 2 → 4 F 7 / 2 The transition of is dominant and can be used as the optimal excitation wavelength. The strongest excitation peak at 403nm matches well with the output wavelength of commercial NUV-LED based on InGaN. Figure 2 The emission peaks in the emission spectrum are located at 563nm, 600nm, 647nm and 710nm, corresponding to Sm 3+ of 4 G 5 / 2 → 6 H 5 / 2 , 4 G 5 / 2 → 6 H 7 / 2 , 4 G 5 / 2 → 6 H 9 / 2 and 4 G 5 / 2 → 6 H 11 / 2 The orange-red light emitted at 600nm is the strongest. In the field of solid-state lighting and display, it can be used as orange-red fluorescent glass for warm white light LEDs, and can also be directly used as luminescent glass for color light sources.

[0021] Example 2

[0022] 90wt% black talc, 10wt% Na2 O and 1.25wt% Sm 2 O 3 Mix well in a ceramic mortar to obtain a batch material. Pour the batch material into Al 2 O 3 The crucible was placed in a high-temperature muffle furnace and melted at 1600°C for 2 hours to obtain a glass melt. The glass melt was poured onto a preheated stainless steel mold and placed in a low-temperature muffle furnace at 680°C for annealing for 10 hours. The annealing furnace was cooled to room temperature to obtain a black talc-based luminescent glass. The relative value of the integrated intensity of its fluorescence emission was 86.9%, and the value of the fluorescence lifetime was 2.321ms.

[0023] Example 3

[0024] 90wt% black talc, 10wt% Na 2 O and 2.5wt% Sm 2 O 3 Mix well in a ceramic mortar to obtain a batch material. Pour the batch material into Al 2 O 3 The crucible was placed in a high-temperature muffle furnace and melted at 1600°C for 2 hours to obtain a glass melt. The glass melt was poured onto a preheated stainless steel mold and placed in a low-temperature muffle furnace at 680°C for annealing for 10 hours. The annealing furnace was cooled to room temperature to obtain a black talc-based luminescent glass. The relative value of the integrated intensity of its fluorescence emission was 100%, and the value of the fluorescence lifetime was 2.001ms.

[0025] Example 4

[0026] 90wt% black talc, 10wt% Na 2 O and 4wt% Sm 2 O 3 Mix well in a ceramic mortar to obtain a batch material. Pour the batch material into Al 2 O 3 The crucible was placed in a high-temperature muffle furnace and melted at 1600°C for 2 hours to obtain a glass melt. The glass melt was poured onto a preheated stainless steel mold and placed in a low-temperature muffle furnace at 680°C for annealing for 10 hours. The annealing furnace was cooled to room temperature to obtain a black talc-based luminescent glass. The relative value of the integrated intensity of its fluorescence emission was 56.7%, and the value of the fluorescence lifetime was 1.829ms.

[0027] Table 1 Sm prepared in Examples 1-4 3+ Integrated relative intensity and fluorescence lifetime data of fluorescence emission of doped black talc-based luminescent glass

[0028]

Claims

1. A Sm 3+ Doped black talc-based luminescent glass and preparation method thereof, characterized in that: The steps are as follows: (1) black talc, Na2O and Sm2O3 are mixed uniformly in a ceramic mortar according to a pre-designed mass ratio (black talc: 90wt%, Na2O: 10wt%, Sm2O3: 0.5-4wt%), and the mixture is placed in an Al2O3 crucible to obtain a batch material; (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 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 the black talc-based luminescent glass.

2. A Sm according to claim 1 3+ Doped black talc-based luminescent glass and preparation method thereof, characterized in that: The main raw material is black talc.

3. A Sm according to claim 2 3+ A method for preparing doped black talc-based luminescent glass, characterized in that: The melting temperature is 1600℃ / 2h, and the annealing temperature is 680℃ / 10h.

4. A Sm according to claim 2 3+ A method for preparing doped black talc-based luminescent glass, characterized in that: The doping amount of Sm2O3 is 0.5-4wt%.

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