Preparation method and luminescent glass capable of efficiently extracting size-controllable Ag nano particles under low-concentration AgNO3 doping condition

A technology of nanoparticles and luminescent glass, which is applied in the field of transparent luminescent glass, can solve the problems of uneven distribution of materials, harsh requirements of preparation process, unfavorable optical device design, etc., and achieve adjustable size distribution, simple annealing process and short time Effect

Inactive Publication Date: 2015-08-05
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

After the ion exchange process is completed, it still takes a long time (2-48h) heat treatment to precipitate Ag nanoparticles in the glass substrate. The preparation process of this method is complicated, and many control factors are required, and Ag nanoparticles are only precipitated on the glass surface. The overall distribution of the material is uneven, which greatly limits its application range
[0005] In order to solve the problems in the above method, it is reported in the literature that the heat treatment is carried out in a reducing atmosphere, and the reducing atmosphere is beneficial to the Ag in the glass matrix to a certain extent. + reduction, but the reducing atmosphere brings more stringent requirements and higher application costs to the preparation process
In addition, it has been reported in the literature that the introduction of Eu into the glass matrix 3+ It is beneficial to the precipitation of Ag nanoparticles, and the effect is remarkable, but the rare earth ion Eu 3+ It can emit light itself, which is not conducive to the design of other optical devices with specific requirements

Method used

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  • Preparation method and luminescent glass capable of efficiently extracting size-controllable Ag nano particles under low-concentration AgNO3 doping condition
  • Preparation method and luminescent glass capable of efficiently extracting size-controllable Ag nano particles under low-concentration AgNO3 doping condition
  • Preparation method and luminescent glass capable of efficiently extracting size-controllable Ag nano particles under low-concentration AgNO3 doping condition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) According to the following molar ratio ingredients:

[0038] Sample 1 (G1):

[0039] SiO 2 (66)% B 2 o 3 (8)%

[0040] Na 2 O(10)% NaF(8)%

[0041] SrF 2 (4)% YF 3 (4)%

[0042] Ag(0.1)%

[0043] (2) After fully grinding and mixing the two groups of ingredients in step (1), they are melted at 1450°C for 45 minutes under air atmosphere, pressed and annealed at 450°C for 2 hours to obtain silver-containing nano Particles of glass.

[0044] Its absorption spectrum is as figure 1As shown, there is a strong broadband plasmon resonance absorption peak at 415nm. Its TEM image as figure 2 As shown, it can be estimated that the average particle size of Ag nanoparticles precipitated in the glass is 25nm.

Embodiment 2

[0046] (1) According to the following molar ratio ingredients:

[0047] Sample 1 (G2):

[0048] SiO 2 (69)% B 2 o 3 (5)%

[0049] Na 2 O(10)% NaF(8)%

[0050] SrF 2 (8)%Ag(0.3)%

[0051] Sample 2 (G3):

[0052] SiO 2 (69)% B 2 o 3 (5)%

[0053] Na 2 O(10)% NaF(8)%

[0054] YF 3 (8)%Ag(0.3)%

[0055] (2) After fully grinding and mixing the two groups of batch materials in step (1), they are melted at 1500°C for 45 minutes in an air atmosphere, pressed and molded, and annealed at 450°C for 2 hours to obtain silver-containing nanoparticles. Granular glass, respectively named G2, G3.

[0056] Its absorption spectrum is as image 3 As shown, there is a broadband plasmon resonance absorption peak. Among them, the absorption peak intensity of G3 is much higher than that of G2, and the center position of the SPR peak is red-shifted from 417nm to 430nm, indicating that the size of Ag nanoparticles precipitated in G3 glass is larger than that in G2.

Embodiment 3

[0058] (1) According to the following molar ratio ingredients:

[0059] Sample 1 (G4):

[0060] SiO 2 (64)% B 2 o 3 (10)%

[0061] Na 2 O(6)% NaF(12)%

[0062] YF 3 (8)%Ag(0.2)%

[0063] Sample 2 (G5):

[0064] SiO 2 (64)% B 2 o 3 (10)%

[0065] Na 2 O(12)% NaF(6)%

[0066] YF 3 (8)%Ag(0.2)%

[0067] (2) After fully grinding and mixing the two groups of batch materials in step (1), they are melted at 1450°C for 45 minutes in an air atmosphere, pressed and formed, and annealed at 400°C for 2 hours to obtain silver-containing nanoparticles. Granular glass, respectively named G4, G5.

[0068] Its absorption spectrum is as Figure 4 As shown, there is a broadband plasmon resonance absorption peak centered at 425 nm. Among them, the absorption peak intensity of G4 is greater than that of G5, indicating that in F - / O 2 -The average particle size of Ag nanoparticles precipitated in G4 glass with a higher proportion is larger than that in G5.

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Abstract

The invention discloses a preparation method and luminescent glass capable of efficiently extracting size-controllable Ag nano particles under a low-concentration AgNO3 doping condition. The luminescent glass is prepared from the following components in mole ratio: 60-70% of SiO2, 4-14% of B2O3, (18-x)% of X2O (X=Li / Na / K), x% of XF (X=Li / Na / K), y% of MF2 (M=Ca / Sr / Ba), (8-y)% of RF3 (R=Y / Gd) and 0.01-0.5% of Ag, wherein x is greater than zero and not greater than 1 and y is not smaller than zero and not greater than 6. The preparation method comprises the steps: firstly, weighing raw materials according to the mole ratio; secondly, smelting a sufficiently ground and uniformly mixed batch in the air; finally, pressing, molding and annealing, thereby obtaining glass containing Ag nano particles. The luminescent glass containing Ag nano particles has the characteristics of low initial AgNO3 doping content, adjustable size distribution of extracted Ag nano particles and no complex thermal treatment process; smelting and annealing are carried out in the air; cost is low and the luminescent glass has no pollution to the environment.

Description

technical field [0001] The invention relates to transparent luminescent glass, in particular to a low-concentration AgNO 3 A luminescent glass capable of effectively precipitating scale-controllable Ag nanoparticles under doping and a preparation method thereof. Background technique [0002] Nano-metal particles have unique physical and chemical properties such as quantum size effect and surface effect. Combining these metal nanoparticles with other types of materials can endow materials with new functions. Glass materials have excellent characteristics such as adjustable composition properties and stable chemical and physical properties, especially their excellent processing characteristics, such as being able to be processed into arbitrary block shapes, optical fibers, ultra-thin plates, etc., endowing glass materials with a wide range of applications. The combination of nano metal particles and glass materials has broad application prospects in the fields of communicatio...

Claims

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Application Information

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IPC IPC(8): C03C3/112C03C3/095C03C4/12
Inventor 叶松王慧云王德平周萘
Owner TONGJI UNIV
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