Novel rare-earth/L type zeolite luminescent material and preparation method thereof

A luminescent material and zeolite technology, applied in luminescent materials, chemical instruments and methods, etc., can solve the problems of high preparation temperature, complex process, high energy consumption, etc., and achieve strong stability, strong application value, luminous intensity and stability. Enhanced effect

CN102174322AInactive Publication Date: 2011-09-07HEBEI UNIV OF TECH
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Publication Date
2011-09-07
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention belongs to the field of rare-earth functional materials, and particularly relates to a rare-earth / L type zeolite luminescent material and a preparation method thereof. The material consists of L type zeolite, rare-earth ion (Ln) and bismuth ion, wherein 0.0025 to 0.25mmol of the rare-earth ion and 100mg of zeolite are added, and the mole ratio of the rare-earth ion to the bismuth ion is (1 to 250):(40 to 1). The rare-earth ion (Ln) is Nd3<+>, Sm3<+>, Eu3<+>, Tb3<+>, Ho3<+>, Er3<+>, Yb3<+>, Tm3<+> or Dy3<+>. According to the preparation method, the luminous intensity and the stability of the rare-earth / L type zeolite are enhanced through simple ion exchange and baking processes, and the fluorescence lifetime is greatly improved compared with that of other rare-earth doped zeolite. For example, the excited state lifetime of the L type zeolite luminescent material doped with Eu3<+> is above 1.60ms, the stability is very strong at a high temperature, and remarkably dazzling characteristic glow can be emitted under the ultraviolet irradiation. Based on the characteristics, the rare-earth / L type zeolite luminescent material has strong application values in the aspects of plasma display, illumination, falsification prevention and the like.
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Description

technical field

[0001] The invention belongs to the field of rare earth functional materials, in particular to a rare earth / L-type zeolite luminescent material and a preparation method thereof. Background technique

[0002] Due to the unique 4f-layer electronic configuration, rare earth elements have potential application value in metallurgical industry, petrochemical industry, hydrogen storage, glass ceramics, permanent magnet materials, luminescent materials and other fields. Eu 3+ As the luminescence center of red phosphor, it shows good luminescence performance, often in the form of 5 D. 0 → 7 f 1，2 become the main jump. Eu-containing phosphors are commercially produced in large quantities, but the disadvantage is that they are expensive, so it is imperative to find cheap alternatives. However, the substitute must have good optical properties, such as high-efficiency absorption of ultraviolet light at 254nm, high quantum efficiency (>85%), and the like. [0003...

Examples

Embodiment 1

[0032] 1. be that the concentration nitric acid of 65%-68% is diluted into the dilute nitric acid of 2mol / L, dissolve bismuth nitrate pentahydrate crystal with it, be mixed with the Bi(NO of 0.04mol / L 3 ) 3 .5H 2 O solution.

[0033] 2. According to the volume ratio of 9:1, 0.1mol / L EuCl 3 .6H 2 O solution 2.25mL and 0.04mol / LBi(NO 3 ) 3 .5H 2 O solution 0.25mL and mix well.

[0034] 3. Weigh 100 mg of 64T (that is, 0.225 mmol of rare earth ions / 100 mg of zeolite), place it in the mixed solution, and perform ion exchange at a temperature of 80° C. Reflux for 24 hours.

[0035] 4. After the reaction, wash the product of step 3 three times with deionized water. After centrifugation, put it in an oven at 80°C to dry and set aside.

[0036] 5. Take out the dried product of Step 4, grind it, and place it in a tube-type resistance furnace for roasting. The heating rate was 2°C / min, raised to 700°C, and then kept for 1.5h. That is, a rare earth / L-type zeolite luminescent ...

Embodiment 2

[0042] Change the volume ratio of the second step in Example 1 to 8:2, that is, add 0.1mol / L of EuCl 3 .6H 2 O solution 2mL, 0.04mol / L Bi(NO 3 ) 3 .5H 2 O solution 0.5mL (ie 0.2mmol rare earth ion / 100mg zeolite). All the other processes are the same as in Example 1. Finally, a rare earth / L-type zeolite luminescent material (99.1 mg) was obtained.

[0043] Utilize fluorescence spectrum to carry out fluorescence monitoring to embodiment 2, monitor collection of illustrations such as figure 2 Shown:

[0044] Excitation spectrum (detection wavelength: 612nm): 200-480nm

[0045]Emission spectrum (excitation spectrum: 395nm): 611nm, 576nm, 591nm, 653nm, 703nm

[0046] Lifetime: 1.29ms

Embodiment 3

[0048] Change the volume ratio of the second step in Example 1 to 7:3, that is, add 0.1mol / L EuCl 3 .6H 2 O solution 1.75mL, 0.04mol / L Bi(NO 3 ) 3 .5H 2 O solution 0.75mL (ie 0.175mmol rare earth ion / 100mg zeolite). All the other processes are the same as in Example 1. Finally, a rare earth / L-type zeolite luminescent material (99.3 mg) was obtained.

[0049] Utilize fluorescence spectrum to carry out fluorescence monitoring to embodiment 3, monitor collection of illustrations such as image 3 Shown:

[0050] Excitation spectrum (detection wavelength: 612nm): 200-480nm

[0051] Emission spectrum (excitation spectrum: 395nm): 612nm, 578nm, 593nm, 653nm, 702nm

[0052] Lifetime: 1.72ms

[0053] And carried out the detection of scanning electron microscope to embodiment 3, wherein Figure 4a It is a scanning electron micrograph of a rare earth / L-type zeolite luminescent material with a magnification of 20000 times, and b is a scanning electron micrograph of a rare earth / ...