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Lithium ion doped bismuth phosphate samarium fluorescent powder and preparation method thereof

A technology of bismuth samarium phosphate and lithium ions, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of low luminous intensity and low crystallinity of phosphor powder, etc., achieve high luminous intensity, improve luminous performance, and high crystallinity Effect

Inactive Publication Date: 2017-05-10
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] So far, BiPO produced by existing synthetic methods 4 :Sm 3+ Phosphor powder has low crystallinity and low luminous intensity, and no one has proposed a simple and convenient method to enhance its luminescence

Method used

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  • Lithium ion doped bismuth phosphate samarium fluorescent powder and preparation method thereof
  • Lithium ion doped bismuth phosphate samarium fluorescent powder and preparation method thereof

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preparation example Construction

[0034] The preparation method of the present invention comprises the following steps:

[0035] (1)Bi(NO 3 ) 3 ·5H 2 O, Sm(NO 3 ) 3 ·6H 2 O, 0~1.0mmol LiNO 3 and 0.2~0.4mol / L NH 4 h 2 PO 4 solution, spare; where NH 4 h 2 PO 4 The solution is NH 4 h 2 PO 4 Add in deionized water, stir for 20-30 minutes to dissolve, set aside;

[0036] (2) Take step 1) spare Bi(NO 3 ) 3 ·5H 2 O, Sm(NO 3 ) 3 ·6H 2 O and 0~1.0mmol LiNO 3 Mix, dissolve it in a nitric acid solution with a volume fraction of 13% to 13.6%, and stir for 10 to 15 minutes to obtain a uniform mixed solution A, that is, the reaction generates Bi 0.95 NO 3 : 0.05Sm 3+ , Li + , and then add NH dropwise to the mixed solution A 4 h 2 PO 4 solution, continue to stir for 20 to 30 minutes until the reagent is fully dissolved to obtain a mixed solution B; where Bi(NO 3 ) 3 ·5H 2 O, Sm(NO 3 ) 3 ·6H 2 O, LiNO 3 , nitric acid solution and NH 4 h 2 PO 4 The ratio is 3.8mmol:0.2mmol:xmmol:10mL:4mmol...

Embodiment 1

[0049] (1) Take 3.8mmol (1.843g) Bi(NO 3 ) 3 ·5H 2 O, 0.2mmol (0.089g) Sm(NO 3 ) 3 ·6H 2 O and 0.1mmol (0.007g) LiNO 3 Put it into a beaker for mixing, then dissolve it in 10 mL of nitric acid solution with a volume fraction of 13%, and stir it magnetically for 15 minutes to obtain a mixed solution A;

[0050] (2) Weigh 4mmolNH 4 h 2 PO 4 Dissolve in 20mL deionized water, stir for 30min to prepare 0.2mol / L NH 4 h 2 PO 4 Solution, it is added dropwise in the mixed solution A of step (1) gained, stirs 30min, guarantees that it mixes evenly, obtains mixed solution B; Wherein Bi(NO 3 ) 3 , Sm(NO 3 ) 3 ·6H 2 O, LiNO 3 , nitric acid solution and NH 4 h 2 PO 4 The ratio is 3.8mmol:0.2mmol:0.1mmol:10mL:4mmol.

[0051] (3) Adjust the pH of the mixed solution B to 0.5 with dilute nitric acid under stirring conditions to obtain a mixed solution C;

[0052] (4) Stir the above-mentioned mixed solution C for 60 min, transfer it to a stainless steel reaction kettle lined...

Embodiment 2

[0060] (1) Take 3.8mmol (1.843g) Bi(NO 3 ) 3 ·5H 2 O, 0.2mmol (0.089g) Sm(NO 3 ) 3 ·6H 2 O and 0.2mmol (0.014g) LiNO 3 Put it into a beaker for mixing, then dissolve it in 10 mL of nitric acid solution with a volume fraction of 13%, and stir it magnetically for 15 minutes to obtain a mixed solution A;

[0061] (2) Weigh 4mmolNH 4 h 2 PO 4 Dissolve in 20mL deionized water, stir for 25min to prepare 0.2mol / L NH 4 h 2 PO 4 Solution, it is added dropwise in the mixed solution A of step (1) gained, stirs 30min, guarantees that it mixes evenly, obtains mixed solution B; Wherein Bi(NO 3 ) 3 , Sm(NO 3 ) 3 ·6H 2 O, LiNO 3 , nitric acid solution and NH 4 h 2 PO 4 The ratio of 3.8mmol:0.2mmol:0.2mmol:10mL:4mmol.

[0062] (3) Adjust the pH of the mixed solution B to 0.51 with dilute nitric acid under stirring conditions to obtain a mixed solution C;

[0063] (4) Stir the above mixed solution C for 60 min, transfer it to a stainless steel reactor with a polytetrafluoro...

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Abstract

The invention relates to a lithium ion doped bismuth phosphate samarium fluorescent powder and a preparation method thereof. The preparation method comprises the following steps: firstly, mixing solid powder of Bi(NO3)3*5H2O, Sm(NO3)3*6H2O and LiNO3, adding into a nitric acid solution, uniformly stirring to react to generate Bi0.95NO3:0.05Sm<3+> and Li<+>, further dropping a NH4H2PO4 solution into the solution, continuously stirring until the NH4H2PO4 solution is sufficiently dissolved, adjusting the pH value of a mixed solution B to be 0.50-0.55, performing reaction on the mixed solution at a temperature of 180-185 DEG C to generate precipitate, when the precipitate is not increased, naturally cooling to the room temperature, performing centrifugal separation on the obtained precipitate, washing and drying, and finally obtaining the lithium ion doped bismuth phosphate samarium fluorescent powder. The structure and the lighting property of a product can be affected by adjusting the addition amount of LiNO3, and the prepared fluorescent powder is high in crystallization degree and high in lighting intensity.

Description

[0001] 【Technical field】 [0002] The invention relates to the field of rare earth luminescent materials, and relates to a lithium ion-doped bismuth samarium phosphate fluorescent powder and a preparation method thereof. [0003] 【Background technique】 [0004] Rare earth luminescent materials occupy a very important position in the whole field of solid state luminescence, because the special electron layer structure makes rare earth elements have incomparable properties of general elements. In recent years, rare earth phosphates have been widely used in the fields of lighting, quantum optics, color TV and thermoluminescence detection because of their advantages such as strong absorption capacity, high luminous brightness, and moderate synthesis temperature, which has aroused extensive interest of scientific researchers. Therefore, finding a method for rare earth phosphates with simple production process, multifunctional products and special morphology is of great value in both...

Claims

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Application Information

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IPC IPC(8): C09K11/74C09K11/81
CPCC09K11/7759
Inventor 刘运马随艳赵敏竹刘丁菡王凯
Owner SHAANXI UNIV OF SCI & TECH