Single-ion-Dy-doped bismuth-phosphate-based white-light-illuminating fluorescent powder and preparing method thereof
A bismuth phosphate-based hair, single ion technology, applied in the direction of luminescent materials, chemical instruments and methods, sustainable buildings, etc., to achieve the effects of high luminous intensity, simple process flow, and high crystallinity
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[0035] The preparation method of the present invention comprises the following steps:
[0036] (1)Bi(NO 3 ) 3 ·5H 2 O, Dy(NO 3 ) 3 ·6H 2 O and 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;
[0037] (2) Take step 1) spare Bi(NO 3 ) 3 ·5H 2 O and Dy(NO 3 ) 3 ·6H 2 Mix O powder, 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, and stir to form Bi 0.95 NO 3 : 0.05Dy 3+ , 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, Dy(NO 3 ) 3 ·6H 2 O, nitric acid solution and NH 4 h 2 PO 4 The ratio is (4-x)mmol:xmmol:10mL:4mmol, x=0.1~0.3;
[0038] (3) adjusting the pH value of the mixed solution B ...
Embodiment 1
[0044] (1) Take (4-x)mmol of Bi(NO 3 ) 3 ·5H 2 O and 0.2mmol (0.091g) Dy(NO 3 ) 3 ·6H 2 O was mixed in a beaker, then dissolved in 10 mL of nitric acid solution with a volume fraction of 13%, and stirred magnetically for 15 minutes to obtain a mixed solution A;
[0045] (2) Weigh 4mmol of NH 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 , Dy(NO 3 ) 3 ·6H 2 O, nitric acid solution and NH 4 h 2 PO 4 The ratios are (4-x) mmol: x mmol: 10 mL: 4 mmol, x = 0.1, 0.2 and 0.3.
[0046] (3) Adjust the pH of the mixed solution B to 1.00 with dilute nitric acid under stirring conditions to obtain a mixed solution C;
[0047] (4) Stir the above-mentioned mixed solution C for 60 min, transfer it to a stainless steel reaction kettle lined with polytetrafluoroeth...
Embodiment 2
[0055] (1) Take 3.8mmol (1.843g) Bi(NO 3 ) 3 ·5H 2 O and 0.2mmol (0.091g) Dy(NO 3 ) 3 ·6H 2 O was mixed in a beaker, then dissolved in 10 mL of nitric acid solution with a volume fraction of 13.4%, and magnetically stirred for 10 min to obtain a mixed solution A;
[0056] (2) Weigh 4mmolNH 4 h 2 PO 4 Dissolve in 16mL deionized water, stir for 20min to prepare 0.25mol / L NH 4 h 2 PO 4 Solution, it is added dropwise in the mixed solution A of step (1) gained, stirs 20min, guarantees that it mixes evenly, obtains mixed solution B; Wherein Bi(NO 3 ) 3 , Dy(NO 3 ) 3 ·6H 2 O, nitric acid solution and NH 4 h 2 PO 4 The ratio of 3.8mmol:0.2mmol:10mL:4mmol.
[0057] (3) Adjust the pH of the mixed solution B to 1.05 with dilute nitric acid under stirring conditions to obtain a mixed solution C;
[0058] (4) Stir the above mixed solution C for 40 min, transfer it to a stainless steel reaction kettle with a polytetrafluoroethylene lining, seal it, react at 185° C. for 12...
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