Process for preparing water-soluble up-conversion NaYF4:Er<3+>,Yb<3+> nano-crystalline using glycyl alcohol as solvent

A technology of glycerol and nanocrystals, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of easy particle aggregation, difficult size control, and reduced luminous efficiency, so as to avoid particle adhesion, particle size increase, The effect of improving dispersion

Inactive Publication Date: 2008-10-22
NORTHEAST DIANLI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Nano-ZrO 2 , Y 2 o 3 and other materials have attracted attention due to their low phonon energy, but at nanoscale, surface-adsorbed H 2 O and CO 2 Absorbing more excitation light energy reduces the luminous efficiency of the material; at the same time, these materials need to be sintered at more than 1000°C to crystallize, which consumes a lot of energy and the particles are prone to agglomeration, and the size is difficult to control

Method used

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  • Process for preparing water-soluble up-conversion NaYF4:Er&lt;3+&gt;,Yb&lt;3+&gt; nano-crystalline using glycyl alcohol as solvent
  • Process for preparing water-soluble up-conversion NaYF4:Er&lt;3+&gt;,Yb&lt;3+&gt; nano-crystalline using glycyl alcohol as solvent
  • Process for preparing water-soluble up-conversion NaYF4:Er&lt;3+&gt;,Yb&lt;3+&gt; nano-crystalline using glycyl alcohol as solvent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Preparation of upconverting NaYF 4 :Er 3+ , Yb 3+ The method of nanocrystal, reaction is 1h, and reaction temperature is 220 ℃, and n(EDTA) / n(RE) molar ratio is 1: 1, and wherein, n(EDTA) represents the total molar amount of ETDA, and n(RE) represents ( Y 3+ 、Er 3+ , Yb 3+ ) sum of molar consumption; It is made up of following process and steps:

[0037] 1) Take 1.05g NaF and put it into a conical flask, add 150ml glycerol and heat it with an electric furnace, stir while heating to make it all dissolve, and obtain solution A.

[0038] 2) Put 0.7445g of EDTA into a conical flask, add 50ml of glycerol and heat with an electric furnace, stir while heating to make it all dissolve, and obtain solution B.

[0039] 3) Weigh 0.0212g Er(NO 3 ) 3 , 0.1221g Yb(NO 3 ) 3 , 0.4198gY (NO 3 ) 3 Put it into the same Erlenmeyer flask, add 50ml glycerol and heat it with an electric furnace, stir while heating to make it all dissolve, and obtain solution C.

[0040] 4) Mix sol...

Embodiment 2

[0047] Preparation of upconverting NaYF 4 :Er 3+ , Yb 3+ For nanocrystals, the reaction time is 2h, n(EDTA) / n(RE)=1:1, and the reaction temperature is 220°C.

[0048] 1) Take 1.05g NaF and put it into a conical flask, add 150ml glycerol and heat it with an electric furnace, stir while heating to make it all dissolve, and obtain solution A.

[0049] 2) Put 0.7445g of EDTA into a conical flask, add 50ml of glycerol and heat with an electric furnace, stir while heating to make it all dissolve, and obtain solution B.

[0050] 3) Weigh 0.0212g Er(NO 3 ) 3 , 0.1221g Yb(NO 3 ) 3 , 0.4198gY (NO 3 ) 3 Put it into the same Erlenmeyer flask, add 50ml glycerol and heat it with an electric furnace, stir while heating to make it all dissolve, and obtain solution C.

[0051] 4) Mix solution A and solution B to obtain solution D, and transfer it into a three-necked flask.

[0052] 5) Add solution C to solution D, heat with an electric furnace, and stir with an electric stirrer while...

Embodiment 3

[0058] Preparation of upconverting NaYF 4 :Er 3+ , Yb 3+ For nanocrystals, the reaction time is 3 hours, n(EDTA) / n(RE)=1:1, and the reaction temperature is 220°C.

[0059] 1) Take 1.05g NaF and put it into a conical flask, add 150ml glycerol and heat it with an electric furnace, stir while heating to make it all dissolve, and obtain solution A.

[0060] 2) Put 0.7445g of EDTA into a conical flask, add 50ml of glycerol and heat with an electric furnace, stir while heating to make it all dissolve, and obtain solution B.

[0061] 3) Weigh 0.0212g Er(NO 3 ) 3 , 0.1221g Yb(NO 3 ) 3 , 0.4198gY (NO 3 ) 3 Put it into the same Erlenmeyer flask, add 50ml glycerol and heat it with an electric furnace, stir while heating to make it all dissolve, and obtain solution C.

[0062] 4) Mix solution A and solution B to obtain solution D, and transfer it into a three-necked flask.

[0063] 5) Add solution C to solution D, heat with an electric furnace, and stir with an electric stirrer ...

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Abstract

The invention relates to a method for making water-soluble upconversion NaYF4: Er<3+>, Yb<3+> nano crystal through taking glycerol propanetriol as solvent. The method is as follows: NaF is dissolved in glycerol propanetriol solvent to obtain a solution A, and then EDTA is dissolved in glycerol propanetriol to obtain a solution B; Er (NO3) 3, Yb (NO3) 3 and Y (NO3) 3 are dissolved in glycerol propanetriol solvent to obtain a solution C; the solution A and the solution B are mixed to obtain a solution D, and then the solution C is added in the solution D; moreover, n(EDTA) / n(RE) is equal to 1:0.5 to 1:5 (mol), wherein n(EDTA) is the total mol dosage of EDTA, while n(RE) is the sum of the mol dosage of Er<3+>, Yb<3+> and Y<3+>; the solutions are stirred to carry out reaction at the temperature of between 200 and 297 DEG C for 1 to 3 hours; and the product is excitated by 980nm infrared light after drying so as to make the bright fluorescence upconversion NaYF4: Er<3+>, Yb<3+> nano crystal apparent to the naked eye. The method obtains simplified process, energy conservation and improved water solubility.

Description

technical field [0001] The invention belongs to the preparation method of rare earth metal ion up-conversion luminescent material, specifically relates to a kind of using glycerol as solvent to prepare water-soluble up-conversion NaYF 4 :Er 3+ , Yb 3 + nanocrystal approach. Background technique [0002] Rare earth ion up-conversion luminescent materials have good application prospects in laser technology, optical fiber communication technology, fiber amplifier, display technology and anti-counterfeiting. Recently, the use of up-conversion materials as fluorescent labeling probes for biomolecules has attracted widespread attention. Up-conversion materials have the advantages of not being prone to photobleaching, high luminous intensity and low laser intensity, and can greatly improve detection sensitivity and linear range when used in labeling. [0003] As early as 1959, it was reported that 960nm infrared light was used to excite polycrystalline ZnS, and 525nm green emi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85
Inventor 贾若琨杨珊
Owner NORTHEAST DIANLI UNIVERSITY
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