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1064nm lead fluoride based up-conversion luminescence material and preparation method thereof

A technology of luminescent materials and lead fluoride, which is applied in the direction of luminescent materials, chemical instruments and methods, etc., can solve the problems of poor chemical stability and mechanical strength, and achieve the effect of loosening the requirements of the preparation equipment and process and reducing the preparation cost

Inactive Publication Date: 2014-01-22
CHANGCHUN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, as an up-conversion luminescent material, the matrix is ​​also required to have better chemical stability and higher mechanical strength. Compared with inorganic substances such as oxides and fluorides, the organic dyes have lower chemical stability and higher mechanical strength. poor strength

Method used

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  • 1064nm lead fluoride based up-conversion luminescence material and preparation method thereof
  • 1064nm lead fluoride based up-conversion luminescence material and preparation method thereof
  • 1064nm lead fluoride based up-conversion luminescence material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1. Calculate according to the stoichiometric ratio and weigh 0.191g Er 2 o 3 and 1.773gYb 2 o 3 , and put it into a beaker; weigh 2.25ml of nitric acid with a concentration of 8mol / L, add Er 2 o 3 and Yb 2 o 3 In a beaker, the beaker is placed on a heating magnetic stirrer, and Er(NO 3 ) 3 and Yb(NO 3 ) 3 solution.

[0023] 2. Dissolve 8.928gPb(NO 3 ) 2 , to get Pb(NO 3 ) 2 solution.

[0024] 3. Weigh 4.115g of NaF, add deionized water, place it on a magnetic stirrer, stir and dissolve to obtain NaF solution, drop a drop of nitric acid to accelerate the dissolution.

[0025] 4. Mix the solutions obtained in step 1 and step 2, place the formed mixed solution on a magnetic stirrer and stir for 10 minutes, and adjust the pH value to 2.5; add the solution obtained in step 3 to the mixed solution and stir for 1 Hours, the fluorides of the reaction raw materials Yb, Er, and Pb are obtained through the reaction, and the various fluorides exist in the solution i...

Embodiment 2

[0032] 1. Calculate according to the stoichiometric ratio and weigh 0.191g Er 2 o 3 and 1.773gYb 2 o 3 , and put it into a beaker; weigh 2.25ml of nitric acid with a concentration of 8mol / L, add Er 2 o 3 and Yb 2 o 3 In a beaker, the beaker is placed on a heating magnetic stirrer, and Er(NO 3 ) 3 and Yb(NO 3 ) 3 solution.

[0033] 2. Dissolve 11.923gPb(NO 3 ) 2 and 1.045gBa(NO 3 ) 2 , to get Pb(NO 3 ) 2 solution and Ba(NO 3 ) 2 solution.

[0034] 3. Weigh 4.115g of NaF, add deionized water, place it on a magnetic stirrer, stir and dissolve to obtain NaF solution, drop a drop of nitric acid to accelerate the dissolution.

[0035] 4. Mix the solutions obtained in step 1 and step 2, place the formed mixed solution on a magnetic stirrer and stir for 10 minutes, and adjust the pH value to 2.5; add the solution obtained in step 3 to the mixed solution and stir for 1 Hours, the reaction raw materials Yb, Er, Pb fluoride and Ba fluoride are obtained through the rea...

Embodiment 3

[0042] 1. Weigh 3.941gYb 2 o 3 and 0.383gEr 2 o 3 , put them into beakers respectively; weigh 7.5ml and 0.75ml of nitric acid respectively, and add 2 o 3 and Er 2 o 3 Put it in a beaker with a heating magnetic stirrer to make it fully react, and finally obtain a transparent solution.

[0043] 2. Pour the two solutions into plastic cups respectively, and then add an excess of 40.0% analytically pure hydrofluoric acid to it to fully react.

[0044] 3. Put the substance obtained in step 2 into a centrifuge for separation, then pour off the liquid in the upper layer, add deionized water to stir, and then separate twice.

[0045] 4. Transfer the substance obtained in step 3 to a clean beaker, and dry it in an oven at 120°C for 10 hours to obtain ErF 3 and YbF 3 block samples.

[0046] 5. Weigh 7.013gBaF according to the stoichiometric ratio 2 , 1.035gYbF 3 , 0.112gErF 3 , 16%NaF, 8%Na 2 SiF 6 , put it into an agate mortar, grind it repeatedly to make it evenly mixed,...

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Abstract

The invention relates to a 1064nm lead fluoride based up-conversion luminescence material and a preparation method thereof, and belongs to the technical field of luminescence materials. Present fluoride up-conversion luminescence materials are only responsive to 980nm light. The 1064nm lead fluoride based up-conversion luminescence material is characterized in that the general formula of the 1064nm lead fluoride based up-conversion luminescence material is (Pb1-xMx)F2:Er<3+>,Yb<3+>, M is one of Ca, Sr and Ba, x is not greater than 0 and is less than 1, and the 1064nm lead fluoride based up-conversion luminescence material can be excited by 1064nm wavelength light and can emit 551nm wavelength light. The preparation method of the up-conversion luminescence material is a high temperature solid phase method, reaction raw materials comprise fluorides of Yb and Er or comprise the fluorides of Yb and Er and a fluoride of one of Ca, Sr and Ba, and also comprise a fluoride of Pb, and the preparation method comprises the following steps: processing all the reaction raw materials to prepare a (Pb1-xMx)F2:Er<3+>,Yb<3+> precursor, wherein M is one of Ca, Sr and Ba, and x is not greater than 0 and is less than 1; carrying out grinding mixing of the precursor and a fusing assistant NaF to obtain a sintering material base; and putting the sintering material base in a crucible with the bottom spread with a layer of Na2SiF6, and carrying out a high temperature solid phase reaction in an open space to obtain the (Pb1-xMx)F2:Er<3+>,Yb<3+> target product.

Description

technical field [0001] The invention relates to a 1064nm lead fluoride-based up-conversion luminescent material and a preparation method thereof, which can be effectively excited by 1064nm infrared light and emit visible light, and belong to the technical field of luminescent materials. Background technique [0002] Among photoluminescent materials, up-conversion luminescent materials can absorb long-wave radiation with low photon energy and emit short-wave radiation with high photon energy, which belongs to the anti-Stokes effect, that is, the radiated energy is greater than the absorbed energy. This feature can further develop the function of infrared detectors with poor long-wave sensitivity, so up-conversion luminescent materials can be used as display materials for infrared light, such as night vision system materials, infrared quantum counters, up-conversion lasers, three-dimensional display, anti-counterfeiting identification etc. [0003] The up-conversion luminesce...

Claims

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Application Information

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IPC IPC(8): C09K11/66C09K11/61
Inventor 柏朝晖张希艳孙海鹰钱静娴刘全生卢利平米晓云王晓春王能利
Owner CHANGCHUN UNIV OF SCI & TECH
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