Preparation method of visible light absorption type upper conversion luminescent material

A luminescent material and absorption type technology, applied in the directions of luminescent materials, chemical instruments and methods, etc., can solve the problem of no up-conversion luminescent material research reports, etc., and achieve the effects of uniform size, uniform doping, and simple process

Inactive Publication Date: 2010-07-14
NORTHWEST UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Nano-TiO doped with rare earth has not been found so far 2 Related

Method used

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  • Preparation method of visible light absorption type upper conversion luminescent material
  • Preparation method of visible light absorption type upper conversion luminescent material
  • Preparation method of visible light absorption type upper conversion luminescent material

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preparation example Construction

[0039] The preparation of solutions B and E can be carried out at the same time. After 6-7 hours, slowly add solution E to solution B dropwise, and then stir at room temperature for another 2 hours to obtain solution F;

[0040] Aging the solution F to obtain the sol, drying the sol in a vacuum drying oven at 50-100°C to obtain a xerogel, after grinding, and then calcining at 200-500°C for about 2 hours, the heating rate is 10°C / min, and finally Grinding to obtain up-conversion powder luminescent material.

[0041] The present invention can also prepare up-conversion thin-film luminescent materials, and the specific method is as follows: the sol obtained in step 6 is used as a substrate with pre-treated clean glass or silicon wafers, and a film is formed by dipping and pulling method or spin coating method, and the thickness of the film is It can be adjusted by adjusting the pulling speed and the number of pulling times or the speed of the glue homogenizer; the wet film is dried...

Embodiment 1

[0043] Embodiment 1: Preparation Y 2 o 3 :Er 3+ +TiO 2 up-conversion luminescent material

[0044] The raw materials used are as follows:

[0045] Tetra-n-butyl titanate: (Ti(OC 4 h 9 ) 4 )6.8ml

[0046] Butanol (C 4 h 9 OH) 7.4ml

[0047] Glacial acetic acid (CH 3 COOH) 4.6ml

[0048] nitric acid (HNO 3 ) 9.0ml

[0049] Yttrium oxide (Y 2 o 3 ) 0.7527g

[0050] Erbium oxide (Er 2 o 3 )0.2532g

[0051] refer to figure 2 As shown, the preparation process of this embodiment is as follows:

[0052] 1) Add 7.4ml of n-butanol to 6.8ml of tetra-n-butyl titanate, mix and stir for 0.5 hours to obtain solution A1;

[0053] 2) Slowly drop 4.6ml of glacial acetic acid into solution A1, stir at room temperature for 6 hours to obtain solution B1, and continue stirring;

[0054] 3) Add 1.8mol of diethanolamine to solution B1 as a catalyst, and continue stirring;

[0055] 4) Weigh 0.7527g of yttrium oxide and 0.2532g of erbium oxide into a beaker, add 9.0ml of nitric...

Embodiment 2

[0060] Embodiment 2: Preparation of NaYF 4 :Er 3+ +TiO 2 up-conversion luminescent material

[0061] The raw materials used are as follows:

[0062] Tetra-n-butyl titanate: (Ti(OC 4 h 9 ) 4 ) 6.8ml

[0063] Butanol (C 4 h 9 OH) 7.4ml

[0064] Glacial acetic acid (CH 3 COOH) 4.6ml

[0065] nitric acid (HNO 3 ) 9.0ml

[0066] Distilled water (H 2 O) 19.0ml

[0067] Sodium fluoride (NaF) 1.1200g

[0068] Yttrium oxide (Y 2 o 3 ) 0.7529g

[0069] Erbium oxide (Er 2 o 3 ) 0.3072g

[0070] refer to image 3 , the preparation process of the present embodiment is as follows:

[0071] 1) Add 7.4ml of n-butanol to 6.4ml of tetra-n-butyl titanate, mix and stir for 0.5 hours to obtain solution A2;

[0072] 2) slowly drop 4.6ml of glacial acetic acid into solution A2 to obtain solution B2, and continue stirring;

[0073] 3) Add 6.8 mol of diethanolamine as a catalyst to solution B2, and stir for 6 hours;

[0074] 4a) Weigh 0.7529g of yttrium oxide and 0.3072g of e...

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Abstract

The invention provides a preparation method of a visible light absorption type upper conversion luminescent material, which comprises the following steps: mixing N-butyl titanate and absolute ethyl alcohol or normal butanol for obtaining a solution A; continuously stirring the solution for 30 minutes; slowly dripping glacial acetic acid or ethanol or ethanol acetic acid or propanol acetic acid in the solution A; stirring the mixture at the room temperature to obtain a solution B; adding a proper amount of diethanolameine to be used as catalysts; stirring the materials for a period; dissolving one or two kinds of materials of yttrium oxide and rare earth compounds in nitric acid to obtain turbid liquid; stirring the turbid liquid to obtain a transparent clarified solution C; placing the transparent clarified solution C at the room temperature to be cooled; slowly dripping the solution C into the solution B which is stirred at a high speed to obtain a mixed solution G; continuously stirring the solution G for two hours; pouring the solution G into a culture dish for stilling standing and ageing for obtaining stable, uniform and transparent rose pink sol; and obtaining the upper conversion luminescent material through drying, grinding and calcining the sol.

Description

technical field [0001] The invention relates to the technical field of synthesis of rare earth luminescent materials, in particular to a preparation method of a rare earth doped up-conversion luminescent material that uses visible light as an excitation source and emits deep ultraviolet, ultraviolet and blue light. Background technique [0002] Rare earth ion-doped up-conversion luminescent materials have always been a hot topic in the field of rare earth luminescent materials. It has broad application prospects in optical storage, optical communication systems, night vision systems, biomarkers, three-dimensional displays and sensors. Rare-earth up-conversion luminescent materials are attracting attention because of the difficulty in preparing such materials and the variety of them. Among them, fluoride is a good upconversion matrix material due to its low phonon energy and strong solubility to rare earth ions, but due to the toxicity, corrosion, and poor chemical and mechan...

Claims

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Application Information

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IPC IPC(8): C09K11/78C09K11/85
Inventor 胡晓云叶岩溪刘恩周樊君
Owner NORTHWEST UNIV
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