Dual mode luminous rare earth doped cerium fluoride nano crystal, preparation method and surface modification method thereof

A rare earth doping, cerium fluoride technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of single surface polarity modification of fluorescent material nanocrystal morphology, single luminescence wavelength, and difficulty in meeting application requirements.

Inactive Publication Date: 2010-06-16
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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Problems solved by technology

However, the rare earth-doped fluorescent material must be single-excited (up-converted excitation) under 980nm laser light, and there is a problem of a single luminescent wavelength.
In addition, the fluorescent material nanocrystals prepared in this patent have a single morphology and surface polarity modification also have certain limitations, making it difficult to meet the needs of various current applications.

Method used

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  • Dual mode luminous rare earth doped cerium fluoride nano crystal, preparation method and surface modification method thereof
  • Dual mode luminous rare earth doped cerium fluoride nano crystal, preparation method and surface modification method thereof
  • Dual mode luminous rare earth doped cerium fluoride nano crystal, preparation method and surface modification method thereof

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preparation example Construction

[0032] According to another embodiment of the present invention, a method for preparing rare earth-doped cerium fluoride nanocrystals with dual-mode light emission is provided, wherein the chemical composition formula of the rare earth-doped cerium fluoride nanocrystals is Ce 0.74 f 3 : 0.2Yb / xTm / (0.06-x) Tb, x=0.01-0.05, described method comprises the following steps:

[0033]a) According to the chemical composition formula, respectively weigh ytterbium oxide, thulium oxide and terbium oxide in a stoichiometric ratio, and dissolve them with concentrated nitric acid, and weigh cerium nitrate in a stoichiometric ratio, and heat and dissolve them in water to obtain the rare earth ions solution, the rare earth ion is an ion in its stable form.

[0034] b) According to the chemical composition formula, weigh the fluoride salt with a stoichiometric excess of less than 5%, and dissolve it in water to obtain a fluoride ion solution. In this step, preferably less than 5% excess fluo...

Embodiment 1

[0051] Embodiment 1: prepare Ce 0.74 f 3 :0.2Yb / 0.05Tm / 0.01Tb nanoparticles

[0052] Measure 1850 μl of the above-prepared Ce(NO 3 ) 3 solution (0.2M), 500 μl of Yb(NO 3 ) 3 solution (0.2M), 125 μl of the Tm(NO 3 ) 3 solution (0.2M) and 25 μl of Tb(NO 3 ) 3 Mix the solution (0.2M) evenly, add 10ml of aqueous solution containing 0.75g KOH, 15ml of absolute ethanol, and 10ml of oleic acid and stir vigorously until transparent, and add a slight excess of 2ml of KF solution, a white emulsion appears quickly and stir thoroughly for 15 Minutes, immediately put the mixed homogeneous emulsion into a 50ml hydrothermal reaction kettle, react at a temperature of 180°C for 8 hours, then cool the completed sample to room temperature, centrifuge, and wash with absolute ethanol / cyclohexane, The residue was removed and dispersed with cyclohexane.

[0053] Ce prepared in this example 0.74 f 3 : The XRD diffraction patterns of 0.2Yb / 0.05Tm / 0.01Tb nanocrystals are as follows figure ...

Embodiment 2

[0054] Embodiment 2: preparation Ce 0.73 f 3 :0.2Yb / 0.03Tm / 0.03Tb nanorods

[0055] Measure 1850 μl of the above-prepared Ce(NO 3 ) 3 solution (0.2M), 500 μl Yb(NO 3 ) 3 solution (0.2M), 75 μl of Tm(NO 3 ) 3 solution (0.2M), 75 μl of Tb(NO 3 ) 3 Mix the solution (0.2M) evenly, add 10ml of aqueous solution containing 0.75g KOH, 15ml of absolute ethanol, and 10ml of oleic acid and stir vigorously until transparent, then add a slight excess of 2ml of KF solution, a white emulsion appears quickly and stir thoroughly for 15 minutes, Immediately put the mixed homogeneous emulsion into a 50ml hydrothermal reactor and react at 180°C for 24 hours. However, the sample after the reaction is cooled to room temperature, centrifuged, and washed with absolute ethanol / cyclohexane to remove the residue, and use cyclohexane dispersion.

[0056] Ce of the sample prepared in this embodiment 2 0.73 f 3 : The X-ray diffraction pattern of 0.2Yb / 0.03Tm / 0.03Tb is similar to figure 1 , sho...

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Abstract

The invention provides a dual mode luminous rare earth doped cerium fluoride nano crystal, a preparation method thereof and a surface modification method thereof. The rare earth doped cerium fluoride nano crystal has a chemical composition formula, namely Ce0.74F3:0.2Yb / xTm / (0.06-x)Tb, wherein x=0.01-0.05. The crystal can realize dual mode luminescence of up-conversion excitation and down-conversion excitation under conditions such as ultraviolet light and a 980nm infrared laser. In addition, the method can prepare the rare earth doped cerium fluoride nano crystal having different structural shapes by controlling technological conditions. Moreover, the surface of the prepared doped cerium fluoride nano crystal can be modified by a surfactant so as to meet various requirements in the technical fields of anti-counterfeiting, biological marking and the like.

Description

technical field [0001] The invention relates to the technical field of inorganic fluorescent materials. Specifically, the present invention relates to a rare-earth-doped cerium fluoride nanocrystal with dual-mode light emission, and its preparation and surface modification methods. Background technique [0002] At present, inorganic fluorescent materials have been widely used in lighting such as white light LEDs, anti-counterfeiting such as anti-counterfeiting inks, biomarkers such as bioprobes, electroluminescence, molecular electronics, lasers and scintillation counting technologies, and are an important class of functional materials. [0003] However, the rare earth-doped fluorescent materials currently used in technical fields such as anti-counterfeiting and biomarkers are mainly fluorescent materials with a single light emitting mode. For example, Chinese patent CN 101195747A discloses a red up-conversion fluorescent material NaY 1-x-y-z (Yb x Ho y Ce z ) F 4 (whe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85
Inventor 孙家跃杜海燕先建波夏志国
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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