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Highly doped rare earth up-conversion fluorescent nano material and preparation method thereof

A technology for up-conversion of fluorescent nanomaterials and rare earths, applied in the direction of luminescent materials, chemical instruments and methods, etc., can solve problems such as reduction of luminous intensity, practicality and universality limitations, quenching, etc., to increase doping concentration and improve quenching The effect of killing concentration

Inactive Publication Date: 2017-04-26
CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

[0004] Obviously, increasing the doping concentration of rare earth ions in nanoparticles is expected to increase their luminous intensity, but we have noticed that in practical applications, the doping concentration of rare earth ions in the matrix is ​​still at a low level, generally only 2% ~5%, this is because the rare earth ions with high doping concentration are prone to strong cross-relaxation and concentration quenching effects, resulting in high doping concentration usually causing a decrease in luminous intensity
Although there are recent reports in the literature at very high power densities (10 6 W / cm 2 ) excitation, or in a special matrix structure (KYb 2 f 7 ), the quenching concentration of rare earth ions can be greatly improved, but these methods are still limited in practicability and universality. , is a very important practical requirement

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  • Highly doped rare earth up-conversion fluorescent nano material and preparation method thereof
  • Highly doped rare earth up-conversion fluorescent nano material and preparation method thereof
  • Highly doped rare earth up-conversion fluorescent nano material and preparation method thereof

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preparation example Construction

[0034] The present invention also provides a preparation method of the above-mentioned highly doped rare earth up-conversion fluorescent nano material, which includes the following steps:

[0035] A) Preparation of up-conversion nanoparticles doped with rare earth ions;

[0036] B) Shell-coating the nanoparticles obtained in step A).

[0037] The preparation of the above-mentioned up-conversion nanoparticles doped with rare earth ions is a technique well known to those skilled in the art. Specifically, the chloride-oleic acid precursor method or the trifluoroacetate decomposition method can be used.

[0038] Then, the prepared nanoparticles are added to the inert shell material, and the temperature is increased from 300°C to 330°C to form nanoparticles with a core-shell structure.

[0039] Take NaYF 4 Inert shell as an example,

[0040] The above step B) is specifically: adding YCl 3 .6H 2 O powder is dissolved in the mixed solution of oleic acid and 1-octadecene, and then mixed with the...

Embodiment 1

[0046] Er single doped 3+ NaYF 4 Preparation of the naked core of nanoparticles: ErCl in a certain proportion according to the doping concentration 3 ·6H 2 O and YCl 3 ·6H 2 O (the two are 1 millimoles, doped with Er 3+ Concentrations are 5%, 10%, 20%, 40%, 80%) The powder is placed in a 100ml three-necked flask, 6ml oleic acid and 15ml 1-octadecene liquid are added, and the temperature is raised to 155℃ under the protection of inert gas After dissolving completely, let it cool to room temperature naturally, and then drip into 6ml containing 100mg NaOH and 148mg NH 4 The methanol solution of F is fully stirred and then the temperature is raised to 70°C to remove the methanol, and then the temperature is gradually raised to 300-330°C under the protection of inert gas, the reaction is carried out for 90 minutes, and then it is naturally cooled to room temperature. Wash the resulting solution three times with acetone and ethanol by centrifugation, and disperse the remaining solid (a...

Embodiment 2

[0054] The preparation method of homogeneous core-shell structure nanoparticles: 152mg YCl 3 ·6H 2 Put the O powder in a 100ml three-necked flask, add 6ml of oleic acid and 15ml of 1-octadecene liquid, under the protection of inert gas, raise the temperature to 150℃ to make it completely dissolved, then cool to room temperature naturally, and then drop 4ml containing 75mg Er-doped prepared in Example 1 3+ NaYF 4 Naked core nanoparticles (Er doped 3+ Concentrations of 5%, 10%, 20%, 40%, 80%) in cyclohexane solution, slowly increase the temperature to 80°C to remove the cyclohexane, then cool to room temperature, drop 3ml containing 50mg NaOH and 74mg NH 4 The methanol solution of F is heated to 70°C to remove the methanol, and then gradually heated to 300-330°C under the protection of inert gas, reacted for 60 minutes, and then naturally cooled to room temperature. Wash the resulting solution three times with acetone and ethanol by centrifugation, and disperse the remaining solid ...

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Abstract

The invention provides a highly doped rare earth up-conversion fluorescent nano material. The highly doped rare earth up-conversion fluorescent nano material consists of rare earth ions-doped up-conversion nano-particles serving as a nuclear structure and a shell structure which coats the nuclear structure; the doping concentration of rare earth ions is greater than 5 percent. According to the highly doped rare earth up-conversion fluorescent nano material, the quenching concentration of the doped rare earth ions is improved by utilizing the shell layer, and the cross relaxation of the doped rare earth ions is reduced, so that the light intensity of the up-conversion nano-particles is further improved through a mode of effectively increasing the doping concentration of the rare earth ions in a light emitting centre. On the other hand, the emission intensity of each energy level of the rare earth ions can be effectively regulated by utilizing the strong cross relaxation produced by high doping; therefore, controllable multi-colour light emitting of the highly doped rare earth up-conversion fluorescent nano material is realized.

Description

Technical field [0001] The invention relates to the technical field of luminescent materials, in particular to a highly doped rare earth up-conversion fluorescent nano material and a preparation method thereof. Background technique [0002] Rare earth doped up-conversion fluorescent material is a fluorescent material that uses lanthanide ion doping to convert near-infrared light into visible light and ultraviolet light. It has a wide range of applications in solar energy utilization, data storage, three-dimensional display, biological tissue imaging and detection, and drug delivery. Taking the biological detection direction as an example, compared with traditional organic fluorescent dyes or semiconductor quantum dots, rare earth-doped upconversion materials have the advantages of low toxicity, high chemical stability, no photobleaching phenomenon, and long energy level life. Moreover, because its excitation wavelength can be located within the "optical window" of the human body...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85C09K11/02
CPCC09K11/7773C09K11/02
Inventor 刘晓敏孔祥贵张友林涂浪平常钰磊薛彬
Owner CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI
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