Yttrium-cerium composite oxide-based up-conversion luminescent material and preparation method thereof

Abstract

In order to solve the problems that an oxide-based up-conversion luminescent material in the field of up-conversion luminescent materials has low luminous efficiency and luminescent intensity which cannot meet the practical application requirement, the invention provides an yttrium-cerium composite oxide-based up-conversion luminescent material and a preparation method thereof. The luminescent material has a chemical formula as Y(2-x-y)RExYbyCeO5, wherein x is larger than or equal to 0.0002 and smaller than or equal to 0.035, and y is larger than or equal to 0.01 and smaller than or equal to 0.25. The preparation method comprises the steps of adopting a sol-gel method for preparing a precursor, drying, grinding, calcining at 900 to 1300 DEG C for 1 to 4h, and obtaining a series of rare-earth-doped yttrium-cerium composite oxide-based up-conversion luminescent material. The luminescent material has the advantages of simple preparation process, small powder particle, single material phase, good chemical stability, high luminescent intensity under 980nm infrared light stimulation and the like, can meet the requirement of practical application fields such as anti-counterfeit technology, and has a wide application prospect.

Description

Technical field

[0001] The invention relates to a high luminous intensity yttrium-cerium composite oxide-based up-conversion luminescent material excited by 980nm infrared light and a preparation method thereof, and belongs to the field of luminescent materials. Background technique

[0002] Up-conversion luminescent material is an important luminescent material, which can convert long-wavelength excitation light into short-wavelength emission light through a multiphoton mechanism. Since the discovery of up-conversion in the 1960s, up-conversion has been extensively studied. Rare-earth ion-doped up-conversion luminescent materials are used in up-conversion lasers, fiber amplifiers, three-dimensional displays, anti-counterfeiting, infrared imaging, and biological detection. And other fields have broad application prospects.

[0003] Upconversion luminescent materials can be roughly classified into fluorides, oxides, sulfides, and oxyhalides according to different host components. ...

Examples

Embodiment 1

[0018] Preparation of Er by sol-gel method 3+ , Yb 3+ Double-doped yttrium-cerium composite oxide-based upconversion luminescent material Y 1.97 Er 0.01 Yb 0.02 CeO 5 , The specific operations are as follows:

[0019] Calculate the ratio of various raw materials according to the mole fraction of each metal element in the material composition. Weigh 3.2713g Ce(NO 3 ) 3 ·6H 2 O, 5.6865g Y(NO 3 ) 3 ·6H 2 O, 0.0334g Er(NO 3 ) 3 ·5H 2 O, 0.0698g Yb(NO 3 )·6H 2 Put O into the beaker, add 70mL of distilled water, stir to fully dissolve it to form a uniform mixed solution, add 8.692g of citric acid to the mixed solution and stir evenly, slowly add 2mol / L to the mixed solution at a certain speed under stirring Ammonia water reaches the pH value of the solution at 4 to 5 to make a transparent sol, and the beaker containing the sol is placed in a constant temperature water bath for gelation reaction. The gelation temperature is 60° C. and the time is 5 to 8 hours. After the gel is formed, p...

Embodiment 2

[0022] Preparation of Er by sol-gel method 3+ , Yb 3+ Double-doped yttrium-cerium composite oxide-based upconversion luminescent material Y 1.81 Er 0.01 Yb 0.18 CeO 5 ,details as follows:

[0023] Weigh 3.2713g Ce(NO 3 ) 3 ·6H 2 O, 5.2246g Y(NO 3 ) 3 ·6H 2 O, 0.0334gEr(NO 3 ) 3 ·5H 2 O, 0.6282g Yb(NO 3 )·6H 2 Put O into the beaker, and the remaining steps are the same as in Example 1.

[0024] image 3 Er 3+ , Yb 3+ Double-doped yttrium-cerium composite oxide-based upconversion luminescent material Y 1.81 Er 0.01 Yb 0.18 CeO 5 The up-conversion fluorescence spectrum of At room temperature, the powdered sample was irradiated with a 30mw 980nm semiconductor laser, and the bright red light was observed by naked eyes.

Embodiment 3

[0026] Preparation of Ho by sol-gel method 3+ , Yb 3+ Double-doped yttrium-cerium composite oxide-based upconversion luminescent material Y 1.945 Ho 0.005 Yb 0.05 CeO 5 , The specific operations are as follows:

[0027] Calculate the ratio of various raw materials according to the mole fraction of each metal element in the material composition. Weigh 3.4382g Ce(NO 3 ) 3 ·6H 2 O, 6.0661g Y(NO 3 ) 3 ·6H 2 O, 0.0175g Ho(NO 3 ) 3 ·5H 2 O, 0.1479g Yb(NO 3 ) 3 ·6H 2 Put O into the beaker, add 70mL of distilled water, stir to fully dissolve it to form a uniform mixed solution, add 8.692g of citric acid to the mixed solution and stir evenly, slowly add 2mol / L dropwise to the mixed solution at a certain speed under stirring conditions To make a transparent sol, the beaker containing the sol is placed in a constant temperature water bath for gelation reaction, the gelation temperature is 60°C, and the time is 5-8h. After the gel is formed, place it in an oven at 110°C and dry it for 12-18 ...

Technical field

[0001] The invention relates to a high luminous intensity yttrium-cerium composite oxide-based up-conversion luminescent material excited by 980nm infrared light and a preparation method thereof, and belongs to the field of luminescent materials. Background technique

[0002] Up-conversion luminescent material is an important luminescent material, which can convert long-wavelength excitation light into short-wavelength emission light through a multiphoton mechanism. Since the discovery of up-conversion in the 1960s, up-conversion has been extensively studied. Rare-earth ion-doped up-conversion luminescent materials are used in up-conversion lasers, fiber amplifiers, three-dimensional displays, anti-counterfeiting, infrared imaging, and biological detection. And other fields have broad application prospects.

[0003] Upconversion luminescent materials can be roughly classified into fluorides, oxides, sulfides, and oxyhalides according to different host components. ...

Examples

Embodiment 1

[0018] Preparation of Er by sol-gel method 3+ , Yb 3+ Double-doped yttrium-cerium composite oxide-based upconversion luminescent material Y 1.97 Er 0.01 Yb 0.02 CeO 5 , The specific operations are as follows:

[0019] Calculate the ratio of various raw materials according to the mole fraction of each metal element in the material composition. Weigh 3.2713g Ce(NO 3 ) 3 ·6H 2 O, 5.6865g Y(NO 3 ) 3 ·6H 2 O, 0.0334g Er(NO 3 ) 3 ·5H 2 O, 0.0698g Yb(NO 3 )·6H 2 Put O into the beaker, add 70mL of distilled water, stir to fully dissolve it to form a uniform mixed solution, add 8.692g of citric acid to the mixed solution and stir evenly, slowly add 2mol / L to the mixed solution at a certain speed under stirring Ammonia water reaches the pH value of the solution at 4 to 5 to make a transparent sol, and the beaker containing the sol is placed in a constant temperature water bath for gelation reaction. The gelation temperature is 60° C. and the time is 5 to 8 hours. After the gel is formed, p...

Embodiment 2

[0022] Preparation of Er by sol-gel method 3+ , Yb 3+ Double-doped yttrium-cerium composite oxide-based upconversion luminescent material Y 1.81 Er 0.01 Yb 0.18 CeO 5 ,details as follows:

[0023] Weigh 3.2713g Ce(NO 3 ) 3 ·6H 2 O, 5.2246g Y(NO 3 ) 3 ·6H 2 O, 0.0334gEr(NO 3 ) 3 ·5H 2 O, 0.6282g Yb(NO 3 )·6H 2 Put O into the beaker, and the remaining steps are the same as in Example 1.

[0024] image 3 Er 3+ , Yb 3+ Double-doped yttrium-cerium composite oxide-based upconversion luminescent material Y 1.81 Er 0.01 Yb 0.18 CeO 5 The up-conversion fluorescence spectrum of At room temperature, the powdered sample was irradiated with a 30mw 980nm semiconductor laser, and the bright red light was observed by naked eyes.

Embodiment 3

[0026] Preparation of Ho by sol-gel method 3+ , Yb 3+ Double-doped yttrium-cerium composite oxide-based upconversion luminescent material Y 1.945 Ho 0.005 Yb 0.05 CeO 5 , The specific operations are as follows:

[0027] Calculate the ratio of various raw materials according to the mole fraction of each metal element in the material composition. Weigh 3.4382g Ce(NO 3 ) 3 ·6H 2 O, 6.0661g Y(NO 3 ) 3 ·6H 2 O, 0.0175g Ho(NO 3 ) 3 ·5H 2 O, 0.1479g Yb(NO 3 ) 3 ·6H 2 Put O into the beaker, add 70mL of distilled water, stir to fully dissolve it to form a uniform mixed solution, add 8.692g of citric acid to the mixed solution and stir evenly, slowly add 2mol / L dropwise to the mixed solution at a certain speed under stirring conditions To make a transparent sol, the beaker containing the sol is placed in a constant temperature water bath for gelation reaction, the gelation temperature is 60°C, and the time is 5-8h. After the gel is formed, place it in an oven at 110°C and dry it for 12-18 ...

Images