Hydroxyapatite-based fluorescent ceramic material and preparation method thereof

Abstract

The invention relates to a hydroxyapatite-based fluorescent ceramic material and a preparation method thereof. The hydroxyapatite-based fluorescent ceramic material is prepared from the following raw materials in percentages by weight: 95-99% of hydroxyapatite matrix and 1-5% of fluorescent powder. The preparation method comprises the steps of mixing the hydroxyapatite matrix with the fluorescent powder evenly; loading the mixed raw materials into a graphite mold, putting the graphite mold into a spark plasma sintering furnace, sintering in a vacuum environment to obtain transparent ceramic; and finally grinding and polishing to obtain the hydroxyapatite-based fluorescent ceramic material. By adopting hydroxyapatite nano powder, the sintering temperature of the fluorescent ceramic is effectively reduced, the sintering time of the fluorescent ceramic is effectively shortened, the luminescence characteristic of fluorescent powder can be effectively reserved; meanwhile, by adopting the ceramic as the matrix, the thermal conductivity of an LED packaging material can be significantly improved, and the heat resistance and the stability of the fluorescent ceramic material are effectively improved; the preparation technology is simple and convenient; and the hydroxyapatite-based fluorescent ceramic material can be directly used as a packaging material to replace a traditional organic polymer or silica gel packaging material, and has a good application prospect.

Description

technical field

[0001] The invention belongs to the field of fluorescent materials, in particular to a hydroxyapatite-based fluorescent ceramic material and a preparation method thereof. Background technique

[0002] As a lighting source, semiconductor light-emitting diode (Light-Emitting Diode, LED) is known as the fourth-generation lighting source that is expected to surpass incandescent lamps, fluorescent lamps and high-pressure gas discharge lamps due to its advantages of energy saving, environmental protection, long life, and fast response. , will gradually become one of the representative high-tech products in the field of lighting in the 21st century. Among them, white LED is the top priority in the development of semiconductor lighting.

[0003] In recent years, as the lumen efficiency of high-power white LEDs continues to increase and the manufacturing cost continues to decrease, it has become possible for them to be widely used in traditional lighting and special ...

Examples

Embodiment 1

[0029] Using calcium nitrate and diammonium hydrogen phosphate as raw materials, the concentration of calcium nitrate is 0.9mol / L to prepare solution A, and the concentration of diammonium hydrogen phosphate is 1.8mol / L to prepare solution B; under the ice bath environment, the solution A is prepared according to the ion molar ratio to Ca : P=1.6:1, drop speed 3ml / min, slowly drop into B solution, adjust reaction environment pH>10 with ammonia water during the reaction; react 2h after dropping, obtain C suspension, turn C solution into high pressure Carry out hydrothermal in the reaction kettle, the hydrothermal reaction temperature is 130°C, and the hydrothermal reaction time is 24h; after hydrothermal filtration, the precipitate is washed with water and alcohol to obtain the precursor of hydroxyapatite powder, which is fully dried in an oven; The powder was calcined in a muffle furnace at a calcining temperature of 250° C., a heating rate of 5° C. / min, and a holding time of 2...

Embodiment 2

[0032]Using calcium nitrate and diammonium hydrogen phosphate as raw materials, the concentration of calcium nitrate is 0.3mol / L to prepare solution A, and the concentration of diammonium hydrogen phosphate to prepare solution B; : P=1.5:1, dripping speed 1ml / min, slowly drop into B solution, adjust the reaction environment pH>10 with ammonia water during the reaction; react for 2h after the drop is completed, obtain C suspension, turn C solution into high pressure Carry out hydrothermal in the reaction kettle, the hydrothermal reaction temperature is 100°C, and the hydrothermal reaction time is 12h; after hydrothermal filtration, the precipitate is washed with water and alcohol to obtain the precursor of hydroxyapatite powder, which is fully dried in an oven; The powder was calcined in a muffle furnace at a calcining temperature of 700° C., a heating rate of 5° C. / min, and a holding time of 2 hours to obtain a hydroxyapatite matrix.

[0033] Grind and mix the commercial red p...

Embodiment 3

[0035] Using calcium nitrate and diammonium hydrogen phosphate as raw materials, the concentration of calcium nitrate is 0.9mol / L to prepare solution A, and the concentration of diammonium hydrogen phosphate is 1.8mol / L to prepare solution B; under the ice bath environment, the solution A is prepared according to the ion molar ratio to Ca : P=2:1, drop speed 2ml / min, slowly drop into solution B, adjust the reaction environment pH>10 with ammonia water during the reaction; react for 2 hours after the addition is completed, obtain C suspension, transfer C solution to high pressure Carry out hydrothermal in the reaction kettle, the hydrothermal reaction temperature is 130°C, and the hydrothermal reaction time is 24h; after hydrothermal filtration, the precipitate is washed with water and alcohol to obtain the precursor of hydroxyapatite powder, which is fully dried in an oven; The powder was calcined in a muffle furnace at a calcining temperature of 250° C., a heating rate of 5° C...

technical field

[0001] The invention belongs to the field of fluorescent materials, in particular to a hydroxyapatite-based fluorescent ceramic material and a preparation method thereof. Background technique

[0002] As a lighting source, semiconductor light-emitting diode (Light-Emitting Diode, LED) is known as the fourth-generation lighting source that is expected to surpass incandescent lamps, fluorescent lamps and high-pressure gas discharge lamps due to its advantages of energy saving, environmental protection, long life, and fast response. , will gradually become one of the representative high-tech products in the field of lighting in the 21st century. Among them, white LED is the top priority in the development of semiconductor lighting.

[0003] In recent years, as the lumen efficiency of high-power white LEDs continues to increase and the manufacturing cost continues to decrease, it has become possible for them to be widely used in traditional lighting and special ...

Examples

Embodiment 1

[0029] Using calcium nitrate and diammonium hydrogen phosphate as raw materials, the concentration of calcium nitrate is 0.9mol / L to prepare solution A, and the concentration of diammonium hydrogen phosphate is 1.8mol / L to prepare solution B; under the ice bath environment, the solution A is prepared according to the ion molar ratio to Ca : P=1.6:1, drop speed 3ml / min, slowly drop into B solution, adjust reaction environment pH>10 with ammonia water during the reaction; react 2h after dropping, obtain C suspension, turn C solution into high pressure Carry out hydrothermal in the reaction kettle, the hydrothermal reaction temperature is 130°C, and the hydrothermal reaction time is 24h; after hydrothermal filtration, the precipitate is washed with water and alcohol to obtain the precursor of hydroxyapatite powder, which is fully dried in an oven; The powder was calcined in a muffle furnace at a calcining temperature of 250° C., a heating rate of 5° C. / min, and a holding time of 2...

Embodiment 2

[0032]Using calcium nitrate and diammonium hydrogen phosphate as raw materials, the concentration of calcium nitrate is 0.3mol / L to prepare solution A, and the concentration of diammonium hydrogen phosphate to prepare solution B; : P=1.5:1, dripping speed 1ml / min, slowly drop into B solution, adjust the reaction environment pH>10 with ammonia water during the reaction; react for 2h after the drop is completed, obtain C suspension, turn C solution into high pressure Carry out hydrothermal in the reaction kettle, the hydrothermal reaction temperature is 100°C, and the hydrothermal reaction time is 12h; after hydrothermal filtration, the precipitate is washed with water and alcohol to obtain the precursor of hydroxyapatite powder, which is fully dried in an oven; The powder was calcined in a muffle furnace at a calcining temperature of 700° C., a heating rate of 5° C. / min, and a holding time of 2 hours to obtain a hydroxyapatite matrix.

[0033] Grind and mix the commercial red p...

Embodiment 3

[0035] Using calcium nitrate and diammonium hydrogen phosphate as raw materials, the concentration of calcium nitrate is 0.9mol / L to prepare solution A, and the concentration of diammonium hydrogen phosphate is 1.8mol / L to prepare solution B; under the ice bath environment, the solution A is prepared according to the ion molar ratio to Ca : P=2:1, drop speed 2ml / min, slowly drop into solution B, adjust the reaction environment pH>10 with ammonia water during the reaction; react for 2 hours after the addition is completed, obtain C suspension, transfer C solution to high pressure Carry out hydrothermal in the reaction kettle, the hydrothermal reaction temperature is 130°C, and the hydrothermal reaction time is 24h; after hydrothermal filtration, the precipitate is washed with water and alcohol to obtain the precursor of hydroxyapatite powder, which is fully dried in an oven; The powder was calcined in a muffle furnace at a calcining temperature of 250° C., a heating rate of 5° C...

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