Method for preparing luminescent material with long persistence of Nano strontium aluminate

Abstract

This invention discloses a method for preparing nanoscale strontium aluminate long-afterglow luminescent material. The method comprises: reacting salt solution containing Al, Sr, Eu and Dy ions with (NH4)2CO3 solution (precipitant) to obtain a suspension of the product precursor, placing the suspension in a hydrothermal kettle, performing hydrothermal treatment at 140-240 deg.C for 4-48 h, filtering, washing, drying, uniformly mixing with H3BO3, and calcining at 1100-1300 deg.C in a reductive atmosphere (N2 96 vol.% + H2 4 vol.%) for 2-5 h to obtain the product. The chemical compositions of the product are SrAl2O4 (monoclinic crystal system) and Sr4Al14O25 (orthorhombic crystal system). The particle sizes of the product are below 100 nm, and there is little aggregation. Besides, the morphology is controllable.

Description

technical field

[0001] The invention relates to a preparation method of a long afterglow luminescent material, in particular to a preparation method of a nanometer strontium aluminate long afterglow luminescent material, belonging to the field of luminescent materials. Background technique

[0002] Common sulfide long-lasting luminescent materials such as ZnS:Cu have shortcomings such as short afterglow time, unstable chemical properties, and need to be coated during use, which limits their application. Compared with sulfide luminescent materials, aluminate luminescent materials have excellent luminescent properties, and are superior to sulfide luminescent materials in terms of luminous brightness and afterglow time, especially the Sr 4 Al 14 o 25 material, its brightness is good and it has good water resistance. The excellent long afterglow performance of aluminate luminescent materials makes it have a wide range of applications, especially in luminescent coatings and sa...

Examples

Embodiment 1

[0030] Prepare 1mol / L Al(NO 3 ) 3 and Sr(NO 3 ) 2 solution, the Eu 2 o 3 and Dy 2 o 3Dissolve in nitric acid solution respectively, adjust the concentration to 0.1mol / L, precipitant NH 4 ) 2 CO 3 The concentration of the solution is 1.0 mol / L. According to chemical formula Sr 3.88 Al 14 o 25 :Eu 0.04 , Dy 0.08 Al(NO 3 ) 3 , Sr(NO 3 ) 2 , Eu(NO 3 ) 3 and Dy(NO 3 ) 3 The mixed solution of each concentration is 0.7M, 0.2M, 0.004M and 0.008M respectively. In a water bath at 60°C, slowly drop (NH 4 ) 2 CO 3 Mix the solution with nitrate (mode (1)), and stir rapidly for 3h.

[0031] Put 25ml of the suspension of the resulting product precursor into a 30ml hydrothermal kettle, treat it at 140°C for 12h, wash the treated suspension with water and alcohol for 3 to 4 times, and dry it in an air oven at 80°C for 24 hours , take out and grind, pass through a 200-mesh sieve and then put in a weak reducing atmosphere (96%N 2 +4%H 2 ), calcined in a high-temperat...

Embodiment 2

[0034] Prepare 1mol / L Al(NO 3 ) 3 and Sr(NO 3 ) 2 solution, the Eu 2 o 3 and Dy 2 o 3 Dissolve in nitric acid solution respectively, and adjust the concentration to 0.1mol / L. According to chemical formula Sr 3.88 Al 14 o 25 :Eu 0.04 , Dy 0.08 Al(NO 3 ) 3 , Sr(NO 3 ) 2 , Eu(NO 3 ) 3 and Dy(NO 3 ) 3 The mixed solution of each concentration is 0.7M, 0.2M, 0.004M and 0.008M respectively. In a water bath at 60°C, slowly drop (NH 4 ) 2 CO 3 Mix solution with nitrate (mode (1)), stir rapidly for 3h, wherein, (NH 4 ) 2 CO 3 The solution was used in excess of 20% required for complete precipitation of the various ions at a concentration of 1.5M.

[0035] Put 25ml of the suspension of the product precursor produced by the reaction into a 30ml hydrothermal kettle, treat at 200°C for 4h, wash the treated suspension with water and alcohol for 3 to 4 times, and dry in an air oven at 80°C for 24 hours , take out and grind, pass through a 200-mesh sieve and then put...

Embodiment 3

[0038] Prepare 1mol / L Al respectively 2 (SO 4 ) 3 and SrSO 4 solution, the Eu 2 o 3 and Dy 2 o 3 Dissolve in sulfuric acid solution respectively, and adjust the concentration to 0.1mol / L. According to chemical formula Sr 3.88 Al 14 o 25 :Eu 0.04 , Dy 0.08 Al(NO 3 ) 3 , SrSO 4 、Eu 2 (SO 4 ) 3 and Dy 2 (SO 4 ) 3 The mixed solution of each concentration is 0.7M, 0.2M, 0.004M and 0.008M respectively. In a water bath at 60°C, slowly drop (NH 4 ) 2 CO 3 (mode (2)), rapid stirring 3h, wherein, (NH 4 ) 2 CO 3 The solution was used in excess of 20% required for complete precipitation of the various ions at a concentration of 1.5M.

[0039] Put 25ml of the resulting product precursor suspension into a 30ml hydrothermal kettle, treat it at 200°C for 4h, wash the hydroheated suspension with water and alcohol for 3 to 4 times, and dry it in an air oven at 80°C for 24 hours , take out the grind and mix with 2%wt H 3 BO 3 , passed through a 200-mesh sieve and th...

technical field

[0001] The invention relates to a preparation method of a long afterglow luminescent material, in particular to a preparation method of a nanometer strontium aluminate long afterglow luminescent material, belonging to the field of luminescent materials. Background technique

[0002] Common sulfide long-lasting luminescent materials such as ZnS:Cu have shortcomings such as short afterglow time, unstable chemical properties, and need to be coated during use, which limits their application. Compared with sulfide luminescent materials, aluminate luminescent materials have excellent luminescent properties, and are superior to sulfide luminescent materials in terms of luminous brightness and afterglow time, especially the Sr 4 Al 14 o 25 material, its brightness is good and it has good water resistance. The excellent long afterglow performance of aluminate luminescent materials makes it have a wide range of applications, especially in luminescent coatings and sa...

Examples

Embodiment 1

[0030] Prepare 1mol / L Al(NO 3 ) 3 and Sr(NO 3 ) 2 solution, the Eu 2 o 3 and Dy 2 o 3Dissolve in nitric acid solution respectively, adjust the concentration to 0.1mol / L, precipitant NH 4 ) 2 CO 3 The concentration of the solution is 1.0 mol / L. According to chemical formula Sr 3.88 Al 14 o 25 :Eu 0.04 , Dy 0.08 Al(NO 3 ) 3 , Sr(NO 3 ) 2 , Eu(NO 3 ) 3 and Dy(NO 3 ) 3 The mixed solution of each concentration is 0.7M, 0.2M, 0.004M and 0.008M respectively. In a water bath at 60°C, slowly drop (NH 4 ) 2 CO 3 Mix the solution with nitrate (mode (1)), and stir rapidly for 3h.

[0031] Put 25ml of the suspension of the resulting product precursor into a 30ml hydrothermal kettle, treat it at 140°C for 12h, wash the treated suspension with water and alcohol for 3 to 4 times, and dry it in an air oven at 80°C for 24 hours , take out and grind, pass through a 200-mesh sieve and then put in a weak reducing atmosphere (96%N 2 +4%H 2 ), calcined in a high-temperat...

Embodiment 2

[0034] Prepare 1mol / L Al(NO 3 ) 3 and Sr(NO 3 ) 2 solution, the Eu 2 o 3 and Dy 2 o 3 Dissolve in nitric acid solution respectively, and adjust the concentration to 0.1mol / L. According to chemical formula Sr 3.88 Al 14 o 25 :Eu 0.04 , Dy 0.08 Al(NO 3 ) 3 , Sr(NO 3 ) 2 , Eu(NO 3 ) 3 and Dy(NO 3 ) 3 The mixed solution of each concentration is 0.7M, 0.2M, 0.004M and 0.008M respectively. In a water bath at 60°C, slowly drop (NH 4 ) 2 CO 3 Mix solution with nitrate (mode (1)), stir rapidly for 3h, wherein, (NH 4 ) 2 CO 3 The solution was used in excess of 20% required for complete precipitation of the various ions at a concentration of 1.5M.

[0035] Put 25ml of the suspension of the product precursor produced by the reaction into a 30ml hydrothermal kettle, treat at 200°C for 4h, wash the treated suspension with water and alcohol for 3 to 4 times, and dry in an air oven at 80°C for 24 hours , take out and grind, pass through a 200-mesh sieve and then put...

Embodiment 3

[0038] Prepare 1mol / L Al respectively 2 (SO 4 ) 3 and SrSO 4 solution, the Eu 2 o 3 and Dy 2 o 3 Dissolve in sulfuric acid solution respectively, and adjust the concentration to 0.1mol / L. According to chemical formula Sr 3.88 Al 14 o 25 :Eu 0.04 , Dy 0.08 Al(NO 3 ) 3 , SrSO 4 、Eu 2 (SO 4 ) 3 and Dy 2 (SO 4 ) 3 The mixed solution of each concentration is 0.7M, 0.2M, 0.004M and 0.008M respectively. In a water bath at 60°C, slowly drop (NH 4 ) 2 CO 3 (mode (2)), rapid stirring 3h, wherein, (NH 4 ) 2 CO 3 The solution was used in excess of 20% required for complete precipitation of the various ions at a concentration of 1.5M.

[0039] Put 25ml of the resulting product precursor suspension into a 30ml hydrothermal kettle, treat it at 200°C for 4h, wash the hydroheated suspension with water and alcohol for 3 to 4 times, and dry it in an air oven at 80°C for 24 hours , take out the grind and mix with 2%wt H 3 BO 3 , passed through a 200-mesh sieve and th...

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