CN103333683A - CaxSiO4Bry:Ce<3+> fluorescent powder and preparation method thereof - Google Patents

CaxSiO4Bry:Ce<3+> fluorescent powder and preparation method thereof Download PDF

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CN103333683A
CN103333683A CN2013102726704A CN201310272670A CN103333683A CN 103333683 A CN103333683 A CN 103333683A CN 2013102726704 A CN2013102726704 A CN 2013102726704A CN 201310272670 A CN201310272670 A CN 201310272670A CN 103333683 A CN103333683 A CN 103333683A
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sio
sintering
fluorescent material
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solid
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毕自贵
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Irico Group Corp
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Abstract

The invention provides a CaxSiO4Bry:Ce<3+> fluorescent powder and a preparation method thereof. The CaxSiO4Bry:Ce<3+> fluorescent powder has the chemical general formula: CaxSiO4Bry:Ce<3+>, wherein 1<=x<=3, and 1<=y<=3. The preparation method comprises the following steps of: uniformly mixing calcium oxide, silica, calcium bromide and cerium oxide according to the stoichiometric ratio of the fluorescent powder; sintering the raw materials in a high temperature furnace at an atmosphere with a reductive gas or an atmosphere with a mixed gas of air and the reductive gas by using a high temperature solid state method; cooling to the room temperature at the same atmosphere; and washing a solid by using concentrated nitric acid, and then, drying the solid to obtain the fluorescent powder, wherein the solid is obtained through sintering. The fluorescent powder is good in chemical stability, high in degradation resistance at high temperature and capable of increasing the color index of an LED (Light Emitting Diode) to over 65 under a single component, effectively prolonging the service life of the LED and emitting blue-green visible light with peak wavelength range from 465nm to 475nm under the excitation of an LED chip with blue light with the wave band range from 455nm to 460nm.

Description

A kind of Ca xSiO 4Br y: Ce 3+Fluorescent material and preparation method thereof
Technical field
The invention belongs to the material field, relate to a kind of fluorescent material, be specifically related to a kind of Ca xSiO 4Br y: Ce 3+Fluorescent material and preparation method thereof.
Background technology
Advantages such as photodiode (LED) is the semiconductor light source of environmental type, has less energy-consumption, long lifetime, and volume is little, and structure is firm, and good directionality, response are fast, and be radiationless.But be subjected to the present stage technical limitation, LED generally is monochromatic source, and is more suitable as decorative light-source, and range blanking is used still certain gap.So be badly in need of to want various types of LED fluorescent material, send the visible light of different-waveband after exciting by led chip, superpose with original led chip light source, form that to drill colour index higher, more close to the illumination light source of natural light.
Summary of the invention
The object of the present invention is to provide a kind of Ca xSiO 4Br y: Ce 3+Fluorescent material and preparation method thereof, this fluorescent material can hard to bear blue-light LED chip excite and launch bluish-green coloured light.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of Ca xSiO 4Br y: Ce 3+Fluorescent material, its chemical general formula are Ca xSiO 4Br y: Ce 3+, 1≤x≤3,1≤y≤3 wherein.
Its blue-light LED chip at 455～460nm wave band excites the visible light that can launch 465～475nm wave band down.
A kind of Ca xSiO 4Br y: Ce 3+The preparation method of fluorescent material may further comprise the steps:
With calcium oxide, silicon-dioxide, Calcium Bromide and cerium oxide according to Ca xSiO 4Br y: Ce 3+Stoichiometric ratio pack into after mixing in the corundum crucible, 1≤x≤3 wherein, 1≤y≤3, again corundum crucible is packed in the High Temperature Furnaces Heating Apparatus, adopt high temperature solid-state method under the mixed atmosphere of reducing gas or air and reducing gas, to carry out sintering, sintering temperature is 1400-1700 ℃, sintering time is 5-10 hour, naturally be down to room temperature after sintering is finished under the mixed atmosphere of identical reducing gas or air and reducing gas, the solid that sintering is obtained namely obtains Ca with concentrated nitric acid washing back oven dry xSiO 4Br y: Ce 3+Fluorescent material.
0.5≤x/y≤3, when x/y=0.5, the add-on of calcium oxide is 0.
Described reducing gas is the gas mixture of gas mixture, ammonia and carbon monoxide of hydrogen, carbon monoxide, nitrogen and hydrogen or the gas mixture of hydrogen and carbon monoxide.
Naturally being down to the required time of room temperature from sintering temperature after described sintering is finished is 10～30h.
The solid that described sintering obtains is with needing before the concentrated nitric acid washing earlier through fragmentation, crosses 100～200 mesh sieves (100～200 mesh sieves refer to look over so as to check number be in 100～200 purpose sieves any one) then.
Described concentrated nitric acid is the nitric acid of pH value＜1.
Described bake out temperature is 100～150 ℃.
With respect to prior art, beneficial effect of the present invention is:
Ca provided by the invention xSiO 4Br y: Ce 3+Fluorescent material (1≤x≤3,1≤y≤3) chemical stability is good, and one-component is drilled the colour index height, and can under one-component, LED be drilled colour index and be promoted to more than 65, and Ca xSiO 4Br y: Ce 3+Fluorescent material antidamping ability at high temperature is strong, can effectively promote the LED life-span.Ce 3+As doped with rare-earth elements, as unique activator, excite Ca xSiO 4Br y: Ce 3+Fluorescent material, and Ca xSiO 4Br y: Ce 3+Fluorescent material can excite at the blue-light LED chip of 455～460nm wave band down as pure phase simplification compound, launches peak wavelength at the blue-greenish colour visible light of 465～475nm wave band, is a kind of potential LED fluorescent material.
Ca provided by the invention xSiO 4Br y: Ce 3+Fluorescent material (1≤x≤3,1≤y≤3) preparation method adopts high temperature solid-state method, calcium oxide, silicon-dioxide, Calcium Bromide and cerium oxide mixed according to the stoichiometric ratio of this fluorescent material and carry out high temperature sintering, raw material is easy to get, technology is simple, easy to operate, be the Ca simply and easily that a kind of industry is suitable for xSiO 4Br y: Ce 3+The preparation method of fluorescent material.
Embodiment
Ca provided by the invention xSiO 4Br y: Ce 3+Fluorescent material, its chemical general formula are Ca xSiO 4Br y: Ce 3+, 1≤x≤3,1≤y≤3 wherein.Ce 3+As doped with rare-earth elements, it is the unique activator of this fluorescent material.
Below in conjunction with specific embodiment to Ca of the present invention xSiO 4Br y: Ce 3+The preparation method of fluorescent material is described in further detail.
Embodiment 1:
Ca 1.5SiO 4Br 2: Ce 3+ 0.1Fluorescent material (x=1.5 in the chemical general formula, preparation method y=2): according to Ca 1.5SiO 4Br 2: Ce 3+ 0.1Stoichiometric ratio, take by weighing the 0.5mol calcium oxide, 1mol silicon-dioxide, the 1mol Calcium Bromide, 0.1mol cerium oxide, pack into after above raw material mixed in the corundum crucible, again corundum crucible is packed in the High Temperature Furnaces Heating Apparatus, adopt high temperature solid-state method under the mixed atmosphere (volumetric concentration of hydrogen is less than 3%) of air and hydrogen, to carry out sintering, sintering temperature is 1600 ℃, and sintering time is 5 hours, after sintering is finished still at the mixed atmosphere (volumetric concentration of hydrogen is less than 3%) of air and hydrogen down with the slow natural room temperature of being down to of time of 30 hours, the solid that sintering is obtained takes out the back fragmentation, cross the accurate sub-sieve of 100 targets, the lower part of screen branch washs in the concentrated nitric acid of pH value＜1, falls remaining acid solution with distilled water wash again after the pickling, 150 ℃ of oven dry, namely obtaining chemical formula is Ca then 1.5SiO 4Br 2: Ce 3+ 0.1Fluorescent material.
Embodiment 2:
CaSiO 4Br 1.5: Ce 3+ 0.1Fluorescent material (x=1 in the chemical general formula, preparation method y=1.5): according to CaSiO 4Br 1.5: Ce 3+ 0.1Stoichiometric ratio, take by weighing the 0.25mol calcium oxide, 1mol silicon-dioxide, 0.75mol Calcium Bromide, 0.1mol cerium oxide, pack into after above raw material mixed in the corundum crucible, again corundum crucible is packed in the High Temperature Furnaces Heating Apparatus, adopt high temperature solid-state method under the mixed atmosphere (volumetric concentration of hydrogen is less than 3%) of air and hydrogen, to carry out sintering, sintering temperature is 1500 ℃, and sintering time is 6 hours, after sintering is finished still at the mixed atmosphere (volumetric concentration of hydrogen is less than 3%) of air and hydrogen down with the slow natural room temperature of being down to of time of 15 hours, the solid that sintering is obtained takes out the back fragmentation, cross the accurate sub-sieve of 100 targets, the lower part of screen branch washs in the concentrated nitric acid of pH value＜1, falls remaining acid solution with distilled water wash again after the pickling, 150 ℃ of oven dry, namely obtaining chemical formula is CaSiO then 4Br 1.5: Ce 3+ 0.1Fluorescent material.
Embodiment 3:
Ca 3SiO 4Br 1.5: Ce 3+ 0.2Fluorescent material (x=3 in the chemical general formula, preparation method y=1.5): according to Ca 3SiO 4Br 1.5: Ce 3+ 0.2Stoichiometric ratio, take by weighing the 2.25mol calcium oxide, 1mol silicon-dioxide, 0.75mol Calcium Bromide, 0.2mol cerium oxide, pack into after above raw material mixed in the corundum crucible, again corundum crucible is packed in the High Temperature Furnaces Heating Apparatus, adopt high temperature solid-state method under carbon monoxide atmosphere, to carry out sintering, sintering temperature is 1400 ℃, and sintering time is 10 hours, after sintering is finished still under carbon monoxide atmosphere with time of 10 hours slowly nature be down to room temperature, the solid that sintering is obtained takes out the back fragmentation, cross the accurate sub-sieve of 100 targets, the lower part of screen branch washs in the concentrated nitric acid of pH value＜1, falls remaining acid solution with distilled water wash again after the pickling, 150 ℃ of oven dry, namely obtaining chemical formula is Ca then 3SiO 4Br 1.5: Ce 3+ 0.2Fluorescent material.
Embodiment 4:
Ca 3SiO 4Br 2: Ce 3+ 0.1Fluorescent material (x=3 in the chemical general formula, preparation method y=2): according to Ca 3SiO 4Br 2: Ce 3+ 0.1Stoichiometric ratio, take by weighing the 2mol calcium oxide, 1mol silicon-dioxide, the 1mol Calcium Bromide, 0.1mol cerium oxide, pack into after above raw material mixed in the corundum crucible, again corundum crucible is packed in the High Temperature Furnaces Heating Apparatus, adopt high temperature solid-state method under the mixed atmosphere of nitrogen and hydrogen, to carry out sintering, sintering temperature is 1700 ℃, and sintering time is 5 hours, after sintering is finished still under the mixed atmosphere of nitrogen and hydrogen with time of 30 hours slowly nature be down to room temperature, the solid that sintering is obtained takes out the back fragmentation, cross the accurate sub-sieve of 100 targets, the lower part of screen branch washs in the concentrated nitric acid of pH value＜1, falls remaining acid solution with distilled water wash again after the pickling, 150 ℃ of oven dry, namely obtaining chemical formula is Ca then 3SiO 4Br 2: Ce 3+ 0.1Fluorescent material.
Embodiment 5:
Ca 1.5SiO 4Br 3: Ce 3+ 0.1Fluorescent material (x=1.5 in the chemical general formula, preparation method y=3): according to Ca 1.5SiO 4Br 3: Ce 3+ 0.1Stoichiometric ratio, take by weighing 1mol silicon-dioxide, 1.5mol Calcium Bromide, 0.1mol cerium oxide, pack into after above raw material mixed in the corundum crucible, again corundum crucible is packed in the High Temperature Furnaces Heating Apparatus, adopt high temperature solid-state method under the mixed atmosphere (volumetric concentration of hydrogen is less than 3%) of air and hydrogen, to carry out sintering, sintering temperature is 1450 ℃, sintering time is 9 hours, after sintering is finished still the mixed atmosphere (volumetric concentration of hydrogen is less than 3%) of air and hydrogen down with time of 12 hours slowly nature be down to room temperature, it is broken that the solid that sintering is obtained takes out the back, the accurate sub-sieve of 100 targets, the lower part of screen branch washs in the concentrated nitric acid of pH value＜1, fall remaining acid solution with distilled water wash again after the pickling, then 150 ℃ of oven dry, namely obtaining chemical formula is Ca 1.5SiO 4Br 3: Ce 3+ 0.1Fluorescent material.
Embodiment 6:
CaSiO 4Br 1.5: Ce 3+ 0.3Fluorescent material (x=1 in the chemical general formula, preparation method y=1.5): according to CaSiO 4Br 1.5: Ce 3+ 0.3Stoichiometric ratio, take by weighing the 0.25mol calcium oxide, 1mol silicon-dioxide, 0.75mol Calcium Bromide, 0.3mol cerium oxide, pack into after above raw material mixed in the corundum crucible, again corundum crucible is packed in the High Temperature Furnaces Heating Apparatus, adopt high temperature solid-state method under the mixed atmosphere (volumetric concentration of hydrogen is less than 3%) of air and hydrogen, to carry out sintering, sintering temperature is 1500 ℃, and sintering time is 8 hours, after sintering is finished still at the mixed atmosphere (volumetric concentration of hydrogen is less than 3%) of air and hydrogen down with the slow natural room temperature of being down to of time of 20 hours, the solid that sintering is obtained takes out the back fragmentation, cross the accurate sub-sieve of 170 targets, the lower part of screen branch washs in the concentrated nitric acid of pH value＜1, falls remaining acid solution with distilled water wash again after the pickling, 110 ℃ of oven dry, namely obtaining chemical formula is CaSiO then 4Br 1.5: Ce 3+ 0.3Fluorescent material.
Embodiment 7:
Ca 2SiO 4Br 2: Ce 3+ 0.1Fluorescent material (x=2 in the chemical general formula, preparation method y=2): according to Ca 2SiO 4Br 2: Ce 3+ 0.1Stoichiometric ratio, take by weighing the 1mol calcium oxide, 1mol silicon-dioxide, the 1mol Calcium Bromide, 0.1mol cerium oxide, pack into after above raw material mixed in the corundum crucible, again corundum crucible is packed in the High Temperature Furnaces Heating Apparatus, adopt high temperature solid-state method under the mixed atmosphere (volumetric concentration of hydrogen is less than 3%) of air and hydrogen, to carry out sintering, sintering temperature is 1550 ℃, and sintering time is 7 hours, after sintering is finished still at the mixed atmosphere (volumetric concentration of hydrogen is less than 3%) of air and hydrogen down with the slow natural room temperature of being down to of time of 18 hours, the solid that sintering is obtained takes out the back fragmentation, cross the accurate sub-sieve of 140 targets, the lower part of screen branch washs in the concentrated nitric acid of pH value＜1, falls remaining acid solution with distilled water wash again after the pickling, 120 ℃ of oven dry, namely obtaining chemical formula is Ca then 2SiO 4Br 2: Ce 3+ 0.1Fluorescent material.
Embodiment 8:
Ca 3SiO 4Br:Ce 3+ 0.1Fluorescent material (x=3 in the chemical general formula, preparation method y=1): according to Ca 3SiO 4Br:Ce 3+ 0.1Stoichiometric ratio, take by weighing the 2.5mol calcium oxide, 1mol silicon-dioxide, 0.5mol Calcium Bromide, 0.1mol cerium oxide is in the corundum crucible of packing into after above raw material mixed, in the High Temperature Furnaces Heating Apparatus of again corundum crucible being packed into, adopt high temperature solid-state method under hydrogen atmosphere, to carry out sintering, sintering temperature is 1650 ℃, and sintering time is 5 hours, after sintering is finished still under hydrogen atmosphere with time of 25 hours slowly nature be down to room temperature, the solid that sintering is obtained takes out the back fragmentation, cross the accurate sub-sieve of 120 targets, the lower part of screen branch washs in the concentrated nitric acid of pH value＜1, falls remaining acid solution with distilled water wash again after the pickling, 130 ℃ of oven dry, namely obtaining chemical formula is Ca then 3SiO 4Br:Ce 3+ 0.1Fluorescent material.
Embodiment 9:
Ca 3SiO 4Br:Ce 3+ 0.2Fluorescent material (x=3 in the chemical general formula, preparation method y=1): according to Ca 3SiO 4Br:Ce 3+ 0.2Stoichiometric ratio, take by weighing the 2.5mol calcium oxide, 1mol silicon-dioxide, 0.5mol Calcium Bromide, 0.2mol cerium oxide, pack into after above raw material mixed in the corundum crucible, again corundum crucible is packed in the High Temperature Furnaces Heating Apparatus, adopt high temperature solid-state method under the mixed atmosphere of ammonia and carbon monoxide, to carry out sintering, sintering temperature is 1600 ℃, and sintering time is 6 hours, after sintering is finished still under the mixed atmosphere of ammonia and carbon monoxide with time of 20 hours slowly nature be down to room temperature, the solid that sintering is obtained takes out the back fragmentation, cross the accurate sub-sieve of 200 targets, the lower part of screen branch washs in the concentrated nitric acid of pH value＜1, falls remaining acid solution with distilled water wash again after the pickling, 140 ℃ of oven dry, namely obtaining chemical formula is Ca then 3SiO 4Br:Ce 3+ 0.2Fluorescent material.
Embodiment 10:
Ca 3SiO 4Br 3: Ce 3+ 0.1Fluorescent material (x=3 in the chemical general formula, preparation method y=3): according to Ca 3SiO 4Br 3: Ce 3+ 0.1Stoichiometric ratio, take by weighing the 1.5mol calcium oxide, 1mol silicon-dioxide, 1.5mol Calcium Bromide, 0.1mol cerium oxide, pack into after above raw material mixed in the corundum crucible, again corundum crucible is packed in the High Temperature Furnaces Heating Apparatus, adopt high temperature solid-state method at air, carry out sintering under the mixed atmosphere of hydrogen and carbon monoxide (volumetric concentration of hydrogen is less than 3%), sintering temperature is 1600 ℃, and sintering time is 5 hours, after sintering is finished still at air, the mixed atmosphere of hydrogen and carbon monoxide (volumetric concentration of hydrogen is less than 3%) is down with the slow natural room temperature of being down to of time of 30 hours, the solid that sintering is obtained takes out the back fragmentation, cross the accurate sub-sieve of 100 targets, the lower part of screen branch washs in the concentrated nitric acid of pH value＜1, falls remaining acid solution with distilled water wash again after the pickling, 150 ℃ of oven dry, namely obtaining chemical formula is Ca then 3SiO 4Br 3: Ce 3+ 0.1Fluorescent material.
Ca provided by the invention xSiO 4Br y: Ce 3+Fluorescent material (1≤x≤3,1≤y≤3) chemical stability is good, and one-component is drilled the colour index height, and can under one-component, LED be drilled colour index and be promoted to more than 65, and Ca xSiO 4Br y: Ce 3+Fluorescent material antidamping ability at high temperature is strong, can effectively promote the LED life-span.And Ca xSiO 4Br y: Ce 3+Fluorescent material can excite at the blue-light LED chip of 455～460nm wave band down as pure phase simplification compound, launches peak wavelength at the blue-greenish colour visible light of 465～475nm wave band.

Claims (9)

1. Ca xSiO 4Br y: Ce 3+Fluorescent material is characterized in that: its chemical general formula is Ca xSiO 4Br y: Ce 3+, 1≤x≤3,1≤y≤3 wherein.
2. Ca according to claim 1 xSiO 4Br y: Ce 3+Fluorescent material is characterized in that: its blue-light LED chip at 455～460nm wave band excites the visible light that can launch 465～475nm wave band down.
3. Ca xSiO 4Br y: Ce 3+The preparation method of fluorescent material is characterized in that, may further comprise the steps:
With calcium oxide, silicon-dioxide, Calcium Bromide and cerium oxide according to Ca xSiO 4Br y: Ce 3+Stoichiometric ratio pack into after mixing in the corundum crucible, 1≤x≤3 wherein, 1≤y≤3, again corundum crucible is packed in the High Temperature Furnaces Heating Apparatus, adopt high temperature solid-state method under the mixed atmosphere of reducing gas or air and reducing gas, to carry out sintering, sintering temperature is 1400-1700 ℃, sintering time is 5-10 hour, naturally be down to room temperature after sintering is finished under the mixed atmosphere of identical reducing gas or air and reducing gas, the solid that sintering is obtained namely obtains Ca with concentrated nitric acid washing back oven dry xSiO 4Br y: Ce 3+Fluorescent material.
4. Ca according to claim 3 xSiO 4Br y: Ce 3+The preparation method of fluorescent material is characterized in that: 0.5≤x/y≤3, when x/y=0.5, the add-on of calcium oxide is 0.
5. Ca according to claim 3 xSiO 4Br y: Ce 3+The preparation method of fluorescent material is characterized in that: described reducing gas is the gas mixture of gas mixture, ammonia and carbon monoxide of hydrogen, carbon monoxide, nitrogen and hydrogen or the gas mixture of hydrogen and carbon monoxide.
6. Ca according to claim 3 xSiO 4Br y: Ce 3+The preparation method of fluorescent material is characterized in that: being down to the required time of room temperature naturally from sintering temperature after described sintering is finished is 10～30h.
7. Ca according to claim 3 xSiO 4Br y: Ce 3+The preparation method of fluorescent material is characterized in that: the solid that described sintering obtains needs elder generation through fragmentation before with the concentrated nitric acid washing, crosses 100～200 mesh sieves then.
8. Ca according to claim 3 xSiO 4Br y: Ce 3+The preparation method of fluorescent material is characterized in that: described concentrated nitric acid is the nitric acid of pH value＜1.
9. Ca according to claim 3 xSiO 4Br y: Ce 3+The preparation method of fluorescent material is characterized in that: described bake out temperature is 100～150 ℃.
CN2013102726704A 2013-07-01 2013-07-01 CaxSiO4Bry:Ce<3+> fluorescent powder and preparation method thereof Pending CN103333683A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114806559A (en) * 2022-04-19 2022-07-29 西安建筑科技大学 Eu (Eu) 2+ Activated ultra-wideband visible-near infrared luminescent material, preparation method and application

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JP2007327070A (en) * 2007-08-22 2007-12-20 Mitsubishi Chemicals Corp Phosphor
US20120068591A1 (en) * 2010-09-16 2012-03-22 Samsung Electronics Co., Ltd. Green phosphors, methods of preparing the green phosphors, and white light-emitting devices including the green phosphors
CN102757787A (en) * 2012-07-30 2012-10-31 轻工业部南京电光源材料科学研究所 Blue light excited green fluorescent powder for white light light-emitting diode (LED) and preparing method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007327070A (en) * 2007-08-22 2007-12-20 Mitsubishi Chemicals Corp Phosphor
US20120068591A1 (en) * 2010-09-16 2012-03-22 Samsung Electronics Co., Ltd. Green phosphors, methods of preparing the green phosphors, and white light-emitting devices including the green phosphors
CN102757787A (en) * 2012-07-30 2012-10-31 轻工业部南京电光源材料科学研究所 Blue light excited green fluorescent powder for white light light-emitting diode (LED) and preparing method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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Application publication date: 20131002