CN102001827B - Inorganic aluminate luminescent microcrystalline glass and preparation method thereof - Google Patents

Inorganic aluminate luminescent microcrystalline glass and preparation method thereof Download PDF

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CN102001827B
CN102001827B CN2009101898548A CN200910189854A CN102001827B CN 102001827 B CN102001827 B CN 102001827B CN 2009101898548 A CN2009101898548 A CN 2009101898548A CN 200910189854 A CN200910189854 A CN 200910189854A CN 102001827 B CN102001827 B CN 102001827B
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sytull
luminous
inorganic aluminate
preparation
glass
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CN102001827A (en
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周明杰
李清涛
马文波
时朝璞
乔延波
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Oceans King Lighting Science and Technology Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
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Abstract

The invention discloses inorganic aluminate luminescent microcrystalline glass and a preparation method thereof. The inorganic aluminate luminescent microcrystalline glass is a substance shown as a chemical formula, namely, X SrO-Y Al2O3-Z SiO2-R Pr2O3, wherein X, Y, Z and R are molar fractions; X is more than or equal to 25 and less than or equal to 40; Y is more than or equal to 25 and less than or equal to 40; Z is more than or equal to 25 and less than or equal to 50; and R is more than or equal to 0.1 and less than or equal to 2. The preparation method comprises the following steps of: grinding strontium carbonate, alumina, silicon dioxide and praseodymium oxide serving as raw materials and mixing; fusing at the temperature of between 1,550 and 1,650 DEG C and molding the raw materials to obtain glass; and thermally treating the molded glass at the temperature of between 800 and 1,150 DEG C in a reducing atmosphere for 8 to 12 hours so as to obtain the inorganic aluminate luminescent microcrystalline glass. The inorganic aluminate luminescent microcrystalline glass has a relatively wide excitation spectrum in a blue light range, pure luminescent chromaticity, a stable physical property, a simple preparation method and low cost.

Description

Luminous sytull of inorganic aluminate and preparation method thereof
Technical field
The invention belongs to luminescent material, illuminating engineering technical field, relate to a kind of luminescent material with and preparation method thereof, relate in particular to luminous sytull of inorganic aluminate and preparation method thereof.This luminescent material can be applicable to semiconductor light-emitting-diode (LED).
Background technology
Along with the develop rapidly of photoelectron technology, the application of luminescent material in light-emitting device and display unit more and more widely.The luminescent material of in means of illumination and display unit, using at present is mainly fluorescent material, but in actual application, finds: the fluorescent material existence is prone to problems such as aging, that stability is not high, greatly reduces the work-ing life of means of illumination and display unit.
Summary of the invention
The technical problem that the present invention will solve is; Be prone to problems such as aging, that stability is not high to fluorescent material in the prior art, and a kind of luminous sytull of PLE, luminescent chromaticity inorganic aluminate pure, that physico-chemical property is stable that in blue light range, has broad is provided.
The technical problem that the present invention further will solve is to provide a kind of preparation method of with low cost, the luminous sytull of the simple inorganic aluminate of preparation technology.
The present invention adopts following technical scheme to solve the problems referred to above: the luminous sytull of a kind of inorganic aluminate is the material of following chemical formula: X SrO-Y Al 2O 3-Z SiO 2-R Pr 2O 3, wherein X, Y, Z, R are molfraction, value is respectively 25≤X≤40,25≤Y≤40,25≤Z≤50,0.1≤R≤2.
The value of said X, Y, Z, R is preferably 30≤X≤40,30≤Y≤40,35≤Z≤45,0.1≤R≤1 respectively.
The preparation method of the luminous sytull of inorganic aluminate is: with Strontium carbonate powder, aluminum oxide, silicon-dioxide and Praseodymium trioxide is raw material; After the above-mentioned raw materials ground and mixed; Process glass in 1550-1650 ℃ of following fusion and moulding; Under reducing atmosphere, the glass of under 800-1150 ℃, this moulding being processed is heat-treated 8-12h then, obtains the luminous sytull of inorganic aluminate.
In the said raw material, the amount of Strontium carbonate powder, aluminum oxide, silicon-dioxide and Praseodymium trioxide is according to chemical formula XSrO-YAl 2O 3-Z SiO 2-R Pr 2O 3The molfraction of institute's corresponding element takes by weighing, wherein 25≤X≤40,25≤Y≤40,25≤Z≤50,0.1≤R≤2.
Among the preparation method of the luminous sytull of inorganic aluminate; After all raw material ground and mixed; Fusion under 1580-1620 ℃ of temperature is then processed glass with fused raw material casting, then under reducing atmosphere; The glass of under 950-1100 ℃, this moulding being processed is heat-treated 9-10h, obtains the luminous sytull of inorganic aluminate.
The purity of said Strontium carbonate powder, aluminum oxide, silicon-dioxide is not less than analytical pure, and the purity of said Praseodymium trioxide is not less than 99.95%.
Described reducing atmosphere is chosen as the mixed gas or the formed atmosphere of CO gas of hydrogen, hydrogen and nitrogen.
Described reducing atmosphere can also refer to have in the reaction system atmosphere of charcoal existence.
The present invention adopts doping with rare-earth ions--the mode of praseodymium ion; Prepare a kind of novel luminous sytull; Because the special 4f electronic structure of rare earth ion, the glass of praseodymium ion doping has good fluorescent characteristic, and has advantages such as luminescent chromaticity is pure, physico-chemical property is stable.Luminous sytull of the present invention still is a kind of crystalline state and non-crystal combination, not only has the luminescent properties of luminescent crystal, and has the stability of glass, can improve the stability of photoluminescence of device greatly.The material that the present invention obtained has wide excitation spectrum at 425-475nm, is suitable for exciting of blue-light LED chip, obtains glaucous light at 480-510nm; This luminous sytull is applied to fields such as fluorescence equipment and semiconductor lighting.
Among the preparation method of the present invention, process step is simple, stable process conditions is reliable, is widely used.
Description of drawings
Below in conjunction with accompanying drawing and embodiment the present invention is described further, in the accompanying drawing:
Fig. 1 is the excitation spectrum of the embodiment of the invention 1;
Fig. 2 is the emmission spectrum of the embodiment of the invention 1;
Fig. 3 is the excitation spectrum of the embodiment of the invention 2;
Fig. 4 is the emmission spectrum of the embodiment of the invention 2;
Fig. 5 is the excitation spectrum of the embodiment of the invention 3;
Fig. 6 is the emmission spectrum of the embodiment of the invention 3;
Fig. 7 is the excitation spectrum of the embodiment of the invention 5;
Fig. 8 is the emmission spectrum of the embodiment of the invention 5.
Embodiment
Embodiment 1
Weighing Strontium carbonate powder 19.52g, aluminum oxide 10.11g, silicon-dioxide 5.95g and Praseodymium trioxide 0.22g perhaps grind alms bowl with above-mentioned raw materials through ball milling and grind, and obtain uniform powder.With the ground raw material alumina crucible of packing into, place 1600 ℃ of insulation 30min down, raw material becomes molten state, and the fused raw material is poured on the stainless-steel sheet, and the quenching moulding makes glass.Place hydrogen reducing atmosphere in 1100 ℃ of following thermal treatment 8h in the glass after the moulding, obtain 40SrO-30Al 2O 3-30SiO 2-0.2Pr 2O 3The crystallite fluorescent glass.
The sytull of present embodiment gained can be by the excited by visible light in the 430-475nm wavelength region, and under the optical excitation of 437nm royal purple, present embodiment sytull glow color presents blue-greenish colour.As shown in Figure 1, present embodiment sytull excitation wavelength range is 430-475nm, and is as shown in Figure 2; Present embodiment sytull emission wavelength ranges is 480-510nm, and its emission main peak is positioned at 492nm, is blue green light; The wide about 15nm of emission peak half-wave, luminescent chromaticity is pure.
Embodiment 2
Weighing Strontium carbonate powder 17.11g, aluminum oxide 11.82g, silicon-dioxide 5.97g and Praseodymium trioxide 0.19g perhaps grind alms bowl with above-mentioned raw materials through ball milling and grind, and obtain uniform powder.With the ground raw material alumina crucible of packing into, place 1620 ℃ of insulation 30min down, raw material becomes molten state, and the fused raw material is poured on the stainless-steel sheet, and the quenching moulding makes glass.The glass that moulding is later is placed in the carbon monoxide reducing atmosphere in 1150 ℃ of following thermal treatment 10h, obtains 35SrO-35Al 2O 3-30SiO 2-0.175Pr 2O 3The crystallite fluorescent glass.
The sytull of present embodiment gained can be by the excited by visible light in the 430-475nm wavelength region, and under the optical excitation of 445nm royal purple, present embodiment sytull glow color presents blue-greenish colour.As shown in Figure 3, present embodiment sytull excitation wavelength range is 430-475nm, and is as shown in Figure 4; Present embodiment sytull emission wavelength ranges is 480-510nm, and its emission main peak is positioned at 485nm, is blue green light; The wide about 14nm of emission peak half-wave, luminescent chromaticity is pure.
Embodiment 3
Weighing Strontium carbonate powder 17.07g, aluminum oxide 11.79g, silicon-dioxide 5.95g and Praseodymium trioxide 0.25g perhaps grind alms bowl with above-mentioned raw materials through ball milling and grind, and obtain uniform powder.With the ground raw material alumina crucible of packing into, place 1600 ℃ of insulation 30min down, raw material becomes molten state, and the fused raw material is poured on the stainless-steel sheet, and the quenching moulding makes glass.The glass that moulding is later places hydrogen reducing atmosphere in 800 ℃ of following thermal treatment 10h, obtains 35SrO-35Al 2O 3-30SiO 2-0.23Pr 2O 3The crystallite fluorescent glass.
The sytull of present embodiment gained can be by the excited by visible light in the 425-475nm wavelength region.Under the optical excitation of 441nm royal purple, present embodiment sytull glow color presents blue-greenish colour.As shown in Figure 5, present embodiment sytull excitation wavelength range is 425-475nm, and is as shown in Figure 6, and present embodiment sytull emission wavelength ranges is 480-510nm, and its emission main peak is positioned at 485nm, blue green light, and the wide about 15nm of emission peak half-wave, luminescent chromaticity is pure.
Embodiment 4
Weighing Strontium carbonate powder 13.06g, aluminum oxide 9.02g, silica 1 0.63g and Praseodymium trioxide 1.2g perhaps grind alms bowl with above-mentioned raw materials through ball milling and grind, and obtain uniform powder.With the ground raw material alumina crucible of packing into, place 1650 ℃ of insulation 30min down, raw material becomes molten state, and the fused raw material is poured on the stainless-steel sheet, and the quenching moulding makes glass.The glass that moulding is later places the carbon monoxide reducing atmosphere in 950 ℃ of following thermal treatment 12h, obtains 25SrO-25Al 2O 3-50SiO 2-1Pr 2O 3The crystallite fluorescent glass.
The sytull of present embodiment gained can be by the excited by visible light in the 430-475nm wavelength region, and under the optical excitation of 451nm royal purple, present embodiment sytull glow color presents blue-greenish colour.Its emission main peak is positioned at 491nm, blue green light.
Embodiment 5
Weighing Strontium carbonate powder 15.66g, aluminum oxide 12.84g, silicon-dioxide 5.97g and Praseodymium trioxide 0.17g perhaps grind alms bowl with above-mentioned raw materials through ball milling and grind, and obtain uniform powder.With the ground raw material alumina crucible of packing into, place 1580 ℃ of insulation 30min down, raw material becomes molten state, and the fused raw material is poured on the stainless-steel sheet, and the quenching moulding makes glass.The glass that moulding is later places hydrogen reducing atmosphere in 1000 ℃ of following thermal treatment 9h, obtains 32SrO-38Al 2O 3-30SiO 2-0.16Pr 2O 3The crystallite fluorescent glass.
The sytull of present embodiment gained can be by the excited by visible light in the 425-475nm wavelength region, and under the optical excitation of 444nm royal purple, present embodiment sytull glow color presents blue-greenish colour.As shown in Figure 7, present embodiment sytull excitation wavelength range is 430-475nm, and is as shown in Figure 8, and present embodiment sytull emission wavelength ranges is 480-510nm, and its emission main peak is positioned at 490nm, blue green light, and the wide about 12nm of emission peak half-wave, luminescent chromaticity is pure.
Embodiment 6
Weighing Strontium carbonate powder 14.19g, aluminum oxide 13.12g, silicon-dioxide 4.8g and Praseodymium trioxide 2.17g perhaps grind alms bowl with above-mentioned raw materials through ball milling and grind, and obtain uniform powder.With the ground raw material alumina crucible of packing into, place 1650 ℃ of insulation 30min down, raw material becomes molten state, and the fused raw material is poured on the stainless-steel sheet, and the quenching moulding makes glass.The glass that moulding is later places reducing atmosphere that the mixed gas of hydrogen and nitrogen forms in 950 ℃ of following thermal treatment 10h, obtains 30SrO-40Al 2O 3-25SiO 2-2Pr 2O 3The crystallite fluorescent glass.
The sytull of present embodiment gained can be by the excited by visible light in the 425-475nm wavelength region, and under the optical excitation of 451nm royal purple, present embodiment sytull emission main peak is positioned at 492nm, is blue-greenish colour.
Embodiment 7
Weighing Strontium carbonate powder 13.37g, aluminum oxide 9.24g, silica 1 0.89g and Praseodymium trioxide 0.49g perhaps grind alms bowl with above-mentioned raw materials through ball milling and grind, and obtain uniform powder.With the ground raw material alumina crucible of packing into, place 1630 ℃ of insulation 30min down, raw material becomes molten state, and the fused raw material is poured on the stainless-steel sheet, and the quenching moulding makes glass.The glass that moulding is later places the carbon monoxide reducing atmosphere in 1000 ℃ of following thermal treatment 10h, obtains 25SrO-25Al 2O 3-50SiO 2-0.4Pr 2O 3The crystallite fluorescent glass.
The sytull of present embodiment gained can be by the excited by visible light in the 425-475nm wavelength region, and under the optical excitation of 447nm royal purple, present embodiment sytull emission main peak is positioned at 492nm, is blue-greenish colour.
Embodiment 8
Weighing Strontium carbonate powder 13.38g, aluminum oxide 12.32g, silicon-dioxide 8.17g and Praseodymium trioxide 0.103g perhaps grind alms bowl with above-mentioned raw materials through ball milling and grind, and obtain uniform powder.With the ground raw material alumina crucible of packing into, place 1550 ℃ of insulation 30min down, raw material becomes molten state, and the fused raw material is poured on the stainless-steel sheet, and the quenching moulding makes glass.The glass that moulding is later places the reaction system of charcoal existence in 1150 ℃ of following thermal treatment 11h, obtains 30SrO-40Al 2O 3-45SiO 2-0.1Pr 2O 3The crystallite fluorescent glass.
The sytull of present embodiment gained can be by the excited by visible light in the 430-475nm wavelength region, and under the optical excitation of 442nm royal purple, present embodiment sytull emission main peak is positioned at 491nm, is blue-greenish colour.

Claims (8)

1. the luminous sytull of inorganic aluminate is characterized in that, is the material of following chemical formula: X SrO-Y Al 2O 3-Z SiO 2-R Pr 2O 3, wherein X, Y, Z, R are molfraction, its value is respectively 25≤X≤40,25≤Y≤40,25≤Z≤50,0.1≤R≤2.
2. the luminous sytull of inorganic aluminate according to claim 1 is characterized in that the value of said X, Y, Z, R is respectively 30≤X≤40,30≤Y≤40,35≤Z≤45,0.1≤R≤1.
3. the preparation method of claim 1 or the luminous sytull of 2 described inorganic aluminates; It is characterized in that, be raw material with Strontium carbonate powder, aluminum oxide, silicon-dioxide and Praseodymium trioxide, after the above-mentioned raw materials ground and mixed; Process glass in 1550-1650 ℃ of following fusion and moulding; Under reducing atmosphere, the glass of under 800-1150 ℃, this moulding being processed is heat-treated 8-12h then, obtains the luminous sytull of inorganic aluminate.
4. the preparation method of the luminous sytull of inorganic aluminate according to claim 3 is characterized in that, in the said raw material, the amount of Strontium carbonate powder, aluminum oxide, silicon-dioxide and Praseodymium trioxide is according to chemical formula XSrO-Y Al 2O 3-Z SiO 2-R Pr 2O 3The molfraction of institute's corresponding element takes by weighing, wherein 25≤X≤40,25≤Y≤40,25≤Z≤50,0.1≤R≤2.
5. the preparation method of the luminous sytull of inorganic aluminate according to claim 4; It is characterized in that, after all raw material ground and mixed, fusion under 1580-1620 ℃ of temperature; Then fused raw material casting is processed glass; Under reducing atmosphere, the glass of under 950-1100 ℃, this moulding being processed is heat-treated 9-10h then, obtains the luminous sytull of inorganic aluminate.
6. the preparation method of the luminous sytull of inorganic aluminate according to claim 5 is characterized in that the purity of said Strontium carbonate powder, aluminum oxide, silicon-dioxide is not less than analytical pure, and the purity of said Praseodymium trioxide is not less than 99.95%.
7. according to the preparation method of any luminous sytull of described inorganic aluminate of claim 3～6, it is characterized in that described reducing atmosphere is chosen as the mixed gas or the formed atmosphere of CO gas of hydrogen, hydrogen and nitrogen.
8. according to the preparation method of any luminous sytull of described inorganic aluminate of claim 3～6, it is characterized in that described reducing atmosphere is meant the atmosphere that has charcoal to exist in the reaction system.
CN2009101898548A 2009-09-02 2009-09-02 Inorganic aluminate luminescent microcrystalline glass and preparation method thereof Expired - Fee Related CN102001827B (en)

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Publication number Priority date Publication date Assignee Title
US6287993B1 (en) * 1998-09-22 2001-09-11 Kabushiki Kaisha Ohara Long-lasting phosphorescent glasses and glass-ceramics
CN1717374A (en) * 2002-11-29 2006-01-04 独立行政法人科学技术振兴机构 Luminescent glass

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6287993B1 (en) * 1998-09-22 2001-09-11 Kabushiki Kaisha Ohara Long-lasting phosphorescent glasses and glass-ceramics
CN1717374A (en) * 2002-11-29 2006-01-04 独立行政法人科学技术振兴机构 Luminescent glass

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