CN101054521A - Red luminescence phosphor - Google Patents

Red luminescence phosphor Download PDF

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Publication number
CN101054521A
CN101054521A CNA2007101057505A CN200710105750A CN101054521A CN 101054521 A CN101054521 A CN 101054521A CN A2007101057505 A CNA2007101057505 A CN A2007101057505A CN 200710105750 A CN200710105750 A CN 200710105750A CN 101054521 A CN101054521 A CN 101054521A
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王海容
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

The invention relates to a red luminous fluorescent powder, the formula of which is MM'aAbOd:Mnx,Ry, wherein M is at least one of Li, Na, K, Rb, Mg, Ca, Sr, Ba, Zn, Zr, Ce and Hf, M' is at least one of Al, Si, B, F, Cl and Br, A is at least one of V and P, R is at least one of Eu, Sm, Dy, Nd, Pr, Ho, Er, Bi and Cr and 0.1<=a<=12, 0.1<=b<=10, 1<=d<=25, 0.0001<=x<=0.5 and 0<=y<=0.5. The red luminous fluorescent powder in the invention is a composite oxide, prepared in high-temperature solid-phase method. The substrate contains no toxic or hazardous chemical components such as precious rare earth, cadmium and sulfer. The invention has the advantages of simple preparing process, low production cost, stable chemical properties, good luminous performance, high thermal-stability, wide excitation wavelength and capable of being effectively excited by ultraviolet light, purple light or blue light LED etc. The invention can be widely used in white light LED.

Description

A kind of red luminescence phosphor
Technical field
The present invention relates to a kind of red luminescence phosphor, particularly a kind of can effectively being excited and produce the fluorescent material of red emission by UV-light, purple light or blue-ray LED.
Background technology
White light-emitting diodes (W-LED, white-light-emitting diode) as a kind of junction semiconductor electroluminescent device, have that operating voltage is low, current consumption is few, light weight, volume is little, the life-span is long, radiationless, pollution-free, series of advantages such as luminescence response fast, shock resistance and security are good and receiving much concern, be referred to as the 4th generation the solid cold light source.White light LEDs is mainly realized white light by two kinds of approach at present: a kind of is the fluorescence conversion hysteria, promptly uses single led chip and phosphor combination luminous; Another kind method is to adopt red, green, blue three-color LED chip portfolio luminous.
White light LEDs has been subjected to showing great attention to of countries in the world as the green illumination light source of energy-conserving and environment-protective of new generation, utilize UV-light, purple light or blue-ray LED excitated fluorescent powder and produce the main flow that white light is present white light LEDs development, the fluorescent material development of technology has important effect to the development of white light LEDs, and its performance directly influences brightness, chromaticity coordinates, colour temperature and the color developing etc. of white light LEDs.The ultraviolet leds technology is still immature at present, and existing red fluorescence powder is relatively poor at the excitating performance of purple light or the luminous wave band of blue-ray LED, and luminous efficiency is lower, becomes the bottleneck of LED with fluorescent material and even white light LEDs development.The LED that has has researched and developed mainly contains Ca with red fluorescence powder 3(VO4) 2: Eu 3+, YVO 4: Eu 3+, Y 2O 3: Eu 3+, Bi 3+, Y 2O 2S:Eu 3+, CaO:Eu 3+, CaMoO 4: Eu 3+, (Gd, Y, Eu) 2(MoO 4) 3: Sm 3+, (Sr, Ca) S:Eu 2+, Ca 5(SiO4) 2Cl 2: Eu 2+, Sr 2Si 5N 8: Eu 2+All also do not reach requirement of actual application Deng, these red fluorescence powders luminous efficiency, thermostability and chemical stability under purple light or blue-ray LED excite, so the LED of development of new becomes the focus of domestic and international research with red luminescence phosphor.
Summary of the invention
The objective of the invention is at the problems referred to above, propose that a kind of chemical property is stable, good luminous performance, Heat stability is good, can effectively be excited by UV-light, purple light or blue-ray LED and produce the fluorescent material of red emission.
The objective of the invention is to be achieved through the following technical solutions:
The chemical formula of a kind of red luminescence phosphor of the present invention is: MM ' aA bO d: Mn x, R y,
Wherein, M is at least a among Li, Na, K, Rb, Mg, Ca, Sr, Ba, Zn, Zr, Ce, the Hf;
M ' is at least a among Al, Si, B, F, Cl, the Br;
A is at least a among V or the P;
R is at least a among Eu, Sm, Dy, Nd, Pr, Ho, Er, Bi, the Cr;
0≤a≤12，0.1≤b≤10，1≤d≤25，0.0001≤x≤0.5，0≤y≤0.5。
Compared with prior art, red luminescence phosphor of the present invention is a kind of composite oxide material, the advantage that have that preparation technology is simple, production cost is low, chemical property is stable, good luminous performance, Heat stability is good, excitation wavelength range are wide, can effectively be excited by UV-light, purple light or blue-ray LED can be widely used in white light LEDs.
Ultraviolet leds of the present invention is meant that emission wavelength is the photodiode of 200nm～380nm;
Purple LED of the present invention is meant that emission wavelength is the photodiode of 380nm～420nm;
Blue-ray LED of the present invention is meant that emission wavelength is the photodiode of 420nm～490nm.
Red luminescence phosphor of the present invention can adopt prepared such as high temperature solid phase synthesis, sol-gel method, microwave sintering synthesis method, the technological process of its high temperature solid phase synthesis is: ground and mixed is even in proportion with various raw materials, in air or reducing atmosphere in 500～1600 ℃ of following sintering 1～10 hour, with the gained sinter levigate the finished product.
Description of drawings
Fig. 1 is the emmission spectrum figure of fluorescent material under the 398nm wavelength excites in the embodiment of the invention 1
Fig. 2 is the exciting light spectrogram of fluorescent material in 200～500nm wavelength region in the embodiment of the invention 1
Embodiment
Embodiment 1: take by weighing Quilonum Retard (Li 2CO 3) 1.1g, Vanadium Pentoxide in FLAKES (V 2O 5) 1.82g, Manganse Dioxide (MnO 2) 0.012g, europiumsesquioxide (Eu 2O 3) 0.035g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 650 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.Its emmission spectrum is seen Fig. 1, and main emission peak also has very strong emission in 665～715nm scope about 618nm, totally present pure red emission; Its excitation spectrum is seen Fig. 2, and main excitation peak can effectively be excited by the UV-light in 200～500nm scope, purple light or blue light near 398nm, particularly at 390～410nm purple light wave band and 460～500nm blue wave band very strong absorption is arranged.
Embodiment 2: take by weighing Quilonum Retard (Li 2CO 3) 1.1g, Vanadium Pentoxide in FLAKES (V 2O 5) 1.82g, Manganse Dioxide (MnO 2) 0.012g, samarium sesquioxide (Sm 2O 3) 0.035g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 650 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.
Embodiment 3: take by weighing Strontium carbonate powder (SrCO 3) 4.4g, Vanadium Pentoxide in FLAKES (V 2O 5) 1.45g, Secondary ammonium phosphate ((NH 4) 2HPO 4) 0.6g, Manganse Dioxide (MnO 2) 0.012g, europiumsesquioxide (Eu 2O 3) 0.035g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 750 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.
Embodiment 4: take by weighing Strontium carbonate powder (SrCO 3) 4.4g, Vanadium Pentoxide in FLAKES (V 2O 5) 1.45g, Secondary ammonium phosphate ((NH 4) 2HPO 4) 0.6g, Manganse Dioxide (MnO 2) 0.012g, samarium sesquioxide (Sm 2O 3) 0.035g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 750 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.
Embodiment 5: take by weighing lime carbonate (CaCO 3) 2.0g, Quilonum Retard (Li 2CO 3) 0.37g, Vanadium Pentoxide in FLAKES (V 2O 5) 1.45g, Secondary ammonium phosphate ((NH 4) 2HPO 4) 0.6g, Manganse Dioxide (MnO 2) 0.012g, europiumsesquioxide (Eu 2O 3) 0.035g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 700 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.
Embodiment 6: take by weighing lime carbonate (CaCO 3) 2.0g, Quilonum Retard (Li 2CO 3) 0.37g, Vanadium Pentoxide in FLAKES (V 2O 5) 1.45g, Secondary ammonium phosphate ((NH 4) 2HPO 4) 0.6g, Manganse Dioxide (MnO 2) 0.012g, samarium sesquioxide (Sm 2O 3) 0.035g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 700 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.
Embodiment 7: take by weighing lime carbonate (CaCO 3) 2.0g, Quilonum Retard (Li 2CO 3) 0.37g, Vanadium Pentoxide in FLAKES (V 2O 5) 1.82g, Manganse Dioxide (MnO 2) 0.012g, europiumsesquioxide (Eu 2O 3) 0.035g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 700 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.
Embodiment 8: take by weighing lime carbonate (CaCO 3) 2.0g, Quilonum Retard (Li 2CO 3) 0.37g, Vanadium Pentoxide in FLAKES (V 2O 5) 1.82g, Manganse Dioxide (MnO 2) 0.012g, samarium sesquioxide (Sm 2O 3) 0.035g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 700 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.
Embodiment 9: take by weighing zirconium dioxide (ZrO 2) 2.46g, Quilonum Retard (Li 2CO 3) 0.37g, Vanadium Pentoxide in FLAKES (V 2O 5) 1.82g, Manganse Dioxide (MnO 2) 0.012g, europiumsesquioxide (Eu 2O 3) 0.035g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 700 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.
Embodiment 10: take by weighing zirconium dioxide (ZrO 2) 2.46g, Quilonum Retard (Li 2CO 3) 0.37g, Vanadium Pentoxide in FLAKES (V 2O 5) 1.82g, Manganse Dioxide (MnO 2) 0.012g, samarium sesquioxide (Sm 2O 3) 0.035g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 700 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.
Embodiment 11: take by weighing lime carbonate (CaCO 3) 3.0g, Vanadium Pentoxide in FLAKES (V 2O 5) 1.45g, Secondary ammonium phosphate ((NH 4) 2HPO 4) 0.6g, Manganse Dioxide (MnO 2) 0.012g, europiumsesquioxide (Eu 2O 3) 0.035g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 750 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.
Embodiment 12: take by weighing lime carbonate (CaCO 3) 3.0g, Vanadium Pentoxide in FLAKES (V 2O 5) 1.45g, Secondary ammonium phosphate ((NH 4) 2HPO 4) 0.6g, Manganse Dioxide (MnO 2) 0.012g, samarium sesquioxide (Sm 2O 3) 0.035g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 750 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.
Embodiment 13: weighing sodium carbonate (Na 2CO 3) 1.59g, Vanadium Pentoxide in FLAKES (V 2O 5) 1.82g, Manganse Dioxide (MnO 2) 0.012g, europiumsesquioxide (Eu 2O 3) 0.035g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 650 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.
Embodiment 14: weighing sodium carbonate (Na 2CO 3) 1.59g, Vanadium Pentoxide in FLAKES (V 2O 5) 1.82g, Manganse Dioxide (MnO 2) 0.012g, samarium sesquioxide (Sm 2O 3) 0.035g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 650 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.
Embodiment 15: take by weighing Quilonum Retard (Li 2CO 3) 0.74g, aluminum oxide (Al 2O 3) 1.8g, boric acid (H 3BO 3) 0.25g, Secondary ammonium phosphate ((NH 4) 2HPO 4) 2.8g, Manganse Dioxide (MnO 2) 0.02g, europiumsesquioxide (Eu 2O 3) 0.07g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 850 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.
Embodiment 16: take by weighing Quilonum Retard (Li 2CO 3) 0.74g, aluminum oxide (Al 2O 3) 1.8g, boric acid (H 3BO 3) 0.25g, Secondary ammonium phosphate ((NH 4) 2HPO 4) 2.8g, Manganse Dioxide (MnO 2) 0.02g, samarium sesquioxide (Sm 2O 3) 0.07g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 850 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.
Embodiment 17: take by weighing Quilonum Retard (Li 2CO 3) 0.74g, aluminum oxide (Al 2O 3) 3.6g, boric acid (H 3BO 3) 0.5g, Secondary ammonium phosphate ((NH 4) 2HPO 4) 2.8g, silicon-dioxide (SiO 2) 1.2g, Manganse Dioxide (MnO 2) 0.02g, europiumsesquioxide (Eu 2O 3) 0.07g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 1000 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.
Embodiment 18: take by weighing Quilonum Retard (Li 2CO 3) 0.74g, aluminum oxide (Al 2O 3) 3.6g, boric acid (H 3BO 3) 0.5g, Secondary ammonium phosphate ((NH 4) 2HPO 4) 2.8g, silicon-dioxide (SiO 2) 1.2g, Manganse Dioxide (MnO 2) 0.02g, samarium sesquioxide (Sm 2O 3) 0.07g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 1000 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.
Embodiment 19: take by weighing lime carbonate (CaCO 3) 2.0g, aluminum oxide (Al 2O 3) 1.8g, boric acid (H 3BO 3) 0.25g, Secondary ammonium phosphate ((NH 4) 2HPO 4) 2.8g, Manganse Dioxide (MnO 2) 0.02g, europiumsesquioxide (Eu 2O 3) 0.07g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 1150 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.
Embodiment 20: take by weighing lime carbonate (CaCO 3) 2.0g, aluminum oxide (Al 2O 3) 1.8g, boric acid (H 3BO 3) 0.25g, Secondary ammonium phosphate ((NH 4) 2HPO 4) 2.8g, Manganse Dioxide (MnO 2) 0.02g, samarium sesquioxide (Sm 2O 3) 0.07g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 1150 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.
Embodiment 21: take by weighing magnesium fluoride (MgF 2) 0.86g, aluminum oxide (Al 2O 3) 1.8g, boric acid (H 3BO 3) 0.25g, Secondary ammonium phosphate ((NH 4) 2HPO 4) 2.8g, Manganse Dioxide (MnO 2) 0.02g, europiumsesquioxide (Eu 2O 3) 0.07g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 850 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.
Embodiment 22: take by weighing magnesium fluoride (MgF 2) 0.86g, aluminum oxide (Al 2O 3) 1.8g, boric acid (H 3BO 3) 0.25g, Secondary ammonium phosphate ((NH 4) 2HPO 4) 2.8g, Manganse Dioxide (MnO 2) 0.02g, samarium sesquioxide (Sm 2O 3) 0.07g, after abundant ground and mixed was even, the alumina crucible roasting in air of packing into was in 850 ℃ of insulations 3 hours, with the levigate the finished product that get of gained sinter.

Claims (2)

1, a kind of red luminescence phosphor is characterized in that: its chemical formula is: MM ' aA bO d: Mn x, R y,
Wherein, M is at least a among Li, Na, K, Rb, Mg, Ca, Sr, Ba, Zn, Zr, Ce, the Hf;
M ' is at least a among Al, Si, B, F, Cl, the Br;
A is at least a among V or the P;
R is at least a among Eu, Sm, Dy, Nd, Pr, Ho, Er, Bi, the Cr;
0≤a≤12，0.1≤b≤10，1≤d≤25，0.0001≤x≤0.5，0≤y≤0.5。
2, a kind of red luminescence phosphor according to claim 1 is characterized in that: described red luminescence phosphor can effectively be excited by UV-light, purple light or blue-ray LED and produce red emission.
CNA2007101057505A 2007-05-29 2007-05-29 Red luminescence phosphor Pending CN101054521A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102399558A (en) * 2011-11-24 2012-04-04 苏州大学 Vanadate red phosphor, preparation method and application
CN103013511A (en) * 2013-01-14 2013-04-03 福州大学 Red fluorescent powder for white-light LEDs (light-emitting diodes), and preparation method and application thereof
CN107384392A (en) * 2017-06-28 2017-11-24 陕西科技大学 Using vanadate as Er ions yellowish green fluorescent powder of matrix and preparation method thereof
CN107384391A (en) * 2017-06-28 2017-11-24 陕西科技大学 Using vanadate as dysprosium doped white fluorescent powder of matrix and preparation method thereof
CN113387567A (en) * 2020-03-13 2021-09-14 包头稀土研究院 Red fluorescent glass and preparation method thereof
CN113387568A (en) * 2020-03-13 2021-09-14 包头稀土研究院 Red fluorescent glass material and preparation method and application thereof
CN115298141A (en) * 2020-03-31 2022-11-04 松下知识产权经营株式会社 Method for producing halide

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102399558A (en) * 2011-11-24 2012-04-04 苏州大学 Vanadate red phosphor, preparation method and application
CN103013511A (en) * 2013-01-14 2013-04-03 福州大学 Red fluorescent powder for white-light LEDs (light-emitting diodes), and preparation method and application thereof
CN107384392A (en) * 2017-06-28 2017-11-24 陕西科技大学 Using vanadate as Er ions yellowish green fluorescent powder of matrix and preparation method thereof
CN107384391A (en) * 2017-06-28 2017-11-24 陕西科技大学 Using vanadate as dysprosium doped white fluorescent powder of matrix and preparation method thereof
CN113387567A (en) * 2020-03-13 2021-09-14 包头稀土研究院 Red fluorescent glass and preparation method thereof
CN113387568A (en) * 2020-03-13 2021-09-14 包头稀土研究院 Red fluorescent glass material and preparation method and application thereof
CN113387568B (en) * 2020-03-13 2022-03-18 包头稀土研究院 Red fluorescent glass material and preparation method and application thereof
CN113387567B (en) * 2020-03-13 2022-03-18 包头稀土研究院 Red fluorescent glass and preparation method thereof
CN115298141A (en) * 2020-03-31 2022-11-04 松下知识产权经营株式会社 Method for producing halide

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