CN104152142A - Red fluorescent material and preparation method thereof - Google Patents
Red fluorescent material and preparation method thereof Download PDFInfo
- Publication number
- CN104152142A CN104152142A CN201410393991.4A CN201410393991A CN104152142A CN 104152142 A CN104152142 A CN 104152142A CN 201410393991 A CN201410393991 A CN 201410393991A CN 104152142 A CN104152142 A CN 104152142A
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- red fluorescence
- fluorescent material
- preparation
- red fluorescent
- gram
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- 239000000463 material Substances 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000126 substance Substances 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000011575 calcium Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium oxide Inorganic materials O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims description 2
- PVADDRMAFCOOPC-UHFFFAOYSA-N oxogermanium Chemical compound [Ge]=O PVADDRMAFCOOPC-UHFFFAOYSA-N 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 23
- 230000005284 excitation Effects 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract description 5
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 2
- 150000002910 rare earth metals Chemical class 0.000 abstract description 2
- 229910052693 Europium Inorganic materials 0.000 abstract 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 abstract 1
- 239000006104 solid solution Substances 0.000 abstract 1
- 229910005793 GeO 2 Inorganic materials 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 238000001354 calcination Methods 0.000 description 9
- 238000000695 excitation spectrum Methods 0.000 description 9
- 239000004570 mortar (masonry) Substances 0.000 description 9
- 238000000295 emission spectrum Methods 0.000 description 8
- 241001025261 Neoraja caerulea Species 0.000 description 3
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Abstract
The invention discloses a red fluorescent material and a preparation method thereof. The invention relates to the technical field of rare earth luminescent material. The red fluorescent material provided by the invention is europium-activated fluorescent powder, and is a solid solution. The material has a chemical general formula of Ca2-x-yGe7O16:xA,yB. In the formula, A is Eu; B is at least one of Li, Na, and K; x is greater than 0 and no greater than 0.15; and y is no smaller than 0 and no greater than 0.15. The preparation method of the red fluorescent material comprises the following steps: various materials are weighed according to the ratio in the chemical general formula, and are ground and well mixed; the mixture is calcined for 10-16h under a temperature of 900-1050 DEG C; and the product is cooled and pulverized, such that the red fluorescent material is obtained. The fluorescent powder provided by the invention has good chemical stability, high excitation efficiency, and high thermal stability. The material can match near-ultraviolet and blue-light LED, and is a type of novel red fluorescent powder used in a white-light LED.
Description
Technical field
The present invention relates to a kind of red fluorescence material and preparation method thereof, belong to rare earth luminescent material technical field.
Background technology
The birth of semiconductor light emitting diode device (LED) is that green illumination is pointed out new hope.LED is owing to having the features such as less energy-consumption, high-level efficiency, long lifetime, has significant advantage compared with the conventional lighting source such as incandescent light, electricity-saving lamp in the past.At present have following several taking LED as the white light implementation of main a new generation's illumination system: the first, by by integrated the LED chip of different colours (normally red-green-blue) and be mixed into white light.But the bias voltage difference of different chips, circuit control is had relatively high expectations, and cost is very high.The second is the lighting theory of using for reference luminescent lamp, applies fluorescent material at LED chip surface, obtains white light.As this year day in 1996, first Ya company of Japan developed yttrium aluminum garnet (YAG) fluorescent material of Yellow light-emitting low temperature, coordinated blue-ray LED to obtain high efficiency white light source.Blue light excitation YAG fluorescent material, part blue light is absorbed by fluorescent material and inspires gold-tinted, and rest part blue light becomes white light with yellow light mix.This white light implementation cost is lower, be the mode extensively adopting at present, but this fluorescent material lacks ruddiness composition, so colour rendering index is bad, and its colour temperature is higher, and is difficult to regulate, and can not obtain warm white.Also having the auxiliary mode that produces white light of a kind of fluorescent material is to utilize near ultraviolet LED to excite red-green-blue fluorescent material to mix to realize white light, this ultraviolet leds has stronger excitation intensity and the efficiency of conversion of Geng Gao, but wherein red fluorescence powder is lower with respect to bluish-green light-emitting phosphor efficiency, as Y
2o
2s:Eu
3+fluorescent material, energy conversion efficiency is low, and poor heat stability.At present, still lack excellent performance on market, the white-light illuminating LED three primary colors fluorescent powder based near ultraviolet or blue light diode, especially can be by near-ultraviolet light and blue-light excited red fluorescence powder.
Summary of the invention
The object of this invention is to provide a kind of near ultraviolet or blue-light excited high thermal stability red fluorescence material and preparation method thereof, make it solve in prior art the ruddiness composition of emmission spectrum few and make its colour rendering index on the low side, can not synthesize the problem of single white light, and make its chemical stability good, launching efficiency is high, thermostability is high, can be simultaneously by near ultraviolet and blue-light excited.
The chemical general formula of red fluorescence powder of the present invention is Ca
2-x-yge
7o
16: xA, yB, wherein A is Eu, B is the one in Li, Na, K, 0<x≤0.2,0≤y≤0.2.
The preparation method of red fluorescence powder of the present invention is:
(1) take following raw material by the proportioning in chemical general formula: the oxide compound of calcium carbonate, A, the carbonate of B, germanium oxide;
(2) former abrasive lapping step (1) being taken also mixes;
(3) raw material mixing is calcined to 10-16h at 900 DEG C-1050 DEG C, be then cooled to room temperature, grind and get final product.
While grinding in step of the present invention (2), in raw material, add raw material total mass 3-4 ethanol doubly, can make grinding more abundant, easily mix.
Beneficial effect of the present invention is:
Red fluorescence powder chemical heat good stability of the present invention, launching efficiency is high, can excite lower acquisition to be positioned at the emitting red light of 618nm left and right near ultraviolet (395nm), blue light (466nm), can mate with near ultraviolet and blue-ray LED, be a kind of novel white light LEDs red fluorescence powder.
Brief description of the drawings
Fig. 1 is the Ca that embodiment 1 prepares
2ge
7o
16: Eu
3+the absorption spectrum of fluorescent material and exciting light spectrogram;
Fig. 2 is the utilizing emitted light spectrogram of fluorescent material in embodiment of the present invention 1-6;
Fig. 3 is the graph of relation of luminous intensity and the x value of fluorescent material;
Fig. 4 is the utilizing emitted light spectrogram of fluorescent material in embodiment of the present invention 7-9;
Fig. 5 is the thermostability utilizing emitted light spectrogram of fluorescent material in the embodiment of the present invention 7;
Fig. 6 is thermostability and the commercial powder Y of fluorescent material in the embodiment of the present invention 7
2o
3: Eu
3+contrast.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail, but protection scope of the present invention is not limited to described content.
Embodiment 1
The chemical general formula of red fluorescence material prepared by the present embodiment is Ca
1.99ge
7o
16: 0.01Eu
3+.
Described in the present embodiment, the preparation method of red fluorescence material is: take CaCO
3(analytical pure) 0.199 gram, GeO
2(analytical pure) 0.7325 gram, Eu
2o
3(99.99%) 0.0017 gram; Add 2 grams of ethanol, fully grind with agate mortar, send into powder stove at 900 DEG C of calcining 10h after mixing, cooling rear grinding obtains red fluorescence material.
The excitation spectrum of gained fluorescent material is shown in Fig. 1, its excitation peak is at 395nm as seen from Figure 1, there is stronger exciting at 466nm place, the f-f transition that all comes from Eu ion excites, its excitation wavelength is just in time positioned near ultraviolet and blue light position, mate with LED chip excitation wavelength, be applicable near ultraviolet and blue-ray LED and excite.
Embodiment 2
The chemical general formula of red fluorescence material prepared by the present embodiment is Ca
1.97ge
7o
16: 0.03Eu
3+
Described in the present embodiment, the preparation method of red fluorescence material is: take CaCO
3(analytical pure) 0.197 gram, GeO
2(analytical pure) 0.7325 gram, Eu
2o
3(99.99%) 0.0053 gram.Add 2.2 grams of ethanol, fully grind with agate mortar, send into powder stove at 920 DEG C of calcining 11h after mixing, cooling rear grinding obtains red fluorescence material.
The excitation spectrum of gained fluorescent material is shown in Fig. 2, and the main emission peak of its emission spectrum, at 618nm, sends bright red light.
Embodiment 3
The chemical general formula of red fluorescence material prepared by the present embodiment is Ca
1.95ge
7o
16: 0.05Eu
3+
Described in the present embodiment, the preparation method of red fluorescence material is: take CaCO
3(analytical pure) 0.195 gram, GeO
2(analytical pure) 0.7325 gram, Eu
2o
3(99.99%) 0.0087 gram.Add 2.3 grams of ethanol, fully grind with agate mortar, send into powder stove at 910 DEG C of calcining 11.5h after mixing, cooling rear grinding obtains red fluorescence material.
The excitation spectrum of gained fluorescent material is shown in Fig. 2, and the main emission peak of its emission spectrum, at 618nm, sends bright red light.
Embodiment 4
The chemical general formula of red fluorescence material prepared by the present embodiment is Ca
1.91ge
7o
16: 0.09Eu
3+
Described in the present embodiment, the preparation method of red fluorescence material is: take CaCO
3(analytical pure) 0.191 gram, GeO
2(analytical pure) 0.7325 gram, Eu
2o
3(99.99) 0.0157 grams.Add 2.4 grams of ethanol, fully grind with agate mortar, after mixing, send into powder stove at 940 DEG C of calcining 12h, obtain red fluorescence material.
The excitation spectrum of gained fluorescent material is shown in Fig. 2, and the main emission peak of its emission spectrum, at 618nm, sends bright red light.
Embodiment 5
The chemical general formula of red fluorescence material prepared by the present embodiment is Ca
1.88ge
7o
16: 0.12Eu
3+
Described in the present embodiment, the preparation method of red fluorescence material is: take CaCO
3(analytical pure) 0.188 gram,, GeO
2(analytical pure) 0.7325 gram, Eu
2o
3(99.99%) 0.0211 gram.Add 2.5 grams of ethanol, fully grind with agate mortar, after mixing, send into powder stove at 950 DEG C of calcining 12.5h, obtain red fluorescence material.
The excitation spectrum of gained fluorescent material is shown in Fig. 2, and the main emission peak of its emission spectrum, at 618nm, sends bright red light.
Embodiment 6
The chemical general formula of red fluorescence material prepared by the present embodiment is Ca
1.85ge
7o
16: 0.15Eu
3+
Described in the present embodiment, the preparation method of red fluorescence material is: take CaCO
3(analytical pure) 0.185 gram, GeO
2(analytical pure) 0.7325 gram, Eu
2o
3(99.99%) 0.0264 gram.Add 2.6 grams of ethanol, fully grind with agate mortar, after mixing, send into powder stove at 970 DEG C of calcining 13h, obtain red fluorescence material.
The excitation spectrum of gained fluorescent material is shown in Fig. 2, and the main emission peak of its emission spectrum, at 618nm, sends bright red light.By getting x values different between 0<x≤0.15, can prepare the Ca of different x values in order to upper method
2-x-yge
7o
16: xA, yB fluorescent material, fluorescent material Ca
2-x-yge
7o
16: xA, the value graph of relation of the luminous intensity of yB and x is shown in Fig. 3, and as seen from Figure 3, luminous intensity increases with the increase of x value, and in the time that x value exceedes 0.12, luminous intensity starts to decline, and the optimum value of x value is between 0.10-0.12.
Embodiment 7
The chemical general formula of red fluorescence material prepared by the present embodiment is Ca
1.76ge
7o
16: 0.12Eu
3+, 0.12Li
+
Described in the present embodiment, the preparation method of red fluorescence material is: take CaCO
3(analytical pure) 0.188 gram, GeO
2(analytical pure) 0.7325 gram, Li
2cO
3(99.99%) 0.0044 gram, Eu
2o
3(99.99%) 0.0211 gram, add 2.7 grams of ethanol, fully grind with agate mortar, after mixing, send into powder stove at 1000 DEG C of calcining 14h, obtain red fluorescence material.
The excitation spectrum of gained fluorescent material is shown in Fig. 4, and the main emission peak of its emission spectrum, at 618nm, sends bright red light.Fig. 5 is the thermostability utilizing emitted light spectrogram of the fluorescent material for preparing of embodiment 7, and along with the rising of temperature, emissive porwer reduces gradually, and in the time that temperature reaches 230 degree, it is original 63% that emissive porwer is reduced to, and than commercial powder Y
2o
2: Eu
3+(when temperature reaches 230 when spending, commercial powder Y
2o
2: Eu
3+emissive porwer be reduced to original intensity 56%), as shown in Figure 6, think that the red fluorescence powder that the present invention prepares has higher thermostability.
Embodiment 8
The chemical general formula of red fluorescence material prepared by the present embodiment is Ca
1.76ge
7o
16: 0.12Eu
3+, 0.12Na
+
Take CaCO
3(analytical pure) 0.188 gram, GeO
2(analytical pure) 0.7325 gram, Na
2cO
3(99.99%) 0.0064, Eu
2o
3gram (99.99%) 0.0211 gram, add 2.7 grams of ethanol, fully grind with agate mortar, after mixing, send into powder stove at 1020 DEG C of calcining 15h, obtain red fluorescence material.
The excitation spectrum of gained fluorescent material is shown in Fig. 4, and the main emission peak of its emission spectrum, at 618nm, sends bright red light.
Embodiment 9
The chemical general formula of red fluorescence material prepared by the present embodiment is Ca
1.76ge
7o
16: 0.12Eu
3+, 0.12K
+
Take CaCO
3(analytical pure) 0.188 gram, GeO
2(analytical pure) 0.7325 gram, K
2cO
3(99.99%) 0.0089, Eu
2o
3gram (99.99%) 0.0211 gram.Add 2.7 grams of ethanol, fully grind with agate mortar, after mixing, send into powder stove at 1050 DEG C of calcining 16h, obtain red fluorescence material.
The excitation spectrum of gained fluorescent material is shown in Fig. 4, and the main emission peak of its emission spectrum, at 618nm, sends bright red light, as seen from Figure 4, and Li
+do charge compensation agent with respect to K
+, Na
+effect is best, and three kinds of charge compensation agent can make the luminous of fluorescent material be enhanced, and it excites and transmitting figure spectral shape does not change.
Claims (3)
1. a red fluorescence material, is characterized in that, the chemical general formula of described red fluorescence material is Ca
2-x-yge
7o
16: xA, yB, wherein A is Eu, B is the one in Li, Na, K, 0<x≤0.15,0≤y≤0.15.
2. the preparation method of red fluorescence material described in claim 1, is characterized in that, specifically comprises the steps:
(1) take following raw material by the proportioning in chemical general formula: the oxide compound of calcium carbonate, A, the carbonate of B, germanium oxide;
(2) former abrasive lapping step (1) being taken also mixes;
(3) raw material mixing is calcined to 10-16h at 900 DEG C-1050 DEG C, be then cooled to room temperature, grind and get final product.
3. the preparation method of red fluorescence material according to claim 2, is characterized in that: while grinding in step (2), in raw material, add raw material total mass 3-4 ethanol doubly.
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|---|---|---|---|
| CN201410393991.4A CN104152142B (en) | 2014-08-12 | 2014-08-12 | A kind of red fluorescence material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410393991.4A CN104152142B (en) | 2014-08-12 | 2014-08-12 | A kind of red fluorescence material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104152142A true CN104152142A (en) | 2014-11-19 |
| CN104152142B CN104152142B (en) | 2016-05-25 |
Family
ID=51877774
Family Applications (1)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109705864A (en) * | 2018-11-23 | 2019-05-03 | 长春理工大学 | A kind of red fluorescence powder and preparation method thereof that luminous efficiency is high |
| CN113388395A (en) * | 2020-03-13 | 2021-09-14 | 包头稀土研究院 | Red fluorescent material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020038861A1 (en) * | 2000-09-29 | 2002-04-04 | Sumitomo Chemical Company, Limited | Fluorescent substances for vacuum ultraviolet radiation excited light-emitting devices |
| CN101956237A (en) * | 2010-09-30 | 2011-01-26 | 安徽工业大学 | Calcium germinate nanowire and preparation method thereof |
-
2014
- 2014-08-12 CN CN201410393991.4A patent/CN104152142B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020038861A1 (en) * | 2000-09-29 | 2002-04-04 | Sumitomo Chemical Company, Limited | Fluorescent substances for vacuum ultraviolet radiation excited light-emitting devices |
| CN101956237A (en) * | 2010-09-30 | 2011-01-26 | 安徽工业大学 | Calcium germinate nanowire and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| 易守军 等: "Cd2Ge7O16中Tb的长余辉发光特性", 《无机化学学报》 * |
| 易守军 等: "Pb在锗酸镉基质中的长余辉发光特性", 《高等学校化学学报》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109705864A (en) * | 2018-11-23 | 2019-05-03 | 长春理工大学 | A kind of red fluorescence powder and preparation method thereof that luminous efficiency is high |
| CN113388395A (en) * | 2020-03-13 | 2021-09-14 | 包头稀土研究院 | Red fluorescent material and preparation method and application thereof |
| CN113388395B (en) * | 2020-03-13 | 2023-07-21 | 包头稀土研究院 | Red fluorescent material and preparation method and application thereof |
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| Publication number | Publication date |
|---|---|
| CN104152142B (en) | 2016-05-25 |
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