CN106635017B - Titanate-based red fluorescent powder and preparation method thereof - Google Patents
Titanate-based red fluorescent powder and preparation method thereof Download PDFInfo
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Abstract
A titanate-based red fluorescent powder and a preparation method thereof, belonging to the field of red fluorescent powder and the preparation method thereof. The chemical general formula of the phosphor is Mg1‑xEuxAl8Ti6O25Wherein x is Eu3+The stoichiometric fraction of doping, x is more than or equal to 0.001 and less than or equal to 0.20. The method comprises the following steps: (1) according to chemical composition Mg1‑xEuxAl8Ti6O25The stoichiometric ratio of each element in the magnesium alloy, wherein x is more than or equal to 0.001 and less than or equal to 0.20, and Mg containing magnesium ions are respectively weighed2+Compound of (1), Eu ion-containing Eu3+Compound of (2), Al containing aluminum ion3+Compound of (2), containing titanium ion Ti4+Grinding and mixingMixing uniformly; (2) pre-calcining the mixture obtained in the step (1) in an air atmosphere at the temperature of 400-900 ℃ for 3-20 hours; (3) naturally cooling the mixture obtained by the precalcination in the step (2), grinding and uniformly mixing, and calcining in air at the calcining temperature of 900-1400 ℃ for 3-12 hours; and then cooling to room temperature, grinding and uniformly mixing to obtain the fluorescent powder. The advantages are that: simple process, no pollution, environmental protection and suitability for industrial production.
Description
Technical field
The present invention relates to a kind of red fluorescence powder and preparation method thereof, especially a kind of titanate base red fluorescent powder and its
Preparation method.
Background technique
Light emitting diode (LED) can effectively be converted to electric energy as one of higher solid state light emitters of efficiency
Luminous energy.Since the 1960s comes out, because it is long with the service life, energy conversion efficiency is high, have good stability, price is low
The advantages that honest and clean and be widely used in display and lighting area.After developing white light LEDs for the first time from 1996 Nian Ya companies, with
LED solid state light emitter substitution conventional illumination sources are the main trends of current lighting engineering development, and each state all pays close attention,
Development plan has been formulated one after another, step up to develop and has been developed.
At present using the GaN base chip collocation YAG that most extensive and very mature technology white light LEDs are mainly with blue light-emitting:
The fluorescent powder of Ce emits yellow light and blue light by excitation YAG:Ce to realize, high-efficient, manufacturing cost is low, but
It is especially not high in red area luminous efficiency due to lacking green and red color components in its emission spectrum, cause its colour developing to refer to
Number is relatively low, and color reducibility is poor, the colder tone of tone, so that its application is subject to certain restrictions.
Summary of the invention
In view of the above-mentioned problems of the prior art, the purpose of the present invention is to provide a kind of stability height, luminous efficiency
Height, preparation is simple, low in cost, and the titanate base red fluorescent powder and preparation method thereof of no pollution to the environment.
To achieve the above object, the technical solution adopted by the present invention is that: a kind of white light LEDs metatitanic acid alkali red fluorescence
Powder, chemical general formula Mg1-xEuxAl8Ti6O25, wherein x is Eu3+The stoichiometry score of doping, 0.001≤x≤0.20；?
Under the excitation of 250-550nm wavelength, fluorescent powder can launch red fluorescence.
A kind of preparation method of titanate base red fluorescent powder, includes the following steps:
(1) chemical composition Mg is pressed1-xEuxAl8Ti6O25The stoichiometric ratio of middle each element, wherein 0.001≤x≤0.20, point
Also known as take containing magnesium ion Mg2+Compound, contain europium ion Eu3+Compound, contain aluminium ion Al3+Compound, contain
Titanium ion Ti4+Compound, grind and be uniformly mixed；
(2) the mixture precalcining in air atmosphere for obtaining step (1), temperature are 400~900 DEG C, sintering time
It is 3~20 hours；
(3) the mixture natural cooling for obtaining step (2) precalcining, grind and after mixing, carry out in air
Calcining, calcination temperature are 900~1400 DEG C, and calcination time is 3~12 hours；It then cools to room temperature, grind and is uniformly mixed,
Obtain the fluorescent powder.
Described contains titanium ion Ti4+Compound be titanium dioxide TiO2；Contain aluminium ion Al3+Compound be oxidation
Aluminium Al2O3, aluminum nitrate Al (NO3)3•9H2O, aluminium carbonate Al2(CO3)3Or aluminium hydroxide Al (OH)3One of；Described contains
Magnesium ion Mg2+Compound be magnesia MgO, magnesium hydroxide Mg (OH)2, magnesium nitrate Mg (NO3)3•6H2O and basic magnesium carbonate
4MgCO3•Mg(OH)2•5H2One of O；Described contains europium ion Eu3+Compound be europium oxide, europium nitrate, europium carbonate,
One of europium sulfate, Europium chloride.
Beneficial effect, as the above scheme is adopted, the red fluorescence powder material being prepared can be by 250-550 nanometers
Nearby there is very strong excitation, coincide very much with the launch wavelength of near ultraviolet LED chip or blue-light LED chip, in black light
Under excitation, which can launch bright red fluorescence, and launch wavelength is based on 613 nm；And obtained granularity is equal
Even, luminous efficiency is high, and chemical stability is good, will not generate the toxic gases such as sulfide under uv irradiation, environmentally friendly,
Applied to white light LEDs and other illumination fields；Compound containing element needed for synthetic material is mixed in proportion, using high temperature
Solid phase method preparation prepares the simple process of the material, without any pollution, environmentally friendly, suitable industrialized production.
It realizes in ultraviolet, near ultraviolet or blue light equal excitation light source activation, launches the material of red fluorescence, i.e. Eu3+
The metatitanic acid magnalium fluorescent material MgAl of ion doping8Ti6O25:xEu3+, wherein x is Eu3+The molar ratio of doping, 0.001≤x≤
0.20, the preparation applied to LED illumination device.Meanwhile the material has preparation process simple, production cost is low, without any dirt
It contaminates, and the advantage that the light conversion material performance synthesized is stable, and there is no report at present.
Advantage: 1, titanate base red fluorescent material provided by the invention has good physical and chemical properties, and shine effect
Rate is high, can be widely applied to prepare high-power LED.
2, prepared new red phosphors can effectively absorb near ultraviolet (250~550 receive to green wavelength
Rice) light, and transfer energy to the trivalent europium ion Eu being entrained in host material3+, launch red near 613 nanometers
Light, coloration is pure, and brightness is high, by it with proper amount of green, blue colour fluorescent powder, applies and is packaged in outside InGaN diode, can
Prepare efficient white light LEDs illuminating device.
3, titanate base red fluorescent powder provided by the invention, preparation process is simple, without any pollution, environmentally friendly.
Detailed description of the invention:
Fig. 1 is that the embodiment of the present invention 1 prepares sample Mg0.99Eu0.01Al8Ti6O25X-ray powder diffraction pattern.
Fig. 2 is that the embodiment of the present invention 1 prepares sample Mg0.99Eu0.01Al8Ti6O25Scanning electron microscope diagram.
Fig. 3 is that the embodiment of the present invention 1 prepares sample Mg0.99Eu0.01Al8Ti6O25Excitation under the monitoring of 613 nano wave lengths
Spectrogram.
Fig. 4 is that the embodiment of the present invention 1 prepares sample Mg0.99Eu0.01Al8Ti6O25Transmitting under the excitation of 365 nano wave lengths
Spectrogram.
Fig. 5 is that the embodiment of the present invention 1 prepares sample Mg0.99Eu0.01Al8Ti6O25In the excitation of 316 nano wave lengths, 613 nanometers
Decay of luminescence curve under wavelength monitoring.
Fig. 6 is that the embodiment of the present invention 4 prepares sample Mg0.8Eu0.1Al8Ti6O25Scanning electron microscope diagram.
Fig. 7 is that the embodiment of the present invention 4 prepares sample Mg0.8Eu0.1Al8Ti6O25Exciting light under the monitoring of 613 nano wave lengths
Spectrogram.
Fig. 8 is that the embodiment of the present invention 4 prepares sample Mg0.8Eu0.1Al8Ti6O25Transmitting light under the excitation of 365 nano wave lengths
Spectrogram.
Fig. 9 is that the embodiment of the present invention 4 prepares sample Mg0.8Eu0.1Al8Ti6O25In the excitation of 316 nano wave lengths, 613 nanometer waves
Decay of luminescence curve under long monitoring.
Specific embodiment
A kind of white light LEDs titanate base red fluorescent powder, chemical general formula Mg1-xEuxAl8Ti6O25, wherein x is Eu3+
The stoichiometry score of doping, 0.001≤x≤0.20；Under the excitation of 250-550nm wavelength, fluorescent powder can launch red
Fluorescence.
A kind of preparation method of titanate base red fluorescent powder, includes the following steps:
(1) chemical composition Mg is pressed1-xEuxAl8Ti6O25The stoichiometric ratio of middle each element, wherein 0.001≤x≤0.20, point
Also known as take containing magnesium ion Mg2+Compound, contain europium ion Eu3+Compound, contain aluminium ion Al3+Compound, contain
Titanium ion Ti4+Compound, grind and be uniformly mixed；
(2) the mixture precalcining in air atmosphere for obtaining step (1), temperature are 400~900 DEG C, sintering time
It is 3~20 hours；
(3) the mixture natural cooling for obtaining step (2) precalcining, grind and after mixing, carry out in air
Calcining, calcination temperature are 900~1400 DEG C, and calcination time is 3~12 hours；It then cools to room temperature, grind and is uniformly mixed,
Obtain the fluorescent powder.
Described contains titanium ion Ti4+Compound be titanium dioxide TiO2；Contain aluminium ion Al3+Compound be oxidation
Aluminium Al2O3, aluminum nitrate Al (NO3)3•9H2O, aluminium carbonate Al2(CO3)3Or aluminium hydroxide Al (OH)3One of；Described contains
Magnesium ion Mg2+Compound be magnesia MgO, magnesium hydroxide Mg (OH)2, magnesium nitrate Mg (NO3)3•6H2O and basic magnesium carbonate
4MgCO3•Mg(OH)2•5H2One of O；Described contains europium ion Eu3+Compound be europium oxide, europium nitrate, europium carbonate,
One of europium sulfate, Europium chloride.
The invention will be further described with reference to the accompanying drawings and examples.
Embodiment 1: according to chemical formula Mg0.99Eu0.01Al8Ti6O25The stoichiometric ratio of middle each element weighs oxidation respectively
MgO:0.242 grams of magnesium, aluminium oxide Al2O3: 2.472 grams, europium oxide Eu2O3: 0.011 gram, titanium dioxide TiO2: 2.934 grams, in Ma
Be added in Nao mortar suitable acetone mixed grinding it is uniform after, precalcining is carried out in air atmosphere, is calcined at 850 DEG C 10 small
When furnace cooling after, take out sample by the raw material of precalcining again with identical method be sufficiently mixed grinding uniformly, in air gas
It is calcined again in atmosphere, is calcined 10 hours at 1350 DEG C, be cooled to room temperature, be fully ground after taking-up and obtain sample.
Referring to attached drawing 1, it is the X-ray powder diffraction pattern that the present embodiment technical solution prepares sample, XRD test result
It has been shown that, prepared titanate Mg0.99Eu0.01Al8Ti6O25For monophase materials, exist without other miscellaneous phases, and crystallinity compared with
It is good, show trivalent europium ion Eu3+Doping on the structure of matrix without influence.
Referring to attached drawing 2, it is the SEM(scanning electron microscope that the present embodiment technical solution prepares sample) map, from figure
In as can be seen that gained sample particle dispersion it is more uniform.
Referring to attached drawing 3, it is to prepare sample Mg by the sample of the present embodiment technical solution preparation0.99Eu0.01Al8Ti6O25
Exciting light spectrogram under the monitoring of 613 nano wave lengths, has broad peak appearance, at 320 nanometers and 464 in 250 ~ 550 nanometer ranges
Nanometer has strong peak to occur, and shows that the material can be excited effectively by the light of near ultraviolet to blue region, is suitable for white light LEDs.
Referring to attached drawing 4, it is the transmitting light by the sample of the present embodiment technical solution preparation under the excitation of 365 nano wave lengths
Spectrogram, it can be seen from the figure that the launch wavelength of the material is the feux rouges of 613 nano waveband ranges.
Referring to attached drawing 5, it be excite by the sample of the present embodiment technical solution preparation in 316 nano wave lengths, 613 nanometer waves
Decay of luminescence curve under long monitoring, can be calculated die-away time is 1.5 milliseconds.
Embodiment 2: preparation Mg0.999Eu0.001Al8Ti6O25, according to chemical formula Mg0.999Eu0.001Al8Ti6O25Middle each element
Stoichiometric ratio, weigh basic magnesium carbonate 4MgCO respectively3•Mg(OH)2•5H2O:0.588 grams, aluminium carbonate Al2(CO3)3:
5.673 grams, titanium oxide TiO2: 2.934 grams, europium nitrate Eu (NO3)3•6H2O:0.002 grams.It grinds and mixes in the agate mortar
After uniformly, air atmosphere precalcining is selected, precalcining temperature is 750 DEG C, and precalcination time is 8 hours, is then cooled to room temperature, takes
Obtained presoma is sufficiently mixed grinding uniformly, is calcined among the air at 1250 DEG C, calcination time is 8 by sample out
Hour, it is cooled to room temperature, takes out sample grinding and obtain required fluorescent material.
Sample manufactured in the present embodiment, X-ray powder diffraction pattern, primary structure pattern, excitation spectrum, emission spectrum
And decay of luminescence curve is similar to Example 1.
Embodiment 3: preparation Mg0.95Eu0.05Al8Ti6O25, according to chemical formula Mg0.95Eu0.05Al8Ti6O25The change of middle each element
Metering ratio is learned, weighs magnesium hydroxide Mg (OH) respectively2: 0.336 gram, aluminium hydroxide Al (OH)3: 3.782 grams, titanium oxide TiO2:
2.934 grams, europium carbonate Eu2(CO3)3•H2O:0.075 grams.In the agate mortar grinding and after mixing, selection air atmosphere
Precalcining, precalcining temperature are 600 DEG C, and precalcination time is 6 hours, is then cooled to room temperature, sample are taken out, obtained forerunner
Body is sufficiently mixed grinding uniformly, among air, is calcined at 1100 DEG C, calcination time is 6 hours, is cooled to room temperature, takes
Sample grinding out obtains required titanate fluorescent material.
Sample manufactured in the present embodiment, X-ray powder diffraction pattern, primary structure pattern, excitation spectrum, emission spectrum
And decay of luminescence curve is similar to Example 1.
Embodiment 4: preparation Mg0.9Eu0.1Al8Ti6O25, according to chemical formula Mg0.9Eu0.1Al8Ti6O25The chemistry of middle each element
Ratio is measured, weighs magnesium nitrate Mg (NO respectively3)3•6H2O:1.399 grams, aluminum nitrate Al (NO3)3•9H2O:18.188 grams, Europium chloride
EuCl3: 0.155 gram, titanium dioxide TiO2: 2.934 grams.In the agate mortar grinding and after mixing, selection air atmosphere it is pre-
Calcining, precalcining temperature are 450 DEG C, and precalcination time is 4 hours, is then cooled to room temperature, sample are taken out, obtained presoma
It is sufficiently mixed grinding uniformly, among air atmosphere, is calcined at 950 DEG C, calcination time is 4 hours, is cooled to room temperature, takes
Sample grinding out obtains required fluorescent material.
It is the SEM photograph by the sample of this implementation technical solution preparation referring to attached drawing 6.
It is the excitation spectrum by the sample of the present embodiment technical solution preparation under the monitoring of 613 nano wave lengths referring to attached drawing 7
Figure has strong peak to occur it can be seen from the figure that there is broad peak appearance in 250 ~ 550 nanometer ranges at 320 nanometers and 465 nanometers,
Show that the material can be excited effectively by the light of near ultraviolet to blue region, is suitable for white light LEDs.
Referring to attached drawing 8, it is the transmitting light by the sample of the present embodiment technical solution preparation under the excitation of 365 nano wave lengths
Spectrogram, it can be seen from the figure that the launch wavelength of the material is the feux rouges of 613 nano waveband ranges.
Referring to attached drawing 9, it be excite by the sample of the present embodiment technical solution preparation in 316 nano wave lengths, 613 nanometer waves
Decay of luminescence curve under long monitoring, can be calculated die-away time is 1.4 milliseconds.
Embodiment 5: preparation Mg0.85Eu0.15Al8Ti6O25, according to chemical formula Mg0.85Eu0.15Al8Ti6O25The change of middle each element
Metering ratio is learned, weighs MgO:0.208 grams of magnesia respectively, aluminium oxide Al2O3: 2.472 grams, europium sulfate Eu2(SO4)3•H2O:
0.266 gram, titanium dioxide TiO2: 2.934 grams.In the agate mortar grinding and after mixing, selection air atmosphere precalcining,
Precalcining temperature is 750 DEG C, and precalcination time is 4 hours, is then cooled to room temperature, takes out sample, and obtained presoma is abundant
Mixed grinding is uniform, among air, is calcined at 1300 DEG C, and calcination time is 10 hours, is cooled to room temperature, and takes out sample
Grinding obtains required titanate fluorescent material.
Sample manufactured in the present embodiment, primary structure pattern, excitation spectrum, emission spectrum and decay of luminescence curve with
Embodiment 4 is similar.
Embodiment 6: preparation Mg0.8Eu0.2Al8Ti6O25, according to chemical formula Mg0.8Eu0.2Al8Ti6O25The chemistry of middle each element
Ratio is measured, weighs magnesium hydroxide Mg (OH) respectively2: 0.283 gram, europium carbonate Eu2(CO3)3•H2O:0.301 grams, aluminium hydroxide Al
(OH)3: 3.782 grams, titanium dioxide TiO2: 2.934 grams.In the agate mortar grinding and after mixing, selection air atmosphere it is pre-
Calcining, precalcining temperature are 700 DEG C, and precalcination time is 6 hours, is then cooled to room temperature, sample are taken out, obtained presoma
It is sufficiently mixed grinding uniformly, among air, is calcined at 1100 DEG C, calcination time is 12 hours, is cooled to room temperature, and is taken out
Sample grinding obtains required tantalite fluorescent material.
Sample manufactured in the present embodiment, primary structure pattern, excitation spectrum, emission spectrum and decay of luminescence curve with
Embodiment 4 is similar.
Claims (3)
1. a kind of titanate base red fluorescent powder, it is characterized in that: the red fluorescence powder, chemical general formula Mg1-xEuxAl8Ti6O25,
Wherein x is Eu3+The stoichiometry score of doping, 0.001≤x≤0.20；Under the excitation of 250-550nm wavelength, fluorescent powder can be with
Launch red fluorescence.
2. the preparation method of a kind of titanate base red fluorescent powder described in claim 1, it is characterized in that: a kind of metatitanic acid alkali is red
The preparation method of color fluorescent powder, includes the following steps:
(1) chemical composition Mg is pressed1-xEuxAl8Ti6O25The stoichiometric ratio of middle each element, wherein 0.001≤x≤0.20, claims respectively
It takes containing magnesium ion Mg2+Compound, contain europium ion Eu3+Compound, contain aluminium ion Al3+Compound, containing titanium from
Sub- Ti4+Compound, grind and be uniformly mixed；
(2) the mixture precalcining in air atmosphere for obtaining step (1), temperature be 400~900 DEG C, sintering time be 3~
20 hours；
(3) the mixture natural cooling for obtaining step (2) precalcining, grind and after mixing, calcined in air,
Calcination temperature is 900~1400 DEG C, and calcination time is 3~12 hours；It then cools to room temperature, grind and is uniformly mixed, obtain
The fluorescent powder.
3. the preparation method of a kind of titanate base red fluorescent powder according to claim 2, it is characterized in that: described contains
Titanium ion Ti4+Compound be titanium dioxide TiO2；Contain aluminium ion Al3+Compound be aluminium oxide Al2O3, aluminum nitrate Al
(NO3)3•9H2O, aluminium carbonate Al2(CO3)3Or aluminium hydroxide Al (OH)3One of；Described contains magnesium ion Mg2+Chemical combination
Object is magnesia MgO, magnesium hydroxide Mg (OH)2, magnesium nitrate Mg (NO3)3•6H2O and basic magnesium carbonate 4MgCO3•Mg(OH)2•
5H2One of O；Described contains europium ion Eu3+Compound be europium oxide, europium nitrate, europium carbonate, europium sulfate, Europium chloride
One of.
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| CN109233826B (en) * | 2018-10-23 | 2021-03-16 | 江苏师范大学 | Europium ion activated titanium aluminate fluorescent powder and preparation method and application thereof |
| CN109762564B (en) * | 2019-03-13 | 2021-04-20 | 常州工程职业技术学院 | Europium ion Eu3+Activated titanate red fluorescent powder, preparation method and application thereof |
| CN111138185B (en) * | 2019-12-27 | 2022-02-08 | 江苏师范大学 | Eu (Eu)3+Ion activated aluminum phosphate fluorescent ceramic and preparation method and application thereof |
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