CN106635017A - 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 mixing 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, particularly a kind of titanate base red fluorescent powder and its
Preparation method.
Background technology
Light emitting diode (LED) effectively can change into electric energy as one of higher solid state light emitters of efficiency
Luminous energy.Since coming out from the sixties in 20th century, because it has, life-span length, energy conversion efficiency are high, have good stability, price is low
Honest and clean the advantages of and be widely used in show and lighting field.Develop first after white light LEDs from 1996 Nian Ya companies, with
LED solid state light emitters substitute the main trend that conventional illumination sources are current lighting engineering development, and each state all pays close attention, confusingly
Development plan is confusingly formulated, has been stepped up to develop and is developed.
At present using the most extensive and very ripe white light LEDs of technology mainly with the GaN base chip collocation YAG of blue light-emitting：
The fluorescent material of Ce, by exciting YAG：What Ce was realized to launch gold-tinted with blue light, its efficiency high, low cost of manufacture, 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
Than relatively low, color reducibility is poor, the colder tone of tone for number, so that it is applied being subject to certain restrictions.
The content of the invention
For the problem that above-mentioned prior art is present, it is an object of the invention to provide a kind of stability is high, luminous efficiency
Height, preparation is simple, with low cost, and the titanate base red fluorescent powder of environmentally safe and preparation method thereof.
For achieving the above object, the technical solution used in the present invention is：A kind of white light LEDs metatitanic acid alkali red fluorescence
Powder, chemical general formula is Mg1-xEuxAl8Ti6O25, wherein x is Eu3+The stoichiometry fraction of doping, 0.001≤x≤0.20；
250-550nm wavelength is excited down, and fluorescent material can launch red fluorescence.
A kind of preparation method of titanate base red fluorescent powder, comprises the steps：
(1) by chemical composition Mg1-xEuxAl8Ti6O25The stoichiometric proportion of middle each element, wherein 0.001≤x≤0.20, point
Another name is taken containing magnesium ion Mg2+Compound, containing europium ion Eu3+Compound, containing aluminium ion Al3+Compound, contain
Titanium ion Ti4+Compound, grind and be well mixed；
(2) the mixture precalcining in air atmosphere for obtaining step (1), temperature is 400～900 DEG C, sintering time
For 3～20 hours；
(3) the mixture natural cooling for obtaining step (2) precalcining, after grinding and being well mixed, is carried out in atmosphere
Calcining, calcining heat is 900～1400 DEG C, and calcination time is 3～12 hours；Room temperature is subsequently cooled to, is ground and is well mixed,
Obtain described fluorescent material.
It is described containing titanium ion Ti4+Compound be titanium dioxide TiO2；Containing aluminium ion Al3+Compound for oxidation
Aluminium Al2O3, aluminum nitrate Al (NO3)3·9H2O, aluminium carbonate Al2(CO3)3Or aluminium hydroxide Al (OH)3In one kind；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 kind in O；It is described containing europium ion Eu3+Compound be europium oxide, europium nitrate, carbonic acid
One kind in europium, europium sulfate, Europium chloride.
Beneficial effect, as a result of such scheme, the red fluorescence powder material for preparing can be by 250-550 nanometers
Nearby have it is very strong excite, coincide very much with the launch wavelength of near ultraviolet LED chip or blue-light LED chip, in black light
Excite down, the fluorescent material can launch bright red fluorescence, and launch wavelength is based on 613nm；And the granularity that obtains is equal
Even, luminous efficiency is high, and chemical stability is good, and the toxic gases such as sulfide will not be produced under uv irradiation, environmentally friendly,
It is applied to white light LEDs and other illumination fields；Compound containing element needed for synthesising biological material is mixed in proportion, is adopted
Prepared by high temperature solid-state method, prepare the process is simple of the material, without any pollution, environmentally friendly, is adapted to industrialized production.
Realize in ultraviolet, near ultraviolet or blue light equal excitation light source activation, launch the material of red fluorescence, i.e. Eu3+
The metatitanic acid magnalium fluorescent material MgAl of ion doping8Ti6O25:xEu3+, wherein x is Eu3+The mol ratio of doping, 0.001≤x≤
0.20, it is applied to the preparation of LED illumination device.Meanwhile, the material has preparation process is simple, low production cost, without any dirt
Dye, and the advantage of the light-converting material stable performance for synthesizing, and report is there is no at present.
Advantage：1st, the titanate base red fluorescent material that the present invention is provided, there is good process based prediction model, and light effect
Rate is high, can be widely applied to prepare high-power LED.
2nd, prepared new red phosphors can effectively absorb near ultraviolet (250～550 receive to green wavelength
Rice) light, and the trivalent europium ion Eu for transferring energy to be entrained in host material3+, launch the red of 613 nms
Light, colourity is pure, and brightness is high, is matched somebody with somebody proper amount of green, blue colour fluorescent powder, applies and be packaged in outside InGaN diodes, can
Prepare efficient White-light LED illumination device.
3rd, the tantalates base red fluorescent powder that the present invention is provided, preparation process is simple, without any pollution is environmentally friendly.
Description of the drawings：
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 Mg0.99Eu0.01Al8Ti6O25Exciting 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 in the case where 365 nano wave lengths are excited
Spectrogram.
Fig. 5 is that the embodiment of the present invention 1 prepares sample Mg0.99Eu0.01Al8Ti6O25Excite in 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 Mg0.8Eu0.1Al8Ti6O25Launching light in the case where 365 nano wave lengths are excited
Spectrogram.
Fig. 9 is that the embodiment of the present invention 4 prepares sample Mg0.8Eu0.1Al8Ti6O25Excite in 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 is Mg1-xEuxAl8Ti6O25, wherein x is Eu3+
The stoichiometry fraction of doping, 0.001≤x≤0.20；In the case where 250-550nm wavelength is excited, fluorescent material can launch redness
Fluorescence.
A kind of preparation method of titanate base red fluorescent powder, comprises the steps：
(1) by chemical composition Mg1-xEuxAl8Ti6O25The stoichiometric proportion of middle each element, wherein 0.001≤x≤0.20, point
Another name is taken containing magnesium ion Mg2+Compound, containing europium ion Eu3+Compound, containing aluminium ion Al3+Compound, contain
Titanium ion Ti4+Compound, grind and be well mixed；
(2) the mixture precalcining in air atmosphere for obtaining step (1), temperature is 400～900 DEG C, sintering time
For 3～20 hours；
(3) the mixture natural cooling for obtaining step (2) precalcining, after grinding and being well mixed, is carried out in atmosphere
Calcining, calcining heat is 900～1400 DEG C, and calcination time is 3～12 hours；Room temperature is subsequently cooled to, is ground and is well mixed,
Obtain described fluorescent material.
It is described containing titanium ion Ti4+Compound be titanium dioxide TiO2；Containing aluminium ion Al3+Compound for oxidation
Aluminium Al2O3, aluminum nitrate Al (NO3)3·9H2O, aluminium carbonate Al2(CO3)3Or aluminium hydroxide Al (OH)3In one kind；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 kind in O；It is described containing europium ion Eu3+Compound be europium oxide, europium nitrate, carbonic acid
One kind in europium, europium sulfate, Europium chloride.
With reference to the accompanying drawings and examples the invention will be further described.
Embodiment 1：According to chemical formula Mg0.99Eu0.01Al8Ti6O25The stoichiometric proportion of middle each element, weighs respectively oxidation
Magnesium MgO：0.242 gram, aluminium oxide Al2O3：2.472 grams, europium oxide Eu2O3：0.011 gram, titanium dioxide TiO2：2.934 grams, in agate
After adding appropriate acetone mixed grinding uniform in Nao mortars, precalcining is carried out in air atmosphere, calcining 10 is little at 850 DEG C
When along with the furnace cooling after, taking out sample, that again the raw material of precalcining is sufficiently mixed into grinding with identical method is uniform, in air gas
Calcine again in atmosphere, calcine 10 hours at 1350 DEG C, be cooled to room temperature, be fully ground after taking-up and obtain sample.
Referring to accompanying drawing 1, it is the X-ray powder diffraction pattern that the present embodiment technical scheme prepares sample, XRD test results
Show, prepared titanate Mg0.99Eu0.01Al8Ti6O25For monophase materialses, exist without other dephasigns, and degree of crystallinity compared with
It is good, show trivalent europium ion Eu3+Doping on the structure of matrix without impact.
Referring to accompanying drawing 2, it is SEM (SEM) collection of illustrative plates that the present embodiment technical scheme prepares sample, from figure
In as can be seen that gained sample particle dispersion it is more uniform.
Referring to accompanying drawing 3, it is that the sample prepared by the present embodiment technical scheme is preparing sample Mg0.99Eu0.01Al8Ti6O25
Exciting light spectrogram under the monitoring of 613 nano wave lengths, has broad peak to occur, 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, it is adaptable to white light LEDs.
Referring to accompanying drawing 4, it is the launching light by the sample of the present embodiment technical scheme preparation in the case where 365 nano wave lengths are excited
Spectrogram, it can be seen that the launch wavelength of the material is the ruddiness of 613 nano waveband scopes.
Referring to accompanying drawing 5, it is the sample for preparing by the present embodiment technical scheme excites in 316 nano wave lengths, 613 nanometer waves
Decay of luminescence curve under long monitoring, can be calculated die-away time for 1.5 milliseconds.
Embodiment 2：Prepare Mg0.999Eu0.001Al8Ti6O25, according to chemical formula Mg0.999Eu0.001Al8Ti6O25Middle each element
Stoichiometric proportion, basic magnesium carbonate 4MgCO is weighed respectively3·Mg(OH)2·5H2O：0.588 gram, aluminium carbonate Al2(CO3)3：
5.673 grams, titanium oxide TiO2：2.934 grams, europium nitrate Eu (NO3)3·6H2O：0.002 gram.Grind in agate mortar and mix
After uniform, air atmosphere precalcining is selected, precalcining temperature is 750 DEG C, and precalcination time is 8 hours, is then cooled to room temperature, is taken
Go out sample, the presoma for obtaining is sufficiently mixed grinding uniformly, calcined at 1250 DEG C among air, calcination time is 8
Hour, room temperature is cooled to, take out sample grinding and obtain required fluorescent material.
Sample manufactured in the present embodiment, its X-ray powder diffraction pattern, primary structure pattern, excitation spectrum, emission spectrum
And decay of luminescence curve is similar to Example 1.
Embodiment 3：Prepare Mg0.95Eu0.05Al8Ti6O25, according to chemical formula Mg0.95Eu0.05Al8Ti6O25The change of middle each element
Metering ratio is learned, magnesium hydroxide Mg (OH) is weighed 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 gram.After grinding and be well mixed in agate mortar, air atmosphere is selected
Precalcining, precalcining temperature is 600 DEG C, and precalcination time is 6 hours, is then cooled to room temperature, sample is taken out, the forerunner for obtaining
Body is sufficiently mixed grinding uniformly, among air, is calcined at 1100 DEG C, and calcination time is 6 hours, is cooled to room temperature, is taken
Go out sample grinding and obtain required titanate fluorescent material.
Sample manufactured in the present embodiment, its X-ray powder diffraction pattern, primary structure pattern, excitation spectrum, emission spectrum
And decay of luminescence curve is similar to Example 1.
Embodiment 4：Prepare Mg0.9Eu0.1Al8Ti6O25, according to chemical formula Mg0.9Eu0.1Al8Ti6O25The chemistry of middle each element
Metering ratio, weighs respectively magnesium nitrate Mg (NO3)3·6H2O：1.399 grams, aluminum nitrate Al (NO3)3·9H2O:18.188 gram, chlorination
Europium EuCl3：0.155 gram, titanium dioxide TiO2：2.934 gram.After grinding and be well mixed in agate mortar, air atmosphere is selected
Precalcining, precalcining temperature is 450 DEG C, and precalcination time is 4 hours, is then cooled to room temperature, sample is taken out, the forerunner for obtaining
Body is sufficiently mixed grinding uniformly, among air atmosphere, is calcined at 950 DEG C, and calcination time is 4 hours, is cooled to room temperature,
Take out sample grinding and obtain required fluorescent material.
It is the SEM photograph of the sample prepared by this enforcement technical scheme referring to accompanying drawing 6.
It is excitation spectrum of the sample prepared by the present embodiment technical scheme under the monitoring of 613 nano wave lengths referring to accompanying drawing 7
Figure, it can be seen that having broad peak to occur in 250～550 nanometer ranges, has strong peak to go out at 320 nanometers and 465 nanometers
It is existing, show that the material can be excited effectively by the light of near ultraviolet to blue region, it is adaptable to white light LEDs.
Referring to accompanying drawing 8, it is the launching light by the sample of the present embodiment technical scheme preparation in the case where 365 nano wave lengths are excited
Spectrogram, it can be seen that the launch wavelength of the material is the ruddiness of 613 nano waveband scopes.
Referring to accompanying drawing 9, it is the sample for preparing by the present embodiment technical scheme excites in 316 nano wave lengths, 613 nanometer waves
Decay of luminescence curve under long monitoring, can be calculated die-away time for 1.4 milliseconds.
Embodiment 5：Prepare Mg0.85Eu0.15Al8Ti6O25, according to chemical formula Mg0.85Eu0.15Al8Ti6O25The change of middle each element
Metering ratio is learned, magnesia MgO is weighed respectively：0.208 gram, aluminium oxide Al2O3：2.472 grams, europium sulfate Eu2(SO4)3·H2O：
0.266 gram, titanium dioxide TiO2：2.934 gram.After grinding and be well mixed in agate mortar, air atmosphere precalcining is selected,
Precalcining temperature is 750 DEG C, and precalcination time is 4 hours, is then cooled to room temperature, takes out sample, and the presoma for obtaining 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, takes out sample
Grinding obtains required titanate fluorescent material.
Sample manufactured in the present embodiment, its primary structure pattern, excitation spectrum, emission spectrum and decay of luminescence curve with
Embodiment 4 is similar.
Embodiment 6：Prepare Mg0.8Eu0.2Al8Ti6O25, according to chemical formula Mg0.8Eu0.2Al8Ti6O25The chemistry of middle each element
Metering ratio, weighs respectively magnesium hydroxide Mg (OH)2：0.283 gram, europium carbonate Eu2(CO3)3·H2O：0.301 gram, aluminium hydroxide Al
(OH)3：3.782 grams, titanium dioxide TiO2：2.934 gram.After grinding and be well mixed in agate mortar, select air atmosphere pre-
Calcining, precalcining temperature is 700 DEG C, and precalcination time is 6 hours, is then cooled to room temperature, sample is taken out, the presoma for obtaining
It is sufficiently mixed grinding uniform, among air, is calcined at 1100 DEG C, calcination time is 12 hours, is cooled to room temperature, takes out
Sample grinding obtains required tantalite fluorescent material.
Sample manufactured in the present embodiment, its 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, is characterized in that：The red fluorescence powder, chemical general formula is Mg1-xEuxAl8Ti6O25,
Wherein x is Eu3+The stoichiometry fraction of doping, 0.001≤x≤0.20；In the case where 250-550nm wavelength is excited, fluorescent material can be with
Launch red fluorescence.
2. a kind of preparation method of the titanate base red fluorescent powder described in claim 1, is characterized in that：A kind of metatitanic acid alkali is red
The preparation method of color fluorescent material, comprises the steps：
（1）By chemical composition Mg1-xEuxAl8Ti6O25The stoichiometric proportion of middle each element, wherein 0.001≤x≤0.20, claims respectively
Take containing magnesium ion Mg2+Compound, containing europium ion Eu3+Compound, containing aluminium ion Al3+Compound, containing titanium from
Sub- Ti4+Compound, grind and be well mixed；
（2）By step（1）The mixture for obtaining precalcining in air atmosphere, temperature be 400～900 DEG C, sintering time be 3～
20 hours；
（3）By step（2）The mixture natural cooling that precalcining is obtained, after grinding and being well mixed, is calcined in atmosphere,
Calcining heat is 900～1400 DEG C, and calcination time is 3～12 hours；Room temperature is subsequently cooled to, is ground and is well mixed, obtained
Described fluorescent material.
3. a kind of preparation method of titanate base red fluorescent powder according to claim 2, is characterized in that：Described contains
Titanium ion Ti4+Compound be titanium dioxide TiO2；Containing aluminium ion Al3+Compound be aluminium oxide Al2O3, aluminum nitrate Al
(NO3)3•9H2O, aluminium carbonate Al2(CO3)3Or aluminium hydroxide Al (OH)3In one kind；It is described containing magnesium ion Mg2+Chemical combination
Thing is magnesia MgO, magnesium hydroxide Mg (OH)2, magnesium nitrate Mg (NO3)3•6H2O and basic magnesium carbonate 4MgCO3•Mg(OH)2•
5H2One kind in O；It is described containing europium ion Eu3+Compound be europium oxide, europium nitrate, europium carbonate, europium sulfate, Europium chloride
In one kind.
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| CN109370580A (en) * | 2018-10-23 | 2019-02-22 | 江苏师范大学 | A kind of titanium aluminate fluorescent powder and the preparation method and application thereof of bismuth ion activation |
| CN109762564A (en) * | 2019-03-13 | 2019-05-17 | 常州工程职业技术学院 | A kind of europium ion Eu3+The titanate red fluorescence powder of activation, preparation method and applications |
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