CN104119888B - A kind of europium doped with fluorine aluminate substrate fluorescent powder and preparation method thereof - Google Patents
A kind of europium doped with fluorine aluminate substrate fluorescent powder and preparation method thereof Download PDFInfo
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- CN104119888B CN104119888B CN201410383414.7A CN201410383414A CN104119888B CN 104119888 B CN104119888 B CN 104119888B CN 201410383414 A CN201410383414 A CN 201410383414A CN 104119888 B CN104119888 B CN 104119888B
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Abstract
The invention belongs to fluorescent material field, specifically invent a kind of europium doped with fluorine aluminate substrate fluorescent powder and preparation method thereof, comprise the following steps: step one, calcium nitrate, aluminum nitrate, europium nitrate, fluorochemical and water are mixed to get mixed solution, the mol ratio n (Al of aluminium ion and calcium ion in mixed solution3+)/n(Ca2+Mol ratio n (the F of) >=7: 6, fluorion and calcium ion‑)/n(Ca2+) >=1: 6, mixed solution and cross-linking agent mixing, prepare colloidal sol；Step 2, heat described colloidal sol, obtain gel；Step 3, by described gel through calcining after, obtaining atomic ratio is Ca12‑xAl14O32F2∶xEu3+Compound, wherein calcining heat is 950～1300 DEG C, and calcination time is 2～8h.Eu is dopant ion, and the scope of x is 0～0.60.The solid grain size that method therefor of the present invention reaction is gentle, calcining heat is low, energy consumption is low, formed is evenly distributed, for nano-scale particle.
Description
Technical field
The invention belongs to fluorescent material field, specifically invented a kind of europium doped with fluorine aluminate substrate fluorescent powder and
Its preparation method.
Background technology
At present, white light emitting diode (White light emitting diode is called for short WLED) is obtained
Main path has three kinds: the first is to utilize the principle of three primary colours and the most fertile current red, green, blue three
Plant ultra-high brightness LED and mix white in the ratio of light intensity 1: 2: 0.38；The second be utilize super bright
Degree InGaN blue led, its tube core adds fraction of yttrium-aluminium-garnet is the fluorescent material of main body；3rd
Planting is to develop ultraviolet leds, uses ultraviolet excitation three primary colors fluorescent powder or other fluorescent material, and generation is many
The white light of the mixture of colours, its color rendering properties can obtain bigger raising, and this method realizes white light LEDs
Main difficulty is to lack suitable red fluorescence powder.Therefore develop efficient red fluorescence powder and become realization
The key of white light LEDs.
The existing method preparing fluorescent material has high temperature solid phase synthesis, liquid-phase coprecipitation, sol-gal process
Deng.But, in high temperature solid-state method, reactant needs the long-time ability mix homogeneously that grinds, and calcining
Temperature is high, consumes energy higher, and product is easily reunited, particle diameter skewness, and reaction is incomplete, and in product
Containing the most original solid material.Wherein use sol-gal process synthesis Ca12Al14O32F2Base fluorescent powder
There are no report.
Summary of the invention
It is an object of the invention to, it is provided that a kind of europium doped with fluorine aluminate substrate fluorescent powder and preparation method thereof,
Compared with prior art, diameter of particle of the present invention be evenly distributed, course of reaction simple and easily controllable.
The solution of the present invention is:
The preparation method of a kind of europium doped with fluorine aluminate substrate fluorescent powder, comprises the following steps:
Step one, calcium nitrate, aluminum nitrate, europium nitrate, fluorochemical and water are mixed to get mixing molten
Liquid, the mol ratio n (Al of aluminium ion and calcium ion in mixed solution3+)/n(Ca2+) >=7: 6, fluorion and calcium from
Mol ratio n (the F of son-)/n(Ca2+) >=1: 6, mixed solution and cross-linking agent mixing, prepare colloidal sol；
Step 2, heat described colloidal sol, obtain gel；
Step 3, by described gel through calcining after, obtaining atomic ratio is Ca12-xAl14O32F2∶xEu3+'s
Compound, wherein calcining heat is 950～1300 DEG C, and calcination time is 2～8h.
Preferably, in the preparation method of described europium doped with fluorine aluminate substrate fluorescent powder, described step
In three, calcining heat is 1100 DEG C.
Preferably, in the preparation method of described europium doped with fluorine aluminate substrate fluorescent powder, described step
In three, calcination time is 4h.
Preferably, in the preparation method of described europium doped with fluorine aluminate substrate fluorescent powder, mixed solution
Middle europium ion concentration is 1～5%.
Preferably, in the preparation method of described europium doped with fluorine aluminate substrate fluorescent powder, described step
In one, in mixed solution, europium ion concentration is 3%.
Preferably, in the preparation method of described europium doped with fluorine aluminate substrate fluorescent powder, described fluorine-containing
Compound is trifluoroacetic acid, Potassium borofluoride or trifluoromethane sulfonic acid magnesium.
A kind of doped with fluorine aluminate substrate fluorescent powder, by described europium doped with fluorine aluminate substrate fluorescent powder
Preparation method prepares, described fluorescent material be atomic ratio be Ca12-xAl14O32F2∶xEu3+Compound,
Wherein, wherein, 0 ＜ x≤0.6.
Preferably, in described fluorescent material, x value 0.36.
It is an advantage of the current invention that:
1, powder body is nano-particle, and even particle size distribution；
2, answer process simple and easily controllable；
3, reaction is gentle, calcining heat is low, it is low to consume energy.
Accompanying drawing explanation
Fig. 1 is the thermogravimetric differential thermal collection of illustrative plates of dry glue synthesized by sol-gel process
Fig. 2 is the XRD figure spectrum of sample synthesized by different calcining heat
Fig. 3 is the XRD figure spectrum of sample synthesized by different calcination time
Fig. 4 is different CF3The XRD figure spectrum of synthesized sample under COOH concentration
Fig. 5 is Ca12-xAl14O32F2∶xEu3+The XRD figure spectrum of (x=0～0.60)
Fig. 6 is the TEM figure of sample synthesized by sol-gel process
Fig. 7 is Ca11.64Al14O32F2∶0.36Eu3+The excitation spectrum (A) of sample and emission spectrum (B)
Fig. 8 is different CF3The excitation spectrum (A) of synthetic sample and emission spectrum (B) under COOH concentration
Fig. 9 be the emission spectrum (A) of sample synthesized by different calcining heat and temperature glimmering with counter sample
The relation curve (B) of light intensity
Figure 10 be the emission spectrum (A) of sample synthesized by different calcination time and the time glimmering with counter sample
The relation curve (B) of light intensity
Figure 11 is emission spectrum (A) and the europium ion concentration of sample synthesized by the different europium ion concentration of doping
Relation curve (B) with counter sample fluorescence intensity.
Detailed description of the invention
The present invention is described in further detail below in conjunction with the accompanying drawings, to make those skilled in the art's reference
Description word can be implemented according to this.
As shown in Figure 1 to 11, the preparation of a kind of europium doped with fluorine aluminate substrate fluorescent powder of the present invention
Method, comprises the following steps:
Step one, calcium nitrate, aluminum nitrate, europium nitrate, fluorochemical and water are mixed to get mixing molten
Liquid, the mol ratio n (Al of aluminium ion and calcium ion in mixed solution3+)/n(Ca2+) >=7: 6, fluorion and calcium from
Mol ratio n (the F of son-)/n(Ca2+) >=1: 6, mixed solution and cross-linking agent mixing, prepare colloidal sol；
Step 2, heat described colloidal sol, obtain gel；
Step 3, by described gel through calcining after, obtaining atomic ratio is Ca12-xAl14O32F2∶xEu3+'s
Compound, wherein calcining heat is 950～1300 DEG C, and calcination time is 2～8h.
In the preparation method of described europium doped with fluorine aluminate substrate fluorescent powder, in described step 3, calcining
Temperature is 1100 DEG C.
In the preparation method of described europium doped with fluorine aluminate substrate fluorescent powder, in described step 3, calcining
Time is 4h.
In the preparation method of described europium doped with fluorine aluminate substrate fluorescent powder, in mixed solution, europium ion is dense
Degree is 1～5%.
In the preparation method of described europium doped with fluorine aluminate substrate fluorescent powder, in described step one, mixing
In solution, europium ion concentration is 3%.
In the preparation method of described europium doped with fluorine aluminate substrate fluorescent powder, described fluorochemical is three
Fluoroethanoic acid, Potassium borofluoride or trifluoromethane sulfonic acid magnesium.
A kind of doped with fluorine aluminate substrate fluorescent powder, by described europium doped with fluorine aluminate substrate fluorescent powder
Preparation method prepares, described fluorescent material be atomic ratio be Ca12-xAl14O32F2∶xEu3+Compound,
Wherein, wherein, 0 ＜ x≤0.6.
In described fluorescent material, x value 0.36.
Embodiment 1
Weighing calcium nitrate, aluminum nitrate, europium nitrate, trifluoroacetic acid, mol ratio is respectively 3 mMs, and 3.5
MM, 0.09 mM, 6 mMs are mixed to get mixed solution with water, are subsequently adding cross-linking agent and mix
Close uniformly, prepare colloidal sol；Colloidal sol described in heating in water bath, obtains gel；By described gel at 1100 DEG C
After calcining 4h, synthesize Ca11.64Al14O32F2∶0.36Eu3+Fluorescent material.
Embodiment 2
Weighing calcium nitrate, aluminum nitrate, europium nitrate, trifluoroacetic acid, mol ratio is respectively 3 mMs, and 3.5
MM, 0.09 mM, 12 mMs are mixed to get mixed solution with water, are subsequently adding cross-linking agent and mix
Close uniformly, prepare colloidal sol；Colloidal sol described in heating in water bath, obtains gel；By described gel at 1100 DEG C
After calcining 4h, synthesize Ca11.64Al14O32F2∶0.36Eu3+Fluorescent material.
Embodiment 3
Weighing calcium nitrate, aluminum nitrate, europium nitrate, trifluoroacetic acid, mol ratio is respectively 3 mMs, and 3.5
MM, 0.09 mM, 18 mMs are mixed to get mixed solution with water, are subsequently adding cross-linking agent and mix
Close uniformly, prepare colloidal sol；Colloidal sol described in heating in water bath, obtains gel；By described gel at 1100 DEG C
After calcining 4h, synthesize Ca11.64Al14O32F2∶0.36Eu3+Fluorescent material.
Embodiment 4
Weighing calcium nitrate, aluminum nitrate, europium nitrate, trifluoroacetic acid, mol ratio is respectively 3 mMs, and 3.5
MM, 0.09 mM, 24 mMs are mixed to get mixed solution with water, are subsequently adding cross-linking agent and mix
Close uniformly, prepare colloidal sol；Colloidal sol described in heating in water bath, obtains gel；By described gel at 1100 DEG C
After calcining 4h, synthesize Ca11.64Al14O32F2∶0.36Eu3+Fluorescent material.
In embodiment 1～4, the Ca of synthesis11.64Al14O32F2∶0.36Eu3+The XRD figure spectrum number of fluorescent material
According to as shown in Figure 4, it is seen then that work as CF3During COOH addition >=6mmol, the diffraction of synthesized sample
Peak and Ca12Al14O32F2PDF standard diffraction card (53-1232) data the most identical.As fluorine source
CF3COOH is volatile, and during water-bath and dry glue, part is volatilized away, and in burn-in process,
F is partially disengaged reactant the most otherwise.CF selected by experiment3COOH addition is 6mmol.
In embodiment 1～4, the Ca of synthesis11.64Al14O32F2∶0.36Eu3+Excitation spectrum A (the λ of fluorescent material
Em=612nm) data are as shown in Figure 8 for emission spectrum B (λ ex=245nm).As seen from the figure,
Along with CF3The increase of COOH addition, the luminous intensity of fluorescent material first reduces and strengthens afterwards.
Embodiment 5
Weighing calcium nitrate, aluminum nitrate, europium nitrate, trifluoroacetic acid, mol ratio is respectively 3 mMs, and 3.5
MM, 0.00 mM, 6 mMs are mixed to get mixed solution with water, are subsequently adding cross-linking agent and mix
Close uniformly, prepare colloidal sol；Colloidal sol described in heating in water bath, obtains gel；By described gel at 1100 DEG C
After calcining 4h, synthesize Ca12Al14O32F2Fluorescent material.
Embodiment 6
Weighing calcium nitrate, aluminum nitrate, europium nitrate, trifluoroacetic acid, mol ratio is respectively 3 mMs, and 3.5
MM, 0.03 mM, 6 mMs are mixed to get mixed solution with water, are subsequently adding cross-linking agent and mix
Close uniformly, prepare colloidal sol；Colloidal sol described in heating in water bath, obtains gel；By described gel at 1100 DEG C
After calcining 4h, synthesize Ca11.88Al14O32F2∶0.12Eu3+Fluorescent material.
Embodiment 7
Weighing calcium nitrate, aluminum nitrate, europium nitrate, trifluoroacetic acid, mol ratio is respectively 3 mMs, and 3.5
MM, 0.06 mM, 6 mMs are mixed to get mixed solution with water, are subsequently adding cross-linking agent and mix
Close uniformly, prepare colloidal sol；Colloidal sol described in heating in water bath, obtains gel；By described gel at 1100 DEG C
After calcining 4h, synthesize Ca11.76Al14O32F2∶0.24Eu3+Fluorescent material.
Embodiment 8
Weighing calcium nitrate, aluminum nitrate, europium nitrate, trifluoroacetic acid, mol ratio is respectively 3 mMs, and 3.5
MM, 0.12 mM, 6 mMs are mixed to get mixed solution with water, are subsequently adding cross-linking agent and mix
Close uniformly, prepare colloidal sol；Colloidal sol described in heating in water bath, obtains gel；By described gel at 1100 DEG C
After calcining 4h, synthesize Ca11.52Al14O32F2∶0.48Eu3+Fluorescent material.
Embodiment 9
Weighing calcium nitrate, aluminum nitrate, europium nitrate, trifluoroacetic acid, mol ratio is respectively 3 mMs, and 3.5
MM, 0.15 mM, 6 mMs are mixed to get mixed solution with water, are subsequently adding cross-linking agent and mix
Close uniformly, prepare colloidal sol；Colloidal sol described in heating in water bath, obtains gel；By described gel at 1100 DEG C
After calcining 4h, synthesize Ca11.40Al14O32F2∶0.60Eu3+Fluorescent material.
In embodiment 1 and embodiment 5～9, the Eu of doping3+Concentration is synthesized by variable
Ca12-xAl14O32F2∶xEu3+The XRD figure modal data of (0≤x≤0.6) is as shown in Figure 5.As seen from the figure,
The diffraction maximum of fluorescent material synthesized by the range of 0≤x≤0.6 and Ca12Al14O32F2PDF standard diffraction
Card (53-1232) data consistent, illustrates Eu3+A small amount of doping of ion does not affect the phase structure of product,
The Eu adulterated3+Ionic portions replaces substrate Ca2+The case of ion.
In embodiment 1 and embodiment 6～9, the Eu of doping3+Concentration is synthesized by variable
Ca12-xAl14O32F2∶xEu3+The emission spectrum A (λ ex=245nm) of (0≤x≤0.6) and Eu3+
At concentration and counter sample 612nm, the relation curve B spectrum data of fluorescence intensity is as shown in figure 11, sends out
Ejected wave is a length of.As seen from the figure, along with the increase of europium ion-doped concentration, the luminous intensity of fluorescent material is gradually
Strengthening, when concentration reaches 3% (X=0.36), the luminous intensity of fluorescent material reaches the strongest, then as
The increase of europium doped ion concentration, the luminous intensity of fluorescent material gradually weakens.
Embodiment 10
Weighing calcium nitrate, aluminum nitrate, europium nitrate, trifluoroacetic acid, mol ratio is respectively 3 mMs, and 3.5
MM, 0.09 mM, 6 mMs are mixed to get mixed solution with water, are subsequently adding cross-linking agent and mix
Close uniformly, prepare colloidal sol；Colloidal sol described in heating in water bath, obtains gel；By described gel at 1000 DEG C
After calcining 4h, synthesize Ca11.64Al14O32F2∶0.36Eu3+Fluorescent material.
Embodiment 11
Weighing calcium nitrate, aluminum nitrate, europium nitrate, trifluoroacetic acid, mol ratio is respectively 3 mMs, and 3.5
MM, 0.09 mM, 6 mMs are mixed to get mixed solution with water, are subsequently adding cross-linking agent and mix
Close uniformly, prepare colloidal sol；Colloidal sol described in heating in water bath, obtains gel；By described gel at 900 DEG C
After calcining 4h, synthesize Ca11.64Al14O32F2∶0.36Eu3+Fluorescent material.
Embodiment 12
Weighing calcium nitrate, aluminum nitrate, europium nitrate, trifluoroacetic acid, mol ratio is respectively 3 mMs, and 3.5
MM, 0.09 mM, 6 mMs are mixed to get mixed solution with water, are subsequently adding cross-linking agent and mix
Close uniformly, prepare colloidal sol；Colloidal sol described in heating in water bath, obtains gel；By described gel at 1200 DEG C
After calcining 4h, synthesize Ca11.64Al14O32F2∶0.36Eu3+Fluorescent material.
In embodiment 1 and embodiment 10～12, the temperature of calcining is synthesized by variable
Ca11.64Al14O32F2∶0.36Eu3+XRD figure modal data as shown in Figure 2.As seen from the figure, when calcining temperature
When spending >=900 DEG C, synthesized product and Ca12Al14O32F2PDF standard diffraction card (53-1232) number
According to the most identical, but by concrete contrast, the XRD of sample when calcining heat is 900 DEG C and 1200 DEG C
Collection of illustrative plates is at the 2 obvious miscellaneous peaks of appearance, θ=32 °, and sample when calcining heat is 1000 DEG C and 1100 DEG C
XRD diffraction maximum fits like a glove with standard card, so calcining heat is chosen as 1000 DEG C or 1100 DEG C.
But in embodiment 1 and embodiment 10～12, the temperature of calcining is synthesized by variable
Ca11.64Al14O32F2∶0.36Eu3+Emission spectrum A (λ ex=233nm) and 612nm at fluorescence
Intensity to integral curve (B) spectrum data of calcining heat as it is shown in figure 9, transmitted wave is a length of.Can by figure
Seeing, along with the rising of temperature, the luminous intensity of fluorescent material gradually rises and reduces, when calcining heat is 1100
DEG C time, the luminous intensity of fluorescent material is the strongest.
Thermogravimetric curve (TGA) data as shown in Figure 1 are it can be seen that temperature is increased to 600 DEG C from 22 DEG C
During this, the weight of sample drastically reduces, and this is due to combustion decomposition such as C, H, the N in dry glue
Caused；600 DEG C to 900 DEG C, the weight of sample is basically unchanged, and forms mesophase；900 DEG C to 950 DEG C,
Example weight drastically reduces again, has moieties to decompose；950 DEG C～1300 DEG C, the weight of sample is the most not
Become, form stable thing phase.From differential thermal curve (DSC) it can be seen that there be the strongest putting at 564 DEG C
Thermal spike, the formation with mesophase is relevant, and the most unformed dry glue forms metastable centre through calcining
Phase；The exothermic peak of the last one is had, with Ca at 939 DEG C12Al14O32F2Crystalline formation relevant, i.e. mesophase
It is converted into Ca12Al14O32F2Crystalline phase.
Embodiment 13
Weighing calcium nitrate, aluminum nitrate, europium nitrate, trifluoroacetic acid, mol ratio is respectively 3 mMs, and 3.5
MM, 0.09 mM, 6 mMs are mixed to get mixed solution with water, are subsequently adding cross-linking agent and mix
Close uniformly, prepare colloidal sol；Colloidal sol described in heating in water bath, obtains gel；By described gel at 1100 DEG C
After calcining 2h, synthesize Ca11.64Al14O32F2∶0.36Eu3+Fluorescent material.
Embodiment 14
Weighing calcium nitrate, aluminum nitrate, europium nitrate, trifluoroacetic acid, mol ratio is respectively 3 mMs, and 3.5
MM, 0.09 mM, 6 mMs are mixed to get mixed solution with water, are subsequently adding cross-linking agent and mix
Close uniformly, prepare colloidal sol；Colloidal sol described in heating in water bath, obtains gel；By described gel at 1100 DEG C
After calcining 6h, synthesize Ca11.64Al14O32F2∶0.36Eu3+Fluorescent material.
Embodiment 15
Weighing calcium nitrate, aluminum nitrate, europium nitrate, trifluoroacetic acid, mol ratio is respectively 3 mMs, and 3.5
MM, 0.09 mM, 6 mMs are mixed to get mixed solution with water, are subsequently adding cross-linking agent and mix
Close uniformly, prepare colloidal sol；Colloidal sol described in heating in water bath, obtains gel；By described gel at 1100 DEG C
After calcining 8h, synthesize Ca11.64Al14O32F2∶0.36Eu3+Fluorescent material.
In embodiment 1 and embodiment 13～15, calcination time is synthesized by variable
Ca11.64Al14O32F2∶0.36Eu3+XRD figure modal data as shown in Figure 3.As seen from the figure: upon calcination
Between >=2h time, the diffraction maximum of synthesized sample and Ca12Al14O32F2PDF standard diffraction card (53-1232)
Data are the most identical, but by concrete contrast, when calcination time is respectively 2h, 6h and 8h,
Sample occurs miscellaneous peak near 2 θ=32 °, and the sample that calcination time is 4h does not occur miscellaneous near this
Peak or the most inconspicuous, so the calcination time of experiment elects 4h as.
In embodiment 1 and embodiment 13～15, calcination time is synthesized by variable
Ca11.64Al14O32F2∶0.36Eu3+Emission spectrum A (λ ex=245nm) and 612nm at fluorescence strong
Spend integral curve (B) spectrum data to calcination time as shown in Figure 10.As seen from the figure, along with calcining
The prolongation of time, the luminous intensity of fluorescent material gradually strengthens, upon calcination between when being 4h, fluorescent material
Luminous intensity reaches the strongest, and the continuation then as calcination time increases, and the luminous intensity of fluorescent material is gradually
Weaken.
In embodiment 1, by the Ca synthesized by sol-gal process11.64Al14O32F2∶0.36Eu3+Fluorescent material
Granule rounded, its particle diameter meansigma methods is about 40～100nm.With reference to Fig. 6.
In embodiment 1, by the Ca synthesized by sol-gal process11.64Al14O32F2∶0.36Eu3+Fluorescent material pair
The excitation spectrum A answered and emission spectrum B data are as shown in Figure 7.When monitoring wavelength and being 612nm,
Excitation spectrum has a strong broad peak that excites in 220～280nm scopes, has near 350-400nm simultaneously
Several weak narrow cutting edges of a knife or a sword, the former belongs to O2--Eu3+Charge migration absorb, the latter belongs to Eu3+F-f
Transition absorption, wherein the excitation peak at 393nm corresponds to Eu3+'s7F0→5L6Transition.Work as excitation wave
During a length of 233nm, can significantly see the emission peak at 586,598 and 612nm, these peaks are all
It is Eu3+Typical characteristic peak, be respectively belonging to5D1→7F3、5D0→7F1With5D0→7F2Energy level transition.
Although embodiment of the present invention are disclosed as above, but it is not restricted to description and embodiment party
In formula, listed utilization, for those skilled in the art, is easily achieved other amendment, because of
This is under the general concept limited without departing substantially from claim and equivalency range, and the present invention is not limited to specific
Details and shown here as with describe legend.
Claims (5)
1. the preparation method of an europium doped with fluorine aluminate substrate fluorescent powder, it is characterised in that
Comprise the following steps:
Step one, calcium nitrate, aluminum nitrate, europium nitrate, fluorochemical and water are mixed to get
Mixed solution, the mol ratio n (Al of aluminium ion and calcium ion in mixed solution3+)/n(Ca2+) >=7:6,
Mol ratio n (the F of fluorion and calcium ion-)/n(Ca2+) >=1:6, mixed solution and cross-linking agent mixing,
Preparing colloidal sol, wherein, described fluorochemical is trifluoroacetic acid, Potassium borofluoride or trifluoromethyl
Sulfonic acid magnesium；
Step 2, heat described colloidal sol, obtain gel；
Step 3, by described gel through calcining after, obtaining atomic ratio is
Ca12-xAl14O32F2:xEu3+Compound, wherein calcining heat is 950～1300 DEG C, during calcining
Between be 2～8h.
2. the preparation method of europium doped with fluorine aluminate substrate fluorescent powder as claimed in claim 1,
It is characterized in that, in described step 3, calcining heat is 1100 DEG C.
3. the preparation method of europium doped with fluorine aluminate substrate fluorescent powder as claimed in claim 2,
It is characterized in that, in described step 3, calcination time is 4h.
4. europium doped with fluorine aluminate substrate fluorescence as claimed any one in claims 1 to 3
The preparation method of powder, it is characterised in that in mixed solution, europium ion molar concentration is 1～5%.
5. the preparation method of europium doped with fluorine aluminate substrate fluorescent powder as claimed in claim 4,
It is characterized in that, in described step one, in mixed solution, europium ion molar concentration is 3%.
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