CN105860971B - Rare earth ion doped zirconium niobate fluorescent powder and preparation method thereof - Google Patents
Rare earth ion doped zirconium niobate fluorescent powder and preparation method thereof Download PDFInfo
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Abstract
The invention relates to rare earth ion doped zirconium niobate fluorescent powder and a preparation method thereof, and the material has a chemical formula of Zr6Nb2O17xEu, wherein x is Eu3+The rare earth ion doped zirconium niobate fluorescent powder is prepared by taking zirconium niobate as a substrate and adding rare earth ions by adopting a high-temperature solid phase method or a chemical synthesis method, has high luminous intensity and good stability, can absorb ultraviolet light near 267 nanometers and convert and emit red light near 613 nanometers, can be applied to the preparation of L ED lighting devices, has the advantages of simple and easy preparation method, no special gas protection, low requirements on production conditions and equipment, low production cost, no waste gas and waste liquid discharge, environmental friendliness and no pollution.
Description
Technical field
The present invention relates to a kind of fluorescent material and preparation method thereof, more particularly to a kind of rare earth ion doped niobic acid zirconium is glimmering
Light powder and preparation method thereof, belongs to phosphor field.
Background technology
As Global Environmental Problems aggravate, energy shortage, energy conservation and environmental protection becomes the important topic that current people face.General
Logical illumination light-emitting field, white light LEDs product become emphasis of concern.It is a kind of new green environment protection illuminating product, tool
There are higher electrical efficiency, less volume, low-power, high life, it is considered to be lighting source of new generation, has very
Good development trend.
White light LEDs, which produce white light, mainly two approach：The first is that three kinds of LED combinations of red, green, blue are produced white light；
Second is to deactivate luminous conversion phosphor with LED to be mixed to form white light, and this approach has two kinds of implementations, wherein comparing into
Ripe method is blue-light LED chip and YAG:Ce yellow fluorescent powders are arranged in pairs or groups to realize white light emission (United States Patent (USP) 5998925), but
Due to lacking red light, compound obtained white light is cool white light, and therefore, the program still needs to add appropriate red fluorescence powder to carry
Its high colour rendering index, another scheme is then with nearly purple LED chip (390-410nm) and red green blue three primary colors fluorescent powder group
Close, therefore red fluorescence powder plays very important effect.And effective excites scope majority of existing red fluorescence powder is short
Ripple UV regions, the launching efficiency under near ultraviolet and blue light are low.Therefore, the black light of efficient stable, blue-ray LED are developed with red
Color fluorescent powder is particularly important.At present, in the market still lacks being excited by black light or blue-light LED chip for excellent performance
Red fluorescence powder.
At present, the red fluorescence powder that application requirement can be all reached in terms of luminous intensity and stability is also rarely found.Example
Such as：Attempt to Y2O2S:Eu3+Applied to WLED fields, however, commercial red fluorescence powder Y at present2O2S:Eu3+There are all
More shortcomings：Luminous efficiency is low under near ultraviolet excitation, and chemical property is unstable, easily decomposes, short life, the precipitation of element sulphur
Corrosive effects can be caused to chip, so as to cause the failure of whole device.In addition, several involved in document and patent report
Class it is main be expected to also have for the red fluorescence powder of LED：Ca3(VO4)2:Eu3+、YVO4:Eu3+、Y2O3:Eu3+, Bi3+、CaO:
Eu3+、CaMoO4:Eu3+、(Gd,Y,Eu)2(MoO4)3:Sm3+、Ca5(SiO4)2Cl2:Eu2+、Sr2Si5N8:Eu2+Deng.Its middle rare earth
The stability high-luminous-efficiency of the nitrogen oxides of activation is good and is taken seriously, such as：Sr2Si5N8:Eu2+、SrSi2O2N2:Eu2+, but
The matrix synthesis of this kind of material needs to complete under the high nitrogen of high temperature (1600-1700 DEG C) or ammonia pressure (10atm), to production
The requirement of equipment is very harsh.
At this stage, on niobates for matrix fluorescent powder document report and patent it is seldom, Chinese invention patent
CN201310089492.1 reports a kind of metal nano particle-doped niobate luminescent material and preparation method thereof, this shines
Material can be applied to feds.Chinese patent CN201310580990.6 reports a kind of europium terbium codope aluminium niobates
Luminescent material, light-emitting film made of the europium terbium codope aluminium niobate luminescent material in 490 nanometers and 510 nm wavelength regions all
There is very strong glow peak, can be applied in thin-film electroluminescent displays.
The content of the invention
In view of the above-mentioned problems of the prior art, it is an object of the invention to provide a kind of illumination effect is good, stability
It is good, it can be applied to the rare earth ion doped niobic acid zirconium fluorescent powder of LED illumination device preparation；Another object of the present invention is to
There is provided it is a kind of prepare simple, energy consumption less, the preparation method of the low rare earth ion doped niobic acid zirconium fluorescent powder of production cost.
To achieve the above object, the technical solution adopted by the present invention is：A kind of rare earth ion doped niobic acid zirconium fluorescent powder,
The chemical formula of material is Zr6Nb2O17:XEu, wherein x are Eu3+The mole percent of doping, 0.0001≤x≤0.5.
The present invention also provides a kind of preparation method of above-mentioned rare earth ion doped niobic acid zirconium fluorescent powder, consolidated using high temperature
Xiang Fa, includes the following steps：
(1) chemical formula Zr is pressed6Nb2O17:Stoichiometric ratio in xEu, wherein 0.0001≤x≤0.5, weigh respectively containing
Zirconium ion Zr4+Compound, contain niobium ion Nb5+Compound, contain europium ion Eu3+Compound, grind and mix
It is even, obtain mixture；
(2) mixture that step (1) obtains is subjected to precalcining in air atmosphere, precalcining temperature is 300~700
DEG C, when precalcination time is 2~12 small；
(3) the mixture natural cooling for obtaining step (2), grinds and after mixing, calcines, forge in air atmosphere
It is 700~1100 DEG C to burn temperature, when calcination time is 2~12 small；
(4) the mixture natural cooling for obtaining step (3), grinds and after mixing, is carried out most in air atmosphere
Eventually calcining, calcining heat be 1100~1500 DEG C, calcination time for 2~12 it is small when, naturally cool to room temperature, that is, obtain rare earth from
The niobic acid zirconium fluorescent powder of son doping.
As the preferred solution of the above method, the precalcining temperature of step (2) is 350~650 DEG C, precalcination time 4
~10 it is small when.
As the preferred solution of the above method, the calcining heat of step (3) is 750~1050 DEG C, and calcination time is 4~10
Hour.
As the preferred solution of the above method, the calcining heat of step (4) is 1150~1450 DEG C, calcination time for 4~
10 it is small when.
It is above-mentioned to contain zirconium ion Zr4+Compound be zirconium oxide ZrO2, zirconium nitrate Zr (NO3)4·5H2O, zirconium hydroxide Zr
(OH)4, zirconium chloride ZrCl4In one kind；Described contains niobium ion Nb5+Compound be niobium pentaoxide Nb2O5, hydroxide
Niobium Nb (OH)5With niobium chloride NbCl5In one kind；Described contains europium ion Eu3+Compound be europium oxide Eu2O3, europium nitrate
Eu(NO3)3·6H2O, europium carbonate Eu2(CO3)3In one kind.
The present invention also provides the preparation method of another above-mentioned rare earth ion doped niobic acid zirconium fluorescent powder at the same time, using change
Synthetic method is learned, is included the following steps：
(1) chemical formula Zr is pressed6Nb2O17:Stoichiometric ratio in xEu, wherein 0.0001≤x≤0.5, weighs containing zirconium respectively
Ion Zr4+Compound, contain niobium ion Nb5+Compound, contain europium ion Eu3+Compound, they are dissolved separately in
In dilute nitric acid solution, respective clear solution is obtained；Complexing agent lemon is added respectively by 0.5~2.0wt% of each reactant quality
Lemon acid or oxalic acid, stir evenly under 50~100 DEG C of temperature conditionss；
(2) the various solution that step (1) obtains are slowly mixed together, it is small that 1~2 is stirred under 50~100 DEG C of temperature conditionss
Shi Hou, stands, and drying, obtains fluffy presoma；
(3) presoma is placed in Muffle furnace and calcined, calcining heat is 1100~1400 DEG C, and calcination time is small for 3~12
When, room temperature is naturally cooled to, a kind of powdered phosphor is obtained after grinding uniformly.
Preferably, it is described to contain zirconium ion Zr4+Compound be zirconium oxide ZrO2, zirconium nitrate Zr (NO3)4·5H2O, hydrogen-oxygen
Change zirconium Zr (OH)4, zirconium chloride ZrCl4In one kind；Described contains niobium ion Nb5+Compound be niobium pentaoxide Nb2O5、
Niobium hydroxide Nb (OH)5With niobium chloride NbCl5In one kind；Described contains europium ion Eu3+Compound be europium oxide Eu2O3、
Europium nitrate Eu (NO3)3·6H2O and europium carbonate Eu2(CO3)3In one kind.
Compared with prior art, technical solution of the present invention advantage is：The rare earth ion doped niobic acid of the present invention
Zirconium light-emitting phosphor intensity is high, stability is good, can absorb the ultraviolet light near 267 nanometers, switching emission goes out near 613 nanometers
Feux rouges, can be applied to the preparation of LED illumination device；Preparation method is simply easily operated, is also protected without using special gas,
Not high to working condition and equipment requirement, production cost is low, no waste gas and waste liquid discharge, environmental-friendly pollution-free.
Brief description of the drawings
Fig. 1 is the X-ray powder diffraction pattern that the embodiment of the present invention 1 prepares sample；
Fig. 2 is that the embodiment of the present invention 1 prepares exciting light spectrogram of the sample under the monitoring of 613 nano wave lengths；
Fig. 3 is that the embodiment of the present invention 1 prepares luminescent spectrum figure of the sample under the excitation of 267 nano wave lengths；
Fig. 4 is the decay of luminescence curve that the embodiment of the present invention 1 prepares sample；
Fig. 5 is the scanning electron microscope microphoto that the embodiment of the present invention 1 prepares sample；
Fig. 6 is the X-ray powder diffraction pattern that the embodiment of the present invention 5 prepares sample；
Fig. 7 is that the embodiment of the present invention 5 prepares exciting light spectrogram of the sample under the monitoring of 613 nano wave lengths；
Fig. 8 is that the embodiment of the present invention 5 prepares luminescent spectrum figure of the sample under the excitation of 267 nano wave lengths；
Fig. 9 is the decay of luminescence curve that the embodiment of the present invention 5 prepares sample；
Figure 10 is the scanning electron microscope microphoto that the embodiment of the present invention 5 prepares sample.
Embodiment
The invention will be further described with reference to the accompanying drawings and examples.
Embodiment 1
According to chemical formula Zr6Nb2O17:0.0001Eu weighs zirconium oxide ZrO2：7.392 grams, europium oxide Eu2O3：0.001 gram,
Niobium pentaoxide Nb2O5：2.658 grams, added in agate mortar suitable acetone mixed grinding it is uniform after, in air atmosphere
Precalcining is carried out, when calcining 4 is small at 350 DEG C after furnace cooling, takes out sample by the raw material of precalcining again with identical side
Method is sufficiently mixed grinding uniformly, is calcined again in air atmosphere, when calcining 4 is small at 750 DEG C, is cooled to room temperature, and takes out sample.
Mixed grinding is uniform again, among air atmosphere, when finally calcining 4 is small at 1150 DEG C, is cooled to room temperature, is fully ground after taking-up
Mill obtains sample.
It is the X-ray powder diffraction pattern that the present embodiment technical solution prepares sample referring to Fig. 1；XRD test results are shown
Show, prepared sample crystallinity is preferable, is single phase pure material.
It is the exciting light by sample prepared by the present embodiment technical solution under the monitoring of 613 nano wave length light referring to Fig. 2
Spectrum, test result show that sample can absorb the ultraviolet light near 267 nanometers.
Fig. 3 is the launching light spectrogram under the excitation of 267 nano wave length light by sample prepared by the present embodiment technical solution, is surveyed
Test result shows that sample launches light of the centre wavelength at 613 nanometers, obtained material under 267 nanometers nearby excitation of light
Transmitting feux rouges can effectively be converted ultraviolet light into.
It is the decay of luminescence curve that the embodiment of the present invention 1 prepares sample referring to Fig. 4, can be calculated die-away time as 1.899
Millisecond.
It is the scanning electron microscope microphoto that the embodiment of the present invention 1 prepares sample referring to Fig. 5, gained sample granularity disperses
Even, its average grain diameter is 1.69 microns.
Embodiment 2
According to chemical formula Zr6Nb2O17:0.01Eu weighs zirconium nitrate Zr (NO3)4·5H2O：6.433 grams, europium carbonate Eu2
(CO3)3：0.004 gram, niobium hydroxide Nb (OH)5：0.890 gram, it is uniform that suitable acetone mixed grinding is added in agate mortar
Afterwards, precalcining is carried out in air atmosphere, when precalcining 2 is small at 300 DEG C after furnace cooling, takes out sample by the original of precalcining
Material is sufficiently mixed grinding uniformly with identical method again, is calcined again in air atmosphere, when calcining 2 is small at 700 DEG C, cooling
To room temperature, sample is taken out.Mixed grinding is uniform again, among air atmosphere, when finally calcining 2 is small at 1100 DEG C, is cooled to
Room temperature, is fully ground after taking-up and obtains sample.
The present embodiment technical solution prepares the X-ray powder diffraction pattern of sample, exciting light spectrogram, fluorescence spectra, hair
Optical attenuation curve, scanning electron microscope microphoto are consistent with the sample prepared in embodiment 1.
Embodiment 3
According to chemical formula Zr6Nb2O17:0.01Eu weighs zirconium hydroxide Zr (OH)4：3.153 grams, europium nitrate Eu (NO3)3·
6H2O：0.089 gram, niobium chloride NbCl5：1.801 grams, added in agate mortar suitable acetone mixed grinding it is uniform after, in sky
Precalcining is carried out in gas atmosphere, when precalcining 12 is small at 700 DEG C after furnace cooling, take out sample by the raw material of precalcining again
Grinding is sufficiently mixed with identical method uniformly, is calcined again in air atmosphere, when calcining 12 is small at 1100 DEG C, is cooled to room
Temperature, takes out sample.Regrinding is uniform, among air atmosphere, when finally calcining 12 is small at 1500 DEG C, is cooled to room temperature, takes
It is fully ground after going out and obtains sample.
The present embodiment technical solution prepares the X-ray powder diffraction pattern of sample, exciting light spectrogram, fluorescence spectra, hair
Optical attenuation curve, scanning electron microscope microphoto are consistent with the sample prepared in embodiment 1.
Embodiment 4
According to chemical formula Zr6Nb2O17:0.1Eu weighs zirconium chloride ZrCl4：4.198 grams, europium oxide Eu2O3：0.352 gram, five
Aoxidize two niobium Nb2O5：0.886 gram, added in agate mortar suitable acetone mixed grinding it is uniform after, in air atmosphere into
Row precalcining, when precalcining 10 is small at 650 DEG C after furnace cooling, takes out sample by the raw material of precalcining again with identical side
Method is sufficiently mixed grinding uniformly, is calcined again in air atmosphere, when calcining 10 is small at 1050 DEG C, is cooled to room temperature, and takes out sample
Product.Mixed grinding is uniform again, among air atmosphere, when finally calcining 10 is small at 1450 DEG C, is cooled to room temperature, is filled after taking-up
Grinding is divided to obtain sample.
The present embodiment technical solution prepares the X-ray powder diffraction pattern of sample, exciting light spectrogram, fluorescence spectra, hair
Optical attenuation curve, scanning electron microscope microphoto are consistent with the sample prepared in embodiment 1.
Embodiment 5
According to chemical formula Zr6Nb2O17:0.2Eu weighs zirconium oxide ZrO2：1.183 grams, europium carbonate Eu2(CO3)3：0.581 gram,
Niobium hydroxide Nb (OH)5：0.712 gram, and the citric acid of the 1.8wt% of each drug quality of the above is weighed respectively.By what is weighed
Zirconium oxide ZrO2, europium carbonate Eu2(CO3)3, niobium hydroxide Nb (OH)5It is separately added into dilute nitric acid solution until being completely dissolved, then add
Enter the citric acid weighed magnetic agitation under the conditions of 50 DEG C and obtain settled solution for a period of time.Most above-mentioned solution is mixed at last
1.5 it is small when, obtained mixed solution is placed in baking oven, and design temperature is 80 DEG C, dry 12 it is small when after, natural cooling, obtains forerunner
Body.Presoma is placed in Muffle furnace and is calcined, calcining heat is 1100 DEG C, when calcination time is 3 small, is cooled to room temperature, takes out
And it is fully ground and obtains sample.
It is the X-ray powder diffraction pattern that the present embodiment technical solution prepares sample referring to attached drawing 6, the results show that being made
Sample crystallization it is good, no dephasign.
It is the exciting light by sample prepared by the present embodiment technical solution under the monitoring of 613 nano wave lengths referring to attached drawing 7
Spectrum, test result show that sample can absorb the ultraviolet light near 267 nanometers.
Attached drawing 8 is the launching light spectrogram under the excitation of 267 nano wave lengths, institute by sample prepared by the present embodiment technical solution
Obtained material is effectively by ultraviolet light switching emission feux rouges.
It is the decay of luminescence curve that the embodiment of the present invention 5 prepares sample referring to attached drawing 9, can be calculated die-away time is
1.951 millisecond.
It is the scanning electron microscope microphoto that the present embodiment technical solution prepares sample referring to attached drawing 10, the results show that being made
Sample particle it is more tiny, its average grain diameter be 0.11 micron.
Embodiment 6
According to chemical formula Zr6Nb2O17:0.3Eu weighs zirconium nitrate Zr (NO3)4·5H2O：3.606 grams, europium nitrate Eu
(NO3)3·6H2O：1.606 grams, niobium chloride NbCl5：1.081 grams, and weigh the 2.0wt% of each drug quality of the above respectively
Citric acid.Zirconium nitrate Zr (the NO that will be weighed3)4·5H2O, europium nitrate Eu (NO3)3·6H2O, niobium chloride NbCl5It is dissolved in appropriate
Dust technology in, and add the citric acid of the weighing magnetic agitation under the conditions of 100 DEG C and obtain settled solution for a period of time.Most at last
Above-mentioned solution be mixed 1 it is small when, obtained mixed solution is placed in baking oven, and design temperature is 80 DEG C, dry 12 it is small when after, it is natural
Cooling, obtains presoma.Presoma is placed in Muffle furnace and is calcined, calcining heat is 1200 DEG C, cold when calcination time is 6 small
But to room temperature, take out and be fully ground and obtain sample.
The present embodiment technical solution prepares the X-ray powder diffraction pattern of sample, exciting light spectrogram, fluorescence spectra, hair
Optical attenuation curve, scanning electron microscope microphoto are consistent with the sample prepared in embodiment 5.
Embodiment 7
According to chemical formula Zr6Nb2O17:0.4Eu weighs zirconium hydroxide Zr (OH)4：1.147 grams, europium oxide Eu2O3：0.845
Gram, niobium pentaoxide Nb2O5：0.532 gram, and the oxalic acid of the 0.5wt% of each drug quality of the above is weighed respectively.By what is weighed
Zirconium hydroxide Zr (OH)4, europium oxide Eu2O3, niobium pentaoxide Nb2O5It is dissolved separately in suitable dust technology, and adds and weigh
Citric acid under the conditions of 80 DEG C magnetic agitation obtain settled solution for a period of time.Most above-mentioned solution mixing 1.5 is small at last
When, obtained mixed solution is placed in baking oven, and design temperature is 80 DEG C, dry 12 it is small when after, natural cooling, obtains presoma.Will
Presoma is placed in Muffle furnace and calcines, and calcining heat is 1300 DEG C, when calcination time is 9 small, is cooled to room temperature, and takes out simultaneously abundant
Grinding obtains sample.
The present embodiment technical solution prepares the X-ray powder diffraction pattern of sample, exciting light spectrogram, fluorescence spectra, hair
Optical attenuation curve, scanning electron microscope microphoto are consistent with the sample prepared in embodiment 5.
Embodiment 8
According to chemical formula Zr6Nb2O17:The stoichiometric ratio of each element in 0.5Eu, weighs zirconium chloride ZrCl respectively4：1.399
Gram, europium carbonate Eu2(CO3)3：1.452 grams, niobium hydroxide Nb (OH)5：0.712 gram, and each drug quality of the above is weighed respectively
1.8wt% citric acid.The zirconium chloride ZrCl that will be weighed4, europium carbonate Eu2(CO3)3, niobium hydroxide Nb (OH)5It is dissolved separately in
Until being completely dissolved in suitable dust technology, add the citric acid weighed magnetic agitation under the conditions of 100 DEG C and obtain for a period of time
Settled solution, when most above-mentioned solution mixing 2 is small at last, obtained mixed solution is placed in baking oven, and design temperature is 80 DEG C,
Dry 12 it is small when after, natural cooling, take out presoma.Presoma is placed in Muffle furnace and is calcined, 1400 DEG C of calcining heat, during calcining
Between 12 it is small when, be cooled to room temperature, take out and be fully ground and obtain sample.
The present embodiment technical solution prepares the X-ray powder diffraction pattern of sample, exciting light spectrogram, fluorescence spectra, hair
Optical attenuation curve, scanning electron microscope microphoto are consistent with the sample prepared in embodiment 5.
Claims (8)
- A kind of 1. rare earth ion doped niobic acid zirconium fluorescent powder, it is characterised in that：The chemical formula of the material is Zr6Nb2O17: XEu, wherein x are Eu3+The mole percent of doping, 0.0001≤x≤0.5.
- 2. a kind of preparation method of rare earth ion doped niobic acid zirconium fluorescent powder as claimed in claim 1, it is characterised in that adopt With high temperature solid-state method, include the following steps：(1) chemical formula Zr is pressed6Nb2O17:Stoichiometric ratio in xEu, wherein 0.0001≤x≤0.5, weigh respectively containing zirconium from Sub- Zr4+Compound, contain niobium ion Nb5+Compound, contain europium ion Eu3+Compound, grind and be uniformly mixed, obtain To mixture；(2) mixture that step (1) obtains is subjected to precalcining in air atmosphere, precalcining temperature is 300~700 DEG C, in advance When calcination time is 2~12 small；(3) the mixture natural cooling for obtaining step (2), grinds and after mixing, is calcined in air atmosphere, calcining temperature Spend for 700~1100 DEG C, when calcination time is 2~12 small；(4) the mixture natural cooling for obtaining step (3), grinds and after mixing, is finally forged in air atmosphere Burn, calcining heat is 1100~1500 DEG C, when calcination time is 2~12 small, naturally cools to room temperature, that is, obtains rare earth ion and mix Miscellaneous niobic acid zirconium fluorescent powder.
- 3. the preparation method of rare earth ion doped niobic acid zirconium fluorescent powder according to claim 2, it is characterised in that：Step (2) precalcining temperature is 350~650 DEG C, when precalcination time is 4~10 small.
- 4. the preparation method of rare earth ion doped niobic acid zirconium fluorescent powder according to claim 2, it is characterised in that：Step (3) calcining heat is 750~1050 DEG C, when calcination time is 4~10 small.
- 5. the preparation method of rare earth ion doped niobic acid zirconium fluorescent powder according to claim 2, it is characterised in that：Step (4) calcining heat is 1150~1450 DEG C, when calcination time is 4~10 small.
- 6. the preparation method of rare earth ion doped niobic acid zirconium fluorescent powder according to claim 2, it is characterised in that：It is described Contain zirconium ion Zr4+Compound be zirconium oxide ZrO2, zirconium nitrate Zr (NO3)4·5H2O, zirconium hydroxide Zr (OH)4, chlorination Zirconium ZrCl4In one kind；Described contains niobium ion Nb5+Compound be niobium pentaoxide Nb2O5, niobium hydroxide Nb (OH)5With Niobium chloride NbCl5In one kind；Described contains europium ion Eu3+Compound be europium oxide Eu2O3, europium nitrate Eu (NO3)3· 6H2O, europium carbonate Eu2(CO3)3In one kind.
- 7. a kind of preparation method of rare earth ion doped niobic acid zirconium fluorescent powder as claimed in claim 1, it is characterised in that adopt With chemical synthesis, include the following steps：(1) chemical formula Zr is pressed6Nb2O17:Stoichiometric ratio in xEu, wherein 0.0001≤x≤0.5, weighs containing zirconium ion respectively Zr4+Compound, contain niobium ion Nb5+Compound, contain europium ion Eu3+Compound, they are dissolved separately in dilute nitre In acid solution, respective clear solution is obtained；Complexing agent citric acid is added respectively by 0.5~2.0wt% of each reactant quality Or oxalic acid, stirred evenly under 50~100 DEG C of temperature conditionss；(2) the various solution that step (1) obtains are slowly mixed together, under 50~100 DEG C of temperature conditionss stir 1~2 it is small when after, Stand, drying, obtains fluffy presoma；(3) presoma being placed in Muffle furnace and calcined, calcining heat is 1100~1400 DEG C, when calcination time is 3~12 small, from Room temperature is so cooled to, a kind of powdered phosphor is obtained after grinding uniformly.
- 8. the preparation method of rare earth ion doped niobic acid zirconium fluorescent powder according to claim 7, it is characterised in that：It is described Contain zirconium ion Zr4+Compound be zirconium oxide ZrO2, zirconium nitrate Zr (NO3)4·5H2O, zirconium hydroxide Zr (OH)4, chlorination Zirconium ZrCl4In one kind；Described contains niobium ion Nb5+Compound be niobium pentaoxide Nb2O5, niobium hydroxide Nb (OH)5With Niobium chloride NbCl5In one kind；Described contains europium ion Eu3+Compound be europium oxide Eu2O3, europium nitrate Eu (NO3)3· 6H2O and europium carbonate Eu2(CO3)3In one kind.
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