CN105860971A - 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 doping mole percentage is that x is more than or equal to 0.0001 and less than or equal to 0.5. The invention adopts a high-temperature solid phase method or a chemical synthesis method to prepare zirconium niobateIs prepared by adding rare earth ions as a matrix. The rare earth ion doped zirconium niobate fluorescent powder has high luminous intensity and good stability, can absorb ultraviolet light near 267 nanometers, convert and emit red light near 613 nanometers, and can be applied to the preparation of LED lighting devices; the preparation method is simple and easy to operate, does not use special gas protection, has low requirements on production conditions and equipment, has low production cost, does not discharge waste gas and waste liquid, and is environment-friendly and pollution-free.
Description
Technical field
The present invention relates to a kind of fluorescent material and preparation method thereof, particularly to a kind of rare earth ion doped niobic acid zirconium fluorescent material and
Its preparation method, belongs to phosphor field.
Background technology
Along with Global Environmental Problems increases the weight of, energy shortage, energy-conserving and environment-protective become the important topic that current people face.Shine common
Bright illumination field, white light LEDs product becomes emphasis of concern.It is a kind of new green environment protection illuminating product, has relatively
The advantages such as high electrical efficiency, less volume, low-power, high life, it is considered to be a new generation's lighting source, have very well
Development trend.
White light LEDs produces white light mainly two approach: the first is that three kinds of LED combination of red, green, blue are produced white light；
The 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 compares
Ripe method is that blue-light LED chip realizes white light emission (United States Patent (USP) with the collocation of YAG:Ce yellow fluorescent powder
5998925), but owing to lacking red light, the compound white light obtained is cool white light, and therefore, the program still needs to add suitable red
Color fluorescent material improves its color rendering index, and another kind of scheme is then by nearly purple LED chip (390-410nm) and red green blue
Three primary colors fluorescent powder combines, and therefore red fluorescence powder plays very important effect.And effectively the exciting of existing red fluorescence powder
Scope is most in shortwave UV region, and the launching efficiency under near ultraviolet and blue light is low.Therefore, the near ultraviolet of efficient stable is developed
Light, blue-ray LED red fluorescence powder are particularly important.At present, market still lacks excellent performance can by black light or
The red fluorescence powder that blue-light LED chip excites.
At present, it is possible to the red fluorescence powder all reaching application requirement in terms of luminous intensity and stability is the most rarely found.Such as: have
People attempts Y2O2S:Eu3+It is applied to WLED field, but, the most commercial red fluorescence powder Y2O2S:Eu3+Exist many
Shortcoming: luminous efficiency is low under near ultraviolet excitation, chemical property is unstable, easily decomposes, and the life-span is short, the precipitation of element sulphur
Chip can be caused corrosive effects, thus cause the inefficacy of whole device.It addition, relate in document and patent report is several
What class was main be expected also has 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
The stability high-luminous-efficiency of the nitrogen oxides that middle rare earth activates is good and comes into one's own, such as: Sr2Si5N8:Eu2+、
SrSi2O2N2:Eu2+, but the synthesis of the substrate of this kind of material needs in high temperature (1600-1700 DEG C) high nitrogen or ammonia pressure (10atm)
Under complete, to produce equipment requirement the harshest.
Present stage, the document about the fluorescent material that niobates is substrate is reported and patent is little, Chinese invention patent
CN201310089492.1 reports a kind of metal nano particle-doped niobate luminescent material and preparation method thereof, this luminescence material
Material can apply to feds.It is luminous that Chinese patent CN201310580990.6 reports a kind of europium terbium codope aluminum niobates
Material, the light-emitting film that this europium terbium codope aluminum niobate luminescent material is made has very in 490 nanometers and 510 nm wavelength region
Strong glow peak, it is possible to be applied in thin-film electroluminescent displays.
Summary of the invention
The problem existed for above-mentioned prior art, it is an object of the invention to provide that a kind of illumination effect is good, good stability, can
To be applied to rare earth ion doped niobic acid zirconium fluorescent material prepared by LED illumination device；Another object of the present invention is to provide one
Kind prepare simple, power consumption less, the preparation method of rare earth ion doped niobic acid zirconium fluorescent material that production cost is low.
For achieving the above object, the technical solution used in the present invention is: a kind of rare earth ion doped niobic acid zirconium fluorescent material, material
Chemical formula be Zr6Nb2O17: xEu, wherein x is Eu3+The mole percent of doping, 0.0001≤x≤0.5.
The present invention also provides for the preparation method of a kind of above-mentioned rare earth ion doped niobic acid zirconium fluorescent material, uses high temperature solid-state method,
Comprise the steps:
(1) chemical formula Zr is pressed6Nb2O17: the stoichiometric proportion in xEu, wherein 0.0001≤x≤0.5, weigh respectively containing zirconium from
Sub-Zr4+Compound, containing niobium ion Nb5+Compound, containing europium ion Eu3+Compound, grind and mix homogeneously,
Obtain mixture；
(2) mixture that step (1) obtains being carried out precalcining in air atmosphere, precalcining temperature is 300～700 DEG C,
The precalcining time is 2～12 hours；
(3) mixture natural cooling step (2) obtained, grinds and after mix homogeneously, calcines, forge in air atmosphere
Burning temperature is 700～1100 DEG C, and calcination time is 2～12 hours；
(4) mixture natural cooling step (3) obtained, grinds and after mix homogeneously, carries out final in air atmosphere
Calcining, calcining heat is 1100～1500 DEG C, and calcination time is 2～12 hours, naturally cools to room temperature, i.e. obtain rare earth from
The niobic acid zirconium fluorescent material of son doping.
As the preferred version of said method, the precalcining temperature of step (2) is 350～650 DEG C, the precalcining time be 4～
10 hours.
As the preferred version of said method, the calcining heat of step (3) is 750～1050 DEG C, and calcination time is 4～10 little
Time.
As the preferred version of said method, the calcining heat of step (4) is 1150～1450 DEG C, and calcination time is 4～10
Hour.
Above-mentioned containing zirconium ion Zr4+Compound be zirconium oxide ZrO2, zirconium nitrate Zr (NO3)4·5H2O, zirconium hydroxide Zr (OH)4、
Zirconium chloride ZrCl4In one；Described containing niobium ion Nb5+Compound be niobium pentaoxide Nb2O5, niobium hydroxide
Nb(OH)5With niobium chloride NbCl5In one；Described containing europium ion Eu3+Compound be europium oxide Eu2O3, europium nitrate
Eu(NO3)3·6H2O, europium carbonate Eu2(CO3)3In one.
The present invention provides the preparation method of another kind of above-mentioned rare earth ion doped niobic acid zirconium fluorescent material the most simultaneously, uses chemosynthesis
Method, comprises the steps:
(1) chemical formula Zr is pressed6Nb2O17: stoichiometric proportion in xEu, wherein 0.0001≤x≤0.5, weigh respectively containing zirconium ion
Zr4+Compound, containing niobium ion Nb5+Compound, containing europium ion Eu3+Compound, they are dissolved separately in dilute
In salpeter solution, obtain respective clear solution；By the 0.5～2.0wt% of each reactant quality add respectively chelating agent citric acid or
Oxalic acid, stirs under the temperature conditions of 50～100 DEG C；
(2) the various solution that step (1) obtains are slowly mixed together, stir 1～2 hour under the temperature conditions of 50～100 DEG C
After, stand, dry, obtain fluffy presoma；
(3) presoma being placed in Muffle furnace calcining, calcining heat is 1100～1400 DEG C, and calcination time is 3～12 hours,
Naturally cool to room temperature, after grinding uniformly, obtain a kind of powdered phosphor.
Preferably, described containing zirconium ion Zr4+Compound be zirconium oxide ZrO2, zirconium nitrate Zr (NO3)4·5H2O, hydroxide
Zirconium Zr (OH)4, zirconium chloride ZrCl4In one；Described containing niobium ion Nb5+Compound be niobium pentaoxide Nb2O5、
Niobium hydroxide Nb (OH)5With niobium chloride NbCl5In one；Described containing europium ion Eu3+Compound be europium oxide Eu2O3、
Europium nitrate Eu (NO3)3·6H2O and europium carbonate Eu2(CO3)3In one.
Compared with prior art, technical solution of the present invention advantage is: the rare earth ion doped niobic acid zirconium fluorescence of the present invention
Powder luminous intensity is high, good stability, can absorb the ultraviolet light of 267 nm, and switching emission goes out the red of 613 nm
Light, it is possible to be applied to the preparation of LED illumination device；Preparation method is the most easily operated, does not the most use special gas to protect, right
Working condition and equipment requirements are the highest, and production cost is low, discharge without waste gas and waste liquid, and environmental friendliness is pollution-free.
Accompanying drawing explanation
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 sample exciting light spectrogram under 613 nano wave length monitoring；
Fig. 3 is that the embodiment of the present invention 1 prepares sample luminescent spectrum figure under 267 nano wave lengths excite；
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 microphotograph 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 sample exciting light spectrogram under 613 nano wave length monitoring；
Fig. 8 is that the embodiment of the present invention 5 prepares sample luminescent spectrum figure under 267 nano wave lengths excite；
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 microphotograph that the embodiment of the present invention 5 prepares sample.
Detailed description of the invention
The invention will be further described with embodiment below in conjunction with the accompanying drawings.
Embodiment 1
According to chemical formula Zr6Nb2O17: 0.0001Eu weighs zirconium oxide ZrO2: 7.392 grams, europium oxide Eu2O3: 0.001 gram, five
Aoxidize two niobium Nb2O5: 2.658 grams, add in agate mortar appropriate acetone mixed grinding uniformly after, at air
Atmosphere carries out precalcining, after calcining 4 hours furnace cooling at 350 DEG C, takes out sample by the raw material of precalcining
Again it is sufficiently mixed grinding uniformly by identical method, again calcines in air atmosphere, calcine 4 at 750 DEG C little
Time, it is cooled to room temperature, takes out sample.Mixed grinding is uniform again, and among air atmosphere, at 1150 DEG C, final calcining 4 is little
Time, it is cooled to room temperature, is fully ground after taking-up and i.e. obtains sample.
See Fig. 1, be the present embodiment technical scheme X-ray powder diffraction pattern of preparing sample；XRD test result shows,
Prepared sample crystallinity is preferable, for single phase pure material.
See Fig. 2, be the sample prepared by the present embodiment technical scheme excitation spectrum under 613 nano wave length light monitoring, survey
Test result display sample can absorb the ultraviolet light of 267 nm.
Fig. 3 is the sample prepared by the present embodiment technical scheme emission spectrum figure under 267 nano wave length light excite, test knot
Fruit shows, the centre wavelength light in 613 nanometers launched under the exciting of 267 nm light by sample, and obtained material can
Effectively convert ultraviolet light into transmitting HONGGUANG.
Seeing Fig. 4, be the embodiment of the present invention 1 decay of luminescence curve of preparing sample, can be calculated die-away time is 1.899 milliseconds.
Seeing Fig. 5, be the embodiment of the present invention 1 scanning electron microscope microphotograph of preparing sample, gained sample granularity is uniformly dispersed, its
Mean diameter is 1.69 microns.
Embodiment 2
According to chemical formula Zr6Nb2O17: 0.01Eu weighs zirconium nitrate Zr (NO3)4·5H2O:6.433 gram, europium carbonate Eu2(CO3)3:
0.004 gram, niobium hydroxide Nb (OH)5: 0.890 gram, agate mortar adds appropriate acetone mixed grinding uniform
After, air atmosphere carries out precalcining, at 300 DEG C after 2 hours furnace cooling of precalcining, taking out sample will
The raw material of precalcining is sufficiently mixed grinding uniformly by identical method again, again calcines in air atmosphere,
Calcine 2 hours at 700 DEG C, be cooled to room temperature, take out sample.Mixed grinding is uniform again, among air atmosphere, and 1100 DEG C
Lower final calcining 2 hours, is cooled to room temperature, is fully ground and i.e. obtains sample after taking-up.
The present embodiment technical scheme prepares the X-ray powder diffraction pattern of sample, exciting light spectrogram, fluorescence spectrum figure, luminescence decline
Subtract curve, scanning electron microscope microphotograph with in embodiment 1 preparation sample consistent.
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, add in agate mortar appropriate acetone mixed grinding uniformly after,
In air atmosphere, carry out precalcining, at 700 DEG C after 12 hours furnace cooling of precalcining, take out sample by pre-calcined
The raw material burnt is sufficiently mixed grinding uniformly by identical method again, again calcines, 1100 DEG C in air atmosphere
Lower calcining 12 hours, is cooled to room temperature, takes out sample.Regrinding is uniform, among air atmosphere, finally forges at 1500 DEG C
Burn 12 hours, be cooled to room temperature, be fully ground after taking-up and i.e. obtain sample.
The present embodiment technical scheme prepares the X-ray powder diffraction pattern of sample, exciting light spectrogram, fluorescence spectrum figure, luminescence decline
Subtract curve, scanning electron microscope microphotograph with in embodiment 1 preparation sample consistent.
Embodiment 4
According to chemical formula Zr6Nb2O17: 0.1Eu weighs zirconium chloride ZrCl4: 4.198 grams, europium oxide Eu2O3: 0.352 gram, five oxygen
Change two niobium Nb2O5: 0.886 gram, add in agate mortar appropriate acetone mixed grinding uniformly after, at air gas
Atmosphere carries out precalcining, at 650 DEG C after 10 hours furnace cooling of precalcining, takes out sample by the raw material of precalcining
Again it is sufficiently mixed grinding uniformly by identical method, again calcines in air atmosphere, at 1050 DEG C, calcine 10
Hour, it is cooled to room temperature, takes out sample.Mixed grinding is uniform again, among air atmosphere, and final calcining 10 at 1450 DEG C
Hour, it is cooled to room temperature, is fully ground after taking-up and i.e. obtains sample.
The present embodiment technical scheme prepares the X-ray powder diffraction pattern of sample, exciting light spectrogram, fluorescence spectrum figure, luminescence decline
Subtract curve, scanning electron microscope microphotograph with in embodiment 1 preparation sample consistent.
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 weigh the citric acid of the 1.8wt% of above each drug quality respectively.By weigh
Zirconium oxide ZrO2, europium carbonate Eu2(CO3)3, niobium hydroxide Nb (OH)5It is separately added in dilute nitric acid solution until the most molten
Solving, adding the citric acid weighed magnetic agitation a period of time under the conditions of 50 DEG C obtains settled solution.The most at last
Above-mentioned solution mix and blend 1.5 hours, in the mixed solution obtained placement baking oven, design temperature is 80 DEG C, after drying 12 hours,
Natural cooling, obtains presoma.Presoma is placed in Muffle furnace calcining, and calcining heat is 1100 DEG C, and calcination time is 3 little
Time, it is cooled to room temperature, takes out and be fully ground and i.e. obtain sample.
Seeing accompanying drawing 6, be the present embodiment technical scheme X-ray powder diffraction pattern of preparing sample, result shows, prepares
Sample good crystallinity, without dephasign.
See accompanying drawing 7, be the sample prepared by the present embodiment technical scheme excitation spectrum under 613 nano wave lengths monitoring, survey
Test result display sample can absorb the ultraviolet light of 267 nm.
Accompanying drawing 8 is the sample prepared by the present embodiment technical scheme emission spectrum figure under 267 nano wave lengths excite, obtained
Material is effectively by ultraviolet light switching emission HONGGUANG.
Seeing accompanying drawing 9, be the embodiment of the present invention 5 decay of luminescence curve of preparing sample, can be calculated die-away time is 1.951 millis
Second.
Seeing accompanying drawing 10, be the present embodiment technical scheme scanning electron microscope microphotograph of preparing sample, result shows, the sample prepared
Product granule is the most tiny, and its mean diameter is 0.11 micron.
Embodiment 6
According to chemical formula Zr6Nb2O17: 0.3Eu weighs zirconium nitrate Zr (NO3)4·5H2O:3.606 gram, europium nitrate Eu (NO3)3·6H2O:
1.606 grams, niobium chloride NbCl5: 1.081 grams, and weigh the citric acid of the 2.0wt% of above each drug quality respectively.To claim
Zirconium nitrate Zr (the NO taken3)4·5H2O, europium nitrate Eu (NO3)3·6H2O, niobium chloride NbCl5It is dissolved in appropriate dust technology
In, and the citric acid magnetic agitation a period of time under the conditions of 100 DEG C adding weighing obtain settled solution.The most at last
Above-mentioned solution mix and blend 1 hour, in the mixed solution obtained placement baking oven, design temperature is 80 DEG C, after drying 12 hours,
Natural cooling, obtains presoma.Presoma is placed in Muffle furnace calcining, and calcining heat is 1200 DEG C, and calcination time is 6 little
Time, it is cooled to room temperature, takes out and be fully ground and i.e. obtain sample.
The present embodiment technical scheme prepares the X-ray powder diffraction pattern of sample, exciting light spectrogram, fluorescence spectrum figure, luminescence decline
Subtract curve, scanning electron microscope microphotograph with in embodiment 5 preparation sample consistent.
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 weigh the oxalic acid of the 0.5wt% of above each drug quality respectively.The hydrogen that will weigh
Zirconium oxide Zr (OH)4, europium oxide Eu2O3, niobium pentaoxide Nb2O5It is dissolved separately in appropriate dust technology, and adds
Entering the citric acid weighed magnetic agitation a period of time under the conditions of 80 DEG C obtains settled solution.The most above-mentioned solution mixes
Closing stirring 1.5 hours, the mixed solution obtained is placed in baking oven, and design temperature is 80 DEG C, after drying 12 hours, and natural cooling,
Obtain presoma.Presoma is placed in Muffle furnace calcining, and calcining heat is 1300 DEG C, and calcination time is 9 hours, is cooled to
Room temperature, takes out and is fully ground and i.e. obtain sample.
The present embodiment technical scheme prepares the X-ray powder diffraction pattern of sample, exciting light spectrogram, fluorescence spectrum figure, luminescence decline
Subtract curve, scanning electron microscope microphotograph with in embodiment 5 preparation sample consistent.
Embodiment 8
According to chemical formula Zr6Nb2O17: the stoichiometric proportion of each element in 0.5Eu, weigh zirconium chloride ZrCl respectively4: 1.399 grams,
Europium carbonate Eu2(CO3)3: 1.452 grams, niobium hydroxide Nb (OH)5: 0.712 gram, and weigh above each drug quality respectively
The citric acid of 1.8wt%.The zirconium chloride ZrCl that will weigh4, europium carbonate Eu2(CO3)3, niobium hydroxide Nb (OH)5Dissolve respectively
Until being completely dissolved in appropriate dust technology, add the citric acid magnetic agitation one under the conditions of 100 DEG C weighed
The section time obtains settled solution, the most above-mentioned solution mix and blend 2 hours, and the mixed solution obtained is placed in baking oven, if
Fixed temperature is 80 DEG C, after drying 12 hours, natural cooling, takes out presoma.Presoma is placed in Muffle furnace calcining, calcining
Temperature 1400 DEG C, calcination time 12 hours, it is cooled to room temperature, takes out and be fully ground and i.e. obtain sample.
The present embodiment technical scheme prepares the X-ray powder diffraction pattern of sample, exciting light spectrogram, fluorescence spectrum figure, luminescence decline
Subtract curve, scanning electron microscope microphotograph with in embodiment 5 preparation sample consistent.
Claims (8)
1. a rare earth ion doped niobic acid zirconium fluorescent material, it is characterised in that: the chemical formula of described material is Zr6Nb2O17: xEu,
Wherein x is Eu3+The mole percent of doping, 0.0001≤x≤0.5.
2. the preparation method of a rare earth ion doped niobic acid zirconium fluorescent material as claimed in claim 1, it is characterised in that
Use high temperature solid-state method, comprise the steps:
(1) chemical formula Zr is pressed6Nb2O17: the stoichiometric proportion in xEu, wherein 0.0001≤x≤0.5, weigh respectively containing zirconium from
Sub-Zr4+Compound, containing niobium ion Nb5+Compound, containing europium ion Eu3+Compound, grind and mix homogeneously,
Obtain mixture；
(2) mixture that step (1) obtains being carried out precalcining in air atmosphere, precalcining temperature is 300～700 DEG C,
The precalcining time is 2～12 hours；
(3) mixture natural cooling step (2) obtained, grinds and after mix homogeneously, calcines, forge in air atmosphere
Burning temperature is 700～1100 DEG C, and calcination time is 2～12 hours；
(4) mixture natural cooling step (3) obtained, grinds and after mix homogeneously, carries out final in air atmosphere
Calcining, calcining heat is 1100～1500 DEG C, and calcination time is 2～12 hours, naturally cools to room temperature, i.e. obtain rare earth from
The niobic acid zirconium fluorescent material of son doping.
The preparation method of rare earth ion doped niobic acid zirconium fluorescent material the most according to claim 2, it is characterised in that: step
Suddenly the precalcining temperature of (2) is 350～650 DEG C, and the precalcining time is 4～10 hours.
The preparation method of rare earth ion doped niobic acid zirconium fluorescent material the most according to claim 2, it is characterised in that: step
Suddenly the calcining heat of (3) is 750～1050 DEG C, and calcination time is 4～10 hours.
The preparation method of rare earth ion doped niobic acid zirconium fluorescent material the most according to claim 2, it is characterised in that: step
Suddenly the calcining heat of (4) is 1150～1450 DEG C, and calcination time is 4～10 hours.
The preparation method of rare earth ion doped niobic acid zirconium fluorescent material the most according to claim 2, it is characterised in that: institute
State containing zirconium ion Zr4+Compound be zirconium oxide ZrO2, zirconium nitrate Zr (NO3)4·5H2O, zirconium hydroxide Zr (OH)4, chlorine
Change zirconium ZrCl4In one；Described containing niobium ion Nb5+Compound be niobium pentaoxide Nb2O5, niobium hydroxide
Nb(OH)5With niobium chloride NbCl5In one；Described containing europium ion Eu3+Compound be europium oxide Eu2O3, europium nitrate
Eu(NO3)3·6H2O, europium carbonate Eu2(CO3)3In one.
7. the preparation method of a rare earth ion doped niobic acid zirconium fluorescent material as claimed in claim 1, it is characterised in that
Use chemical synthesis, comprise the steps:
(1) chemical formula Zr is pressed6Nb2O17: stoichiometric proportion in xEu, wherein 0.0001≤x≤0.5, weigh respectively containing zirconium ion
Zr4+Compound, containing niobium ion Nb5+Compound, containing europium ion Eu3+Compound, they are dissolved separately in dilute
In salpeter solution, obtain respective clear solution；By the 0.5～2.0wt% of each reactant quality add respectively chelating agent citric acid or
Oxalic acid, stirs under the temperature conditions of 50～100 DEG C；
(2) the various solution that step (1) obtains are slowly mixed together, stir 1～2 hour under the temperature conditions of 50～100 DEG C
After, stand, dry, obtain fluffy presoma；
(3) presoma being placed in Muffle furnace calcining, calcining heat is 1100～1400 DEG C, and calcination time is 3～12 hours,
Naturally cool to room temperature, after grinding uniformly, obtain a kind of powdered phosphor.
The preparation method of rare earth ion doped niobic acid zirconium fluorescent material the most according to claim 7, it is characterised in that: institute
State containing zirconium ion Zr4+Compound be zirconium oxide ZrO2, zirconium nitrate Zr (NO3)4·5H2O, zirconium hydroxide Zr (OH)4, chlorine
Change zirconium ZrCl4In one；Described containing niobium ion Nb5+Compound be niobium pentaoxide Nb2O5, niobium hydroxide
Nb(OH)5With niobium chloride NbCl5In one；Described containing europium ion Eu3+Compound be europium oxide Eu2O3, europium nitrate
Eu(NO3)3·6H2O and europium carbonate Eu2(CO3)3In one.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110372036A (en) * | 2019-08-23 | 2019-10-25 | 中国人民解放军国防科技大学 | Ternary transition metal oxide powder and preparation method thereof |
| CN112225560A (en) * | 2020-10-23 | 2021-01-15 | 陕西天璇涂层科技有限公司 | Solid phase method for preparing low-thermal-conductivity high-temperature thermal barrier ceramic CaMoNb2O9Method (2) |
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