CN107523300A - A kind of Er3+Vanadium germanate light-converting material of doping and preparation method thereof - Google Patents
A kind of Er3+Vanadium germanate light-converting material of doping and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of Er3+Vanadium germanate light-converting material of doping and preparation method thereof.The chemical formula of the vanadium germanate is La11GeV3O26, adulterate Er3+Turning into afterwards can be with near-infrared luminous fluorescent material, and its chemical general formula is La11‑11xEr11xGeV3O26, whereinxFor Er3+The mol ratio of doping, 0.0001≤x≤0.45.The invention discloses the preparation method of this material, using chemical synthesis sol-gal process or coprecipitation method, the material granule fine uniform being prepared by this method, in the case where ultraviolet black light light excites, 1500~1600 nanometers of near infrared light can be launched, effectively realize the lower conversion of light, and luminous efficiency is high, stability is good, can be applied to hot-cast socket, laser output, field of information communication.
Description
Technical field
The present invention relates to a kind of ultraviolet-black light sensitization Er3+Ion simultaneously realizes that the vanadium germanate light of near-infrared radiation turns
Conversion materials and preparation method thereof, belong to phosphor technical field.
Background technology
Near infrared light generally refers to electromagnetic wave of the wave-length coverage at 0.78~2.526 micron, that is, between visible ray and
Emission band between mid-infrared light.The specific wave-length coverage of near infrared light so that it has some monopolizing characteristics and advantage.Example
Such as, on the one hand, near infrared light has penetration depth, and the material of nature is comparatively very low to the absorptivity of near infrared light,
Therefore near infrared light can be avoided because the interference that external substance absorbs and brings among communication process；On the other hand, it is near red
External radiation light has good fuel factor.Infrared ray be bound in the air occur material atom and molecule there is alternant polarization
Phenomenon so that the vibration of atom and molecule is accelerated and collides and rub, that is, adds energy of thermal motion, here it is infrared ray
Fuel factor.Near-infrared high sensitivity, ambient interferences are small, play the role of in many fields the characteristics of based on heat radiation important.
Therefore, widely studied and concern has been carried out in terms of near-infrared light-emitting material both at home and abroad.
Rare earth ion has extremely abundant 4f energy levels, is to realize near-infrared luminous important active ions；Numerous dilute
In native ion, the research for near-infrared light emitting ionic above all concentrates on Nd3+And Er3+Two kinds of ions, erbium ion Er3+
Can realize from4I13/2Energy level arrives4I15/2Ground state level transition, it is 1.55 microns to realize emission wavelength, and the near infrared band is swashing
Light, biological heat sensing analysis, detection, communication, etc. field be widely applied.The various near-infrared fluorescent materials of er-doped are wide
General research and use.
Er3+Ion has very low resonance efficiency in Uv and visible light section in itself, absorbs very weak.Therefore, by seeking
Look for suitable sensitization matrix, realize matrix to rare earth Er3+The energy transmission of ion, improve Er3+Near infrared luminous intensity, be
A kind of important method and approach.
The content of the invention
Limitation of the present invention present in existing inorganic light-emitting host material, there is provided a kind of suitable sensitization matrix,
Realize matrix to rare earth Er3+The energy transmission of ion, Er can be effectively improved3+Near infrared luminous intensity Er3+Adulterate vanadium germanic acid
Salt light-converting material and preparation method thereof.
Realize that one of technical scheme of the object of the invention is to provide a kind of Er3+The vanadium germanate light-converting material of doping, it
Chemical general formula be La11-11xEr11xGeV3O26, wherein,xFor Er3+The mol ratio of doping, 0.0001≤x≤0.45；Described light
Transition material is under ultraviolet-near ultraviolet excitation, the near infrared light of 1500~1600 nanometers of transmitting.
Technical solution of the present invention also includes Er as described above3+The preparation method of the vanadium germanate light-converting material of doping,
Using chemical synthesis sol-gal process or coprecipitation method.
Er is prepared using chemical synthesis sol-gal process3+The step of vanadium germanate light-converting material of doping, is as follows：
1. press chemical formula La11-11xEr11xGeV3O26The stoichiometric proportion of middle each element, wherein 0.0001≤x≤0.45, weighs and contain
There is lanthanum ion La3+Compound, contain erbium ion Er3+Compound, contain germanium ion Ge4+Compound and contain vanadium ion
V5+Compound, lanthanum ion La will be contained3+Compound and contain erbium ion Er3+Compound to be dissolved separately in dust technology molten
In liquid, germanium ion Ge will be contained4+Compound and contain vanadium ion V5+Compound be dissolved separately in deionized water；
To each solution in, complexing agent citric acid or oxalic acid are added respectively by 1.5~2.5 times of each reactant molal quantity, in temperature
Spend to stir under conditions of 50~100 DEG C；
2. the various solution that step 1 is obtained are slowly mixed together, after being stirred 1~5 hour under conditions of being 50~100 DEG C in temperature,
Stand, drying, obtain fluffy presoma；
Calcined 3. presoma is placed in Muffle furnace, calcining heat is 1100~1300 DEG C, and calcination time is 1~15 hour；From
Room temperature so is cooled to, obtains a kind of Er3+The vanadium germanate light-converting material of doping.
The preferable scheme of chemical synthesis sol-gal process step 3 is：Calcining heat is 1150~1250 DEG C, and calcination time is
8~12 hours.
Er is prepared using coprecipitation method3+The step of vanadium germanate light-converting material of doping, is as follows：
1. press chemical formula La11-11xEr11xGeV3O26The stoichiometric proportion of middle each element, wherein 0.0001≤x≤0.45, claims respectively
Take containing lanthanum ion La3+Compound, contain erbium ion Er3+Compound, contain germanium ion Ge4+Compound and contain vanadium
Ion V5+Compound；
2. contain lanthanum ion La by what step 1 weighed3+Compound, contain erbium ion Er3+Compound and contain germanium ion
Ge4+Compound be dissolved in respectively in dust technology；
3. contain vanadium ion V by what step 1 weighed5+Compound, be dissolved in ammoniacal liquor, temperature be 50~100 DEG C under conditions of
Stirring 1~2 hour；
4. the solution that step 2 and 3 are obtained is mutually mixed dropwise, adjust the pH value of solution to 9~11, by obtained sediment and
Turbid solution is placed in ceramic crucible, is heated under 70~90 DEG C of temperature conditionss, drying, obtains powder；
Calcined 5. the powder that step 4 is obtained is placed in Muffle furnace, calcining heat is 950~1250 DEG C, and calcination time is 1~15
Hour；Room temperature is naturally cooled to, obtains a kind of Er3+Ion-activated vanadium germanate light-converting material.
In coprecipitation method step 5, preferable scheme is：Calcining heat be 1050~1150 DEG C, calcination time be 8~
12 hours.
In the present invention, described contains lanthanum ion La3+Compound be lanthana La2O3, lanthanum nitrate La (NO3)3·6H2O
In one kind；Contain erbium ion Er3+Compound be erbium oxide Er2O3, erbium nitrate Er (NO3)3·5H2One kind in O；Contain
Germanium ion Ge4+Compound be germanium chloride GeCl4；Contain vanadium ion V5+Compound be ammonium metavanadate NH4VO3。
The present invention is with a kind of vanadium germanic acid salt material La11GeV3O26As host material, Er3+As active ions, base is realized
The band gap light absorbs of matter are to Er3+The sensibilization of ion.Host material provided by the present invention has obvious advantage, due to it
Er in matrix3+Substitute La3+Can realize high-concentration dopant, lattice structure be stable, lattice has abundant optical activity center,
Thermal property is good etc., most important of which is that parent lattice is to Er3+1.55 microns of near-infrared luminous sensibilizations of ion.Should
Material has that preparation technology is simple, environmentally friendly without any pollution, and the near-infrared light-emitting material stable performance synthesized
Advantage.
Meaning of the present invention is that Er can be sensitized by ultraviolet-black light by providing one kind3+Ion simultaneously realizes near-infrared
The vanadium germanate light-converting material of radiation, technical solution of the present invention have the advantages of following notable：
1. ultraviolet-black light sensitization Er of the present invention3+Ion and the vanadium germanate light-converting material for realizing near-infrared radiation,
There is very strong absorption in black light, can be very good to utilize sunshine.
2. ultraviolet-black light sensitization Er of the present invention3+Ion and the vanadium germanate light conversion material for realizing near-infrared radiation
Material, transmitting main peak are located at 1550 nanometers, and light conversion efficiency is high.
3. ultraviolet-black light sensitization Er of the present invention3+Ion and the vanadium germanate light conversion material for realizing near-infrared radiation
Material, raw material sources are extensive, and production cost is low, and the thing that sample is made is mutually pure, no dephasign, is evenly distributed.
4. preparation technology of the present invention is simple, no waste gas and waste liquid discharge, is a kind of environment-friendly phosphor.
Brief description of the drawings
Fig. 1 is that the embodiment of the present invention 1 prepares sample La10.9989Er0.0011GeV3O26X-ray powder diffraction pattern；
Fig. 2 embodiment of the present invention 1 prepares sample La10.9989Er0.0011GeV3O26SEM figure；
Fig. 3 embodiment of the present invention 1 prepares sample La10.9989Er0.0011GeV3O26Excitation spectrum under the monitoring of 1550 nano wave lengths
Figure；
Fig. 4 embodiments 1 prepare sample La10.9989Er0.0011GeV3O26Luminescent spectrum figure in the case where 390 nano wave lengths excite；
Fig. 5 is that the embodiment of the present invention 5 prepares sample La8.8Er2.2GeV3O26X-ray powder diffraction pattern；
Fig. 6 is that the embodiment of the present invention 5 prepares sample La8.8Er2.2GeV3O26SEM figure；
Fig. 7 is that the embodiment of the present invention 5 prepares sample La8.8Er2.2GeV3O26Exciting light spectrogram under the monitoring of 1550 nano wave lengths；
Fig. 8 is that the embodiment of the present invention 5 prepares sample La8.8Er2.2GeV3O26Luminescent spectrum figure in the case where 390 nano wave lengths excite.
Embodiment
The technology of the present invention method is further described with reference to the accompanying drawings and examples.
Embodiment 1
According to chemical formula La10.9989Er0.0011GeV3O26The stoichiometric proportion of middle each element, lanthanum nitrate La (NO are weighed respectively3)3·
6H2O：7.9375 grams, erbium nitrate Er (NO3)3·5H2O：0.0008 gram, germanium chloride GeCl4：0.3573 gram, ammonium metavanadate
NH4VO3：0.5849 gram.Lanthanum nitrate and erbium nitrate are dissolved in appropriate dust technology, and add the 5.2839 grams of lemons weighed
Acid obtains settled solution for a period of time in 70 DEG C of magnetic agitations, and germanium chloride and ammonium metavanadate are dissolved in deionized water solution,
Add 1.9214 grams of citric acids and obtain settled solution in 70 DEG C of stirrings.
The solution of above-mentioned preparation is mixed 1.5 hours in 50 DEG C, obtained mixed solution is placed in baking oven, setting temperature
Spend for 80 DEG C, drying and processing is after 12 hours, natural cooling, takes out presoma.Precursor is placed in Muffle furnace, in air atmosphere
Middle calcining, sintering temperature are 1150 DEG C, and calcination time is 8 hours, is cooled to room temperature, take out and are fully ground and obtain a kind of purple
Outside-black light sensitization Er3+Ion realizes the vanadium germanate light-converting material of near-infrared radiation.
It is the X-ray powder diffraction pattern that sample is prepared by the present embodiment technical scheme referring to accompanying drawing 1.XRD test results
It has been shown that, prepared sample crystallinity is good, is monophase materialses.
Referring to accompanying drawing 2, it is that the SEM that sample is prepared by the present embodiment technical scheme schemes, gained sample particle better crystallinity degree, does not have
There is dephasign, particle diameter is 5~10 microns.
Referring to accompanying drawing 3, swashed by what sample prepared by the present embodiment technical scheme obtained under the monitoring of 1550 nano wave lengths
Luminous spectrogram, it was demonstrated that have good luminous efficiency near ultraviolet.
It is emission spectrum of the sample prepared by the present embodiment technical scheme in the case where 390 nano wave lengths excite referring to accompanying drawing 4
Figure.As seen from the figure, there is the near-infrared luminous of 1550 nano wavebands in emission spectrum, and obtained material can be effectively by ultraviolet light
Be converted to near-infrared luminous.
Embodiment 2
According to chemical formula La6.05Er4.95GeV3O26The stoichiometric proportion of middle each element, lanthana La is weighed respectively2O3：1.6428
Gram, erbium oxide Er2O3：1.5779 gram, germanium chloride GeCl4：0.3573 gram, vanadic anhydride V2O5：0.455 gram.By lanthana and
Erbium oxide is dissolved in appropriate dust technology, and is added the 3.287 grams of oxalic acid weighed and obtained for a period of time in 100 DEG C of magnetic agitations
Settled solution, germanium chloride and vanadic anhydride are dissolved in deionized water solution, add 1.21 grams of oxalic acid and stirred in 100 DEG C
To settled solution.
Most both above-mentioned solution mix 1 hour in 100 DEG C at last, and obtained mixed solution is placed dries in baking oven,
Natural cooling, presoma is taken out, precursor is placed in Muffle furnace, calcined in air atmosphere, sintering temperature is 1200 DEG C, is forged
It is 10 hours to burn the time, is cooled to room temperature, takes out and is fully ground and obtains a kind of ultraviolet-black light sensitization Er3+Ion core
The vanadium germanate light-converting material of existing near-infrared radiation.
The present embodiment technical scheme prepares the X-ray powder diffraction pattern of sample, SEM figures, exciting light spectrogram, luminescent spectrum
Figure is consistent with the sample prepared in embodiment 1.
Embodiment 3
According to chemical formula La10.45Er0.55GeV3O26The stoichiometric proportion of middle each element, lanthana La is weighed respectively2O3：2.8375
Gram, erbium nitrate Er (NO3)3·5H2O：0.4064 gram, germanium chloride GeCl4：0.3573 gram, ammonium metavanadate NH4VO3：0.5849 gram；
Lanthana is dissolved in appropriate dust technology, and adds the 3.93 grams of oxalic acid weighed and obtain settled solution in 80 DEG C of stirrings；Will
Erbium nitrate is dissolved among deionized water, and 0.5 gram of oxalic acid of addition obtains settled solution in 85 DEG C of stirrings；By germanium chloride and metavanadic acid
Ammonium is dissolved in deionized water solution, is added 1.5 grams of oxalic acid and is obtained settled solution in 85 DEG C of stirrings.
Most above-mentioned solution mixes 5 hours in 50 DEG C at last, and obtained mixed solution is placed dries in baking oven, naturally cold
But, presoma is taken out, precursor is placed in Muffle furnace, calcined in air atmosphere, sintering temperature is 1250 DEG C, calcination time
For 12 hours, room temperature is cooled to, takes out and is fully ground and obtain a kind of ultraviolet-black light sensitization Er3+Ion is realized near red
The vanadium germanate light-converting material of external radiation.
The present embodiment technical scheme prepares the X-ray powder diffraction pattern of sample, SEM figures, exciting light spectrogram, luminescent spectrum
Figure is consistent with the sample prepared in embodiment 1.
Embodiment 4
According to chemical formula La9.9Er1.1GeV3O26The stoichiometric proportion of middle each element, lanthanum nitrate La (NO are weighed respectively3)3·6H2O
：7.1445 gram, erbium oxide Er2O3：0.3506 gram, germanium chloride GeCl4：0.3573 gram, ammonium metavanadate NH4VO3：0.5849 gram；Will
Erbium oxide is dissolved in appropriate dust technology, and is added the 0.5 gram of oxalic acid weighed and obtained settled solution in 85 DEG C of stirrings；By nitric acid
Lanthanum is dissolved among deionized water, and 2.97 grams of oxalic acid of addition obtain settled solution in 85 DEG C of stirrings；By germanium chloride and ammonium metavanadate
It is dissolved in deionized water solution, adds 1.7 grams of oxalic acid and obtain settled solution in 85 DEG C of stirrings.
Most above-mentioned solution mixes 3 hours in 75 DEG C at last, and obtained mixed solution is placed dries in baking oven, naturally cold
But, presoma is taken out, precursor is placed in Muffle furnace, calcined in air atmosphere, sintering temperature is 1250 DEG C, calcination time
For 10 hours, room temperature is cooled to, takes out and is fully ground and obtain a kind of ultraviolet-black light sensitization Er3+Ion is realized near red
The vanadium germanate light-converting material of external radiation.
The present embodiment technical scheme prepares the X-ray powder diffraction pattern of sample, SEM figures, exciting light spectrogram, luminescent spectrum
Figure is consistent with the sample prepared in embodiment 1.
Embodiment 5
By chemical formula La8.8Er2.2GeV3O26The stoichiometric proportion of middle each element, weigh lanthana La2O3：2.3895 gram, nitric acid
Erbium Er (NO3)3·5H2O：1.6254 gram, germanium chloride GeCl4：0.3573 gram, it is dissolved among dust technology.By chemical formula
La8.8Er2.2GeV3O26The stoichiometric proportion of middle each element, weigh ammonium metavanadate NH4VO3：0.5849 gram, it is dissolved among ammoniacal liquor, in
Stirred 2 hours under 50 DEG C of temperature conditionss.
Lanthana, erbium nitrate and germanium chloride are dissolved to obtain solution, are added dropwise to the solution that ammonium metavanadate dissolves to obtain
Among, while ammoniacal liquor is added dropwise, the pH value of solution is obtained the turbid solution of many precipitations, is put among ceramic crucible to 9,
In 70 degree of heating, dryings；Obtained powder, which is placed in Muffle furnace, to be calcined, and temperature is 1050 DEG C, and the time is 10 hours, natural cooling
To room temperature, a kind of ultraviolet-black light sensitization Er is obtained3+Ion realizes the vanadium germanate light-converting material of near-infrared radiation.
It is the X-ray powder diffraction pattern that sample is prepared by the present embodiment technical scheme referring to accompanying drawing 5.XRD test results
It has been shown that, prepared sample crystallinity is good, is monophase materialses.
Referring to accompanying drawing 6, it is that the SEM that sample is prepared by the present embodiment technical scheme schemes, gained sample particle better crystallinity degree, does not have
There is dephasign, particle diameter is 0.2 micron.
Referring to accompanying drawing 7, swashed by what sample prepared by the present embodiment technical scheme obtained under the monitoring of 1550 nano wave lengths
Luminous spectrogram, it was demonstrated that have good luminous efficiency near ultraviolet；
It is launching light spectrogram of the sample prepared by the present embodiment technical scheme in the case where 390 nano wave lengths excite referring to accompanying drawing 8.
As seen from the figure, there is the near-infrared luminous of 1550 nano wavebands in emission spectrum, and obtained material effectively can turn ultraviolet light
It is changed to near-infrared luminous.
Embodiment 6
By chemical formula La7.7Er3.3GeV3O26The stoichiometric proportion of middle each element, weigh lanthanum nitrate La (NO3)3·6H2O：5.5568
Gram, erbium oxide Er2O3：1.0519 gram, germanium chloride GeCl4：0.3573 gram, it is dissolved among dust technology.By chemical formula
La8.8Er2.2GeV3O26The stoichiometric proportion of middle each element, weigh ammonium metavanadate NH4VO3：0.5849 gram, it is dissolved among ammoniacal liquor, in
Stirred 1 hour under 100 DEG C of temperature conditionss.Lanthanum nitrate, erbium oxide and germanium chloride are dissolved to obtain solution, are added dropwise to inclined vanadium
Among sour ammonium dissolves obtained solution, while ammoniacal liquor is added dropwise, the pH value of solution is obtained the muddy molten of many precipitations to 10
Liquid, it is put among ceramic crucible, in 90 degree of heating, dryings；Obtained powder, which is placed in Muffle furnace, to be calcined, and temperature is 1150 DEG C, when
Between be 12 hours, naturally cool to room temperature, obtain a kind of ultraviolet-black light sensitization Er3+Ion realizes the vanadium of near-infrared radiation
Germanate light-converting material.
The present embodiment technical scheme prepares the X-ray powder diffraction pattern of sample, SEM figures, exciting light spectrogram, luminescent spectrum
Figure is consistent with the sample prepared in embodiment 5.
Embodiment 7
By chemical formula La6.05Er4.95GeV3O26The stoichiometric proportion of middle each element, weigh lanthanum nitrate La (NO3)3·6H2O：
4.3661 grams, erbium nitrate Er (NO3)3·5H2O：3.6572 gram, germanium chloride GeCl4：0.3573 gram, it is dissolved among dust technology.
By chemical formula La8.8Er2.2GeV3O26The stoichiometric proportion of middle each element, weigh ammonium metavanadate NH4VO3：0.5849 gram, it is dissolved in ammonia
Among water, stirred 1 hour under 90 DEG C of temperature conditionss.
Lanthanum nitrate, erbium nitrate and germanium chloride are dissolved to obtain solution, are added dropwise to the solution that ammonium metavanadate dissolves to obtain
Among, while ammoniacal liquor is added dropwise, the pH value of solution is obtained the turbid solution of many precipitations, is put among ceramic crucible to 11,
In 90 degree of heating, dryings；Obtained powder, which is placed in Muffle furnace, to be calcined, and temperature is 1100 DEG C, and the time is 10 hours, natural cooling
To room temperature, a kind of ultraviolet-black light sensitization Er is obtained3+Ion realizes the vanadium germanate light-converting material of near-infrared radiation.
The present embodiment technical scheme prepares the X-ray powder diffraction pattern of sample, SEM figures, exciting light spectrogram, luminescent spectrum
Figure is consistent with the sample prepared in embodiment 5.
Claims (7)
- A kind of 1. Er3+The vanadium germanate light-converting material of doping, it is characterised in that：Its chemical general formula is La11- 11xEr11xGeV3O26, wherein,xFor Er3+The mol ratio of doping, 0.0001≤x≤0.45；Under ultraviolet-near ultraviolet excitation, hair Penetrate 1500~1600 nanometers of near infrared light.
- A kind of 2. Er as claimed in claim 13+The preparation method of the vanadium germanate light-converting material of doping, using chemical synthesis Sol-gal process, it is characterised in that comprise the following steps：（1）By chemical formula La11-11xEr11xGeV3O26The stoichiometric proportion of middle each element, wherein 0.0001≤x≤0.45, is weighed Contain lanthanum ion La3+Compound, contain erbium ion Er3+Compound, contain germanium ion Ge4+Compound and containing vanadium from Sub- V5+Compound, lanthanum ion La will be contained3+Compound and contain erbium ion Er3+Compound be dissolved separately in dust technology In solution, germanium ion Ge will be contained4+Compound and contain vanadium ion V5+Compound be dissolved separately in deionized water； In obtained each solution, complexing agent citric acid or oxalic acid are added respectively by 1.5~2.5 times of each reactant molal quantity, Temperature stirs under conditions of being 50~100 DEG C；（2）By step（1）Obtained various solution are slowly mixed together, and are stirred 1~5 hour under conditions of being 50~100 DEG C in temperature Afterwards, stand, drying, obtain fluffy presoma；（3）Presoma is placed in Muffle furnace and calcined, calcining heat is 1100~1300 DEG C, and calcination time is 1~15 hour；From Room temperature so is cooled to, obtains a kind of Er3+The vanadium germanate light-converting material of doping.
- A kind of 3. Er according to claim 23+The preparation method of the vanadium germanate light-converting material of doping, its feature exist In：Step（3）Calcining heat be 1150~1250 DEG C, calcination time be 8~12 hours.
- A kind of 4. Er according to claim 23+The preparation method of the vanadium germanate light-converting material of doping, its feature exist In：Contain lanthanum ion La3+Compound be lanthana La2O3, lanthanum nitrate La (NO3)3·6H2One kind in O；Contain erbium ion Er3+Compound be erbium oxide Er2O3, erbium nitrate Er (NO3)3·5H2One kind in O；Contain germanium ion Ge4+Compound be Germanium chloride GeCl4;Contain vanadium ion V5+Compound be vanadic anhydride V2O5, ammonium metavanadate NH4VO3In one kind.
- A kind of 5. Er as claimed in claim 13+The preparation method of the vanadium germanate light-converting material of doping, closed using co-precipitation Cheng Fa, it is characterised in that comprise the following steps：（1）By chemical formula La11-11xEr11xGeV3O26The stoichiometric proportion of middle each element, wherein 0.0001≤x≤0.45, respectively Weigh containing lanthanum ion La3+Compound, contain erbium ion Er3+Compound, contain germanium ion Ge4+Compound and contain Vanadium ion V5+Compound；（2）By step（1）What is weighed contains lanthanum ion La3+Compound, contain erbium ion Er3+Compound and contain germanium ion Ge4+Compound be dissolved in respectively in dust technology；（3）By step（1）What is weighed contains vanadium ion V5+Compound, be dissolved in ammoniacal liquor, be 50~100 DEG C of condition in temperature Lower stirring 1~2 hour；（4）By step（2）With（3）Obtained solution is mutually mixed dropwise, adjusts the pH value of solution to 9~11, heavy by what is obtained Starch and turbid solution are placed in ceramic crucible, are heated under 70~90 DEG C of temperature conditionss, drying, obtain powder；（5）By step（4）Obtained powder, which is placed in Muffle furnace, to be calcined, and calcining heat is 950~1250 DEG C, calcination time 1 ~15 hours；Room temperature is naturally cooled to, obtains a kind of Er3+Ion-activated vanadium germanate light-converting material.
- A kind of 6. Er according to claims 53+The preparation method of the vanadium germanate light-converting material of doping, its feature exist In：Step（5）In calcining heat be 1050~1150 DEG C, calcination time be 8~12 hours.
- A kind of 7. Er according to claims 53+The preparation method of the vanadium germanate light-converting material of doping, its feature exist In：Described contains lanthanum ion La3+Compound be lanthana La2O3, lanthanum nitrate La (NO3)3·6H2One kind in O；Contain Erbium ion Er3+Compound be erbium oxide Er2O3, erbium nitrate Er (NO3)3·5H2One kind in O；Contain germanium ion Ge4+Change Compound is germanium chloride GeCl4；Contain vanadium ion V5+Compound be ammonium metavanadate NH4VO3。
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| CN106118647A (en) * | 2016-06-13 | 2016-11-16 | 郑甘裕 | A kind of neodymium doping chlorine germanate up-conversion luminescent material, preparation method and applications |
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