CN102559186A - Infrared up-conversion fluorescent powder and preparation method thereof - Google Patents
Infrared up-conversion fluorescent powder and preparation method thereof Download PDFInfo
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- CN102559186A CN102559186A CN2010106024980A CN201010602498A CN102559186A CN 102559186 A CN102559186 A CN 102559186A CN 2010106024980 A CN2010106024980 A CN 2010106024980A CN 201010602498 A CN201010602498 A CN 201010602498A CN 102559186 A CN102559186 A CN 102559186A
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Abstract
The invention provides infrared up-conversion fluorescent powder and a preparation method thereof. The infrared up-conversion fluorescent powder is characterized in that the system of red up-conversion fluorescent powder is NaY1-x-yYbxEryF4, wherein x is not smaller than 0.1 but is not greater than 0.25, and y is not smaller than 0.01 but is not greater than 0.08. A target product of the infrared up-conversion fluorescent powder is spherical, the monocrystal particle size is between 200nm and 400nm, bright macroscopic green light exists under the irradiation of infrared light of 980nm, and the luminous intensity is 1.36 times that of a product obtained by a traditional like technology. Compared with the prior art, the mixture ratio of the components of the product can be accurately controlled, the appearance of the particles of the product is regular and is spherical, the synthesizing process is simple, and the equipment cost is low; and the infrared up-conversion fluorescent powder has stable quality and strong repeatability and is suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of infrared up-conversion phosphor and preparation method thereof, or rather, is up-conversion phosphor of the infrared ray excited macroscopic green glow of emitting bright down of a kind of 980nm and preparation method thereof.
Background technology
Infrared up-conversion luminous material is a kind of material that infrared light is converted into visible light.The photon energy that is characterized in launching is greater than the photon energy that absorbs.Infrared up-conversion luminous material has wide practical use at night vision system material, infrared quantum counter, photodiode, 3 D stereo demonstration, biological fluorescent labelling material, aspect such as false proof.The infrared up-conversion luminous material that uses at present mainly is the complex fluoride of rare-earth ion activated rare earth fluorine, rare earth metal and earth alkali metal, and their phonon energy is low, has reduced the loss of radiationless transition, therefore has higher last efficiency of conversion.In converting luminescent material of fluoride, NaYF
4: Yb, Er be because its luminous efficiency is high, good stability and being used widely.
The main preparation methods of up-conversion luminescent material has high temperature solid-state method, hydrothermal method, the precipitator method.
High temperature solid-state method prepares NaYF
4: Yb, Er are through rare earth fluorine and Sodium Silicofluoride 98min reaction, under protection of inert gas, carry out.Thereby cause environmental pollution because rare earth fluorine complicated process of preparation and its produce a large amount of silicon tetrafluoride toxic gases with Sodium Silicofluoride 98min in the process of reaction, therefore, improve its preparation method is the direction that people study always.
Wherein: hydrothermal method is low because of its synthesis temperature, mild condition and receive extensive concern.
CN 101195747A discloses a kind of red up-conversion phosphor NaY that under 180~220 ℃ hydrothermal condition, prepares
1-x-y-z(Yb
xHo
yCe
z) F
4Method since the preparation process in the reaction be under high pressure to carry out, the cycle is longer, and the luminous efficiency of the luminescent material of preparing is lower, therefore, this method is not suitable for large-scale industrial production.
CN 101260561A has announced a kind of hydrothermal growing method at the light activated up-conversion fluoride crystal of near infrared, and complexing agent disperses and coating through adding, and obtains the NaYF of six side's phases
4Host crystal.Because added complexing agent among this preparation method, cost is higher, therefore be unfavorable for industrial production.
The precipitator method are convenient because of it, during joint, the sample purity advantages of higher of preparation becomes method commonly used in the luminescent material preparation.
CN101289616A has announced that a kind of is that solvent prepares the water-soluble conversion NaYF that goes up with the USP Kosher
4: Er
3+, Yb
3+Nanocrystalline method is with NaF, EDTA and Er (NO
3)
3, Yb (NO
3)
3, Y (NO
3)
3USP Kosher solution mix, at 200~297 ℃ of reaction 1~3h, after its product drying with 980nm when infrared ray excited, the visible up-conversion fluorescence that becomes clear of naked eyes.This preparation method has used organic solvent and complexing agent, and cost is higher.
CN 101020824A discloses a kind of infrared ray excited complex fluoride up-conversion luminescent material and preparation method thereof, and chemical constitution formula is NaY
1-x-yYb
xRe
yF
4, 0.05≤x≤0.3,0.001≤y≤0.1 wherein, Re is Er or Tm.With NaF is precipitation agent, in the aqueous solution, generates NaY with rare earths salt
1-x-yYb
xRe
yF
4, in protective atmosphere, to handle 1~10 hour in 500~700 ℃ then, cooling promptly obtains said luminescent material.Because the solubleness of NaF in water is smaller, cause producing in this preparing method's production process a large amount of waste water.And the sodium ion used of this method is a large amount of excessive, and unfavorable to the thing phase purity of product, background impurities peak at random appears in the X diffracting spectrum of product, causes the luminous intensity of product still on the low side.
Therefore the technology of preparing of existing infrared up-conversion phosphor, condition are relatively harsher, in the preparation process, add organic solvent or complexing agent, and cost is higher, is not suitable for industrial production.
Summary of the invention
The object of the present invention is to provide a kind of infrared up-conversion phosphor and preparation method thereof, to overcome defectives such as working condition harshness that prior art exists, cost height.
Infrared up-conversion phosphor of the present invention, at the infrared ray excited up-conversion phosphor that sends bright macroscopic green glow down of 980nm, characteristic is that the system of red up-conversion phosphor is NaY for a kind of
1-x-yYb
xEr
yF
4
Wherein: 0.1≤x≤0.25,0.01≤y≤0.08.
The preparation method of red up-conversion phosphor of the present invention comprises the steps:
1) according to chemical formula NaY
1-x-yYb
xEr
yF
4, 0.1≤x≤0.25,0.01≤y≤0.08, preparation mixed solution of rare earth A;
Rare earth ion source in the described mixed solution of rare earth is selected from the soluble salt of nitrate salt or the muriate and so on of yttrium, ytterbium and erbium, or makes it to be converted into oxide compound, oxyhydroxide or the carbonate cpds of yttrium, ytterbium and the erbium of soluble salt through nitric acid or hydrochloric acid; The soluble salt of preferred yttrium, ytterbium and erbium;
Said mixed solution of rare earth A middle-weight rare earths ionic total concn is 0.5~1.0mol/L;
2) press trivalent rare earth fluorochemical chemical formula ReF
3The metering ratio, add NH to mixed solution of rare earth A
4F solution, precipitin reaction gets suspension-s;
Wherein: Re is rare earth element y, Yb and Er;
Said NH
4The concentration of F solution is 3~10mol/L;
3) suspension filtered, washing place 60~120 ℃ of down dry 2~12h with filter cake again, get solid B;
4) with solid B and the fusing assistant that contains Na and F, according to N
Na/ N
Re=0.98~1.10, N
F/ N
Na>=1.0 mole number metering is than mixing;
The fusing assistant of described Na of containing and F is selected from NH
4F and Na
2CO
3Mixture, NH
4F and NaHCO
3Mixture, NaF or Na
2SiF
6In one or both, preferred NaF;
N wherein
NaAnd N
FMole number for Na in the fusing assistant and F; N
ReBe Y, Yb and Er REE total mole number;
5) step 4) gained mixture is placed specific atmosphere, 300~750 ℃ of following roasting 0.5~6h collect described infrared up-conversion phosphor product then.
Said specific atmosphere is H
2, N
2Or H
2And N
2Mixed gas or carbon reducing agent atmosphere; Preferred atmosphere is N
2
The preparation method of a kind of infrared up-conversion luminous material provided by the invention; The target product that is obtained is for spherical; The single crystal particle size has bright macroscopic green glow under the irradiation of 980nm infrared light between 200~400nm, luminous intensity is 1.36 times of existing similar technological products therefrom.Compared with prior art, beneficial effect of the present invention: the set of dispense ratio of product can accurately be controlled, and product granule-morphology rule is spherical in shape; Synthesis technique is simple, and cost of equipment is low; Steady quality, repeatability is strong, is suitable for scale operation.
Description of drawings
Fig. 1 is the X-ray diffractogram of the product of embodiment 1.
Fig. 2 is TEM (transmission electron microscope) photo of the product of embodiment 1.
Fig. 3 is that product and the product in Comparative Examples switching emission spectrogram: a under the 980nm laser excitation of embodiment 3 is the last convert light spectrogram of embodiment 3 preparing products, and b is the last convert light spectrogram of Comparative Examples preparing product.
Embodiment
With the rare earth oxide is raw material, takes by weighing 89.20g Y
2O
3, 39.41g Yb
2O
3, 1.91g Er
2O
3Adding in the 200ml deionized water, does the back that stirs add the 295.3g weight concentration and does? The nitric acid of %, insulation are at 70 ℃, and stirring is dissolved rare earth oxide fully, adds deionized water, is mixed with the 1000ml rare earth nitrate solution;
Get 112.0g NH
4F adds the 300ml deionized water makes its dissolving form NH
4F solution is added drop-wise to it in rare earth nitrate solution of continuous stirring then, leaves standstill, filters, washs after dripping, and dry 12h under 60 ℃ gets mixture, in N after fully grinding with 41.99g NaF then
2The following 500 ℃ of thermal treatment 1h of atmosphere, the cooling after pulverize the invention product:
NaY
0.79Yb
0.20Er
0.01F
4。
X-ray diffractogram is seen Fig. 1.TEM (transmission electron microscope) photo is seen Fig. 2.
Embodiment 2
With the rare earth nitrate is raw material, takes by weighing 200.68g Y (NO respectively
3)
3, 89.76g Yb (NO
3)
3, 7.07g Er (NO
3)
3Add deionized water, be mixed with into the 1600ml rare earth nitrate solution.Get 112.0gNH
4F adds makes its dissolving form NH in the 500ml deionized water
4F solution is added drop-wise to it in rare earth nitrate solution of continuous stirring then, and leave standstill, filter, wash after dripping, and in 120 ℃ of following dry 2h, then with 94.03g Na
2SiF
6Comminution by gas stream gets mixture, in H
2The following 300 ℃ of thermal treatment 6h of atmosphere, the cooling after pulverize the invention product:
NaY
0.73Yb
0.25Er
0.02F
4。
Embodiment 3
With the rare earth carbonate is raw material, takes by weighing 159.24g Y respectively
2(CO
3)
3, 26.31g Yb
2(CO
3)
3, 2.57g Er
2(CO
3)
3Add the 200ml deionized water, the back that stirs adds the 295.3g concentrated nitric acid, and dissolving fully adds deionized water, is mixed with the 2000ml rare earth nitrate solution.Get 113.0g NH
4F adds the 300ml deionized water makes its dissolving form NH
4F solution is added drop-wise to it in rare earth nitrate solution of continuous stirring then, and leave standstill, filter, wash after dripping, and in 80 ℃ of following dry 6h, then with 37.04g NH
4F, 84.01g NaHCO
3Behind ball milling, get mixture, in N
2The following 600 ℃ of thermal treatment 1h of atmosphere, the cooling after pulverize the invention product: NaY
0.89Yb
0.10Er
0.01F
4
Embodiment 4
With the rare-earth hydroxide is raw material, takes by weighing 100.75g Y (OH) respectively
3, 44.81g Yb (OH)
3, 17.46g Er (OH)
3Add in the 200ml deionized water, the back that stirs adds the 295.3g concentrated nitric acid, and dissolving adds deionized water fully, is mixed with the 1500ml rare earth nitrate solution.Get 123.0g NH
4F adds makes its dissolving form NH in the 1000ml deionized water
4F solution; Then it is added drop-wise in the rare earth nitrate solution of continuous stirring; Leave standstill after dripping, filter, wash, and, get mixture after fully grinding with 41.99g NaF then in 100 ℃ of following dry 4h; 750 ℃ of thermal treatment 0.5h under the air atmosphere that carbon dust provides, the cooling after pulverize the invention product: NaY
0.72Yb
0.20Er
0.08F
4
Embodiment 5
With the rare earth chloride is raw material, takes by weighing 136.69g YCl respectively
3, 69.85g YbCl
3, 13.68gErCl
3Add in the deionized water, be mixed with the 1200ml rare-earth chloride solution.Getting in the 113.0g NH4F adding 600ml deionized water makes its dissolving form NH
4F solution is added drop-wise to it in rare-earth chloride solution of continuous stirring then, and leave standstill, filter, wash after dripping, and in 120 ℃ of following dry 2h, then with 94.03g Na
2SiF
6Get mixture after fully grinding, in H
2The following 300 ℃ of thermal treatment 6h of atmosphere, the cooling after pulverize the invention product:
NaY
0.70Yb
0.25Er
0.05F
4。
Comparative Examples 1
According to the described preparation method of patent CN 101020824A, preparation is formed identical up-conversion with the embodiment of the invention 3.Take by weighing 15.92g Y respectively
2(CO
3)
3, 2.63g Yb
2(CO
3)
3, 0.26gEr
2(CO
3)
3Add in the 100ml deionized water, the back that stirs adds an amount of concentrated nitric acid to dissolving fully, forms rare earth nitrate solution; Get 4.20g NaF and be dissolved in and obtain the NaF aqueous solution in the 300ml deionized water, rare-earth ion solution is added drop-wise in the NaF solution of continuous stirring gradually forms deposition then, leave standstill after continuing to stir for some time; Outwell supernatant; Filter, wash throw out, throw out is in 120 ℃ of dry 2h down, again at N
2The following 600 ℃ of thermal treatment 1h of atmosphere, cool off, pulverize, wash, dry the contrast product:
NaY
0.89Yb
0.10Er
0.01F
4。
Adopting JEM-1200EX II type transmission electron microscope (TEM) to observe particle diameter, the pattern of product, is excitaton source with 980nm LD laser apparatus, the up-conversion luminescence of Fluorolog-3-P type ultraviolet-visible-near-infrared fluorescent spectrophotometer product.The single crystal particle size of embodiment 1 has bright macroscopic green glow under the irradiation of 980nm infrared light between 200~400nm, luminous intensity is 1.33 times of comparative example 1.The single crystal particle size of embodiment 2 has bright macroscopic green glow under the irradiation of 980nm infrared light between 200~350nm, luminous intensity is 1.28 times of comparative example 1.The single crystal particle size of embodiment 3 has bright macroscopic green glow under the irradiation of 980nm infrared light between 300~400nm, luminous intensity is 1.36 times of comparative example 1.The single crystal particle size of embodiment 4 has bright macroscopic green glow under the irradiation of 980nm infrared light between 250~400nm, luminous intensity is 1.21 times of comparative example 1.The single crystal particle size of embodiment 5 has bright macroscopic green glow under the irradiation of 980nm infrared light between 200~400nm, luminous intensity is 1.18 times of comparative example 1.
Claims (8)
1. infrared up-conversion phosphor is characterized in that, the system that is red up-conversion phosphor is NaY
1-x-yYb
xEr
yF
4Wherein: 0.1≤x≤0.25,0.01≤y≤0.08.
2. the preparation method of red up-conversion phosphor according to claim 1 comprises the steps:
1) according to chemical formula NaY
1-x-yYb
xEr
yF
4, 0.1≤x≤0.25,0.01≤y≤0.08, preparation mixed solution of rare earth A;
Rare earth ion source in the described mixed solution of rare earth is selected from the soluble salt of nitrate salt or the muriate and so on of yttrium, ytterbium and erbium, or makes it to be converted into oxide compound, oxyhydroxide or the carbonate cpds of yttrium, ytterbium and the erbium of soluble salt through nitric acid or hydrochloric acid;
2) press trivalent rare earth fluorochemical chemical formula ReF
3The metering ratio, add NH to mixed solution of rare earth A
4F solution, precipitin reaction gets suspension-s;
Wherein: Re is rare earth element y, Yb and Er;
3) suspension filtered, washing place 60~120 ℃ of down dry 2~12h with filter cake again, get solid B;
4) with solid B and the fusing assistant that contains Na and F, according to N
Na/ N
Re=0.98~1.10, N
F/ N
Na>=1.0 mole number metering is than mixing;
5) step 4) gained mixture is placed specific atmosphere, 300~750 ℃ of following roasting 0.5~6h collect described infrared up-conversion phosphor product then.
3. method according to claim 2 is characterized in that, the rare earth ion source in the described mixed solution of rare earth is the soluble salt of yttrium, ytterbium and erbium.
4. method according to claim 3 is characterized in that, said mixed solution of rare earth A middle-weight rare earths ionic total concn is 0.5~1.0mol/L.
5. method according to claim 2 is characterized in that, said NH
4The concentration of F solution is 3~10mol/L.
6. method according to claim 2 is characterized in that the fusing assistant of described Na of containing and F is selected from NH
4F and Na
2CO
3Mixture, NH
4F and NaHCO
3Mixture, NaF or Na
2SiF
6In one or both.
7. method according to claim 2 is characterized in that, the fusing assistant of described Na of containing and F is NaF.
8. according to each described method of claim 2~7, it is characterized in that said specific atmosphere is H
2, N
2Or H
2And N
2Mixed gas or carbon reducing agent atmosphere.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102585829A (en) * | 2011-12-15 | 2012-07-18 | 上海华明高纳稀土新材料有限公司 | Infrared up-conversion rare earth luminescent material and preparation method thereof |
CN105112056A (en) * | 2015-09-16 | 2015-12-02 | 福州大学 | Preparation method for Er<3+>-Yb<3+>-co-doped NaYF4 fluorescent powder |
CN106947470A (en) * | 2017-03-31 | 2017-07-14 | 英特美光电(苏州)有限公司 | LED and remote fluorescence device small size salt a kind of novel processing step |
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CN101020824A (en) * | 2007-03-12 | 2007-08-22 | 中国科学院长春应用化学研究所 | Infrared ray excited up-conversion luminescent material and its prepn |
CN101289616A (en) * | 2008-05-30 | 2008-10-22 | 东北电力大学 | Process for preparing water-soluble up-conversion NaYF4:Er<3+>,Yb<3+> nano-crystalline using glycyl alcohol as solvent |
CN101575515A (en) * | 2009-06-08 | 2009-11-11 | 北京工商大学 | Method for preparing NaYF4 type up-conversion materials |
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2010
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CN101020824A (en) * | 2007-03-12 | 2007-08-22 | 中国科学院长春应用化学研究所 | Infrared ray excited up-conversion luminescent material and its prepn |
CN101289616A (en) * | 2008-05-30 | 2008-10-22 | 东北电力大学 | Process for preparing water-soluble up-conversion NaYF4:Er<3+>,Yb<3+> nano-crystalline using glycyl alcohol as solvent |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102585829A (en) * | 2011-12-15 | 2012-07-18 | 上海华明高纳稀土新材料有限公司 | Infrared up-conversion rare earth luminescent material and preparation method thereof |
CN105112056A (en) * | 2015-09-16 | 2015-12-02 | 福州大学 | Preparation method for Er<3+>-Yb<3+>-co-doped NaYF4 fluorescent powder |
CN105112056B (en) * | 2015-09-16 | 2017-09-22 | 福州大学 | A kind of Er3+, Yb3+It is co-doped with NaYF4The preparation method of fluorescent material |
CN106947470A (en) * | 2017-03-31 | 2017-07-14 | 英特美光电(苏州)有限公司 | LED and remote fluorescence device small size salt a kind of novel processing step |
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