CN103173221A - Upconversion fluorescent material and preparation method thereof - Google Patents
Upconversion fluorescent material and preparation method thereof Download PDFInfo
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- CN103173221A CN103173221A CN2013100885091A CN201310088509A CN103173221A CN 103173221 A CN103173221 A CN 103173221A CN 2013100885091 A CN2013100885091 A CN 2013100885091A CN 201310088509 A CN201310088509 A CN 201310088509A CN 103173221 A CN103173221 A CN 103173221A
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Abstract
The invention provides an upconversion fluorescent material. According to the material, GaN serves as a basic substance, Yb<3+> serves as a sensitizing agent, the chemical composition of the material is Ga(1-x-y-x)YbyRexSiZN, wherein Re is selected from arbitrary one of rare earth metals such as Er, Tm, Ho, Pr, Sm and Dy, 0.1%<=x<=2%, x<=y<=5x, and 0.01%<=z<=0.1%. In addition, the invention further provides a preparation method of the upconversion fluorescent material. According to the upconversion fluorescent material provided by invention, GaN serves as the basic substance, the good thermal stability, high melting point and easy rare earth ion doping performance of the GaN are effectively utilized; and moreover, the GaN serves as the basic substance, the upconversion efficiency is increased, so that the prepared upconversion fluorescent material has good thermal stability and high upconversion efficiency.
Description
Technical field
The invention belongs to field of photovoltaic materials, relate to a kind of upconverting fluorescent material and preparation method thereof.
Background technology
Upconverting fluorescent material can excite lower emission visible light at ir radiation, UV-light even, be with a wide range of applications in the full fields such as short wavelength's excitor, 3 D stereo demonstration, biomolecules fluorescence labelling, infrared detective of solidifying, just caused researchist's very big concern since the seventies.
Third generation semiconductor material GaN and related device thereof due to show in light display, optical storage, Laser Printing, optical illumination and medical treatment and the field such as military have broad application prospects, therefore the third generation semiconductor material take GaN as representative is described as the new engine of IT industry.Compare with traditional fluorescent material matrix, GaN have good chemical stability, fusing point high, be easy to realize the advantages such as rare earth ion doped.Singly mixing rare earth GaN is to utilize rare earth ion f-f forbidden transition, and energy conversion rate is low, and upper efficiency of conversion is not high.
Rare earth ion ytterbium Yb
3+Be the very good active ions of a kind of luminescent properties, and level structure is very simple, Yb
3+It is within the wavelength region between 0.1～1 micron that the characteristic light of ion absorbs, and has the Absorber Bandwidth of non-constant width, Yb
3+Ion excited state excites metastable state higher than active ions, so doping Yb
3+The material of ion can be with the infrared photon transmission ofenergy that absorbs to these active ions, occur that two-photon or multi-photon add and, efficiency of conversion in raising; In addition, doping Yb
3+There is not excited state absorption in the laserable material of ion, and fluorescence efficiency is very high usually, and fluorescence lifetime is longer.Therefore, doping Yb
3+The laserable material of ion is the focus that people study always.
The GaN substrate material has good physical and chemical performance, Yb
3+Ion has quite wide absorption crosssection near 980nm among this substrate material, therefore, can improve upper efficiency of conversion, and these characteristics all make it become a kind of good up-conversion luminescence substrate material.At present, with trivalent Yb
3+The up-conversion luminescent material of ion-activated GaN there is not yet bibliographical information.
Summary of the invention
The purpose of this invention is to provide high upconverting fluorescent material of a kind of upper efficiency of conversion and preparation method thereof, by take GaN as matrix, the Yb of doping
3+Be sensitizing agent, obtain upconverting fluorescent material by solid state reaction.
For achieving the above object, the present invention has adopted following technical scheme:
A kind of upconverting fluorescent material, described upconverting fluorescent material be take GaN as matrix, Yb
3+Be sensitizing agent, the chemical constitution of described upconverting fluorescent material is
Ga
1-x-y-zYb
yRe
xSi
ZN
Wherein, Re is any one in rare earth metal Er, Tm, Ho, Pr, Sm or Dy, 0.1%≤x≤2%, x≤y≤5x, 0.01%≤z≤0.1%.
In addition, the present invention also provides a kind of preparation method of upconverting fluorescent material, comprises the steps:
Be (1-x-y-z): y:x:z weighing metal Ga, metal Yb, Re and Si respectively in molar ratio, wherein, Re is any one in rare earth metal Er, Yb, Tm, Ho, Pr, Sm or Dy, 0.1%≤x≤2%, x≤y≤5x, 0.01%≤z≤0.1%;
In glass test tube, wherein, the mole number of described catalyst B i is t, 0.001(1-x-y-z with above-mentioned load weighted metal Ga, metal Yb, Re, Si and catalyst B i Vacuum Package)≤t≤0.005(1-x-y-z);
Described glass test tube is positioned in rare gas element, calcines 9～15h in 700 ℃～900 ℃ temperature, obtain mixture;
Described mixture is positioned in rare gas element heats up, when temperature rises to 600 ℃, described rare gas element is switched to a NH
3And be warming up to 900 ℃～1000 ℃, insulation 3～5h; When continuing to be warming up to 1030 ℃, with a described NH
3Switch to the 2nd NH
3, naturally cool to normal temperature after insulation 2～4h, and with described the 2nd NH
3Switch to described rare gas element;
Take out reactant and obtain described upconverting fluorescent material after grinding, rinse, drying.
In embodiment provided by the invention, described rare gas element is N
2, Ar or N
2Mixed gas with Ar.
In embodiment provided by the invention, the flow of a described NH3 is 200-400sccm, described the 2nd NH
3Flow be 400-600sccm.
In embodiment provided by the invention, described flushing is to use successively rare nitric acid, distilled water flushing.
Adopt technique scheme, beneficial effect of the present invention is:
Upconverting fluorescent material provided by the invention, take GaN as matrix, effectively utilized the Heat stability is good of GaN, fusing point high, be easy to realize rare earth ion doped performance, simultaneously, with Yb
3+As sensitizing agent, improved the efficiency of conversion of upper conversion, make the upconverting fluorescent material Heat stability is good of preparation, upper efficiency of conversion high.
Owing to also having added micro-Si in preparation in above-mentioned upconverting fluorescent material, thereby improved the conductivity of GaN.
In addition, adopt nitric acid to rinse solid-phase reactant in the above-mentioned upconverting fluorescent material of preparation, thereby metal and the catalyst B i of complete reaction do not remove, improved the purity of the GaN of doping, strengthened luminous efficiency.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with specific embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
Upconverting fluorescent material provided by the invention, take GaN as matrix, Yb
3+Be sensitizing agent, its chemical constitution is Ga
1-x-y-zYb
yRe
xSi
ZN, wherein, Re is any one in rare earth metal Er, Tm, Ho, Pr, Sm or Dy, 0.1%≤x≤2%, x≤y≤5x, 0.01%≤z≤0.1%.
Be appreciated that, this upconverting fluorescent material is compared with traditional fluorescent material matrix take GaN as matrix, GaN have good chemical stability, fusing point higher, be easy to realize rare earth ion doped, therefore, to adopt GaN be the upconverting fluorescent material Heat stability is good of matrix composition in the present invention.
In addition, this upconverting fluorescent material is with Yb
3+As sensitizing agent, due to Yb
3+Be the very good active ions of a kind of luminescent properties, and have the Absorber Bandwidth of non-constant width, Yb
3+Ion excited state excites metastable state higher than active ions, so doping Yb
3+The material of ion can be with the infrared photon transmission ofenergy that absorbs to these active ions, occur that two-photon or multi-photon add and, thereby improve upper efficiency of conversion.
The present invention also provides the preparation method of above-mentioned upconverting fluorescent material, comprises the steps:
Step S110: be (1-x-y-z): y:x:z weighing metal Ga, metal Yb, Re and Si respectively in molar ratio, wherein, Re is any one in rare earth metal Er, Tm, Ho, Pr, Sm or Dy, 0.1%≤x≤2%, x≤y≤5x, 0.01%≤z≤0.1%.
Step S120: in glass test tube, wherein, the mole number of described catalyst B i is t, 0.001(1-x-y-z with above-mentioned load weighted metal Ga, metal Yb, Re, Si and catalyst B i Vacuum Package)≤t≤0.005(1-x-y-z).
Be appreciated that because rear-earth-doped GaN electroconductibility is bad, in embodiment provided by the invention, the Si of doping trace in above-mentioned upconverting fluorescent material, thus improved the conductivity of this upconverting fluorescent material.
In addition, in the solid state reaction process that generates GaN, because the GaN that generates can cover metal Ga surface, thereby stop the further generation of GaN, make the purity of GaN not high, therefore, added catalyst B i in embodiment provided by the invention, make reaction proceed under the effect of catalyst B i, thereby output and the purity of GaN are provided.
Step S130: above-mentioned glass test tube is positioned in rare gas element, calcines 9～15h in 700 ℃～900 ℃ temperature, obtain mixture.
In the present embodiment, rare gas element is preferably N
2, Ar or N
2Mixed gas with Ar.Be appreciated that under the effect of rare gas element, this mixture has avoided oxidized.
Step S140: said mixture is positioned in rare gas element heats up, when temperature rises to 600 ℃, rare gas element is switched to a NH
3And be warming up to 900 ℃～1000 ℃, insulation 3～5h; When continuing to be warming up to 1030 ℃, with a NH
3Switch to the 2nd NH
3, naturally cool to normal temperature after insulation 2～4h, and with the 2nd NH
3Switch to described rare gas element.
In the present embodiment, the mixture that obtains in step S130 is placed in the corundum bateau, the corundum bateau that holds mixture is put into tube furnace, and to pass into flow be 200-600sccm inert gas purge tube furnace one hour, be warming up to 600 ℃.Be appreciated that pass into rare gas element after, this moment, the ambiance of reactive system was inert atmosphere, thereby had avoided mixture oxidation in the process that heats up.
In the present embodiment, a NH
3Flow be preferably 200-400sccm.When the question response system temperature is warming up to 600 ℃, the inert atmosphere of reaction system is switched to a NH
3, a NH
3Flow be 200-400sccm, and continue to heat up, when the question response system is warming up to 900 ℃～1000 ℃, constant temperature insulation 3～5h.Be appreciated that in above-mentioned temperature-rise period NH
3With mixture generation chemical reaction.
In the present embodiment, the 2nd NH
3Flow be 400-600sccm.When the question response system temperature is warming up to 1030 ℃, with a NH
3Switch to the 2nd NH
3, the 2nd NH
3Flow be 400-600sccm, and naturally cool to normal temperature after being incubated 2～4h, and with the 2nd NH
3Switch to rare gas element.Be appreciated that at the 2nd NH
3Effect under, can guarantee NH
3Produce reactant with the mixture complete reaction, simultaneously, catalyst B i in mixture is discharged, improved reactant productive rate and purity; Simultaneously with the 2nd NH
3Again switch to rare gas element, the reactant after so just having avoided generating is oxidized.
Step S150: take out reactant and obtain upconverting fluorescent material after grinding, rinse, drying.
In the present embodiment, take out the reactant that obtains through above-mentioned steps, and after grinding, then use successively rare nitric acid, distilled water flushing, obtain upconverting fluorescent material after oven dry.Be appreciated that and adopt nitric acid to rinse solid-phase reactant, thereby metal and the catalyst B i of complete reaction do not remove, improved the purity of the GaN of doping, strengthened luminous efficiency.
Below in conjunction with specific embodiment, above-mentioned upconverting fluorescent material of the present invention and preparation method thereof is described in detail.
Embodiment 1
According to described preparation method, in the present embodiment, choose x=0.1%, y=0.1%, z=0.01%, t=0.09979%, Re are rare earth metal Er.Above-mentioned load weighted raw material is packed into mix the final vacuum encapsulation in glass test tube; The glass test tube that vacuum seal installs is put into tube furnace, and be positioned over atmosphere of inert gases N
2In, at the temperature lower calcination 9h of 700 ℃; Burnt glass test tube is opened, taken out the mixture in test tube, mixture is placed in the corundum bateau.Above-mentioned corundum bateau is placed in tube furnace, and to pass into flow be 200sccm rare gas element N
2When being warming up to 600 ℃ after purging tube furnace 1h, with N
2The gas body switches to a NH
3, a NH
3Flow be 200sccm, constant temperature nitrogenize when system is warming up to 1000 ℃, and soaking time 4h; Continue rising temperature to 1030 ℃, with a NH
3Switch to the 2nd NH
3, the 2nd NH
3Flow is at 600sccm, and naturally cools to normal temperature after soaking time 2h, thereby discharges catalyst B i, and with the 2nd NH
3Switch to rare gas element N
2Take out the reactant of corundum bateau, the reactant in the corundum bateau is fully ground, then rinse with rare nitric acid, use afterwards distilled water flushing again, the oven dry sample obtains the upper conversion of the GaN powder that Yb, Er mix altogether.
Embodiment 2
According to described preparation method, in the present embodiment, choose x=0.1%, y=0.5%, z=0.1%, t=0.0993%, Re are rare earth metal Tm.Above-mentioned load weighted raw material is packed into mix the final vacuum encapsulation in glass test tube; The glass test tube that vacuum seal installs is put into tube furnace, and be positioned in atmosphere of inert gases Ar, at the temperature lower calcination 10h of 800 ℃; Burnt glass test tube is opened, taken out the mixture in test tube, mixture is placed in the corundum bateau.Above-mentioned corundum bateau is placed in tube furnace, and to pass into flow be 500sccm rare gas element N
2When being warming up to 600 ℃ after purging tube furnace 1h, with N
2The gas body switches to a NH
3, a NH
3Flow be 300sccm, constant temperature nitrogenize when system is warming up to 950 ℃, and soaking time 5h; Continue rising temperature to 1030 ℃, with a NH
3Switch to the 2nd NH
3, the 2nd NH
3Flow is at 600sccm, and naturally cools to normal temperature after soaking time 3h, thereby discharges catalyst B i, and with the 2nd NH
3Switch to rare gas element Ar.Take out the reactant of corundum bateau, the reactant in the corundum bateau is fully ground, then rinse with rare nitric acid, use afterwards distilled water flushing again, the oven dry sample obtains the upper conversion of the GaN powder that Yb, Tm mix altogether.
Embodiment 3
According to described preparation method, in the present embodiment, choose x=0.1%, y=0.1%, z=0.01%, t=0.49895%, Re are rare earth metal Ho.Above-mentioned load weighted raw material is packed into mix the final vacuum encapsulation in glass test tube; The glass test tube that vacuum seal installs is put into tube furnace, and be positioned over atmosphere of inert gases N
2In the mixed gas of Ar, at the temperature lower calcination 12h of 900 ℃; Burnt glass test tube is opened, taken out the mixture in test tube, mixture is placed in the corundum bateau.Above-mentioned corundum bateau is placed in tube furnace, and to pass into flow be 400sccm rare gas element N
2When being warming up to 600 ℃ after purging tube furnace 1h, with N
2The gas body switches to a NH
3, a NH
3Flow be 200sccm, constant temperature nitrogenize when system is warming up to 980 ℃, and soaking time 4h; Continue rising temperature to 1030 ℃, with a NH
3Switch to the 2nd NH
3, the 2nd NH
3Flow is at 600sccm, and naturally cools to normal temperature after soaking time 4h, thereby discharges catalyst B i, and with the 2nd NH
3Switch to rare gas element N
2Mixed gas with Ar.Take out the reactant of corundum bateau, the reactant in the corundum bateau is fully ground, then rinse with rare nitric acid, use afterwards distilled water flushing again, the oven dry sample obtains the upper conversion of the GaN powder that Yb, Ho mix altogether.
Embodiment 4
According to described preparation method, in the present embodiment, choose x=2%, y=2%, z=0.01%, t=0.47995%, Re are rare earth metal Dy.Above-mentioned load weighted raw material is packed into mix the final vacuum encapsulation in glass test tube; The glass test tube that vacuum seal installs is put into tube furnace, and be positioned over atmosphere of inert gases N
2In, at the temperature lower calcination 13h of 750 ℃; Burnt glass test tube is opened, taken out the mixture in test tube, mixture is placed in the corundum bateau.Above-mentioned corundum bateau is placed in tube furnace, and to pass into flow be 400sccm rare gas element N
2When being warming up to 600 ℃ after purging tube furnace 1h, with N
2The gas body switches to a NH
3, a NH
3Flow be 200sccm, constant temperature nitrogenize when system is warming up to 930 ℃, and soaking time 5h; Continue rising temperature to 1030 ℃, with a NH
3Switch to the 2nd NH
3, the 2nd NH
3Flow is at 600sccm, and naturally cools to normal temperature after soaking time 2h, thereby discharges catalyst B i, and with the 2nd NH
3Switch to rare gas element N
2Take out the reactant of corundum bateau, the reactant in the corundum bateau is fully ground, then rinse with rare nitric acid, use afterwards distilled water flushing again, the oven dry sample obtains the upper conversion of the GaN powder that Yb, Dy mix altogether.
Embodiment 5
According to described preparation method, in the present embodiment, choose x=2%, y=10%, z=0.1%, t=0.4395%, Re are rare earth metal Pr.Above-mentioned load weighted raw material is packed into mix the final vacuum encapsulation in glass test tube; The glass test tube that vacuum seal installs is put into tube furnace, and be positioned in atmosphere of inert gases Ar, at the temperature lower calcination 14h of 850 ℃; Burnt glass test tube is opened, taken out the mixture in test tube, mixture is placed in the corundum bateau.Above-mentioned corundum bateau is placed in tube furnace, and to pass into flow be 400sccm rare gas element N
2When being warming up to 600 ℃ after purging tube furnace 1h, with N
2The gas body switches to a NH
3, a NH
3Flow be 200sccm, constant temperature nitrogenize when system is warming up to 940 ℃, and soaking time 5h; Continue rising temperature to 1030 ℃, with a NH
3Switch to the 2nd NH
3, the 2nd NH
3Flow is at 600sccm, and naturally cools to normal temperature after soaking time 3h, thereby discharges catalyst B i, and with the 2nd NH
3Switch to rare gas element N
2Take out the reactant of corundum bateau, the reactant in the corundum bateau is fully ground, then rinse with rare nitric acid, use afterwards distilled water flushing again, the oven dry sample obtains the upper conversion of the GaN powder that Yb, Pr mix altogether.
Embodiment 6
According to described preparation method, in the present embodiment, choose x=2%, y=10%, z=0.1%, t=0.0879%, Re are rare earth metal Sm.Above-mentioned load weighted raw material is packed into mix the final vacuum encapsulation in glass test tube; The glass test tube that vacuum seal installs is put into tube furnace, and be positioned in atmosphere of inert gases Ar, at the temperature lower calcination 15h of 900 ℃; Burnt glass test tube is opened, taken out the mixture in test tube, mixture is placed in the corundum bateau.Above-mentioned corundum bateau is placed in tube furnace, and to pass into flow be 400sccm rare gas element N
2When being warming up to 600 ℃ after purging tube furnace 1h, with N
2The gas body switches to a NH
3, a NH
3Flow be 200sccm, constant temperature nitrogenize when system is warming up to 960 ℃, and soaking time 5h; Continue rising temperature to 1030 ℃, with a NH
3Switch to the 2nd NH
3, the 2nd NH
3Flow is at 600sccm, and naturally cools to normal temperature after soaking time 4h, thereby discharges catalyst B i, and with the 2nd NH
3Switch to rare gas element N
2Take out the reactant of corundum bateau, the reactant in the corundum bateau is fully ground, then rinse with rare nitric acid, use afterwards distilled water flushing again, the oven dry sample obtains the upper conversion of the GaN powder that Yb, Sm mix altogether.
the above, it is only preferred embodiment of the present invention, be not that the present invention is done any pro forma restriction, although the present invention discloses as above with preferred embodiment, yet be not to limit the present invention, any those skilled in the art, within not breaking away from the technical solution of the present invention scope, when the technology contents that can utilize above-mentioned announcement is made a little change or is modified to the equivalent embodiment of equivalent variations, in every case be not break away from the technical solution of the present invention content, any simple modification that foundation technical spirit of the present invention is done above embodiment, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (5)
1. a upconverting fluorescent material, is characterized in that, described upconverting fluorescent material is take GaN as matrix, Yb
3+Be sensitizing agent, the chemical constitution of described upconverting fluorescent material is
Ga
1-x-y-zYb
yRe
xSi
ZN
Wherein, Re is any one in rare earth metal Er, Yb, Tm, Ho, Pr, Sm or Dy, 0.1%≤x≤2%, x≤y≤5x, 0.01%≤z≤0.1%.
2. the preparation method of a upconverting fluorescent material, is characterized in that, comprises the steps:
Be (1-x-y-z): y:x:z weighing metal Ga, metal Yb, Re and Si respectively in molar ratio, wherein, Re is any one in rare earth metal Er, Tm, Ho, Pr, Sm or Dy, 0.1%≤x≤2%, x≤y≤5x, 0.01%≤z≤0.1%;
In glass test tube, wherein, the mole number of described catalyst B i is t, 0.001(1-x-y-z with above-mentioned load weighted metal Ga, metal Yb, Re, Si and catalyst B i Vacuum Package)≤t≤0.005(1-x-y-z);
Described glass test tube is positioned in rare gas element, calcines 9～15h in 700 ℃～900 ℃ temperature, obtain mixture;
Described mixture is positioned in rare gas element heats up, when temperature rises to 600 ℃, described rare gas element is switched to a NH
3And be warming up to 900 ℃～1000 ℃, insulation 3～5h; When continuing to be warming up to 1030 ℃, with a described NH
3Switch to the 2nd NH
3, naturally cool to normal temperature after insulation 2～4h, and with described the 2nd NH
3Switch to described rare gas element;
Take out reactant and obtain described upconverting fluorescent material after grinding, rinse, drying.
3. the preparation method of upconverting fluorescent material according to claim 2, is characterized in that, described rare gas element is N
2, Ar or N
2Mixed gas with Ar.
4. the preparation method of upconverting fluorescent material according to claim 2, is characterized in that, a described NH
3Flow be 200-400sccm, described the 2nd NH
3Flow be 400-600sccm.
5. the preparation method of upconverting fluorescent material according to claim 2, is characterized in that, described flushing is to use successively rare nitric acid, distilled water flushing.
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| CN104449689A (en) * | 2014-12-14 | 2015-03-25 | 励春亚 | Preparation method of rare-earth doped GaN material |
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