CN102585828A - Yb3+-doped vanadate up-conversion fluorescent material and preparation method thereof - Google Patents
Yb3+-doped vanadate up-conversion fluorescent material and preparation method thereof Download PDFInfo
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- CN102585828A CN102585828A CN2012100173798A CN201210017379A CN102585828A CN 102585828 A CN102585828 A CN 102585828A CN 2012100173798 A CN2012100173798 A CN 2012100173798A CN 201210017379 A CN201210017379 A CN 201210017379A CN 102585828 A CN102585828 A CN 102585828A
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Abstract
The invention relates to a Yb3+-doped vanadate up-conversion fluorescent material and a preparation method of the material, belonging to the field of luminous materials and preparation technology of the luminous materials. The chemical composition of the Yb3+-doped vanadate up-conversion fluorescent material is expressed by the general formula: Ca9Ln(1-x)Ybx(VO4)7, wherein x is the molar percentage of Yb3+ doping amount, x is greater than 0.0001 and is less than or equal to 1.0, and Ln is at least one of La3+, Gd3+, Lu3+ and Y3+; and the preparation method is a high-temperature solid-phase method or chemical solution method. The fluorescent material can realize up-conversion luminescence of a blue green color under the excitation of 980nm infrared laser, and can be applied to the detection of infrared light and also can be used for the fields of goods anti-counterfeiting, biological mark and the like.
Description
Technical field
The present invention relates to a kind of upconverting fluorescent material and preparation method thereof, particularly a kind of at the infrared ray excited up-conversion that sends the visible blue green light down, belong to the luminescent material technical field.
Background technology
Rare earth ion ytterbium Yb
3+Be the very good active ions of a kind of luminescent properties, its maximum characteristics are that level structure is very simple, have only
2F
7/2With
2F
5/2Two isolated energy levels, Yb
3+It is within the wavelength region between the 0.1-1.0 micron that the ionic characteristic light absorbs, and has the absorption bandwidth of non-constant width, so Yb
3+The material of ion doping can effectively be coupled with InGaAs semi-conductor pump light source; In addition, doping Yb
3+There is not excited state absorption in the ionic laserable material, and fluorescence efficiency is very high usually, and the life-span of fluorescence is very long.Therefore Yb mixes
3+The ionic laserable material always is the focus that people study.
Up-conversion luminescent material under infrared ray excited is a kind of at the infrared ray excited material that can send visible light down, and up-conversion luminescent material all has good application background in the detection of antiforge, three-dimensional stereo display, short wavelength's all solid state laser and ir radiation or the like field.
Nakazawa E in 1970 and Shinonnya S are at YbPO
4In at first reported Yb
3+Ion is at the cooperation up-conversion luminescence behavior of blue green light wave band, Yb
3+Ionic up-conversion luminescence behavior is relatively unique, Yb
3+Pair ion is not that the mode through excited state absorption realizes up-conversion luminescence, but through excited state two near Yb
3+The ion colleague's de excitation that is coupled mutually is dealt into ground state and realizes luminous.The solid laser that the up-conversion luminescence of this uniqueness can be used to develop optical bistability, high-speed computer and blue wave band or the like novel optics; Wherein blue green light wave band of laser modulator material has huge potential application foreground in fields such as high density data storage, optical communication and demonstration, laser medicine, laser anti-counterfeit, induced with laser, so Yb
3+Ion has caused people's research and concern in the up-conversion luminescence behavior of visible light blue green light wave band.
It is more to study more up-conversion luminescent material kind at present; Study more main mostly be to be the body material of matrix with fluorochemical or oxyfluoride, though the efficient of its up-conversion luminescence is higher, the preparation of fluorochemical is extremely complicated; The pollution of preparation process is quite serious; The environmental requirement of producing is very harsh, thereby production cost is also very high, and these have all seriously hindered the practical application of up-conversion luminescent material.The up-conversion luminescent material that with the oxide compound is matrix has a lot of good characteristics, and for example the technology of preparation is very simple, and is also lower to the requirement of envrionment conditions, and luminous temperature performance, the thermal stability of material are fine.
Rare earth vanadic acid calcium substrate material has good physical and chemical performance, Yb
3+Ion has quite wide absorption band near 980 nanometers among this substrate material, therefore can improve the pumping efficiency of infrared laser, and these characteristics all make it become a kind of good up-conversion luminescence substrate material.At present, do not see bibliographical information with the up-conversion luminescence of the ion-activated vannadate of trivalent ytterbium.
Summary of the invention
It is high to the purpose of this invention is to provide a kind of percent crystallinity, and substrate material is thermally-stabilised good, prepares simple, free of contamination vannadate fluorescent material and preparation method thereof, through Yb
3+Ionic mixes, and is implemented in the infrared ray excited blue-greenish colour up-conversion fluorescence that obtains becoming clear down.
For reaching above purpose, the technical scheme that the present invention adopts is: a kind of doping Yb is provided
3+The vannadate upconverting fluorescent material, its active ions are ytterbium ion Yb
3+, under the exciting of 980 nanometer infrared lights, the emission wavelength of said fluorescent material is near the blue-greenish colour fluorescence 475 nanometers and 523 nanometers; The chemical formula of the matrix of said fluorescent material is Ca
9Ln
1-xYb
x(VO
4)
7, wherein, Ln is rare earth ruthenium ion Y
3+, lanthanum ion La
3+, gadolinium ion Gd
3+, lutetium ion Lu
3+In a kind of, or their arbitrary combination;
xBe ytterbium ion Yb
3+Adulterated molar percentage coefficient, 0.0001＜x≤1.0.
A kind of doping Yb
3+The preparation method of vannadate upconverting fluorescent material, adopt high temperature solid phase synthesis, comprise the steps:
(1) to contain calcium ion Ca
2+, rare earth ion lutetium ion Ln, vanadium ion V
5+, ytterbium ion Yb
3+Compound be raw material, press chemical formula Ca
9Ln
1-xYb
x(VO
4)
7In the mol ratio of each element take by weighing each raw material, grind and mix, obtain mixture; Described rare earth ion Ln is rare earth ruthenium ion Y
3+, lanthanum ion La
3+, gadolinium ion Gd
3+, lutetium ion Lu
3+In a kind of, or their arbitrary combination;
(2) with the mixture that obtains presintering 1～2 time under air atmosphere, pre-sintering temperature is 250～700 ℃, and the presintering time each time is 1～10 hour;
(3) behind the naturally cooling, grind and mix, in air atmosphere, finally calcine, calcining temperature is 900～1100 ℃, and the calcining soaking time is 3～10 hours, naturally cools to room temperature, obtains a kind of doping Yb
3+The vannadate upconverting fluorescent material.
Another kind of doping Yb
3+The preparation method of vannadate upconverting fluorescent material, it is characterized in that adopting the chemical solution synthesis method, comprise the steps:
(1) presses chemical formula Ca
9Ln
1-xYb
x(VO
4)
7In the Mol ratio of each element, wherein 0.0001＜x≤1.0 take by weighing reactant respectively and contain calcium ion Ca
2+, rare earth ion Ln, ytterbium ion Yb
3+Compound, described rare earth ion Ln is rare earth ruthenium ion Y
3+, lanthanum ion La
3+, gadolinium ion Gd
3+, lutetium ion Lu
3+In a kind of, or their arbitrary combination; They are dissolved in respectively in zero(ppm) water or the nitric acid, obtain clear solution; 0.5～2.0 wt% by each reactant quality adds complexing agent Hydrocerol A or oxalic acid respectively in each clear solution again, is heated to 50～100 ℃, stirs 0.5～3 hour, obtains the transparent mixture liquid of various respective reaction things; The pH value of regulating them is 5～6;
(2) press chemical formula Ca
9Ln
1-xYb
x(VO
4)
7In the Mol ratio of each element, take by weighing and contain vanadium ion V
5+Compound, be dissolved in zero(ppm) water or the nitric acid, obtain clear solution; 0.5～2.0 wt% that presses the reactant quality again adds complexing agent Hydrocerol A or oxalic acid complexing vanadium ion V
5+, be heated to 50～100 ℃, stirred 0.5～3 hour, obtain corresponding transparent mixture liquid; Regulating the pH value is 7～8;
(3) the various mixture that step (1) and (2) obtained are mixed, and stir, and under 50～100 ℃ temperature condition, stir 1～2 hour again, leave standstill, and dry, and obtain fluffy presoma;
(4) place retort furnace to calcine presoma, processing condition are: be warming up to 400～700 ℃ earlier, insulation was greater than 2 hours; Then be warmed up to 850～1100 ℃ and finally calcine, calcination time 3～10 hours naturally cools to room temperature, obtains a kind of doping Yb
3+The vannadate upconverting fluorescent material.
The described calcium ion Ca that contains
2+Compound be a kind of in quicklime, lime carbonate, nitrocalcite, calcium sulfate, the caoxalate, or their arbitrary combination.
The described compound that contains rare earth ion Ln is rare earth ruthenium ion Y
3+, lanthanum ion La
3+, gadolinium ion Gd
3+, lutetium ion Lu
3+Oxide compound, nitrate salt in a kind of, or their arbitrary combination.
The described rare earth ion ytterbium ion Yb that contains
3+Compound be a kind of in rare earth ruthenium ion ytterbium oxide, the ytterbium nitrate, or their arbitrary combination.
The described vanadium ion V that contains
5+Compound be a kind of in Vanadium Pentoxide in FLAKES, the vanadic acid ammonia, or two kinds combination.
In the present invention, pre-burning is become 1 time, and pre-sintering temperature is 350～550 ℃, and the presintering time is 3～5 hours.Final incinerating temperature is 950～1050 ℃, and calcination time is 5～8 hours.
Description of drawings
Fig. 1 is the comparison of the X-ray powder diffraction collection of illustrative plates and the standard card PDF#46-0410 of sample in the embodiment of the invention 1;
Fig. 2 is the Ca that the embodiment of the invention 1 provides
9La
0.9Yb
0.1(VO
4)
7Sample is the luminescent spectrum figure under 0.7 watt the excitation at 980nm, power;
Fig. 3 is the Ca that the embodiment of the invention 2 provides
9La
0.2Yb
0.8(VO
4)
7Sample is the luminescent spectrum figure under 0.7 watt the excitation at 980nm, power;
Fig. 4 is the Ca that the embodiment of the invention 6 provides
9Yb (VO
4)
7Sample is the luminescent spectrum figure under 0.7 watt the excitation at 980nm, power;
Fig. 5 is the Ca that the embodiment of the invention 7 provides
9Yb (VO
4)
7Sample is the luminescent spectrum figure under 0.7 watt the excitation at 980nm, power.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is further described.
Embodiment 1
Preparation up-conversion luminescent material Ca
9La
0.9Yb
0.1(VO
4)
7
Take by weighing lime carbonate CaCO
3: 4.5041 grams, lanthanum trioxide La
2O
3: 0.7331 gram, ytterbium oxide Yb
2O
3: 0.1 gram and vanadic acid ammonia NH
4VO
3: 4.0943 grams, after in agate mortar, grinding and mixing, select air atmosphere to calcine for the first time, temperature is 300 ℃, calcination time 3 hours is chilled to room temperature then, takes out sample.After first time incinerating raw material, grind the compound thorough mixing evenly once more, among air atmosphere, 630 ℃ of sintering for the second time down, sintering time is 5 hours, cooling causes room temperature; Grind the compound thorough mixing evenly once more, among air atmosphere, sintering for the third time under 1000 ℃, sintering time is 6 hours, cooling causes room temperature; Promptly obtain powder shaped Yb
3+Rare earth doped vanadic acid calcium base upconverting fluorescent material.
Referring to accompanying drawing 1, the X-ray powder diffraction collection of illustrative plates and the standard card PDF#46-0410 comparative result that prepare sample by the present embodiment technical scheme show that prepared material is a monophase materials.
Referring to accompanying drawing 2, be by the sample of the present embodiment technical scheme preparation up-conversion luminescence spectrum under 0.7 watt of 980 excited, be presented on the blue-greenish colour fluorescence of 475 nanometers and 523 nanometers.
Embodiment 2
Preparation up-conversion luminescent material Ca
9La
0.2Yb
0.8(VO
4)
7
Take by weighing lime carbonate CaCO
3: 4.5041 grams, lanthanum trioxide La
2O
3: 0.163 gram, ytterbium oxide Yb
2O
3: 0.7882 gram and vanadic acid ammonia NH
4VO
3: 4.0943 grams, after in agate mortar, grinding and mixing, select air atmosphere to calcine for the first time, temperature is 450 ℃, calcination time 5 hours is chilled to room temperature then, takes out sample.After first time incinerating raw material, grind the compound thorough mixing evenly once more, among air atmosphere, 950 ℃ of sintering for the second time down, sintering time is 10 hours, cooling causes room temperature; Promptly obtain powder shaped Yb
3+Rare earth doped vanadic acid calcium base upconverting fluorescent material.
Referring to accompanying drawing 3, it is by the sample of the present embodiment technical scheme preparation up-conversion luminescence spectrogram under 0.7 watt of 980 excited, is presented on the blue-greenish colour fluorescence of 475 nanometers and 523 nanometers.
Embodiment 3
Preparation up-conversion luminescent material Ca
9Gd
0.2Yb
0.8(VO
4)
7
Take by weighing lime carbonate CaCO
3: 4.5041 grams, gadolinium sesquioxide Gd
2O
3: 0.1813 gram, ytterbium oxide Yb
2O
3: 0.7882 gram and vanadic acid ammonia NH
4VO
3: 4.0943 grams, after in agate mortar, grinding and mixing, select air atmosphere to calcine for the first time, temperature is 500 ℃, calcination time 6 hours is chilled to room temperature then, takes out sample.Grind the compound thorough mixing evenly once more, among air atmosphere, 1050 ℃ of sintering for the second time down, sintering time is 7 hours, cooling causes room temperature; Promptly obtain powder shaped Yb
3+Rare earth doped vanadic acid calcium base upconverting fluorescent material.Up-conversion luminescence spectrum and legend 3 that the present embodiment technical scheme prepares sample are approximate.
Embodiment 4
Preparation up-conversion luminescent material 4 Ca
9Y
0.2Yb
0.8(VO
4)
7
Take by weighing lime carbonate CaCO
3: 4.5041 grams, yttrium oxide Y
2O
3: 0.113 gram, ytterbium oxide Yb
2O
3: 0.7882 gram and vanadic acid ammonia NH
4VO
3: 4.0943 grams, after in agate mortar, grinding and mixing, select air atmosphere to calcine for the first time, temperature is 300 ℃, calcination time 10 hours is chilled to room temperature then, takes out sample.Grind the compound thorough mixing evenly once more, among air atmosphere, 1100 ℃ of sintering for the second time down, sintering time is 4 hours, cooling causes room temperature; Promptly obtain powder shaped Yb
3+Rare earth doped vanadic acid calcium base upconverting fluorescent material.Up-conversion luminescence spectrum and legend 3 that the present embodiment technical scheme prepares sample are approximate.
Embodiment 5
Preparation up-conversion luminescent material Ca
9Lu
0.1Yb
0.9(VO
4)
7
Take by weighing lime carbonate CaCO
3: 4.5041 grams, lutecium oxide Lu
2O
3: 0.1 gram, ytterbium oxide Yb
2O
3: 0.8867 gram and vanadic acid ammonia NH
4VO
3: 4.0943 grams, after in agate mortar, grinding and mixing, select air atmosphere to calcine for the first time, temperature is 350 ℃, calcination time 8 hours is chilled to room temperature then, takes out sample.Grind the compound thorough mixing evenly once more, among air atmosphere, 800 ℃ of sintering for the second time down, sintering time is 3 hours, cooling causes room temperature; Grind the compound thorough mixing evenly once more, among air atmosphere, sintering for the third time under 1000 ℃, sintering time is 5 hours, cooling causes room temperature; Promptly obtain powder shaped Yb
3+Rare earth doped vanadic acid calcium base upconverting fluorescent material.Up-conversion luminescence spectrum and legend 3 that the embodiment technical scheme prepares sample are approximate.
Embodiment 6
Preparation up-conversion luminescent material Ca
9Yb (VO
4)
7
Take by weighing lime carbonate CaCO
3: 9.01 grams, ytterbium oxide Yb
2O
3: 1.971 gram and vanadic acid ammonia NH
4VO
3: 8.1886 grams, after in agate mortar, grinding and mixing, select air atmosphere to calcine for the first time, temperature is 400 ℃, calcination time 4 hours is chilled to room temperature then, takes out sample.Grind the compound thorough mixing evenly once more, among air atmosphere, 1000 ℃ of sintering for the second time down, sintering time is 8 hours, cooling causes room temperature; Promptly obtain powder shaped vanadic acid ytterbium calcium upconverting fluorescent material.Fig. 4 is embodiment 6 Ca
9Yb (VO
4)
7The up-conversion luminescence spectrum of sample under 980nm excites, exciting light is 0.7 watt.Be presented on the blue-greenish colour fluorescence of 475 nanometers and 523 nanometers.
Embodiment 7
Preparation up-conversion luminescent material Ca
9Yb (VO
4)
7
Take by weighing four water-calcium nitrate Ca (NO
3)
2.4H
2The O:10.627 gram is dissolved in zero(ppm) water; Take by weighing ytterbium oxide Yb
2O
3: 0.9853 gram, heating 80-100 degree is dissolved in nitric acid, mixes two kinds of solution, adds Hydrocerol A 0.12 gram, regulates pH value to 5.5, obtains clear solution 1.Take by weighing vanadic acid ammonia NH
4VO
3: 4.0943 grams, be dissolved in zero(ppm) water, be heated to 80 ℃, stirred 1.5 hours, obtain clear solution 2, regulate pH value to 7.5.Solution 1 and solution 2 are mixed, after stirring 2 hours under 50～100 ℃ the temperature condition, leave standstill, among baking oven, dry, obtain presoma; Place retort furnace to calcine the presoma that obtains: at first to be warmed up to 650 degree, to be incubated 5 hours; Then be warmed up to 1000 ℃ again, calcination time is 8 hours.Promptly obtain powder shaped vanadic acid ytterbium calcium upconverting fluorescent material.Legend 5 is embodiment 7 Ca
9Yb (VO
4)
7The up-conversion luminescence spectrum of sample under 980nm excites, exciting light is 0.7 watt, and sample has bright up-conversion luminescence, and luminous main peak is in 475 nanometers and 523 nanometers.
Claims (9)
1. doping Yb
3+The vannadate upconverting fluorescent material, it is characterized in that: its active ions are ytterbium ion Yb
3+, under the exciting of 980 nanometer infrared lights, the emission wavelength of said fluorescent material is near the blue-greenish colour fluorescence 475 nanometers and 523 nanometers; The chemical formula of the matrix of said fluorescent material is Ca
9Ln
1-xYb
x(VO
4)
7, wherein, Ln is rare earth ruthenium ion Y
3+, lanthanum ion La
3+, gadolinium ion Gd
3+, lutetium ion Lu
3+In a kind of, or their arbitrary combination;
xBe ytterbium ion Yb
3+Adulterated molar percentage coefficient, 0.0001＜x≤1.0.
2. doping Yb as claimed in claim 1
3+The preparation method of vannadate upconverting fluorescent material, it is characterized in that adopting high temperature solid phase synthesis, comprise the steps:
(1) to contain calcium ion Ca
2+, rare earth ion lutetium ion Ln, vanadium ion V
5+, ytterbium ion Yb
3+Compound be raw material, press chemical formula Ca
9Ln
1-xYb
x(VO
4)
7In the mol ratio of each element take by weighing each raw material, grind and mix, obtain mixture; Described rare earth ion Ln is rare earth ruthenium ion Y
3+, lanthanum ion La
3+, gadolinium ion Gd
3+, lutetium ion Lu
3+In a kind of, or their arbitrary combination;
(2) with the mixture that obtains presintering 1～2 time under air atmosphere, pre-sintering temperature is 250～700 ℃, and the presintering time each time is 1～10 hour;
(3) behind the naturally cooling, grind and mix, in air atmosphere, finally calcine, calcining temperature is 900～1100 ℃, and the calcining soaking time is 3～10 hours, naturally cools to room temperature, obtains a kind of doping Yb
3+The vannadate upconverting fluorescent material.
3. doping Yb as claimed in claim 1
3+The preparation method of vannadate upconverting fluorescent material, it is characterized in that adopting the chemical solution synthesis method, comprise the steps:
(1) presses chemical formula Ca
9Ln
1-xYb
x(VO
4)
7In the Mol ratio of each element, wherein 0.0001＜x≤1.0 take by weighing reactant respectively and contain calcium ion Ca
2+, rare earth ion Ln, ytterbium ion Yb
3+Compound, described rare earth ion Ln is rare earth ruthenium ion Y
3+, lanthanum ion La
3+, gadolinium ion Gd
3+, lutetium ion Lu
3+In a kind of, or their arbitrary combination; They are dissolved in respectively in zero(ppm) water or the nitric acid, obtain clear solution; 0.5～2.0 wt% by each reactant quality adds complexing agent Hydrocerol A or oxalic acid respectively in each clear solution again, is heated to 50～100 ℃, stirs 0.5～3 hour, obtains the transparent mixture liquid of various respective reaction things; The pH value of regulating them is 5～6;
(2) press chemical formula Ca
9Ln
1-xYb
x(VO
4)
7In the Mol ratio of each element, take by weighing and contain vanadium ion V
5+Compound, be dissolved in zero(ppm) water or the nitric acid, obtain clear solution; 0.5～2.0 wt% that presses the reactant quality again adds complexing agent Hydrocerol A or oxalic acid complexing vanadium ion V
5+, be heated to 50～100 ℃, stirred 0.5～3 hour, obtain corresponding transparent mixture liquid; Regulating the pH value is 7～8;
(3) the various mixture that step (1) and (2) obtained are mixed, and stir, and under 50～100 ℃ temperature condition, stir 1～2 hour again, leave standstill, and dry, and obtain fluffy presoma;
(4) place retort furnace to calcine presoma, processing condition are: be warming up to 400～700 ℃ earlier, insulation was greater than 2 hours; Then be warmed up to 850～1100 ℃ and finally calcine, calcination time 3～10 hours naturally cools to room temperature, obtains a kind of doping Yb
3+The vannadate upconverting fluorescent material.
4. according to claim 2 or 3 described a kind of doping Yb
3+The preparation method of vannadate upconverting fluorescent material, it is characterized in that: the described calcium ion Ca that contains
2+Compound be a kind of in quicklime, lime carbonate, nitrocalcite, calcium sulfate, the caoxalate, or their arbitrary combination.
5. according to claim 2 or 3 described a kind of doping Yb
3+The preparation method of vannadate upconverting fluorescent material, it is characterized in that: the described compound that contains rare earth ion Ln is rare earth ruthenium ion Y
3+, lanthanum ion La
3+, gadolinium ion Gd
3+, lutetium ion Lu
3+Oxide compound, nitrate salt in a kind of, or their arbitrary combination.
6. according to claim 2 or 3 described a kind of doping Yb
3+The preparation method of vannadate upconverting fluorescent material, it is characterized in that: the described rare earth ion ytterbium ion Yb that contains
3+Compound be a kind of in rare earth ruthenium ion ytterbium oxide, the ytterbium nitrate, or their arbitrary combination.
7. according to claim 2 or 3 described a kind of doping Yb
3+The preparation method of vannadate upconverting fluorescent material, it is characterized in that: the described vanadium ion V that contains
5+Compound be a kind of in Vanadium Pentoxide in FLAKES, the vanadic acid ammonia, or two kinds combination.
8. a kind of doping Yb according to claim 2
3+The preparation method of vannadate upconverting fluorescent material, it is characterized in that: pre-burning is become 1 time, pre-sintering temperature is 350～550 ℃, the presintering time is 3～5 hours.
9. according to claim 2 or 3 described a kind of doping Yb
3+The preparation method of vannadate upconverting fluorescent material, it is characterized in that: final incinerating temperature is 950～1050 ℃, and calcination time is 5～8 hours.
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| CN102925148A (en) * | 2012-11-15 | 2013-02-13 | 电子科技大学 | White fluorescent powder for LED (Light Emitting Diode) excited through ultraviolet and infrared modes and preparation method |
| CN102942929A (en) * | 2012-11-30 | 2013-02-27 | 苏州大学 | Ytterbium ion Yb<3+> activated borotungstate upconversion luminescent material and preparation method thereof |
| CN102994082A (en) * | 2012-12-13 | 2013-03-27 | 昆明理工大学 | Bismuth ion-doped germinate white light phosphor and preparation method thereof |
| CN103113891A (en) * | 2013-03-14 | 2013-05-22 | 苏州大学 | Vanadate green emitting phosphor as well as preparation method and application thereof |
| CN104910914A (en) * | 2015-05-08 | 2015-09-16 | 江苏师范大学 | Lanthanum boron vanadate-based red fluorescent material and preparation method thereof |
| CN108927140A (en) * | 2018-04-04 | 2018-12-04 | 山东大学 | It is a kind of with upper conversion Shan Hong light emitting and the rear-earth-doped vanadic acid bismuth material of photocatalysis double function characteristic and its preparation method and application |
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