CN102660802B - Preparation method for erbium and ytterbium double-doped up-conversion luminescence nano-fiber - Google Patents
Preparation method for erbium and ytterbium double-doped up-conversion luminescence nano-fiber Download PDFInfo
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- CN102660802B CN102660802B CN201210044206.5A CN201210044206A CN102660802B CN 102660802 B CN102660802 B CN 102660802B CN 201210044206 A CN201210044206 A CN 201210044206A CN 102660802 B CN102660802 B CN 102660802B
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Abstract
The invention relates to a preparation method for an erbium and ytterbium double-doped up-conversion luminescence nano-fiber and belongs to the field of nano-material preparation, comprising the steps of (1) preparing a spinning solution; (2) preparing a PVP/metal nitrate composite fiber using a static spinning technique; (3) preparing a mixed oxide nano-fiber; and (4) preparing a LiYF4:Er3+, Yb3+ up-conversion luminescence nano-fiber. Fluorination of the mixed oxide nano-fiber with ammonium bifluoride by a double-crucible method is performed, and the LiYF4:Er3+, Yb3+ up-conversion luminescence nano-fiber having a diameter of 202.7+/-21.7nm and a length greater than 50 [mu]m with good crystallinity is obtained. The up-conversion luminescence nano-fiber is a nano luminescent material having significant application value. The preparation method is simple to operate and suitable for mass production, having a broad application prospect.
Description
Technical field
The present invention relates to nano material preparation research field, relate to specifically the two preparation methods that mix tetrafluoro yttrium lithium up-conversion luminescence nanofiber of a kind of erbium ytterbium.
Background technology
Nanofiber refers to the filamentary material of bidimensional in nanoscale on the three dimensions yardstick of material, and radial dimension is nanometer scale conventionally, and length is larger.Because the radial dimension of nanofiber is little of nanometer scale, demonstrate series of characteristics, the most outstanding is that specific area is large, thereby its surface can increase with active, and then produce small-size effect, surface or interfacial effect, quantum size effect, macro quanta tunnel effect etc., and therefore show the specificity of a series of chemistry, physics (heat, light, sound, electricity, magnetic etc.) aspect.In the prior art, there is the method for much preparing nanofiber, such as the method for reeling off raw silk from cocoons, template synthetic method, split-phase method and self-assembly method etc.In addition, also has arc evaporation, laser high temperature inustion, compound pyrolysismethod.These three kinds of methods are in fact all at high temperature to make after compound (or simple substance) evaporation, through pyrolysis (or directly condensation), make nanofiber or nanotube, from essence, all belong to compound steam sedimentation.
Up-conversion luminescence process refers to that material absorbs the process of sending higher-energy photon compared with energy photons, and this special nature that up-conversion has makes it in laser technology, optical fiber communication technology, fibre amplifier, Display Technique and the numerous areas such as false proof, have broad application prospects.Up-conversion generally includes activator, sensitizer and matrix.Erbium ion Er
3+have abundant energy level, and part is longer the life time of the level, upper conversion efficiency is very high, is the activator of the more up-conversion of research at present.With Er
3+ion is that the up-conversion of activator adopts ytterbium ion Yb conventionally
3+for sensitizer.Rare earth tetrafluoride, owing to having abundant 4f energy level and lower phonon energy, is one of matrix of current rare earth ion doped efficient up-conversion luminescent material.The two tetrafluoro yttrium lithium LiYF that mix of erbium ytterbium
4: Er
3+, Yb
3+be a kind of important up-conversion luminescent material, there is important application prospect.Adopt the methods such as microemulsion method, presoma pyrolysismethod, hydro-thermal and solvent-thermal method, the precipitation method, sol-gel process, polyalcohol method, higher boiling ligand solvent method, prepared LiYF
4: Er
3+, Yb
3+the nano materials such as nanocrystalline, nanometer rods, sheet, cube is nanocrystalline, hexahedron is nanocrystalline, octahedra nanocrystalline, hollow tubular structures, nano wire, spindle.The two tetrafluoro yttrium lithium LiYF that mix of erbium ytterbium
4: Er
3+, Yb
3+up-conversion luminescence nanofiber is a kind of novel luminescent material, will obtain important application in fields such as luminous and demonstration, false proof, medical science detection, biomarker, solar cell, chemistry and biology sensor, nano-devices, has broad application prospects.At present, have no the two tetrafluoro yttrium lithium LiYF that mix of erbium ytterbium
4: Er
3+, Yb
3+the report of up-conversion luminescence nanofiber.
The patent No. is the technical scheme that 1975504 United States Patent (USP) discloses a relevant electrospinning process (electrospinning), the method is to prepare a kind of effective ways of continuous, to have macro length micro nanometer fiber, by Formhals, in 1934, is first proposed.This method is mainly used to prepare high polymer nanometer fiber, it is characterized in that making charged Polymer Solution or melt in electrostatic field, are subject to the traction of electrostatic force and are sprayed by nozzle, invest the receiving screen on opposite, thereby realize wire drawing, then, solvent evaporation at normal temperatures, or melt cooling solidifies to normal temperature, obtains micro nanometer fiber.Over nearly 10 years, at inorfil preparing technical field, occurred adopting electrospinning process to prepare inorganic compound as the technical scheme of oxidate nano fiber, described oxide comprises TiO
2, ZrO
2, Y
2o
3, Y
2o
3: RE
3+(RE
3+=Eu
3+, Tb
3+, Er
3+, Yb
3+/ Er
3+), NiO, Co
3o
4, Mn
2o
3, Mn
3o
4, CuO, SiO
2, Al
2o
3, V
2o
5, ZnO, Nb
2o
5, MoO
3, CeO
2, LaMO
3(M=Fe, Cr, Mn, Co, Ni, Al), Y
3al
5o
12, La
2zr
2o
7deng metal oxide and composite oxide of metal.The employing electrostatic spinning techniques such as Wang Jinxian have been prepared rare earth fluoride/rare earth oxyfluoride composite nano fibre (Chinese invention patent, grant number: ZL200810050959.0); The employing electrostatic spinning techniques such as Dong Xiangting have been prepared and have been mixed europium Y
7o
6f
9nanofiber (Chinese invention patent, grant number: ZL201010550196.3); The employing electrostatic spinning techniques such as Wang Jinxian have been prepared trifluorides nanofiber (Chinese invention patent, grant number: ZL201010107993.4); Wang Ce etc. adopt electrostatic spinning technique to pass through R (CF
3cO
2)
3/ PVP (R=Eu, Ho) composite nano fiber is heat-treated, and has synthesized ROF (R=Eu, Ho) nanofiber (J.Nanosci.Nanotechnol., 2009,9 (2): 1522-1525).Electrospinning process can continuous production big L/D ratio micrometer fibers or nanofiber.Have no at present and adopt electrostatic spinning technique to combine with fluorination technology to prepare LiYF
4: Er
3+, Yb
3+the report of up-conversion luminescence nanofiber.
While utilizing electrostatic spinning technique to prepare nano material, the composition of the kind of raw material, the molecular weight of high polymer templates, spinning solution, spinning process parameter and Technology for Heating Processing have material impact to the pattern of final products and size.The present invention first adopts electrostatic spinning technique, with a hydronium(ion) oxidation lithium LiOHH
2o, yittrium oxide Y
2o
3, erbium oxide Er
2o
3with ytterbium oxide Yb
2o
3for raw material, with evaporating after nitric acid dissolve, obtain lithium nitrate LiNO
3, yttrium nitrate Y (NO
3)
3, erbium nitrate Er (NO
3)
3with ytterbium nitrate Yb (NO
3)
3mixed crystal, adds solvent DMF DMF and high polymer templates polyvinylpyrrolidone PVP, obtains carrying out electrostatic spinning after spinning solution, under best experiment condition, prepares PVP/[LiNO
3+ Y (NO
3)
3+ Er (NO
3)
3+ Yb (NO
3)
3] composite fibre, it is heat-treated in air, obtain mixed oxide nanoparticle fiber, adopt double crucible method, with ammonium acid fluoride NH
4hF
2for fluorization agent, fluoridize, prepared the LiYF of novel structure pure phase
4: Er
3+, Yb
3+up-conversion luminescence nanofiber.
Summary of the invention
Various in background technology are prepared in the method for nanofiber, the shortcoming of the method for reeling off raw silk from cocoons be solution viscosity is required too harsh; The shortcoming of template synthetic method is to prepare the continuous fibers of root root separation; Split-phase method and self-assembly method production efficiency are all lower; And compound steam sedimentation is due to the demand to high temperature, so process conditions are difficult to control, and nanofiber major diameter prepared by above-mentioned several method is than little.Use electrostatic spinning technique in background technology has been prepared metal oxide, composite oxide of metal nanofiber, rare earth fluoride/rare earth oxyfluoride composite nano fibre, has been mixed europium Y
7o
6f
9nanofiber, trifluorides nanofiber and ROF (R=Eu, Ho) nanofiber.Prior art adopts the methods such as microemulsion method, presoma pyrolysismethod, hydro-thermal and solvent-thermal method, the precipitation method, sol-gel process, polyalcohol method, higher boiling ligand solvent method, has prepared LiYF
4: Er
3+, Yb
3+the nano materials such as nanocrystalline, nanometer rods, sheet, cube is nanocrystalline, hexahedron is nanocrystalline, octahedra nanocrystalline, hollow tubular structures, nano wire, spindle.For a kind of novel up-conversion luminescence nano-fiber material is provided in nanofiber field, we combine electrostatic spinning technique with fluorination technology, invented LiYF
4: Er
3+, Yb
3+the preparation method of up-conversion luminescence nanofiber.
The present invention is achieved in that the spinning solution with certain viscosity of first preparing for electrostatic spinning, and application electrostatic spinning technique carries out electrostatic spinning, under best experiment condition, prepares PVP/[LiNO
3+ Y (NO
3)
3+ Er (NO
3)
3+ Yb (NO
3)
3] composite fibre, it is heat-treated in air, obtained mixed oxide nanoparticle fiber, adopt double crucible method, with ammonium acid fluoride NH
4hF
2for fluorization agent, fluoridize, prepared the LiYF of novel structure pure phase
4: Er
3+, Yb
3+up-conversion luminescence nanofiber.In the present invention, the erbium ion Er of doping
3+with ytterbium ion Yb
3+mole percent be respectively 1% and 20%.The steps include:
(1) preparation spinning solution
That Li Yuan,Yi Yuan,Er Yuan Heyi source is used is a hydronium(ion) oxidation lithium LiOHH
2o, yittrium oxide Y
2o
3, erbium oxide Er
2o
3with ytterbium oxide Yb
2o
3, high polymer templates adopts polyvinylpyrrolidone PVP, and molecular weight is 1300000, and adopting DMF DMF is solvent, takes an a certain amount of hydronium(ion) oxidation lithium LiOHH
2o, yittrium oxide Y
2o
3, erbium oxide Er
2o
3with ytterbium oxide Yb
2o
3, Li wherein
+, Y
3+, Er
3+and Yb
3+mol ratio be 100: 79: 1: 20, i.e. erbium ion Er
3+with ytterbium ion Yb
3+mole percent be 1% and 20%, use nitric acid HNO
3after dissolving, evaporation, obtains LiNO
3, Y (NO
3)
3, Er (NO
3)
3and Yb (NO
3)
3mixed crystal, add appropriate N, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP, in room temperature lower magnetic force, stir 6h, and standing 4h, forming spinning solution, the mass percent of this each part of spinning solution is: nitrate content 5%, PVP content 13%, solvent DMF content 82%;
(2) PVP/[LiNO
3+ Y (NO
3)
3+ Er (NO
3)
3+ Yb (NO
3)
3] composite fibre
The spinning solution preparing is added in the liquid storage pipe of device for spinning, carry out electrostatic spinning, shower nozzle internal diameter 0.7mm, the angle of adjusting shower nozzle and horizontal plane is 20 °, applies the DC voltage of 12kV, solidifies apart from 18cm, 18～25 ℃ of room temperatures, relative humidity is 55%～75%, obtains PVP/[LiNO
3+ Y (NO
3)
3+ Er (NO
3)
3+ Yb (NO
3)
3] composite fibre;
(3) prepare mixed oxide nanoparticle fiber
By described PVP/[LiNO
3+ Y (NO
3)
3+ Er (NO
3)
3+ Yb (NO
3)
3] composite fibre is put in temperature programmed control stove and heat-treats, heating rate is 1 ℃/min, at 600 ℃ of constant temperature 4h, then is cooled to 200 ℃ with the speed of 1 ℃/min, naturally cools to room temperature afterwards with body of heater, obtains mixed oxide nanoparticle fiber;
(4) prepare LiYF
4: Er
3+, Yb
3+up-conversion luminescence nanofiber
Fluorination reagent is used ammonium acid fluoride NH
4hF
2adopt double crucible method, ammonium acid fluoride is put into monkey, cover carbon-point above, described mixed oxide nanoparticle fiber is placed on above carbon-point, monkey is put into larger crucible, between interior outer crucible, add excessive ammonium acid fluoride, on outer crucible, add that crucible lid puts into tube furnace, heating rate with 2 ℃/min is warming up to 280 ℃ of insulation 2h, then is warmed up to 500 ℃ of insulation 3h, and finally the rate of temperature fall with 1 ℃/min is cooled to 200 ℃, with body of heater, naturally cool to room temperature afterwards, obtain LiYF
4: Er
3+, Yb
3+up-conversion luminescence nanofiber, diameter is 202.7 ± 21.7nm, length is greater than 50 μ m.
At the LiYF described in said process
4: Er
3+, Yb
3+up-conversion luminescence nanofiber has good crystallinity, and diameter is 202.7 ± 21.7nm, and length is greater than 50 μ m, has realized goal of the invention.
Accompanying drawing explanation
Fig. 1 is LiYF
4: Er
3+, Yb
3+the XRD spectra of up-conversion luminescence nanofiber;
Fig. 2 is LiYF
4: Er
3+, Yb
3+the SEM photo of up-conversion luminescence nanofiber, this figure doubles as Figure of abstract;
Fig. 3 is LiYF
4: Er
3+, Yb
3+the diameter distribution histogram of up-conversion luminescence nanofiber;
Fig. 4 is LiYF
4: Er
3+, Yb
3+the EDS spectrogram of up-conversion luminescence nanofiber;
Fig. 5 is LiYF
4: Er
3+, Yb
3+the upper switching emission spectrogram of up-conversion luminescence nanofiber;
Fig. 6 is LiYF
4: Er
3+, Yb
3+the upper switching emission spectrogram of up-conversion luminescence nanofiber when the diode laser of different exciting powers excites;
Fig. 7 is LiYF
4: Er
3+, Yb
3+two natural logrithm figure between the Up-conversion Intensity of up-conversion luminescence nanofiber and the exciting power of diode laser.
The specific embodiment
The yittrium oxide Y that the present invention is selected
2o
3, erbium oxide Er
2o
3with ytterbium oxide Yb
2o
3purity be 99.99%, polyvinylpyrrolidone PVP, molecular weight 1300000, DMF DMF, carbon-point, a hydronium(ion) oxidation lithium LiOHH
2o, ammonium acid fluoride NH
4hF
2with nitric acid HNO
3be commercially available analysis net product; Glass apparatus used, crucible and equipment are instrument and equipments conventional in laboratory.
Embodiment: take an a certain amount of hydronium(ion) oxidation lithium LiOHH
2o, yittrium oxide Y
2o
3, erbium oxide Er
2o
3with ytterbium oxide Yb
2o
3, Li wherein
+, Y
3+, Er
3+and Yb
3+mol ratio be 100: 79: 1: 20, i.e. erbium ion Er
3+with ytterbium ion Yb
3+mole percent be 1% and 20%, use nitric acid HNO
3after dissolving, evaporation, obtains LiNO
3, Y (NO
3)
3, Er (NO
3)
3and Yb (NO
3)
3mixed crystal, add appropriate N, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP, in room temperature lower magnetic force, stir 6h, and standing 4h, forming spinning solution, the mass percent of this each part of spinning solution is: nitrate content 5%, PVP content 13%, solvent DMF content 82%; The spinning solution preparing is added in the liquid storage pipe of device for spinning, carry out electrostatic spinning, shower nozzle internal diameter 0.7mm, the angle of adjusting shower nozzle and horizontal plane is 20 °, applies the DC voltage of 12kV, solidifies apart from 18cm, 18～25 ℃ of room temperatures, relative humidity is 55%～75%, obtains PVP/[LiNO
3+ Y (NO
3)
3+ Er (NO
3)
3+ Yb (NO
3)
3] composite fibre; By described PVP/[LiNO
3+ Y (NO
3)
3+ Er (NO
3)
3+ Yb (NO
3)
3] composite fibre is put in temperature programmed control stove and heat-treats, heating rate is 1 ℃/min, at 600 ℃ of constant temperature 4h, then is cooled to 200 ℃ with the speed of 1 ℃/min, naturally cools to room temperature afterwards with body of heater, obtains mixed oxide nanoparticle fiber; Fluorination reagent is used ammonium acid fluoride NH
4hF
2adopt double crucible method, ammonium acid fluoride is put into monkey, cover carbon-point above, described mixed oxide nanoparticle fiber is placed on above carbon-point, monkey is put into larger crucible, between interior outer crucible, add excessive ammonium acid fluoride, on outer crucible, add that crucible lid puts into tube furnace, heating rate with 2 ℃/min is warming up to 280 ℃ of insulation 2h, then is warmed up to 500 ℃ of insulation 3h, and finally the rate of temperature fall with 1 ℃/min is cooled to 200 ℃, with body of heater, naturally cool to room temperature afterwards, obtain LiYF
4: Er
3+, Yb
3+up-conversion luminescence nanofiber.Described LiYF
4: Er
3+, Yb
3+up-conversion luminescence nanofiber, has good crystallinity, the d value of its diffraction maximum and relative intensity and LiYF
4the listed d value of PDF standard card (77-0816) consistent with relative intensity, belong to tetragonal crystal system, space group is I41/a, as shown in Figure 1.Described LiYF
4: Er
3+, Yb
3+the diameter of up-conversion luminescence nanofiber is even, is fibrous, and length is greater than 50 μ m, as shown in Figure 2.By Shapiro-Wilk method to LiYF
4: Er
3+, Yb
3+the diameter of up-conversion luminescence nanofiber carries out normal distribution-test, under 95% confidence level, and LiYF
4: Er
3+, Yb
3+the diameter of up-conversion luminescence nanofiber distributes and belongs to normal distribution, and diameter is 202.7 ± 21.7nm, as shown in Figure 3.LiYF
4: Er
3+, Yb
3+up-conversion luminescence nanofiber forms (the Au conductive layer of plated surface when Au derives from SEM sample preparation, Li element can not detect by EDS spectrum) by Y, F, Er and Yb element, as shown in Figure 4.With wavelength be the diode laser of 980nm, power 549mW as excitation source, obtain LiYF
4: Er
3+, Yb
3+the upper switching emission spectrum of up-conversion luminescence nanofiber, the bands of a spectrum that are respectively 407nm, 520nm, 548nm and 650nm by peak value form, wherein the corresponding Er of the blue emission at 407nm place
3+ion
2h
9/2→
4i
15/2transition transmitting, the corresponding Er of green emission at 520nm and 548nm place
3+ion
2h
11/2→
4i
15/2with
4s
3/2→
4i
15/2transition transmitting, and the corresponding Er of the red emission at 650nm place
3+ion
4f
9/2→
4i
15/2transition transmitting, as shown in Figure 5.LiYF
4: Er
3+, Yb
3+the upper switching emission spectrum of up-conversion luminescence nanofiber strengthens along with the increase of the exciting power of diode laser, as shown in Figure 6.By LiYF
4: Er
3+, Yb
3+green emission in the upper switching emission spectrum of up-conversion luminescence nanofiber
4s
3/2→
4i
15/2transition and red emission
4f
9/2→
4i
15/2the natural logrithm lnP mapping of the natural logrithm lnI of the Up-conversion Intensity of transition to the exciting power of diode laser, obtains two straight lines, wherein
4s
3/2→
4i
15/2transition and
4f
9/2→
4i
15/2the slope n of transition is respectively 1.3361 and 1.3528, shows green emission
4s
3/2→
4i
15/2and red emission
4f
9/2→
4i
15/2be biphotonic process, as shown in Figure 7.
Certainly; the present invention also can have other various embodiments; in the situation that not deviating from spirit of the present invention and essence thereof; those of ordinary skill in the art are when making according to the present invention various corresponding changes and distortion, but these corresponding changes and distortion all should belong to the protection domain of the appended claim of the present invention.
Claims (1)
1. two preparation methods that mix tetrafluoro yttrium lithium up-conversion luminescence nanofiber of an erbium ytterbium, it is characterized in that, the method that adopts electrostatic spinning technique to combine with fluorination technology, using the polyvinylpyrrolidone PVP of molecular weight Mr=1300000 is high polymer templates, adopt N, dinethylformamide DMF is solvent, and fluorination reagent is used ammonium acid fluoride NH
4hF
2, preparing product is the two tetrafluoro yttrium lithium LiYF that mix of erbium ytterbium
4: Er
3+, Yb
3+up-conversion luminescence nanofiber, the steps include:
(1) preparation spinning solution
That Li Yuan,Yi Yuan,Er Yuan Heyi source is used is a hydronium(ion) oxidation lithium LiOHH
2o, yittrium oxide Y
2o
3, erbium oxide Er
2o
3with ytterbium oxide Yb
2o
3, high polymer templates adopts polyvinylpyrrolidone PVP, and adopting DMF DMF is solvent, takes an a certain amount of hydronium(ion) oxidation lithium LiOHH
2o, yittrium oxide Y
2o
3, erbium oxide Er
2o
3with ytterbium oxide Yb
2o
3, Li wherein
+, Y
3+, Er
3+and Yb
3+mol ratio be 100: 79: 1: 20, i.e. erbium ion Er
3+with ytterbium ion Yb
3+mole percent be 1% and 20%, use nitric acid HNO
3after dissolving, evaporation, obtains LiNO
3, Y (NO
3)
3, Er (NO
3)
3and Yb (NO
3)
3mixed crystal, add appropriate N, dinethylformamide DMF solvent and polyvinylpyrrolidone PVP, in room temperature lower magnetic force, stir 6h, and standing 4h, forming spinning solution, the mass percent of this each part of spinning solution is: nitrate content 5%, PVP content 13%, solvent DMF content 82%;
(2) PVP/[LiNO
3+ Y (NO
3)
3+ Er (NO
3)
3+ Yb (NO
3)
3] composite fibre
The spinning solution preparing is added in the liquid storage pipe of device for spinning, carry out electrostatic spinning, shower nozzle internal diameter 0.7mm, the angle of adjusting shower nozzle and horizontal plane is 20 °, applies the DC voltage of 12kV, solidifies apart from 18cm, 18～25 ℃ of room temperatures, relative humidity is 55%～75%, obtains PVP/[LiNO
3+ Y (NO
3)
3+ Er (NO
3)
3+ Yb (NO
3)
3] composite fibre;
(3) prepare mixed oxide nanoparticle fiber
By described PVP/[LiNO
3+ Y (NO
3)
3+ Er (NO
3)
3+ Yb (NO
3)
3] composite fibre is put in temperature programmed control stove and heat-treats, heating rate is 1 ℃/min, at 600 ℃ of constant temperature 4h, then is cooled to 200 ℃ with the speed of 1 ℃/min, naturally cools to room temperature afterwards with body of heater, obtains mixed oxide nanoparticle fiber;
(4) prepare LiYF
4: Er
3+, Yb
3+up-conversion luminescence nanofiber
Fluorination reagent is used ammonium acid fluoride NH
4hF
2adopt double crucible method, ammonium acid fluoride is put into monkey, cover carbon-point above, described mixed oxide nanoparticle fiber is placed on above carbon-point, monkey is put into larger crucible, between interior outer crucible, add excessive ammonium acid fluoride, on outer crucible, add that crucible lid puts into tube furnace, heating rate with 2 ℃/min is warming up to 280 ℃ of insulation 2h, then is warmed up to 500 ℃ of insulation 3h, and finally the rate of temperature fall with 1 ℃/min is cooled to 200 ℃, with body of heater, naturally cool to room temperature afterwards, obtain LiYF
4: Er
3+, Yb
3+up-conversion luminescence nanofiber, diameter is 202.7 ± 21.7nm, length is greater than 50 μ m.
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| CN104562296A (en) * | 2014-12-29 | 2015-04-29 | 长春理工大学 | Er/Yb co-doped dioxo-lanthanum cyanamide up-conversion luminescence nanofibers and preparation method thereof |
| CN108823681B (en) * | 2018-06-08 | 2020-10-16 | 长春理工大学 | Preparation method of silicon dioxide coated ytterbium erbium-doped gadolinium trifluoride tape-in-tape type nanobelt |
| CN108722450B (en) * | 2018-06-21 | 2021-01-29 | 福州大学 | Preparation method of high-strength ultraviolet-emission up-conversion phosphor powder composite photocatalytic material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101348951A (en) * | 2008-07-11 | 2009-01-21 | 长春理工大学 | Preparation of rare earth fluoride/rare earth oxyfluoride composite nano fibre |
| CN101850947A (en) * | 2010-02-09 | 2010-10-06 | 长春理工大学 | Rare-earth ion doped gadolinium gallium garnet porous nano-belt and preparation method thereof |
| CN101798056A (en) * | 2010-02-10 | 2010-08-11 | 长春理工大学 | Rare earth fluoride nanobelt and preparation method thereof |
| CN102251298A (en) * | 2011-06-03 | 2011-11-23 | 大连交通大学 | Preparation method of composite luminescent fiber nanomaterial |
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| JP特开2008-57072A 2008.03.13 |
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