CN102943321A - Europium doped yttrium trifluoride upconversion luminescence hollow nanometer fiber preparation method - Google Patents

Europium doped yttrium trifluoride upconversion luminescence hollow nanometer fiber preparation method Download PDF

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CN102943321A
CN102943321A CN2012104073996A CN201210407399A CN102943321A CN 102943321 A CN102943321 A CN 102943321A CN 2012104073996 A CN2012104073996 A CN 2012104073996A CN 201210407399 A CN201210407399 A CN 201210407399A CN 102943321 A CN102943321 A CN 102943321A
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preparation
hollow nano
pvp
nano fiber
europium
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CN102943321B (en
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董相廷
李丹
于文生
王进贤
刘桂霞
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Changchun University of Science and Technology
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Changchun University of Science and Technology
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Abstract

The present invention relates to a europium doped yttrium trifluoride upconversion luminescence hollow nanometer fiber preparation method, and belongs to the technical field of nanometer material preparation. The preparation method comprises the following four steps: (1) preparing a spinning solution; (2) adopting a uniaxial electrospinning technology to prepare PVP/[Y(NO3)3+Eu(NO3)3] original composite fibers; (3) preparing Y2O3:5%Eu<3+> hollow nanometer fibers, wherein the Y2O3:5%Eu<3+> hollow nanometer fibers are obtained by carrying out a heat treatment on the original composite fibers; and (4) preparing YF3:5%Eu<3+> hollow nanometer fibers, wherein a dual crucible method is adopted, ammonium bifluoride is adopted to carry out a fluorination treatment on the Y2O3:5%Eu<3+> hollow nanometer fibers to obtain the YF3:5%Eu<3+> hollow nanometer fibers, and the YF3:5%Eu<3+> hollow nanometer fibers have excellent crystallinity, a diameter of 154-240 nm and a length of more than 20 mum. The hollow nanometer fibers are an important red fluorescent material. In addition, the preparation method has characteristics of simpleness, easy performing, mass production and broad application prospects.

Description

A kind of preparation method who mixes europium three yttrium fluoride hollow nano fibers
Technical field
The present invention relates to nano material preparation research field, relate to specifically a kind of preparation method who mixes europium three yttrium fluoride hollow nano fibers.
Background technology
Nanofiber refers to have bidimensional to be in the filamentary material of nanoscale at the three dimensions yardstick of material, and radial dimension is nanometer scale usually, and length is then 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 energy and active the increase, 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.Hollow nano fiber will have widely and use owing to have larger specific area.In the prior art, a lot of methods that prepare nanofiber are arranged, 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 in fact all are after at high temperature making compound (or simple substance) evaporation, make nanofiber or nanotube through pyrolysis (or directly condensation), from essence, all belong to the compound steam sedimentation.
The rare earth fluoride phonon energy is low, has good heat endurance and environmental stability, extensively is used as luminescent material matrix, solid electrolyte, lubricant, iron and steel and non-ferrous alloy additive, electrode material, chemical sensor and biology sensor etc.Mix europium three yttrium fluoride YF 3: Eu 3+Nano material is a kind of important red fluorescence material, has broad application prospects, and has become one of focus of nano luminescent material research field.People have adopted the methods such as the precipitation method, microemulsion method, hydro-thermal and solvent-thermal method, sol-gel process, microwave method, supercritical ultrasonics technology, presoma pyrolysismethod, method of electrostatic spinning, have prepared YF 3: Eu 3+The nano material of nano particle, nano wire, nanotube, nanometer rods, nanofiber, nanometer film, the different morphologies such as polyhedron is nanocrystalline, composite construction is nanocrystalline, core-shell structured nanomaterials.Mix europium three yttrium fluoride YF 3: Eu 3+Hollow nano fiber is a kind of novel red illuminating 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 and mix europium three yttrium fluoride YF 3: Eu 3+The report of emitting red light hollow nano fiber.
The patent No. is the technical scheme that 1975504 United States Patent (USP) discloses a relevant electrospinning process (electrospinning), the method is a kind of effective ways that prepare continuous, as to have macro length micro nanometer fiber, is at first proposed in 1934 by Formhals.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, to be subjected to the traction of electrostatic force and sprayed by nozzle, invest the receiving screen on opposite, thereby realization wire drawing, then, at normal temperatures solvent evaporation, perhaps melt cooling solidifies to normal temperature, obtains micro nanometer fiber.Over nearly 10 years, occurred adopting electrospinning process to prepare the technical scheme of inorganic compound such as oxidate nano fiber at the inorfil preparing technical field, 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 single spinning head of the uses such as Wang Jinxian, employing electrostatic spinning technique have 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 prepared mixes europium Y 7O 6F 9Nanofiber [Chinese invention patent, grant number: ZL201010550196.3]; The single spinning head of the uses such as Wang Jinxian, employing electrostatic spinning technique have prepared trifluorides nanofiber [Chinese invention patent, grant number: ZL201010107993.4]; Wang Ce etc. use single spinning head, 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.At present, have no and adopt the single shaft electrostatic spinning technique to combine with fluorination technology to prepare YF 3: Eu 3+The report of emitting red light hollow nano fiber.
When 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 pattern and the size of final products.The present invention adopts first electrostatic spinning technique, with yittrium oxide Y 2O 3With europium oxide Eu 2O 3Be raw material, with evaporating behind the nitric acid dissolve, obtain yttrium nitrate Y (NO 3) 3With europium nitrate Eu (NO 3) 3Mixed crystal adds solvent DMF DMF and high polymer templates polyvinylpyrrolidone PVP, obtains spinning solution, and the viscosity of control spinning solution is most important, carries out electrostatic spinning under the experiment condition of the best, prepares PVP/[Y (NO 3) 3+ Eu (NO 3) 3] original composite fibre, it is heat-treated in air, obtain Y 2O 3: Eu 3+Hollow nano fiber adopts double crucible method, with ammonium acid fluoride NH 4HF 2Fluoridize for fluorization agent, prepared the YF of novel structure pure phase 3: Eu 3+The emitting red light hollow nano fiber.
Summary of the invention
Various in background technology prepare 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 that the root root separates; Split-phase method and self-assembly method production efficiency are all lower; And the compound steam sedimentation is because to the demand of high temperature, so process conditions are difficult to control, and the nanofiber major diameter of above-mentioned several method preparation is than little.Adopt single spinning head in the background technology, used electrostatic spinning technique to prepare metal oxide, composite oxide of metal nanofiber, rare earth fluoride/rare earth oxyfluoride composite nano fibre, mixed europium Y 7O 6F 9Nanofiber, trifluorides nanofiber and ROF (R=Eu, Ho) nanofiber; Prior art adopts the methods such as the precipitation method, microemulsion method, hydro-thermal and solvent-thermal method, sol-gel process, microwave method, supercritical ultrasonics technology, presoma pyrolysismethod, method of electrostatic spinning, has prepared YF 3: Eu 3+The nano material of nano particle, nano wire, nanotube, nanometer rods, nanofiber, nanometer film, the different morphologies such as polyhedron is nanocrystalline, composite construction is nanocrystalline, core-shell structured nanomaterials.For a kind of novel red luminous hollow nano fiber material is provided in the nanofiber field, we combine the single shaft electrostatic spinning technique with fluorination technology, invented YF 3: Eu 3+The preparation method of emitting red light hollow nano fiber.
The present invention is achieved in that the spinning solution with certain viscosity of at first preparing for electrostatic spinning, uses electrostatic spinning technique and carries out electrostatic spinning, under the experiment condition of the best, prepares PVP/[Y (NO 3) 3+ Eu (NO 3) 3] original composite fibre, it is heat-treated in air, obtain Y 2O 3: Eu 3+Hollow nano fiber adopts double crucible method, with ammonium acid fluoride NH 4HF 2Fluoridize for fluorization agent, prepared the YF of novel structure pure phase 3: Eu 3+The emitting red light hollow nano fiber.In the present invention, the mole percent of the europium ion of doping is 5%, is labeled as YF 3: 5%Eu 3+, i.e. that the present invention is prepared is YF 3: 5%Eu 3+The emitting red light hollow nano fiber.The steps include:
(1) preparation spinning solution
That use in yttrium source and europium source is yittrium oxide Y 2O 3With europium oxide Eu 2O 3, high polymer templates adopts polyvinylpyrrolidone PVP, and molecular weight is 10000, and adopting DMF DMF is solvent, takes by weighing a certain amount of yittrium oxide Y 2O 3With europium oxide Eu 2O 3, Y wherein 3+And Eu 3+Mol ratio be 95: 5, namely the mole percent of europium ion is 5%, uses nitric acid HNO 3Evaporation obtains Y (NO after the dissolving 3) 3And Eu (NO 3) 3Mixed crystal adds DMF and PVP, stirs 4h in the room temperature lower magnetic force, and leaves standstill 2h, forms spinning solution, and the mass percent of each part is in this spinning solution: nitrate content 12%, PVP content 39%, solvent DMF content 49%;
(2) preparation PVP/[Y (NO 3) 3+ Eu (NO 3) 3] original composite fibre
Adopt the single shaft electrostatic spinning technique, the 10# stainless steel syringe needle after the spinning head employing is truncated, external diameter is 1.0mm, internal diameter is 0.7mm, the spinning solution for preparing is placed the liquid storage pipe of device for spinning, adopt perpendicular spray mode, spinning head is vertical with horizontal plane, the adjusting DC voltage is 16kV, spinning head is 18cm to the curing distance of receiving screen wire netting, and 18～28 ℃ of indoor temperatures, relative humidity are 40%～70%, along with the volatilization of solvent, on the receiving screen wire netting, can obtain PVP/[Y (NO 3) 3+ Eu (NO 3) 3] original composite fibre;
(3) preparation Y 2O 3: 5%Eu 3+Hollow nano fiber
With described PVP/[Y (NO 3) 3+ Eu (NO 3) 3] original composite fibre is put in the temperature programmed control stove and heat-treats, heating rate is 1 ℃/min, at 700 ℃ of constant temperature 8h, the speed with 1 ℃/min is cooled to 200 ℃ again, naturally cools to room temperature with body of heater afterwards, obtains Y 2O 3: 5%Eu 3+Hollow nano fiber;
(4) preparation YF 3: 5%Eu 3+Hollow nano fiber
Fluorination reagent uses ammonium acid fluoride NH 4HF 2, adopt double crucible method, ammonium acid fluoride is put into monkey, the above covers carbon-point, with described Y 2O 3: 5%Eu 3+Hollow nano fiber is placed on above the carbon-point, monkey is put into larger crucible, between interior outer crucible, add an amount of ammonium acid fluoride, add that at outer crucible the crucible lid puts into tube furnace, heating rate with 2 ℃/min is warming up to 280 ℃ of insulation 2h, is warmed up to 450 ℃ of insulation 3h again, and the rate of temperature fall with 1 ℃/min is cooled to 200 ℃ at last, naturally cool to room temperature with body of heater afterwards, obtain YF 3: 5%Eu 3+Hollow nano fiber, diameter are 197 ± 43nm, and length is greater than 20 μ m.
At the YF described in the said process 3: 5%Eu 3+Hollow nano fiber has good crystallinity, and diameter is 197 ± 43nm, and length has realized goal of the invention greater than 20 μ m.
Description of drawings
Fig. 1 is YF 3: 5%Eu 3+The XRD spectra of hollow nano fiber;
Fig. 2 is YF 3: 5%Eu 3+The SEM photo of hollow nano fiber, this figure doubles as Figure of abstract;
Fig. 3 is YF 3: 5%Eu 3+The diameter distribution histogram of hollow nano fiber;
Fig. 4 is YF 3: 5%Eu 3+The EDS spectrogram of hollow nano fiber;
Fig. 5 is YF 3: 5%Eu 3+The TEM photo of hollow nano fiber;
Fig. 6 is YF 3: 5%Eu 3+The ED photo of hollow nano fiber;
Fig. 7 is YF 3: 5%Eu 3+The exciting light spectrogram of hollow nano fiber;
Fig. 8 is YF 3: 5%Eu 3+The utilizing emitted light spectrogram of hollow nano fiber.
The specific embodiment
The yittrium oxide Y that the present invention is selected 2O 3With europium oxide Eu 2O 3Purity be 99.99%, polyvinylpyrrolidone PVP, molecular weight are 10000, DMF DMF, carbon-point, ammonium acid fluoride NH 4HF 2With nitric acid HNO 3Be commercially available analysis net product; Used glass apparatus, crucible and equipment are instrument and equipments commonly used in the laboratory.
Embodiment: take by weighing a certain amount of yittrium oxide Y 2O 3With europium oxide Eu 2O 3, Y wherein 3+And Eu 3+Mol ratio be 95: 5, namely the mole percent of europium ion is 5%, uses nitric acid HNO 3Evaporation obtains Y (NO after the dissolving 3) 3And Eu (NO 3) 3Mixed crystal adds DMF and PVP, stirs 4h in the room temperature lower magnetic force, and leaves standstill 2h, forms spinning solution, and the mass percent of each part is in this spinning solution: nitrate content 12%, PVP content 39%, solvent DMF content 49%; Adopt the single shaft electrostatic spinning technique, the 10# stainless steel syringe needle after the spinning head employing is truncated, external diameter is 1.0mm, internal diameter is 0.7mm, the spinning solution for preparing is placed the liquid storage pipe of device for spinning, adopt perpendicular spray mode, spinning head is vertical with horizontal plane, the adjusting DC voltage is 16kV, spinning head is 18cm to the curing distance of receiving screen wire netting, and 18～28 ℃ of indoor temperatures, relative humidity are 40%～70%, along with the volatilization of solvent, on the receiving screen wire netting, can obtain PVP/[Y (NO 3) 3+ Eu (NO 3) 3] original composite fibre; With described PVP/[Y (NO 3) 3+ Eu (NO 3) 3] original composite fibre is put in the temperature programmed control stove and heat-treats, heating rate is 1 ℃/min, at 700 ℃ of constant temperature 8h, the speed with 1 ℃/min is cooled to 200 ℃ again, naturally cools to room temperature with body of heater afterwards, obtains Y 2O 3: 5%Eu 3+Hollow nano fiber; Fluorination reagent uses ammonium acid fluoride NH 4HF 2, adopt double crucible method, ammonium acid fluoride is put into monkey, the above covers carbon-point, with described Y 2O 3: 5%Eu 3+Hollow nano fiber is placed on above the carbon-point, monkey is put into larger crucible, between interior outer crucible, add an amount of ammonium acid fluoride, add that at outer crucible the crucible lid puts into tube furnace, heating rate with 2 ℃/min is warming up to 280 ℃ of insulation 2h, is warmed up to 450 ℃ of insulation 3h again, and the rate of temperature fall with 1 ℃/min is cooled to 200 ℃ at last, naturally cool to room temperature with body of heater afterwards, obtain YF 3: 5%Eu 3+Hollow nano fiber.Described YF 3: 5%Eu 3+Hollow nano fiber has good crystallinity, the d value of its diffraction maximum and relative intensity and YF 3The listed d value of PDF standard card (70-1935) consistent with relative intensity, belong to rhombic system, space group is Pnma, as shown in Figure 1.Described YF 3: 5%Eu 3+The diameter of hollow nano fiber is even, is hollow fiber-shaped, and length is greater than 20 μ m, as shown in Figure 2.With the Shapiro-Wilk method to YF 3: 5%Eu 3+The diameter of hollow nano fiber carries out normal distribution-test, under 95% confidence level, and YF 3: 5%Eu 3+The diameter of hollow nano fiber distributes and belongs to normal distribution, and diameter is 197 ± 43nm, as shown in Figure 3.YF 3: 5%Eu 3+Hollow nano fiber is comprised of Y, F and Eu element, the Au conductive layer of plated surface when Au derives from the SEM sample preparation, and C derives from organic carbonization, does not have due to the completing combustion volatilization, and Si derives from the carrier silicon chip, as shown in Figure 4.YF 3: 5%Eu 3+Nanofiber has obvious hollow-core construction, as shown in Figure 5.YF 3: 5%Eu 3+Hollow nano fiber belongs to polycrystalline structure, and electron diffraction diagram has obvious diffraction ring, as shown in Figure 6.When the monitoring wavelength is 593nm, YF 3: 5%Eu 3+The strongest excitation peak of hollow nano fiber is positioned at the 394nm place, corresponding to Eu 3+ 7F 0→ 5L 6Transition, as shown in Figure 7.Under the ultraviolet excitation of 394nm, YF 3: 5%Eu 3+Hollow nano fiber is launched the bright red that main peak is positioned at 593nm, corresponding to Eu 3+Ion 5D 0→ 7F 1, as shown in Figure 8.
Certainly; the present invention also can have other various embodiments; in the situation that does not deviate from spirit of the present invention and essence thereof; those of ordinary skill in the art work as can make 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 (2)

1. preparation method who mixes europium three yttrium fluoride hollow nano fibers, it is characterized in that, the method that adopts the single shaft electrostatic spinning technique to combine with fluorination technology, use polyvinylpyrrolidone PVP to be high polymer templates, adopt N, dinethylformamide DMF is solvent, and fluorination reagent uses ammonium acid fluoride N 4HF 2, the preparation product is europium ion-doped three yttrium fluoride YF 3: 5%Eu 3+Hollow nano fiber the steps include:
(1) preparation spinning solution
That use in yttrium source and europium source is yittrium oxide Y 2O 3With europium oxide Eu 2O 3, high polymer templates adopts polyvinylpyrrolidone PVP, and adopting DMF DMF is solvent, takes by weighing a certain amount of yittrium oxide Y 2O 3With europium oxide Eu 2O 3, Y wherein 3+And Eu 3+Mol ratio be 95: 5, namely the mole percent of europium ion is 5%, uses nitric acid HNO 3Evaporation obtains Y (NO after the dissolving 3) 3And Eu (NO 3) 3Mixed crystal adds DMF and PVP, stirs 4h in the room temperature lower magnetic force, and leaves standstill 2h, forms spinning solution, and the mass percent of each part is in this spinning solution: nitrate content 12%, PVP content 39%, solvent DMF content 49%;
(2) preparation PVP/[Y (NO 3) 3+ Eu (NO 3) 3] original composite fibre
Adopt the single shaft electrostatic spinning technique, the 10# stainless steel syringe needle after the spinning head employing is truncated, external diameter is 1.0mm, internal diameter is 0.7mm, the spinning solution for preparing is placed the liquid storage pipe of device for spinning, adopt perpendicular spray mode, spinning head is vertical with horizontal plane, the adjusting DC voltage is 16kV, spinning head is 18cm to the curing distance of receiving screen wire netting, and 18～28 ℃ of indoor temperatures, relative humidity are 40%～70%, along with the volatilization of solvent, on the receiving screen wire netting, can obtain PVP/[Y (NO 3) 3+ Eu (NO 3) 3] original composite fibre;
(3) preparation Y 2O 3: 5%Eu 3+Hollow nano fiber
With described PVP/[Y (NO 3) 3+ Eu (NO 3) 3] original composite fibre is put in the temperature programmed control stove and heat-treats, heating rate is 1 ℃/min, at 700 ℃ of constant temperature 8h, the speed with 1 ℃/min is cooled to 200 ℃ again, naturally cools to room temperature with body of heater afterwards, obtains Y 2O 3: 5%Eu 3+Hollow nano fiber;
(4) preparation YF 3: 5%Eu 3+Hollow nano fiber
Fluorination reagent uses ammonium acid fluoride NH 4HF 2, adopt double crucible method, ammonium acid fluoride is put into monkey, the above covers carbon-point, with described Y 2O 3: 5%Eu 3+Hollow nano fiber is placed on above the carbon-point, monkey is put into larger crucible, between interior outer crucible, add an amount of ammonium acid fluoride, add that at outer crucible the crucible lid puts into tube furnace, heating rate with 2 ℃/min is warming up to 280 ℃ of insulation 2h, is warmed up to 450 ℃ of insulation 3h again, and the rate of temperature fall with 1 ℃/min is cooled to 200 ℃ at last, naturally cool to room temperature with body of heater afterwards, obtain YF 3: 5%Eu 3+Hollow nano fiber, diameter are 197 ± 43nm, and length is greater than 20 μ m.
2. a kind of preparation method who mixes europium three yttrium fluoride hollow nano fibers according to claim 1 is characterized in that, high polymer templates is the polyvinylpyrrolidone PVP of molecular weight Mr=10000.
CN201210407399.6A 2012-10-24 2012-10-24 Europium doped yttrium trifluoride upconversion luminescence hollow nanometer fiber preparation method Expired - Fee Related CN102943321B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108977936A (en) * 2018-06-08 2018-12-11 长春理工大学 Coated with silica mixes the preparation method of europium gadolinium fluoride pipe sleeve linear nano fiber
CN113755969A (en) * 2020-09-18 2021-12-07 英迪那米(徐州)半导体科技有限公司 Preparation method of europium-doped yttrium trifluoride nanofiber

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6443910A (en) * 1987-08-11 1989-02-16 Toray Industries Superconductive fiber
CN101781818A (en) * 2010-02-10 2010-07-21 长春理工大学 Rare earth fluoride nano-fiber and preparation method thereof
CN101805942A (en) * 2010-03-26 2010-08-18 福建师范大学 Rare earth doped yttrium oxide fluorescent nano-fiber and preparation method thereof
CN102031586A (en) * 2010-11-19 2011-04-27 长春理工大学 Method for preparing europium-doped yttrium fluoride nano fiber/polymer composite nano fiber
CN102041583A (en) * 2010-11-19 2011-05-04 长春理工大学 Method for preparing europium and fluorine-doped yttrium oxide nanofibres
JP2011231959A (en) * 2010-04-26 2011-11-17 Japan Ultra-High Temperature Materials Research Center Air-permeable radiant heat reflector and method for producing the same
CN102031591B (en) * 2010-11-19 2012-01-18 长春理工大学 Europium-doped Y7O6F9 nano fiber and preparation method thereof
CN102618966A (en) * 2012-02-24 2012-08-01 长春理工大学 Method for preparing europium-doped sodium tetrafluoro gadolinium red luminescent nanofiber

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6443910A (en) * 1987-08-11 1989-02-16 Toray Industries Superconductive fiber
CN101781818A (en) * 2010-02-10 2010-07-21 长春理工大学 Rare earth fluoride nano-fiber and preparation method thereof
CN101805942A (en) * 2010-03-26 2010-08-18 福建师范大学 Rare earth doped yttrium oxide fluorescent nano-fiber and preparation method thereof
JP2011231959A (en) * 2010-04-26 2011-11-17 Japan Ultra-High Temperature Materials Research Center Air-permeable radiant heat reflector and method for producing the same
CN102031586A (en) * 2010-11-19 2011-04-27 长春理工大学 Method for preparing europium-doped yttrium fluoride nano fiber/polymer composite nano fiber
CN102041583A (en) * 2010-11-19 2011-05-04 长春理工大学 Method for preparing europium and fluorine-doped yttrium oxide nanofibres
CN102031591B (en) * 2010-11-19 2012-01-18 长春理工大学 Europium-doped Y7O6F9 nano fiber and preparation method thereof
CN102618966A (en) * 2012-02-24 2012-08-01 长春理工大学 Method for preparing europium-doped sodium tetrafluoro gadolinium red luminescent nanofiber

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
于伟利等: "静电纺丝技术制备PVP纳米纤维与表征", 《长春理工大学学报(自然科学版)》 *
侯远等: "YF3∶Eu(3+)纳米纤维/高分子复合纳米纤维的制备与表征", 《高等学校化学学报》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108977936A (en) * 2018-06-08 2018-12-11 长春理工大学 Coated with silica mixes the preparation method of europium gadolinium fluoride pipe sleeve linear nano fiber
CN108977936B (en) * 2018-06-08 2020-10-13 长春理工大学 Preparation method of silica-coated europium-doped gadolinium fluoride pipe sleeved linear nanofiber
CN113755969A (en) * 2020-09-18 2021-12-07 英迪那米(徐州)半导体科技有限公司 Preparation method of europium-doped yttrium trifluoride nanofiber

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