CN102392324A - Method for preparing terbium-doped yttrium oxide sulfide green fluorescent nanometer belt - Google Patents

Method for preparing terbium-doped yttrium oxide sulfide green fluorescent nanometer belt Download PDF

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Publication number
CN102392324A
CN102392324A CN2011102515155A CN201110251515A CN102392324A CN 102392324 A CN102392324 A CN 102392324A CN 2011102515155 A CN2011102515155 A CN 2011102515155A CN 201110251515 A CN201110251515 A CN 201110251515A CN 102392324 A CN102392324 A CN 102392324A
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nanometer
belt
terbium
nano belt
percent
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王进贤
董相廷
杨利颖
于文生
刘桂霞
徐佳
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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 invention relates to a method for preparing a terbium-doped yttrium oxide sulfide green fluorescent nanometer belt, and belongs to the technical field of nanometer material preparation. In the prior art, terbium ion-doped yttrium oxide sulfide nanometer granules, nanometer tubes, nanometer wires, nanometer rods, nanometer flowers and polyhedral nanometer crystals are prepared. In the method, an Y2O2S:5 percent Tb<3+> nanometer belt is prepared by a method of combining an electrostatic spinning technology and a vulcanizing technology. The method comprises the following steps of: (1) preparing an Y2O3:5 percent Tb<3+> nanometer belt, namely preparing polyvinyl pyrrolidone(PVP)/[Y(NO3)3 and Tb(NO3)3] composite nanometer belt by using the electrostatic spinning technology, and performing heat treatment to obtain the Y2O3:5 percent Tb<3+> nanometer belt; and (2) preparing the Y2O2S:5 percent Tb<3+> nanometer belt, namely sulfidizing the Y2O3:5 percent Tb<3+> nanometer belt by using sulfur by using a double-crucible method to obtain a pure-phase Y2O2S:5 percent Tb<3+> nanometer belt. The Y2O2S:5 percent Tb<3+> nanometer belt has a good crystal form, the belt width is between 4.6 and 5.6 micrometers, the thickness is 110 nanometers, and the length is more than 100 micrometers. The method is simple and feasible, and is suitable for volume production. In addition, the terbium ion-doped yttrium oxide sulfide nanometer belt is a novel significant green fluorescent nanometer material and has a wide application prospect.

Description

The method of terbium yttrium oxysulfide green fluorescence nano belt is mixed in a kind of preparation
Technical field
The present invention relates to the nano material preparation technical field, relate to the method that terbium yttrium oxysulfide green fluorescence nano belt is mixed in a kind of preparation specifically.
Background technology
The preparation of inorganic matter nano belt and property research are one of forward position focus of subject researchs such as material science, Condensed Matter Physics, chemistry at present.Nano belt is a kind of nano material that is banded structure of synthesizing with manual method, and its cross section is a rectangular configuration, and its thickness is in nanometer scale, and width can reach micron order, and length can reach the hundreds of micron, even several millimeters.Nano belt is owing to the performances such as novel structure and unique light, electricity, magnetic that it is different from pipe, wire material cause people's great attention.
Yttrium oxysulfide Y 2O 2S has that chemical stability is good, water insoluble, fusing point is high, non-oxidizability is strong and advantage such as efficiency of light absorption and energy transfer efficiency be high, nontoxic, becomes the important matrix of rare-earth ion activated luminescent material.Terbium ion doping yttrium oxysulfide Y 2O 2S:Tb 3+It is the green fluorescent material of one type of important function admirable, extensive use.Y 2O 2S:Tb 3+The research of nano material has caused showing great attention to of people.Adopt hydro-thermal and solvent-thermal method, solid reaction process, firing method, microwave method etc., prepared Y 2O 2S:Tb 3+Nano particle, nanotube, nano wire, nanometer rods, nanometer is colored, polyhedron is nanocrystalline.Y 2O 2S:Tb 3+Nano belt is a kind of important novel green nano luminescent material, will obtain important application in fields such as luminous and demonstration, false proof, biomarker, nano-devices, has broad application prospects.At present, do not see that Y is arranged 2O 2S:Tb 3+The relevant report of nano belt.
The patent No. is the technical scheme that 1975504 United States Patent (USP) discloses a relevant electrospinning process (electrospinning); This 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 mainly is used for preparing high polymer nanometer fiber; It is characterized in that making charged Polymer Solution or melt in electrostatic field, to receive the traction of electrostatic force and spray, invest the receiving screen on opposite, thereby realize wire drawing by nozzle; Then; Solvent evaporation at normal temperatures, perhaps melt is cooled to normal temperature and solidifies, and 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.Existing people utilizes electrostatic spinning technique successfully to prepare high molecular nanometer band (Materials Letters, 2007,61:2325-2328; Journal of Polymer Science:Part B:Polymer Physics, 2001,39:2598-2606).Someone utilizes the organic compound of tin, uses electrostatic spinning technique to combine with the metallo-organic compound decomposition technique and has prepared porous SnO 2Nano belt (Nanotechnology, 2007,18:435704); Someone utilizes electrostatic spinning technique at first to prepare PEO/ stannic hydroxide composite Nano band, and its roasting has been obtained porous SnO 2Nano belt (J.Am.Ceram.Soc., 2008,91 (1): 257-262).Employing electrostatic spinning techniques such as Dong Xiangting prepared rare earth fluoride nanobelt (Chinese invention patent, application number: 201010108039.7), titanium dioxide nano-belts (Chinese invention patent, ZL200810050948.2) and Gd 3Ga 5O 12: Eu 3+Porous nano-belt (SCI, 2010,31 (7), 1291-1296).At present, do not see Y 2O 2S:Tb 3+The report of nano belt.
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 all have material impact to the pattern and the size of final products.The present invention adopts electrostatic spinning technique earlier, with yittrium oxide Y 2O 3With terbium oxide Tb 4O 7Be raw material,, obtain Y (NO with evaporating behind the dilute nitric acid dissolution 3) 3And Tb (NO 3) 3Mixed crystal adds solvent N, and dinethylformamide DMF and high polymer templates polyvinylpyrrolidone PVP obtain carrying out electrostatic spinning behind the spinning solution, under the experiment condition of the best, prepare PVP/ [Y (NO 3) 3+ Tb (NO 3) 3] original nano belt, it is heat-treated in air, obtain Y 2O 3: Tb 3+Nano belt adopts double crucible method, is that vulcanizing agent vulcanizes with sulphur, has prepared the Y of the pure phase of novel structure 2O 2S:Tb 3+Nano belt.
Summary of the invention
Preparation Y in background technology 2O 2S:Tb 3+Nano particle, nanotube, nano wire, nanometer rods, nanometer is colored, polyhedron is nanocrystalline, has adopted hydro-thermal and solvent-thermal method, solid reaction process, firing method, microwave method etc.Use electrostatic spinning technique in the background technology has prepared metal oxide, composite oxide of metal nanofiber, high molecular nanometer band, SnO 2Nano belt, TiO 2Nano belt, Gd 3Ga 5O 12: Eu 3+Porous nano-belt and rare earth fluoride nanobelt.Employed raw material, template and solvent are all different with method of the present invention.For a kind of novel green fluorescence nano carrying material is provided in the nano belt field, we combine electrostatic spinning technique with sulfurization technology, invented Y 2O 2S:Tb 3+The preparation method of nano belt.
The present invention is achieved in that and at first prepares the spinning solution with certain viscosity that is used 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+ Tb (NO 3) 3] original nano belt, it is heat-treated in air, obtain Y 2O 3: Tb 3+Nano belt adopts double crucible method, is that vulcanizing agent vulcanizes with sulphur, has prepared the Y of the pure phase of novel structure 2O 2S:Tb 3+Nano belt.In the present invention, the mole percent of the terbium ion of doping is 5%, is labeled as Y 2O 2S:5%Tb 3+, i.e. that the present invention is prepared is Y 2O 2S:5%Tb 3+Nano belt.The steps include:
(1) preparation Y 2O 3: 5%Tb 3+Nano belt
That use in yttrium source and terbium source is yittrium oxide Y 2O 3With terbium oxide Tb 4O 7, high polymer templates adopts polyvinylpyrrolidone PVP, and molecular weight is 90000, adopts N, and dinethylformamide DMF is a solvent.Take by weighing a certain amount of yittrium oxide and terbium oxide, the mol ratio of ruthenium ion and terbium ion is 19: 1, and promptly the mole percent of terbium ion is 5%, with evaporating behind the dilute nitric acid dissolution, obtains Y (NO 3) 3And Tb (NO 3) 3Mixed crystal adds an amount of DMF solvent, takes by weighing a certain amount of PVP again and joins in the above-mentioned solution, stirs 4h in the room temperature lower magnetic force, and leaves standstill 2h, promptly forms spinning solution.The mass percent of this each part of spinning solution is: rare earth nitrades content 10%, PVP content 20%, solvent DMF content 70%.The spinning solution for preparing is added in the liquid storage pipe of device for spinning, carry out electrostatic spinning, shower nozzle internal diameter 0.7mm adopts perpendicular spray mode; Shower nozzle is vertical with horizontal plane, applies the DC voltage of 8kV, solidifies apart from 15cm; 15～25 ℃ of room temperatures, relative humidity is 60%～80%, obtains PVP/ [Y (NO 3) 3+ Tb (NO 3) 3] the composite Nano band.With described PVP/ [Y (NO 3) 3+ Tb (NO 3) 3] the composite Nano band 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%Tb 3+Nano belt.
(2) preparation Y 2O 2S:5%Tb 3+Nano belt
Sulfuration reagent uses sulphur, adopts double crucible method, and sulphur is put into monkey, covers carbon dust above, with described Y 2O 3: 5%Eu 3+Nano belt is placed on above the carbon dust, and monkey is put into bigger crucible, between interior outer crucible, adds excessive sulphur; Add that on outer crucible the crucible lid puts into tube furnace, when room temperature, feed argon gas 40min, discharge the air in the boiler tube; With the heating rate to 800 of 5 ℃/min ℃, insulation 4h reduces to 200 ℃ with the rate of temperature fall of 5 ℃/min again; Naturally cool to room temperature afterwards, obtain Y 2O 2S:5%Tb 3+Nano belt, bandwidth are 4.6～5.6 μ m, and thickness is 110nm, and length is greater than 100 μ m.
At the Y described in the said process 2O 2S:5%Tb 3+Nano belt has good crystal formation, and bandwidth is 4.6～5.6 μ m, and thickness is 110nm, and length has realized goal of the invention greater than 100 μ m.
Description of drawings
Fig. 1 is Y 2O 2S:5%Tb 3+The XRD spectra of nano belt;
Fig. 2 is Y 2O 2S:5%Tb 3+The SEM photo of nano belt, this figure double as Figure of abstract;
Fig. 3 is Y 2O 2S:5%Tb 3+The EDS spectrogram of nano belt;
Fig. 4 is Y 2O 2S:5%Tb 3+The exciting light spectrogram of nano belt;
Fig. 5 is Y 2O 2S:5%Tb 3+The emission spectrum figure of nano belt.
The specific embodiment
The yittrium oxide Y that the present invention selected for use 2O 3With terbium oxide Tb 4O 7Purity be 99.99%, polyvinylpyrrolidone PVP, molecular weight 90000, N, dinethylformamide DMF, sulphur, carbon dust and nitric acid are 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 and terbium oxide, the mol ratio of ruthenium ion and terbium ion is 19: 1, and promptly the mole percent of terbium ion is 5%, with evaporating behind the dilute nitric acid dissolution, obtains Y (NO 3) 3And Tb (NO 3) 3Mixed crystal adds an amount of DMF solvent, takes by weighing a certain amount of PVP again and joins in the above-mentioned solution, stirs 4h in the room temperature lower magnetic force, and leaves standstill 2h, promptly forms spinning solution.The mass percent of this each part of spinning solution is: rare earth nitrades content 10%, PVP content 20%, solvent DMF content 70%.The spinning solution for preparing is added in the liquid storage pipe of device for spinning, carry out electrostatic spinning, shower nozzle internal diameter 0.7mm adopts perpendicular spray mode; Shower nozzle is vertical with horizontal plane, applies the DC voltage of 8kV, solidifies apart from 15cm; 15～25 ℃ of room temperatures, relative humidity is 60%～80%, obtains PVP/ [Y (NO 3) 3+ Tb (NO 3) 3] the composite Nano band.With described PVP/ [Y (NO 3) 3+ Tb (NO 3) 3] the composite Nano band 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%Tb 3+Nano belt.Sulfuration reagent uses sulphur, adopts double crucible method, and sulphur is put into monkey, covers carbon dust above, with described Y 2O 3: 5%Eu 3+Nano belt is placed on above the carbon dust, and monkey is put into bigger crucible, between interior outer crucible, adds excessive sulphur; Add that on outer crucible the crucible lid puts into tube furnace, when room temperature, feed argon gas 40min, discharge the air in the boiler tube; With the heating rate to 800 of 5 ℃/min ℃, insulation 4h reduces to 200 ℃ with the rate of temperature fall of 5 ℃/min again; Naturally cool to room temperature afterwards, obtain Y 2O 2S:5%Tb 3+Nano belt.Described Y 2O 2S:5%Tb 3+Nano belt has good crystallinity, the d value of its diffraction maximum and relative intensity and Y 2O 2The listed d value of the PDF standard card (24-1424) of S is consistent with relative intensity, belongs to hexagonal crystal system, sees shown in Figure 1.Described Y 2O 2S:5%Tb 3+The bandwidth of nano belt is 4.6～5.6 μ m, and thickness is 110nm, and length is seen shown in Figure 2 greater than 100 μ m.Y 2O 2S:5%Tb 3+Nano belt is formed (the Au conductive layer of surface plating when Au comes from the SEM sample preparation) by Y, O, S and Tb element, sees shown in Figure 3.When the monitoring wavelength is 546nm, Y 2O 2S:5%Tb 3+The excitation spectrum highest peak of nano belt is positioned at the 287nm place, belongs to Tb 3+4f → 5d transition, see shown in Figure 4.Under the ultraviolet excitation of 287nm, Y 2O 2S:5%Tb 3+Nano belt is launched the bright green glow that main peak is positioned at 546nm, and it is corresponding to Tb 3+Ion 5D 4→ 7F 5Transition is seen shown in Figure 5.
Certainly; The present invention also can have other various embodiments; Under 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 various corresponding changes and distortion according to the present invention, but these corresponding changes and distortion all should belong to the protection domain of the appended claim of the present invention.

Claims (5)

1. one kind prepares the method for mixing terbium yttrium oxysulfide green fluorescence nano belt; It is characterized in that the method that adopts electrostatic spinning technique to combine with sulfurization technology uses polyvinylpyrrolidone PVP to be high polymer templates; Adopt N; Dinethylformamide DMF is a solvent, and sulfuration reagent uses sulphur, and the preparation product is terbium ion doping yttrium oxysulfide Y 2O 2S:5%Tb 3+Nano belt the steps include:
(1) preparation Y 2O 3: 5%Tb 3+Nano belt
Take by weighing a certain amount of yittrium oxide and terbium oxide, the mol ratio of ruthenium ion and terbium ion is 19: 1, and promptly the mole percent of terbium ion is 5%, with evaporating behind the dilute nitric acid dissolution, obtains Y (NO 3) 3And Tb (NO 3) 3Mixed crystal adds an amount of DMF solvent, takes by weighing a certain amount of PVP again and joins in the above-mentioned solution, stirs 4h in the room temperature lower magnetic force; And leave standstill 2h, and promptly forming spinning solution, the mass percent of this each part of spinning solution is: rare earth nitrades content 10%, PVP content 20%; Solvent DMF content 70% adds the spinning solution for preparing in the liquid storage pipe of device for spinning, carries out electrostatic spinning, shower nozzle internal diameter 0.7mm; Adopt perpendicular spray mode, shower nozzle is vertical with horizontal plane, applies the DC voltage of 8kV, solidifies apart from 15cm; 15～25 ℃ of room temperatures, relative humidity is 60%～80%, obtains PVP/ [Y (NO 3) 3+ Tb (NO 3) 3] the composite Nano band, with described PVP/ [Y (NO 3) 3+ Tb (NO 3) 3] the composite Nano band 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%Tb 3+Nano belt;
(2) preparation Y 2O 2S:5%Tb 3+Nano belt
Sulfuration reagent uses sulphur, adopts double crucible method, and sulphur is put into monkey, covers carbon dust above, with described Y 2O 3: 5%Eu 3+Nano belt is placed on above the carbon dust, and monkey is put into bigger crucible, between interior outer crucible, adds excessive sulphur; Add that on outer crucible the crucible lid puts into tube furnace, when room temperature, feed argon gas 40min, discharge the air in the boiler tube; With the heating rate to 800 of 5 ℃/min ℃, insulation 4h reduces to 200 ℃ with the rate of temperature fall of 5 ℃/min again; Naturally cool to room temperature afterwards, obtain Y 2O 2S:5%Tb 3+Nano belt, bandwidth are 4.6～5.6 μ m, and thickness is 110nm, and length is greater than 100 μ m.
2. the method for terbium yttrium oxysulfide green fluorescence nano belt is mixed in a kind of preparation according to claim 1, it is characterized in that, that use in yttrium source and terbium source is yittrium oxide Y 2O 3With terbium oxide Tb 4O 7
3. the method for terbium yttrium oxysulfide green fluorescence nano belt is mixed in a kind of preparation according to claim 1, it is characterized in that, high polymer templates is the polyvinylpyrrolidone of molecular weight Mr=90000.
4. the method for terbium yttrium oxysulfide green fluorescence nano belt is mixed in a kind of preparation according to claim 1, it is characterized in that, sulfuration reagent uses sulphur.
5. the method for terbium yttrium oxysulfide green fluorescence nano belt is mixed in a kind of preparation according to claim 1, it is characterized in that the Tb of doping 3+Mole percent is 5%.
CN2011102515155A 2011-08-30 2011-08-30 Method for preparing terbium-doped yttrium oxide sulfide green fluorescent nanometer belt Pending CN102392324A (en)

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* Cited by examiner, † Cited by third party
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CN104774616A (en) * 2015-04-20 2015-07-15 黑龙江大学 Preparation method of Y2O3/Y2O2S: Er<3+ > composite nanorod

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CN104774616A (en) * 2015-04-20 2015-07-15 黑龙江大学 Preparation method of Y2O3/Y2O2S: Er<3+ > composite nanorod

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Application publication date: 20120328