CN109371502B - Preparation method and application of cubic pyrochlore phase nanofiber based on electrostatic spinning method - Google Patents
Preparation method and application of cubic pyrochlore phase nanofiber based on electrostatic spinning method Download PDFInfo
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Abstract
The invention discloses a preparation method of cubic pyrochlore phase nanofibers based on an electrostatic spinning method and application thereof. The doping process of other rare earth ions and the traditional double doping or multi-doping process are avoided, the preparation method is simple and easy to implement, the repeatability is good, and the requirement of batch production can be met. The related green up-conversion luminescent matrix is oxide, has good chemical stability, no toxicity and low price, and can easily meet the requirement of industrial production. The prepared one-dimensional pure pyrochlore phase nano material is expected to play an important role in the fields of display, anti-counterfeiting, biological detection, infrared sensors, solar photovoltaic devices and the like.
Description
Technical Field
The present invention belongs to a rare earth ternary Bi2Ti2O7: the technical field of Er compound one-dimensional nano material preparation and luminescence, in particular to a method for preparing cubic pyrochlore phase nano fibers based on an electrostatic spinning method and application thereof.
Background
The up-conversion luminescent material is a novel optical functional material capable of converting infrared light invisible to naked eyes into visible light, and is also called a multi-photon material. The method has very important application value in the fields of anti-counterfeiting, display, biological detection, imaging, photo-thermal treatment of diseases and the like. The main up-conversion luminescent materials at present can be classified into rare earth fluoride (NaYF) according to the matrix4Etc.), rare earth oxyhalides (represented by YOCl)3Etc.), rare earth oxysulfides (represented by La)2O2S、Y2O2S, etc., as representative), rare earth oxides and composite oxides (represented by Y)2O3Etc. as representative). Among them, the fluoride up-conversion luminescent material doped with rare earth has been widely studied because of its small phonon energy and small non-radiative relaxation. In which hexagonal phase NaYF4The matrix material is the most studied compound of rare earth fluorides due to its high luminous efficiency, but it must pass through the double rare earth elementsAnd doping multiple rare earth elements to realize the excitation of the converted visible light such as red light, green light, blue light and the like.
Bi2Ti2O7: the Er ternary compound has a cubic pyrochlore structure, belongs to the Fd-3m (227) space point group, and has a lattice constant of 10.359 angstroms. So far, Bi has been concerned2Ti2O7The matrix reports mainly include the following aspects: from the application point of view, Bi2Ti2O7The material can act as a photocatalyst; it has very high dielectric constant at the same time, is suitable for being used as the storage medium in the Dynamic Random Access Memory (DRAM); relatively few reports are made on the study of the optical properties. However, no Bi has been added so far2Ti2O7It is a report of the research of the upconversion performance of a matrix through single rare earth doping. The oxide has the advantages of good chemical stability, high mechanical strength, no toxicity and the like. Thus, the field of application of oxides is much broader with respect to fluoride systems. Therefore, it is necessary to research an oxide-based up-conversion material. Meanwhile, the one-dimensional nano material structure has a large specific surface area and a special one-dimensional structure, so that the transmission of photons along the one-dimensional direction is met, the scattering of a disordered interface to the photons is avoided, and the better luminous performance is obtained.
From the production process, for Bi2Ti2O7The materials mainly focus on sol-gel methods, hydrothermal methods, solid-phase reaction methods, various deposition methods (such as laser pulse deposition methods and the like); one-dimensional Bi obtained by electrostatic spinning method2Ti2O7Nanofibers are a major challenge.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a pyrochlore phase Bi based on an electrostatic spinning method, aiming at the defects in the prior art2Ti2O7: the preparation method of the Er nanofiber and the up-conversion luminescence are used for obtaining the one-dimensional nano material precursor by an electrostatic spinning method. Obtaining pure cubic pyrochlore phase Bi by subsequent heat treatment2Ti2O7: the Er ternary compound is used for the first time to obtain green luminescence with upward conversion which can be observed by naked eyes under the condition that no other rare earth elements are doped as a sensitizing agent and an oxide is used as a matrix.
The invention adopts the following technical scheme:
a preparation method of cubic pyrochlore phase nanofibers based on an electrostatic spinning method is characterized in that dimethylformamide is used as a solvent, polyvinylpyrrolidone is added to prepare an electrostatic spinning precursor solution, droplets form Taylor cones under an electrostatic field, a one-dimensional nanomaterial is prepared by the electrostatic spinning method, and then organic matter residues are removed by heating, heat preservation and cooling to prepare the cubic pyrochlore phase Bi2Ti2O7: and (4) Er nano material.
Specifically, the steps for preparing the electrostatic spinning precursor solution are as follows:
s1, mixing and stirring acetic acid and dimethylformamide to prepare a solution A;
s2, stirring the solution A prepared in the step S1 and adding tetrabutyl titanate to prepare a solution B;
s3, stirring the solution B prepared in the step S2 and adding erbium nitrate to prepare a solution C;
s4, adding bismuth nitrate into the solution C prepared in the step S3 to prepare a solution D;
s5, adding polyvinylpyrrolidone into the solution D prepared in the step S4, and stirring to prepare an electrostatic spinning precursor solution.
Further, in step S1, the mass ratio of acetic acid to dimethylformamide is (0.3 to 0.6): 1.
further, in step S2, the mass ratio of the solution a to tetrabutyl titanate is (1.5-2): 1.
further, in step S3, the mass ratio of the solution B to the nitric acid lugs is (14 to 32): 1.
further, in step S4, the mass ratio of the solution C to the bismuth nitrate is (15-34): 1.
further, in step S5, polyvinylpyrrolidone with a mass fraction of 5-20% is added.
Specifically, 18-25 kV high-voltage electricity is applied, the speed of a micro-flow actuator is controlled to be 10-20 mu l/m, and the electrostatic spinning precursor liquid is sprayed onto a collector.
Specifically, the organic residue removal specifically comprises: the heating rate is 4-10 ℃/min, the annealing treatment temperature is 600-800 ℃, the treatment time is 1-3 hours, and then the temperature is naturally cooled to the room temperature.
Pyrochlore phase Bi prepared by method for preparing cubic pyrochlore phase nanofibers based on electrostatic spinning method2Ti2O7: the application of the Er nano material in up-conversion green luminescent nano material is applicable to display devices, anti-counterfeiting devices, biological detection devices, infrared sensors and solar photovoltaic devices.
Compared with the prior art, the invention has at least the following beneficial effects:
the invention relates to a method for preparing pyrochlore phase Bi by using an electrostatic spinning method2Ti2O7: the method of Er nano material includes using dimethyl formamide DMF as solvent, adding proper amount of polyvinylpyrrolidone PVP, dropping in electrostatic field to form Taylor cone, preparing one-dimensional nano material in electrostatic spinning process under the action of liquid surface tension and electric field force, heating, maintaining temperature, cooling and eliminating organic matter to obtain pure cubic pyrochlore phase Bi2Ti2O7: the Er one-dimensional nano material realizes visible light luminescence under near infrared excitation, and is a novel single-doped up-conversion luminescence nano fiber.
Further, in order to meet the requirement of industrial production, acetic acid and DMF are used as solvents, the acetic acid can inhibit the hydrolysis of a titanium source, and the DMF is used as the solvent to fully mix solutes, so that the purpose of accurately controlling the stoichiometric ratio is achieved, and the solution A is obtained; adding a certain amount of tetrabutyl titanate into the solution A and fully dissolving the tetrabutyl titanate so as to introduce a titanium source to obtain a solution B; adding a certain amount of erbium nitrate into the solution B and fully stirring to introduce an erbium source so as to enable the erbium source and tetrabutyl titanate to be mixed at an atomic level and obtain a solution C; adding quantitative bismuth nitrate into the solution C, and fully stirring to introduce a bismuth source and obtain a solution D; and adding a proper amount of PVP (polyvinyl pyrrolidone) to increase the viscosity of the solution and establish the basis for electrostatic spinning.
Further, a high voltage power is applied in order to form a taylor cone at the needle.
Further, the nanowires on the collector are annealed in order to obtain pyrochlore phase Bi of high crystallinity2Ti2O7: and (4) Er nano material.
The invention also discloses an up-conversion green luminescent nano material, which can be obtained without any sensitizer and is expected to play an important role in the fields of display, anti-counterfeiting, biological detection, immunoassay, solar photovoltaic device preparation and the like.
In conclusion, the preparation method is simple and easy to implement, has good repeatability, can meet the requirement of mass production, avoids the doping process of other rare earth ions, and simplifies the traditional double-doping or multi-doping process.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 shows Bi synthesized in example 1 of the present invention2Ti2O7: scanning Electron Microscopy (SEM) images of Er nanomaterials;
FIG. 2 shows Bi synthesized in example 2 of the present invention2Ti2O7: an up-conversion luminescence performance graph of the Er nano-material;
FIG. 3 shows Bi synthesized in example 3 of the present invention2Ti2O7: the X-ray diffraction spectrum of the Er nano material;
FIG. 4 shows Bi synthesized in example 4 of the present invention2Ti2O7: the X-ray diffraction spectrum of the Er nano material;
FIG. 5 shows Bi synthesized in example 5 of the present invention2Ti2O7: the X-ray diffraction spectrum of the Er nano-material.
Detailed Description
The invention provides a cubic pyrochlore phase nanofiber based on an electrostatic spinning methodA process for preparing the crystal of pure cubic pyrochlore phase Bi includes such steps as dissolving dimethyl formamide DMF in PVP, dropping in electrostatic field to form Taylor cone, applying the surface tension of liquid and the action of electric field to obtain one-dimensional nano material, heating, holding the temp and cooling2Ti2O7: and Er one-dimensional nano material. The excitation by a near infrared light source (for example 980 nm) firstly obtains green luminescence with an upper conversion which can be observed by naked eyes under the condition of no doping of other rare earth elements and taking oxide as a matrix.
The invention relates to a method for preparing cubic pyrochlore phase nanofibers based on an electrostatic spinning method, which comprises the following steps:
s1, mixing DMF and acetic acid according to the mass ratio of 1 (0.3-0.6) and stirring to obtain a solution A;
s2, in the process of continuously stirring, mixing the solution A with the solution A in a mass ratio of 1: (1.5-2) adding tetrabutyl titanate into the solution A to obtain a solution B;
s3, the mass ratio of the solution B to the solution B is 1: (14-32) adding erbium nitrate into the solution B to obtain a solution C;
s4, the mass ratio of the solution C to the solution C is 1: (15-34) adding bismuth nitrate into the solution C to obtain a solution D;
s5, adding 5-10% (mass fraction) of PVP into the solution C and stirring to prepare an electrostatic spinning precursor solution;
s6, under the condition that 18-25 kV high-voltage power supply is applied, spraying the precursor liquid onto a collector through a micro-flow processer at a control speed of 10-20 mu l/m to carry out electrostatic spinning;
s7, after the electrostatic spinning is finished, annealing the nano material on the collector to obtain pyrochlore phase Bi with high crystallization performance2Ti2O7: and (4) Er nano material.
The heating rate is 2-10 ℃/min, the annealing temperature is 600-800 ℃, the treatment time is 1-3 hours, and then the temperature is naturally cooled to the room temperature.
Through the illumination of a near-infrared light source (980 nm), green luminescence which can be seen by naked eyes in a visible wave band range is excited, and the up-conversion green luminescent nano material which is not doped with other rare earth elements and takes oxide as a matrix is obtained.
The invention combines the electrostatic spinning method to obtain one-dimensional Bi2Ti2O7: the Er nano material and the realization of the up-conversion process by singly doping the Er have very important significance and practical value
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Mixing DMF and acetic acid according to the mass ratio of 0.3:1, and stirring by magnetic force to form a transparent solution; then 0.8ml of tetrabutyl titanate is added and dissolved sufficiently by stirring; 0.11g of erbium nitrate was added with rapid stirring; and after the precursor solution is fully dissolved, adding 1.05g of bismuth nitrate, fully stirring to dissolve the bismuth nitrate, finally adding 5% of PVP (polyvinyl pyrrolidone) by mass percent, and magnetically stirring to obtain the electrostatic spinning precursor solution. Under the conditions of controlling the voltage to be 18KV and the flow rate to be 10 mul/m, a large amount of nano materials appear on the collector, after the electrostatic spinning is finished, the nano materials on the collector are transferred into a muffle furnace and are heated to 600 ℃ at the speed of 4 ℃/min for heat preservation for 1 hour, and then pyrochlore phase Bi with high crystallization performance can be obtained2Ti2O7: and (4) Er nano material.
FIG. 1 shows the Er obtained2Ti2O7Scanning Electron Microscopy (SEM) images of the nano materials show that the diameters of the nano materials are distributed in the range of 200-500 nanometers.
Example 2
Mixing DMF and acetic acid according to the mass ratio of 0.4:1, and stirring by magnetic force to form a transparent solution; then 0.81ml of tetrabutyl titanate is added and dissolved sufficiently by stirring; 0.13g of erbium nitrate was added with rapid stirring; and after the precursor solution is fully dissolved, adding 1.02g of bismuth nitrate, fully stirring to dissolve the bismuth nitrate, finally adding PVP with the mass fraction of 6%, and magnetically stirring to obtain the electrostatic spinning precursor solution. Under the conditions of controlling the voltage to be 20KV and the flow rate to be 12 mul/m, a large amount of nano materials appear on the collector, after the electrostatic spinning is finished, the nano materials on the collector are transferred into a muffle furnace and are heated to 650 ℃ at the speed of 6 ℃/min for heat preservation for 1.5 hours, and pyrochlore phase Bi with high crystallization performance can be obtained2Ti2O7: and (4) Er nano material.
FIG. 2 shows that the up-conversion luminescence performance obtained by using a 980nm laser as an excitation source has a test wavelength range of 200-900 nm and an integration time of 30 ms.
Example 3
Mixing DMF and acetic acid according to the mass ratio of 0.4:1, and stirring by magnetic force to form a transparent solution; then 0.83ml of tetrabutyl titanate is added and dissolved sufficiently by stirring; 0.13g of erbium nitrate was added with rapid stirring; and after the precursor solution is fully dissolved, adding 1.02g of bismuth nitrate, fully stirring to dissolve the bismuth nitrate, finally adding 8% of PVP (polyvinyl pyrrolidone) by mass percent, and magnetically stirring to obtain the electrostatic spinning precursor solution. Under the conditions that the voltage is controlled to be 22KV and the flow rate is 15 mu l/m, a large amount of nano materials appear on the collector, after the electrostatic spinning is finished, the nano materials on the collector are transferred into a muffle furnace and are heated to 750 ℃ at the speed of 8 ℃/min for heat preservation for 2 hours, and pyrochlore phase Bi with high crystallization performance can be obtained2Ti2O7: and (4) Er nano material.
FIG. 3 shows the X-ray diffraction pattern of the obtained nano material and the X-ray diffraction pattern of the obtained powderScanning at 10-80 deg.c with a ray diffractometer to obtain powder sample with polycrystalline diffraction characteristic, all diffraction peaks and Er2Ti2O7The standard card (PDF #97-009-2Ti2O7Pyrochlore phase. Wherein the 2 theta angle is the strongest peak at 29.854 DEG, corresponding to Bi2Ti2O7The (222) crystal face of the standard card.
Example 4
Mixing DMF and acetic acid according to the mass ratio of 0.5:1, and stirring by magnetic force to form a transparent solution; then 0.84ml of tetrabutyl titanate is added and dissolved sufficiently by stirring; 0.18g of erbium nitrate was added with rapid stirring; and after the precursor solution is fully dissolved, adding 0.97g of bismuth nitrate, fully stirring to dissolve the bismuth nitrate, finally adding 9% of PVP (polyvinyl pyrrolidone) by mass fraction, and magnetically stirring to obtain the electrostatic spinning precursor solution. Under the conditions that the voltage is controlled to be 24KV and the flow rate is 18 mul/m, a large amount of nano materials appear on the collector, after the electrostatic spinning is finished, the nano materials on the collector are transferred into a muffle furnace and are heated to 800 ℃ at the speed of 8 ℃/min for heat preservation for 2 hours, and then pyrochlore phase Bi with high crystallization performance can be obtained2Ti2O7: and (4) Er nano material.
Fig. 4 gives the obtained nanomaterial using X-ray diffraction pattern: all diffraction peaks and Bi2Ti2O7The standard card (PDF #97-009-2Ti2O7Structure of cubic pyrochlore phase.
Example 5
Mixing DMF and acetic acid according to the mass ratio of 0.6:1, and stirring by magnetic force to form a transparent solution; then 0.85ml of tetrabutyl titanate is added and dissolved sufficiently by stirring; 0.15g of erbium nitrate was added with rapid stirring; and after the precursor solution is fully dissolved, adding 0.99g of bismuth nitrate, fully stirring to dissolve the bismuth nitrate, finally adding 10% of PVP (polyvinyl pyrrolidone) by mass percent, and magnetically stirring to obtain the electrostatic spinning precursor solution. Under the conditions of controlling voltage of 25KV and flow rate of 20 mul/m, a large amount of nano material appears on the collector,after the electrostatic spinning is finished, the nano material on the collector is transferred into a muffle furnace and heated to 800 ℃ at the speed of 10 ℃/min for 3 hours, and pyrochlore phase Bi with high crystallization performance can be obtained2Ti2O7: and (4) Er nano material.
Fig. 5 gives the obtained nanomaterial using X-ray diffraction pattern: all diffraction peaks and Bi2Ti2O7The standard card (PDF #97-009-2Ti2O7Structure of cubic pyrochlore phase.
The invention avoids the doping process of other rare earth ions and simplifies the traditional double doping or multi-doping process because the use of a sensitizing agent is not involved, and the adopted one-dimensional nano material preparation method is simple and easy to implement, has good repeatability and can meet the requirement of batch production. The related green up-conversion luminescence can be obtained without any sensitizer, and the adopted matrix is oxide with good chemical stability. Has no toxicity and low price and can easily meet the requirement of industrial production.
Bi of one-dimensional pure pyrochlore phase prepared by the preparation method of the invention2Ti2O7: the Er nano material is expected to play an important role in the fields of display, anti-counterfeiting, biological detection, infrared sensors, solar photovoltaic devices and the like.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (4)
1. A method for preparing cubic pyrochlore phase nanofibers based on an electrostatic spinning method is characterized in that dimethylformamide is used as a solvent, polyvinylpyrrolidone is added to prepare an electrostatic spinning precursor solution, droplets form Taylor cones under an electrostatic field, a one-dimensional nanomaterial is prepared by the electrostatic spinning method, and then organic matter residues are removed by heating, heat preservation and cooling to prepare the cubic pyrochlore phase nanofibersBi2Ti2O7: an Er nano material;
the steps for preparing the electrostatic spinning precursor solution are as follows:
s1, mixing the following components in percentage by mass (0.3-0.6): 1, mixing acetic acid and dimethyl formamide to prepare a solution A;
s2, stirring the solution A prepared in the step S1, and adding tetrabutyl titanate to prepare a solution B, wherein the mass ratio of the solution A to the tetrabutyl titanate is (1.5-2): 1;
s3, stirring the solution B prepared in the step S2, and adding erbium nitrate to prepare a solution C, wherein the mass ratio of the solution B to the nitric acid lugs is (14-32): 1;
s4, adding bismuth nitrate into the solution C prepared in the step S3 to prepare a solution D, wherein the mass ratio of the solution C to the bismuth nitrate is (15-34): 1;
s5, adding 5-20% by mass of polyvinylpyrrolidone into the solution D prepared in the step S4, and stirring to prepare an electrostatic spinning precursor solution.
2. The method for preparing the cubic pyrochlore phase nanofibers based on the electrospinning method according to claim 1, wherein 18-25 kV high voltage is applied, the rate of a micro-flow actuator is controlled to be 10-20 μ l/m, and the electrospinning precursor liquid is sprayed onto a collector.
3. The method for preparing the cubic pyrochlore phase nanofibers according to claim 1, wherein the organic residue removal is specifically: the heating rate is 4-10 ℃/min, the annealing treatment temperature is 600-800 ℃, the treatment time is 1-3 hours, and then the temperature is naturally cooled to the room temperature.
4. The pyrochlore phase Bi prepared by the method for preparing cubic pyrochlore phase nanofibers according to the electrospinning method of claim 12Ti2O7: application of Er nano material in up-conversion green luminescent nano material, and the up-conversion green luminescent nano material is suitable for display devices, anti-counterfeiting devices, biological detection devices, infrared sensors and solar photovoltaic devices。
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