CN101235558A - Method for preparing perovskite-type rare earth composite oxide porous hollow nano fiber - Google Patents
Method for preparing perovskite-type rare earth composite oxide porous hollow nano fiber Download PDFInfo
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- CN101235558A CN101235558A CNA2008100504686A CN200810050468A CN101235558A CN 101235558 A CN101235558 A CN 101235558A CN A2008100504686 A CNA2008100504686 A CN A2008100504686A CN 200810050468 A CN200810050468 A CN 200810050468A CN 101235558 A CN101235558 A CN 101235558A
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Abstract
A method for preparing perovskite type rare-earth compound oxide perforated hollow nanometer fiber belongs to the inorfil preparing technology field, the existing perovskite type rare-earth compound oxide shows with granular or thin film-like, big size and small specific surface area, the existing electrostatic spinning method is utilized to prepare the nanometer fiber of the metallic oxide. The method comprises the following steps: firstly, preparing spinning fluid, wherein the macromolecule template agent adopts polyvinyl pyrrolidone which occupies 45-55% of the macromolecule template agent, secondly, preparing the precursor fiber, adopting the electrostatic spinning method, wherein the technical parameters are that: the voltage is 18-25kV and the solidification distance is 15-25cm, thirdly, preparing the perforated hollow nanometer fiber, the technical parameters of the heat treatment are that: the heating rate is 0.5-2.0DEG C/min, holding the temperature between 600 DEG C and 900DEG C for 5-15h, the products are the perovskite type rare-earth compound oxide perforated hollow nanometer fiber, wherein the external diameter is 500-800nm, the thickness of the tube wall is 50-150nm and the length is more than 100 mu.
Description
Technical field
The present invention relates to a kind of nano-fiber material preparation method, belong to the inorfil preparing technical field.
Background technology
The general formula of perovskite-type rare-earth composite oxides is ABO
3, wherein A is thulium or alkali earth metal, and B is a transition metal, and O is an oxygen element.Perovskite-type rare-earth composite oxides is a kind of important depollution of environment catalyst, and it all has good catalytic action to carbon monoxide, methane, ethane and nitrogen oxide, is used for catalytic combustion, purifying vehicle exhaust and flue gas desulfurization etc.In addition, it also has excellent ferromagnetism, ferroelectricity, piezoelectricity, pyroelectricity, superconductivity, gas sensing property, fluorescence, catalytic activity and giant magnetoresistance effect etc.When the perovskite-type rare-earth composite oxides product of preparation is the hollow nano fiber shape; be also referred to as nanotube; especially when hollow tube wall is distributed with the duct, its Application Areas then contains catalysis, microfluid, purifies, is separated, gas storage, power conversion, drug, sensor and environmental protection etc.The method of existing preparation perovskite-type rare-earth composite oxides hollow nano fiber has hydro-thermal method, solvent-thermal method, evaporation and template.
The patent No. technical scheme of a relevant electrospinning process (electrospinning) that has been 1975504 U.S. Patent Publication, 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 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 spray by nozzle, invest the receiving screen on opposite, thereby realization wire drawing, 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, NiO, Co
3O
4, Mn
2O
3, Mn
3O
4, CuO, SiO
2, Al
2O
3, V
2O
5, ZnO, Nb
2O
5, and MoO
3Deng metal oxide.Electrospinning process can prepare big L/D ratio micro nanometer fiber or nanofiber continuously.By the nozzle arrangements in the redesign electrospinning device, the product of preparation has the hollow fibre pattern.Adopt coaxial nozzle to prepare TiO as people such as Xia Younan
2Hollow nano fiber (U.S. Nano Lett. magazine, 2004,4 (5), 933), the river thunder adopts multichannel nozzle to prepare TiO
2The multichannel hollow nano fiber (U.S. J.Am.Chem.Soc. magazine, 2007,129 (4), 764-765).
Summary of the invention
Adopt the hollow nano fiber draw ratio that method obtained of existing preparation perovskite-type rare-earth composite oxides hollow nano fiber little, and the process conditions harshness, poor repeatability.Need specialized designs, elaborate nozzle and adopt electrospinning process to prepare hollow nano fiber, and the selection of spinning solution raw material is had limitation, as require the precursor fibre ectonexine not dissolve each other, need good contact interface.In addition, prior art is not used for electrospinning process the preparation of perovskite-type rare earth composite oxide porous hollow nano fiber as yet.In order to prepare perovskite-type rare earth composite oxide porous hollow nano fibers in a large number continuously in simple ground, we have invented a kind of perovskite-type rare earth composite oxide porous hollow nano fiber preparation method.
The present invention is achieved in that and selects electrospinning process for use that the preparation product is a perovskite-type rare earth composite oxide porous hollow nano fiber, the steps include:
One, preparation spinning solution
Inorganic salts adopt thulium or nitrate, alkoxide or the acetate of alkali earth metal and nitrate, alkoxide or the acetate of transition metal, and the relative quantity of the two is equaled 1: 1 ratio decision by thulium or two kinds of amount of substance ratios of alkali earth metal and transition metal; High polymer templates adopts polyvinylpyrrolidone (PVP); Described inorganic salts and high polymer templates be dissolved in form spinning solution in the solvent.The weight proportion of each part of this spinning solution is: inorganic salts 8～12%, and polyvinylpyrrolidone 45～55%, all the other are solvent.
Two, preparation inorganic salts/high polymer templates precursor fibre
Adopt electrospinning process, technical parameter is: voltage is 18～25kV; Nozzle is 15～25cm to the curing distance of receiving screen.
Three, preparation perovskite-type rare earth composite oxide porous hollow nano fiber
Inorganic salts/high polymer templates the precursor fibre that is obtained is heat-treated, technical parameter is: heating rate is 0.5～2.0 ℃/min, in 600～900 ℃ of temperature ranges, be incubated 5～15h, naturally cool to room temperature with body of heater afterwards, so far obtain perovskite-type rare earth composite oxide porous hollow nano fiber.
Because being a kind of inorganic salts, high polymer templates, described spinning solution is dissolved in formed colloidal sol behind the solvent, inorganic salts evenly mix with high polymer templates, the precursor fibre that is spinned presents the form of the netted parcel high polymer templates of inorganic salts, after Overheating Treatment, the high polymer templates volatilization, the form of precursor fibre has just become the porous hollow shape.In the electrostatic spinning step, the nozzle in the spinning equipment still is easy single-hole nozzle.The diameter of prepared inorganic salts/high polymer templates precursor fibre is 1～5 μ m in said process, and the perovskite-type rare earth composite oxide porous hollow nano fiber external diameter of final preparation is 500～800nm, thickness of pipe wall 50～150nm, length is greater than 100 μ, judge by the draw ratio that is calculated in view of the above, this is a kind of overlength porous hollow nano fiber, has realized goal of the invention.
Description of drawings
Fig. 1 is LaCoO
3The SEM photo of porous hollow nano fiber.Fig. 2 is LaCoO
3The XRD spectra of porous hollow nano fiber.Fig. 3 is LaFeO
3The SEM photo of porous hollow nano fiber.Fig. 4 is LaFeO
3The XRD spectra of porous hollow nano fiber.Fig. 5 is LaMnO
3The SEM photo of porous hollow nano fiber, this figure double as is a Figure of abstract.Fig. 6 is LaMnO
3The XRD spectra of porous hollow nano fiber.Fig. 7 is LaCrO
3The SEM photo of porous hollow nano fiber.Fig. 8 is LaCrO
3The XRD spectra of porous hollow nano fiber.Fig. 9 is LaNiO
3The SEM photo of porous hollow nano fiber.Figure 10 is LaNiO
3The XRD spectra of porous hollow nano fiber.
The specific embodiment
Thulium or alkali earth metal are selected La, Y, Eu, Ce, Nd or Sr for use, and transition metal is selected Fe, Cr, Mn, Co, Ni or Ti for use.Solvent is selected deionized water or ethanol for use.High polymer templates adopts the polyvinylpyrrolidone of molecular weight Mr=10000.
Embodiment 1: add deionized water to polyvinylpyrrolidone, obtain even, the transparent polyvinylpyrrolidone aqueous solution.With La (NO
3)
36H
2O and Co (CH
3COO)
24H
2O evenly mixes and is dissolved in and obtains inorganic salt solution in the deionized water.With described two kinds of aqueous solution, magnetic agitation 2h at room temperature, ageing 24h then finally obtains even, transparent and the colloidal sol shape [La (NO of certain viscosity is arranged
3)
3+ Co (CH
3COO)
2]/polyvinylpyrrolidone spinning solution, its weight proportion is: polyvinylpyrrolidone 46%, [La (NO
3)
3+ Co (CH
3COO)
2] 10%, all the other are deionized water.With the spinning solution electrostatic spinning, voltage 20kV solidifies apart from 20cm, and nozzle and horizontal angle are 30 °, obtain [La (NO
3)
3+ Co (CH
3COO)
2]/polyvinylpyrrolidone precursor fibre.With 0.5 ℃/min heating rate heat treatment temperature is risen to 600 ℃,, obtain LaCoO precursor fibre sintering 10h
3Porous hollow nano fiber, external diameter 500～800nm, thickness of pipe wall are 100～150nm, length is seen shown in Figure 1 greater than 100 μ m.Product is the LaCoO of pure phase
3, belong to typical perovskite structure, see shown in Figure 2.
Embodiment 2:: add deionized water to polyvinylpyrrolidone, obtain even, the transparent polyvinylpyrrolidone aqueous solution.With La (NO
3)
36H
2O and Fe (NO
3)
39H
2O evenly mixes and is dissolved in and obtains inorganic salt solution in the deionized water.With described two kinds of aqueous solution, magnetic agitation 2h at room temperature, ageing 24h then finally obtains even, transparent and the colloidal sol shape [La (NO of certain viscosity is arranged
3)
3+ Fe (NO
3)
3]/polyvinylpyrrolidone spinning solution, its weight proportion is: polyvinylpyrrolidone 50%, [La (NO
3)
3+ Fe (NO
3)
3] 9%, all the other are deionized water.With the spinning solution electrostatic spinning, voltage 22kV solidifies apart from 22cm, and nozzle and horizontal angle are 30 °, obtain [La (NO
3)
3+ Fe (NO
3)
3]/polyvinylpyrrolidone precursor fibre.With 2 ℃/min heating rate heat treatment temperature is risen to 800 ℃,, obtain LaFeO precursor fibre sintering 6h
3Porous hollow nano fiber, external diameter 500～800nm, thickness of pipe wall are 80～150nm, length is seen shown in Figure 3 greater than 100 μ m.Product is the LaFeO of pure phase
3, belong to typical perovskite structure, see shown in Figure 4.
Embodiment 3: add deionized water to polyvinylpyrrolidone, obtain even, the transparent polyvinylpyrrolidone aqueous solution.With La (NO
3)
36H
2O and Mn (CH
3COO)
24H
2O evenly mixes and is dissolved in and obtains inorganic salt solution in the deionized water.With described two kinds of aqueous solution, magnetic agitation 2h at room temperature, ageing 24h then finally obtains even, transparent and the colloidal sol shape [La (NO of certain viscosity is arranged
3)
3+ Mn (CH
3COO)
2]/polyvinylpyrrolidone spinning solution, its weight proportion is: polyvinylpyrrolidone 55%, [La (NO
3)
3+ Mn (CH
3COO)
2] 12%, all the other are deionized water.With the spinning solution electrostatic spinning, voltage 20kV solidifies apart from 18cm, and nozzle and horizontal angle are 30 °, obtain [La (NO
3)
3+ Mn (CH
3COO)
2]/polyvinylpyrrolidone precursor fibre.With 0.5 ℃/min heating rate heat treatment temperature is risen to 900 ℃,, obtain LaMnO precursor fibre sintering 5h
3Porous hollow nano fiber, external diameter 500～800nm, thickness of pipe wall are 80～150nm, length is seen shown in Figure 5 greater than 100 μ m.Product is the LaMnO of pure phase
3, belong to typical perovskite structure, see shown in Figure 6.
Embodiment 4: add deionized water to polyvinylpyrrolidone, obtain even, the transparent polyvinylpyrrolidone aqueous solution.With La (NO
3)
36H
2O and Cr (NO
3)
39H
2O evenly mixes and is dissolved in and obtains inorganic salt solution in the deionized water.With described two kinds of aqueous solution, magnetic agitation 2h at room temperature, ageing 24h then finally obtains even, transparent and the colloidal sol shape [La (NO of certain viscosity is arranged
3)
3+ Cr (NO
3)
3]/polyvinylpyrrolidone spinning solution, its weight proportion is: polyvinylpyrrolidone 45%, [La (NO
3)
3+ Cr (NO
3)
3] 11%, all the other are deionized water.With the spinning solution electrostatic spinning, voltage 20kV solidifies apart from 20cm, and nozzle and horizontal angle are 30 °, obtain [La (NO
3)
3+ Cr (NO
3)
3]/polyvinylpyrrolidone precursor fibre.With 2 ℃/min heating rate heat treatment temperature is risen to 600 ℃,, obtain LaCrO precursor fibre sintering 15h
3Porous hollow nano fiber, external diameter 500～800nm, thickness of pipe wall are 50～100nm, length is seen shown in Figure 7 greater than 100 μ m.Product is the LaCrO of pure phase
3, belong to typical perovskite structure, see shown in Figure 8.
Embodiment 5: add deionized water to polyvinylpyrrolidone, obtain even, the transparent polyvinylpyrrolidone aqueous solution.With La (NO
3)
36H
2O and Ni (CH
3COO)
24H
2O evenly mixes and is dissolved in and obtains inorganic salt solution in the deionized water.With described two kinds of aqueous solution, magnetic agitation 2h at room temperature, ageing 24h then finally obtains even, transparent and the colloidal sol shape [La (NO of certain viscosity is arranged
3)
3+ Ni (CH
3COO)
2]/polyvinylpyrrolidone spinning solution, its weight proportion is: polyvinylpyrrolidone 50%, [La (NO
3)
3+ Ni (CH
3COO)
2] 8%, all the other are deionized water.With the spinning solution electrostatic spinning, voltage 20kV solidifies apart from 20cm, and nozzle and horizontal angle are 30 °, obtain [La (NO
3)
3+ Ni (CH
3COO)
2]/polyvinylpyrrolidone precursor fibre.With 0.5 ℃/min heating rate heat treatment temperature is risen to 600 ℃,, obtain LaNiO precursor fibre sintering 10h
3Porous hollow nano fiber, external diameter 500～800nm, thickness of pipe wall are 50～100nm, length is seen shown in Figure 9 greater than 100 μ m.Product is the LaNiO of pure phase
3, belong to typical perovskite structure, see shown in Figure 10.
Embodiment 6: polyvinylpyrrolidone is added absolute ethyl alcohol, stir 5h, obtain even, transparent polyvinylpyrrolidone ethanolic solution.With Sr (CH
3COO)
2H
2O and [CH
3(CH
2)
3O] Ti evenly mixes and is dissolved in absolute ethyl alcohol, obtains the inorganic salts ethanolic solution.Described two kinds of ethanolic solutions are mixed, magnetic agitation 5h at room temperature, ageing 2h then finally obtains evenly, oyster white and the colloidal sol shape [Sr (CH of certain viscosity is arranged
3COO)
2+ [CH
3(CH
2)
3O] Ti]/the polyvinylpyrrolidone spinning solution, its weight proportion is: polyvinylpyrrolidone 50%, [Sr (CH
3COO)
2+ [CH
3(CH
2)
3O] Ti] 10%, all the other are absolute ethyl alcohol.With the spinning solution electrostatic spinning, voltage 15kV solidifies apart from 20cm, and nozzle and horizontal angle are 30 °, obtain [Sr (CH
3COO)
2+ [CH
3(CH
2)
3O] Ti]/the polyvinylpyrrolidone precursor fibre.With 1 ℃/min heating rate heat treatment temperature is risen to 800 ℃,, obtain SrTiO precursor fibre sintering 10h
3Porous hollow nano fiber, external diameter 450～800nm, thickness of pipe wall are 50～150nm, length is greater than 100 μ m.Product is the SrTiO of pure phase
3, belong to typical perovskite structure.
Polyvinylpyrrolidone (Mr=10000), Co (CH that such scheme is selected
3COO)
24H
2O, Fe (NO
3)
39H
2O, Mn (CH
3COO)
24H
2O, Cr (NO
3)
39H
2O, Ni (CH
3COO)
24H
2O, [CH
3(CH
2)
3O] Ti and Sr (CH
3COO)
2H
2O is commercially available analysis net product, La (NO
3)
36H
2O purity is 99.99%.
Claims (5)
1, a kind of perovskite-type rare earth composite oxide porous hollow nano fiber preparation method is characterized in that, selects electrospinning process for use, and the preparation product is a perovskite-type rare earth composite oxide porous hollow nano fiber, the steps include:
One, preparation spinning solution
Inorganic salts adopt thulium or nitrate, alkoxide or the acetate of alkali earth metal and nitrate, alkoxide or the acetate of transition metal, and the relative quantity of the two is equaled 1: 1 ratio decision by thulium or two kinds of amount of substance ratios of alkali earth metal and transition metal; High polymer templates adopts polyvinylpyrrolidone; Described inorganic salts and high polymer templates be dissolved in form spinning solution in the solvent; The weight proportion of each part of this spinning solution is: inorganic salts 8～12%, and polyvinylpyrrolidone 45～55%, all the other are solvent;
Two, preparation inorganic salts/high polymer templates precursor fibre
Adopt electrospinning process, technical parameter is: voltage is 18～25kV; Nozzle is 15～25cm to the curing distance of receiving screen;
Three, preparation perovskite-type rare earth composite oxide porous hollow nano fiber
Inorganic salts/high polymer templates the precursor fibre that is obtained is heat-treated, technical parameter is: heating rate is 0.5～2.0 ℃/min, in 600～900 ℃ of temperature ranges, be incubated 5～15h, naturally cool to room temperature with body of heater afterwards, so far obtain perovskite-type rare earth composite oxide porous hollow nano fiber.
2, perovskite-type rare earth composite oxide porous hollow nano fiber preparation method according to claim 1 is characterized in that, thulium or alkali earth metal are selected La, Y, Eu, Ce, Nd or Sr for use.
3, perovskite-type rare earth composite oxide porous hollow nano fiber preparation method according to claim 1 is characterized in that, transition metal is selected Fe, Cr, Mn, Co, Ni or Ti for use.
4, perovskite-type rare earth composite oxide porous hollow nano fiber preparation method according to claim 1 is characterized in that, solvent is selected deionized water or ethanol for use.
5, perovskite-type rare earth composite oxide porous hollow nano fiber preparation method according to claim 1 is characterized in that, high polymer templates employing molecular weight is 10000 polyvinylpyrrolidone.
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