CN103484929A - One-dimensional single-crystal LaFeO3 nanowire and preparation method - Google Patents
One-dimensional single-crystal LaFeO3 nanowire and preparation method Download PDFInfo
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- CN103484929A CN103484929A CN201310432803.XA CN201310432803A CN103484929A CN 103484929 A CN103484929 A CN 103484929A CN 201310432803 A CN201310432803 A CN 201310432803A CN 103484929 A CN103484929 A CN 103484929A
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- deionized water
- nanowire
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Abstract
The invention belongs to the technical field of LaFeO3 nano-structures and provides a one-dimensional single-crystal LaFeO3 nanowire and a preparation method thereof. The one-dimensional single-crystal LaFeO3 nanowire is prepared by the following steps: firstly adopting a hydrothermal synthesis method to prepare a Fe2O3 nanowire, then dissolving lanthanum nitrate hexahydrate into deionized water, adding the Fe2O3 nanowire to serve as a template under stirring, dropwise adding a KOH (potassium hydroxide) solution with the mass concentration of 10 percent under stirring, performing ultrasonic dispersion for 10-15 min, transferring the suspension to a self-pressure kettle with a PTFE (Polytetrafluoroethylene) lining to enable the volume filling degree to be 80 percent, processing the suspension for 12 h at the constant temperature of 180 DEG C, performing suction filtration, using deionized water and absolute ethyl alcohol to wash the product for 3 times respectively, drying the product for 12 h at the temperature of 80 DEG C, and heating the product to 650 or 750 DEG C from a room temperature at a rate of 1 DEG C/min under the air atmosphere in a muffle furnace and keeping the temperature for 4h, to obtain the one-dimensional single-crystal LaFeO3 nanowire. According to the invention, the raw materials are cheap and easy to obtain, the preparation process is simple, and the product morphology is controllable.
Description
Technical field
The present invention relates to a kind of preparation with one-dimensional single crystal perofskite type oxide nano material, relate to Fe specifically
2o
3for template prepares one-dimensional single crystal LaFeO
3the hydrothermal synthesis method of nano wire, belong to LaFeO
3the nanostructure technical field.
Background technology
The development of modern industry has also brought pollution to environment when improving our life.Industrial gaseous waste (volatile organic matter (VOCs) etc.) is the main source that causes topsoil.In the technology of pollute controlling at VOCs, Production by Catalytic Combustion Process is at present the most frequently used removal technology, and by katalysis, VOCs can be burnt under lesser temps (<500 ℃), and its clearance is usually above 95%.In catalyticcombustion, the selection of catalyzer is particularly crucial.The catalyst type that is applied at present the VOCs catalyticcombustion mainly contains carried noble metal, single metal oxide and O composite metallic oxide catalyst etc.Perofskite type oxide is one of complex metal oxides, because it has cheap, advantages such as catalytic activity can compare favourably with precious metal, Heat stability is good, receives much attention.
LaFeO
3belong to uhligite (ABO
3) the type oxide compound, its structure, magnetic and electroconductibility are reported by lot of documents.Because of its special constructional feature extensive application, as do electrode materials, catalyzer, humidity sensor etc., purposes is comparatively extensive.Therefore in recent years, adopt the methods such as hydrothermal/solvent thermal synthesis method, melting salt solid phase synthesis technique, sol-gel method to synthesize LaFeO
3nano material.Deng etc. (J.G.Deng, et al., Environ.Sci.Technol, 2010,44:2618) adopt citric acid complex to prepare a series of perofskite type oxides, LaFeO in conjunction with hydrothermal synthesis method
3there is higher activity in oxidizing reaction to toluene.But and the La of doping Sr and Co
0.6sr
0.4co
0.9fe
0.1o
3the activity of comparing is still very low.Qi etc. (S.Y.Qi, et al., Chem.Res.Chinese Universities, 2008,24:672) adopt solid phase method to prepare bar-shaped La
0.7sr
0.3mnO
3.Wherein the formation of club shaped structure is mainly with fibrous MnO
2as template, the La formed under 950 ℃ of calcination 5h
0.7sr
0.3mnO
3club shaped structure.Study its growth mechanism and learn, La
0.7sr
0.3mnO
3the formation of club shaped structure and fibrous MnO
2template is relevant.Yang etc. (Y.Yang, et al., J.Am.Ceram.Soc., 2008,91:3820) with TiO
2for template, adopt hydrothermal method to prepare PbTiO
3nanotube.And study its growth mechanism and learn, the interpolation of KOH solution dissolves nanotube and at PbTiO
3make its crystallization in the process of dissolution precipitation.Xiao etc. (X.L.Xiao, et al., Nano Res., 2012,5:27) adopt with CoCl
26H
2o and CO (NH
2)
2the Co prepared for raw material
3o
4nano wire is template, mixes LiOH, at 750 ℃ of calcination 2h, prepares LiCoO
2nano wire, have good chemical property.Tang etc. (W.Tang, et al., Nano Lett., 2013,13:2036) at first adopt and take multilayer carbon nanotube and prepare and be coated with MnO as template
2carbon nanotube, then take it as template, mix LiOH and grind in ethanolic soln, after supersound process 5h, after 700 ℃ of calcination 8h, obtain LiMn
2o
4nanotube.
Up to now, there is no document and patent report successfully synthesizes with Fe
2o
3for template prepares one-dimensional single crystal LaFeO
3nano wire.
Summary of the invention
The object of the present invention is to provide a kind of LaFeO with one-dimensional single crystal nanostructure for preparing
3the preparation method.
Adopt hydrothermal method to prepare one-dimensional single crystal LaFeO
3nano wire, is characterized in that, adopts with Fe
2o
3nano wire is the template preparation, and concrete steps comprise as follows: under agitation condition, the content 1:1 metering ratio according to iron and lanthanum, by the lanthanum nitrate hexahydrate deionized water dissolving, add Fe
2o
3line is as template, stir 30min, in above-mentioned mixing solutions, drip mass concentration 10%KOH solution, to pH be 9～11(preferably 10), ultrasonic dispersion 15min then, be transferred to above-mentioned suspension liquid that to make the volume compactedness in the stainless steel self-pressure still (preferred volume 50ml) that liner is tetrafluoroethylene be 80%, and being placed in thermostat container in 180 ℃ of processing 12h, it naturally cools to room temperature to take out relief.The product obtained after processing is filtered, respectively washs 3 times with deionized water and dehydrated alcohol, in 100 ℃ of dry 12h, in retort furnace, with the speed of 1 ℃/min, rise to 650 ℃ or 750 ℃ also after constant temperature 4h, obtain target product one-dimensional single crystal LaFeO
3nano wire.
Preferred every 1.0632g La (NO)
36H
2o 10ml deionized water dissolving.
Template Fe
2o
3the preparation of nano wire is preferred: under agitation condition, by the ferric chloride hexahydrate deionized water dissolving of certain molar weight, then add the Virahol of certain volume to form uniform solution, then add the nitrilotriacetic acid(NTA) of certain molar weight, stir certain hour, wherein corresponding relation is every 1.75mmol FeCl
36H
2the corresponding 15ml deionized water of O, corresponding Virahol 15ml, corresponding nitrilotriacetic acid(NTA) 5mmol; Above-mentioned solution is transferred in the stainless steel self-pressure still (as the 50mL volume) that liner is tetrafluoroethylene, and making the volume compactedness is 60%, and is placed in 180 ℃ of processing 24h of thermostat container, and it naturally cools to room temperature to take out relief.The product obtained after processing is filtered, respectively washs 3 times with deionized water and dehydrated alcohol, and the lower 60 ℃ of dry 12h of vacuum condition rise to 500 ℃ and after 500 ℃ of constant temperature 2h with the speed of 1 ℃/min in retort furnace, obtain Fe
2o
3nano wire.
The present invention has that raw material is cheap and easy to get, and preparation process is simple, product particle morphology, crystalline structure, the feature such as specific surface area is controlled.
One-dimensional single crystal perofskite type oxide LaFeO prepared by the present invention
3there is larger specific surface area, and easily allow the high reactivity crystal face be exposed to catalyst surface, have a good application prospect at aspects such as electrode materials, catalyzer, superconducting material, sensor, synthetic gas production, environmental monitoring materials.Utilize X-ray diffractometer (XRD), scanning electronic microscope (SEM) and selected area electron diffraction (SAED) technology to measure respectively crystal phase structure, particle morphology and the crystal formation of sample.
The accompanying drawing explanation
Fig. 1 is prepared LaFeO
3the XRD spectra of nano wire sample, wherein curve (a), (b) are respectively the XRD spectra of embodiment 1 gained sample under 650 ℃ and 750 ℃ of calcination conditions.
Fig. 2 is prepared LaFeO
3the SEM photo of nano wire sample and SAED pattern, wherein figure (a), (b) is respectively SEM photo and the SAED pattern (built-in figure) of embodiment 1 sample gained sample under 650 ℃ and 750 ℃ of calcination conditions.
Embodiment
In order further to understand the present invention, below with embodiment, elaborate, and provide accompanying drawing and describe the one-dimensional single crystal LaFeO that the present invention obtains
3nano wire.
Embodiment 1: template Fe
2o
3the preparation of nano wire, under agitation condition, by 1.75mmol FeCl
36H
2o 15ml deionized water dissolving, add again the 15ml Virahol to form uniform solution, add the 5mmol nitrilotriacetic acid(NTA), stir 30min, above-mentioned solution is transferred in the 50mL stainless steel self-pressure still that liner is tetrafluoroethylene (the volume compactedness is 60%), and being placed in 180 ℃ of processing 24h of thermostat container, it naturally cools to room temperature to take out relief.The product obtained after processing is filtered, respectively washs 3 times with deionized water and dehydrated alcohol, and the lower 60 ℃ of dry 12h of vacuum condition rise to 500 ℃ and after 500 ℃ of constant temperature 2h with the speed of 1 ℃/min in retort furnace, obtain Fe
2o
3nano wire.
One-dimensional single crystal LaFeO
3the preparation of nano wire: under agitation condition, 1.0632g La (NO)
36H
2o 10ml deionized water dissolving, add 0.1964g Fe
2o
3nano wire, continue to stir 30min, drip 10%KOH solution, to the solution pH value be 10 left and right, then ultrasonic dispersion 15min, above-mentioned suspension liquid is transferred in the 50mL stainless steel self-pressure still that liner is tetrafluoroethylene (the volume compactedness is 80%), and is placed in thermostat container in 180 ℃ of processing 12h, it naturally cools to room temperature to take out relief.The product obtained after processing is filtered, respectively washs 3 times with deionized water and dehydrated alcohol, in 100 ℃ of dry 12h, in retort furnace, with the speed of 1 ℃/min, rise to 650 ℃ or 750 ℃ also after constant temperature 4h, obtain one-dimensional single crystal LaFeO
3nano wire.
Gained one-dimensional single crystal LaFeO
3attached Fig. 1 and 2 is shown in respectively by the XRD spectra of nano wire and SEM photo and SAED pattern.
Claims (6)
1. hydrothermal method is prepared one-dimensional single crystal LaFeO
3the method of nano wire, is characterized in that, adopts with Fe
2o
3nano wire is the template preparation, and concrete steps comprise as follows: under agitation condition, the content 1:1 metering ratio according to iron and lanthanum, by the lanthanum nitrate hexahydrate deionized water dissolving, add Fe
2o
3line is as template, stir 30min, in above-mentioned mixing solutions, drip mass concentration 10%KOH solution, to the solution pH value be 9-11, ultrasonic dispersion 15min then, be transferred to above-mentioned suspension liquid that to make the volume compactedness in the stainless steel self-pressure still that liner is tetrafluoroethylene be 80%, and being placed in thermostat container in 180 ℃ of processing 12h, it naturally cools to room temperature to take out relief; The product obtained after processing is filtered, respectively washs 3 times with deionized water and dehydrated alcohol, in 100 ℃ of dry 12h, in retort furnace, with the speed of 1 ℃/min, rise to 650 ℃ or 750 ℃ also after constant temperature 4h, obtain target product one-dimensional single crystal LaFeO
3nano wire.
2. according to the method for claim 1, it is characterized in that template Fe
2o
3the preparation of nano wire is preferred: under agitation condition, by the ferric chloride hexahydrate deionized water dissolving of certain molar weight, then add the Virahol of certain volume to form uniform solution, then add the nitrilotriacetic acid(NTA) of certain molar weight, stir certain hour, wherein corresponding relation is every 1.75mmolFeCl
3.6H
2the corresponding 15ml deionized water of O, corresponding Virahol 15ml, corresponding nitrilotriacetic acid(NTA) 5mmol; Above-mentioned solution is transferred in the stainless steel self-pressure still that liner is tetrafluoroethylene, and making the volume compactedness is 60%, and is placed in 180 ℃ of processing 24h of thermostat container, and it naturally cools to room temperature to take out relief.The product obtained after processing is filtered, respectively washs 3 times with deionized water and dehydrated alcohol, and the lower 60 ℃ of dry 12h of vacuum condition rise to 500 ℃ and after 500 ℃ of constant temperature 2h with the speed of 1 ℃/min in retort furnace, obtain Fe
2o
3nano wire.
3. according to the method for claim 1, it is characterized in that, add mass concentration 10%KOH solution, to pH be 10.
4. according to the method for claim 1, it is characterized in that, the volume of stainless steel self-pressure still is 50ml.
5. according to the method for claim 1, it is characterized in that preferred every 1.0632gLa (NO)
36H
2o 10ml deionized water dissolving.
6. the one-dimensional single crystal LaFeO prepared according to the described either method of claim 1-5
3nano wire.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107159230A (en) * | 2017-05-23 | 2017-09-15 | 武汉工程大学 | A kind of catalyst that low-concentration nitrogen oxide is removed for constant temperature catalyzing and preparation method thereof |
Citations (2)
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|---|---|---|---|---|
| CN101235558A (en) * | 2008-03-12 | 2008-08-06 | 长春理工大学 | Method for preparing perovskite-type rare earth composite oxide porous hollow nano fiber |
| CN101235556A (en) * | 2008-03-12 | 2008-08-06 | 长春理工大学 | Method for preparing perovskite-type rare earth composite oxide ultra-long nano fiber |
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2013
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101235558A (en) * | 2008-03-12 | 2008-08-06 | 长春理工大学 | Method for preparing perovskite-type rare earth composite oxide porous hollow nano fiber |
| CN101235556A (en) * | 2008-03-12 | 2008-08-06 | 长春理工大学 | Method for preparing perovskite-type rare earth composite oxide ultra-long nano fiber |
Non-Patent Citations (3)
| Title |
|---|
| KWANG-HYEON RYU，等: "Preparation of Porous LaFeO3Nanowires using AAO Template and Their Catalytic Properties", 《BULL. KOREAN CHEM. SOC.》 * |
| WANG JINXIAN，等: "Electrospinning Preparation of LaFeO3 Nanofibers", 《MODERN APPLIED SCIENCE》 * |
| 孙霞，等: "LaFeO3纳米带的制备及其光催化性能", 《硅酸盐学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107159230A (en) * | 2017-05-23 | 2017-09-15 | 武汉工程大学 | A kind of catalyst that low-concentration nitrogen oxide is removed for constant temperature catalyzing and preparation method thereof |
| CN107159230B (en) * | 2017-05-23 | 2019-12-06 | 武汉工程大学 | Catalyst for normal-temperature catalytic removal of low-concentration nitrogen oxides and preparation method thereof |
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