CN104016408A - Synthetic method of sodium niobate nanowire - Google Patents
Synthetic method of sodium niobate nanowire Download PDFInfo
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- CN104016408A CN104016408A CN201410255579.6A CN201410255579A CN104016408A CN 104016408 A CN104016408 A CN 104016408A CN 201410255579 A CN201410255579 A CN 201410255579A CN 104016408 A CN104016408 A CN 104016408A
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Abstract
The invention discloses a synthetic method of a sodium niobate nanowire. The synthetic method comprises the following steps: mixing NaOH and an organic solvent, carrying out hydro-thermal reaction, washing, centrifugally separating and drying. According to the synthetic method, used equipment is simple, reaction conditions are mild, the preparation of an intermediate phase precursor and the later annealing treatment are not needed, reaction raw materials are low in price, and expensive surface active agents are not need to be used as templates. The synthetic method has the main characteristics of simple technological process, capability of saving energy sources, low cost, easy control and operation, good repeatability and the like and can be put into industrial production easily, is capable of effectively shortening synthetic time and improving production efficiency and is an ideal environment-friendly synthetic technology.
Description
Technical field
The present invention relates to a kind of solvent process for thermosynthesizing of sodium niobate nano line, relate in particular to a kind of method of repeatedly one-step synthesis sodium niobate nano line, belong to base metal niobate nano-functional material field.
Background technology
Sodium columbate is a kind of important inorganic non-metallic functional materials, there is typical perovskite structure, because showing the performances such as good optically nonlinearity, ferroelectricity, piezoelectricity, photocatalytic and pyroelectric, there is huge application potential in fields such as energy recovery, intelligent sensing, Conversion of energy and photochemical catalysis, caused the very big concern of scientific research and technical applications.[W. Zeng, X. M. Tao, S. Chen, S. M. Shang, H. L. W. Chan, S. H. Choy,
energy Environ. Sci.,2013,6,2631-2638; M. Blomqvist, S. Khartsev, A. Grishin, A. Petraru, C. Buchal,
appl. Phys. Lett.,2003,82,439.] microtexture of material, the situations such as particle size, pattern and distribution that comprise play conclusive effect to its performance.Due to interfacial effect and dimensional effect, the functional materials of low-dimensional nanometer shows significant performance to be strengthened.Especially, the piezoelectric property of one dimension sodium niobate nanometer powder (comprising nano wire, nanofiber, nanometer rod etc.) and photocatalysis performance have obvious advantage compared with other patterns (nanometer blocks, nanometer ball etc.).[J. Lv, T. Kako, Z. S. Li, Z. G. Zou, J. H. Ye,
j. Phys. Chem. C,2010,114,6157 – 6162; T. Y. Ke, H. A. Chen, H. S. Sheu, J. W. Yeh, H. N. Lin, C. Y. Lee, H. T. Chiu,
j. Phys. Chem. C,2008,112,8827 – 8831.] up to now, synthetic molten-salt growth method, method of electrostatic spinning and the hydrothermal method of mainly containing of one dimension sodium niobate powder.Xu adopts molten-salt growth method first to make K
2nb
8o
21nano wire template, then under fused salt condition, carry out ion-exchange and then obtain sodium niobate nano line, technique is more loaded down with trivial details, and energy consumption is large, and has certain danger; [C. Y. Xu, L. Zhen, R. Yang, Z. L. Wang,
j. Am. Chem. Soc.,2007,129,15444 – 15445.] method of electrostatic spinning can prepare big or small homogeneous, the sodium niobate nano line that size is controlled, but need to depend on expensive equipment, production efficiency is extremely low, is unfavorable for industrialization; [W. Zeng, X. M. Tao, S. Chen, S. M. Shang, H. L. W. Chan, S. H. Choy,
energy Environ. Sci., 2013,6,2631-2638.] and what generally adopt at present is that hydrothermal method adds post annealed processing and prepares sodium niobate nano line, under hydrothermal condition, obtains one dimension intermediate product Na by strict control processing parameter (as temperature, time, basicity etc.)
7(H
3o) Nb
6o
19 .14H
2o or Na
2nb
2o
6, then processing obtains sodium niobate nano line through post annealed.[J. H. Jung, C. Y. Chen, W. W. Wu, J. I. Hong, B. K. Yun, Y. S. Zhou, N. Lee, W. Jo, L. J. Chen, L. J. Chou, Z. L. Wang,
j. Phys. Chem. C,2012,116 (42), 22261 – 22265.] hydrothermal method prepares sodium niobate nano line and has obvious advantage in molten-salt growth method, but one dimension intermediate product is very responsive to reaction environment, reaction conditions needs accurately to control, the calcination processing that simultaneously also needs the later stage, energy consumption is large, and technique is comparatively numerous and diverse.Therefore, adopt simple plant and instrument, by simple processing method, realize that the single stage method of sodium niobate nano line is synthetic to be significant in the application of energy transformation and photocatalysis field for sodium columbate.
Summary of the invention
technical problem
The technical problem to be solved in the present invention is to provide one and realizes an efficiently step solvent process for thermosynthesizing fast of sodium niobate nano line powder, and the sodium niobate nano line powder preparing by the method has excellent photocatalysis performance and piezoelectric property.
technical scheme
In order to solve above-mentioned technical problem, the synthetic method of sodium niobate nano line of the present invention comprises the following steps:
Step 1: add NaOH powder according to the concentration ratio of 0.5 ~ 1.0mol/L in the organic solvents such as ethylene glycol, heat and stir 20 ~ 30min and obtain the mixing solutions of NaOH and organic solvent; After it fully mixes, in above-mentioned mixing solutions, add 0.5 ~ 1.5g raw material Nb
2o
5, heated and stirred 15 ~ 20min, evenly mixes it, forms milky mixing solutions; Wherein, should ensure NaOH and Nb
2o
5the ratio of amount of substance be greater than 1;
Step 2: the mixing solutions of step 1 gained is transferred in polytetrafluoroethyllining lining, then liner is positioned in stainless steel hydrothermal reaction kettle and is sealed, carry out 4 ~ 16h insulation reaction at 120 ~ 200 DEG C, after question response finishes, naturally cool to room temperature and obtain white depositions;
Step 3: adopt respectively deionized water and dehydrated alcohol repeatedly to wash and centrifugation gained white precipitate product, rotating speed is 1000 ~ 3000rpm, and the time is 5 ~ 30min, all washes remaining ion and organic solvent to the greatest extent;
Step 4: carry out drying and processing under 50 ~ 80 DEG C of conditions, the time is 12 ~ 24h, obtains sodium niobate nano line powder.
In technical scheme of the present invention, NaOH should first add in ethylene glycol solvent and carries out stir process, makes as much as possible its dissolving or mixes, and can effectively control like this NaNbO
3the dimensional homogeneity of nano wire.
beneficial effect
Method equipment used of the present invention is simple, and reaction conditions gentleness, without preparation and the post annealed processing of middle phase presoma; Reaction raw materials is cheap, without expensive tensio-active agent as template; There is technical process simple, save energy, with low cost, be easy to operate and control, reproducible, be convenient to the principal features such as suitability for industrialized production, can effectively shorten generated time, enhance productivity, be a kind of desirable green synthesis process.Compared with prior art, the beneficial effect that the inventive method has is:
(1) using complete organic solvent ethylene glycol as reaction medium, a step solvent thermal that realizes sodium niobate nano line is synthetic, and technical process is simple, and combined coefficient is high, is convenient to suitability for industrialized production;
(2) required NaOH concentration is 0.5 ~ 2mol/L, and temperature of reaction is 120 ~ 200 DEG C, reaction conditions gentleness, and energy consumption is low, safe;
(3) alternative of gained sodium niobate nano line and controllability are strong, and NaOH concentration is 0.5 ~ 2.0mol/L, Nb
2o
5content is at 0.5 ~ 1.5g, and the reaction times all can obtain sodium niobate nano line at 4 ~ 16h;
(4) as shown in Figure 1, Figure 2, shown in the collection of illustrative plates and photo of Fig. 3, the size less (10 ~ 20nm) of gained sodium niobate nano line, distribution of sizes narrow range, reacts reproducible.
The sodium niobate nano linear dimension of synthesized of the present invention is little, and narrowly distributing has certain selectivity concurrently simultaneously.This convenient, efficient sodium niobate nano line synthetic method certainly will for the suitability for industrialized production of sodium columbate material with and create new opportunity and power in the application of Conversion of energy and photocatalysis field.
Brief description of the drawings
Fig. 1 is through 8h solvent thermal reaction gained NaNbO at 140 DEG C
3xRD figure spectrum;
Fig. 2 is through 8h solvent thermal reaction gained NaNbO at 180 DEG C
3field emission scanning electron microscope (FE-SEM) photo of nano wire;
Fig. 3 is through 4h solvent thermal reaction gained NaNbO at 200 DEG C
3nanowire size distribution plan, wherein illustration is transmission electron microscope (TEM) photo.
Embodiment
Below in conjunction with specific embodiment, the present invention is specifically described, but the present invention only limits to absolutely not the embodiment described in described embodiment.Every employing solvent thermal is synthesized sodium columbate 1-dimention nano powder, and all distortion of directly being derived or associated by content disclosed by the invention, all should think protection scope of the present invention.
Embodiment mono-
In 50ml ethylene glycol solvent, add 1.6664g NaOH, heated and stirred 20 ~ 30min; After it fully mixes, continue to add 1.5g raw material Nb
2o
5, heated and stirred 15 ~ 20min, evenly mixes it, forms milky mixing solutions.Gained mixing solutions is transferred in polytetrafluoroethyllining lining, then liner is positioned in stainless steel hydrothermal reaction kettle and is sealed, carry out 8h insulation reaction at 140 DEG C, after question response finishes, naturally cool to room temperature.Adopt deionized water and dehydrated alcohol repeatedly to wash and centrifugation gained white precipitate product, rotating speed is 3000rpm, and the time is 10min, ensures that remaining ion and organic solvent all wash to the greatest extent; Under 60 DEG C of conditions, carry out 24h drying and processing, obtain sodium columbate (NaNbO
3) nano wire powder.
Embodiment bis-
In 50ml ethylene glycol solvent, add 1.6664g NaOH, heated and stirred 20 ~ 30min; After it fully mixes, continue to add 1.0g raw material Nb
2o
5, heated and stirred 15 ~ 20min, evenly mixes it, forms milky mixing solutions.Gained mixing solutions is transferred in polytetrafluoroethyllining lining, then liner is positioned in stainless steel hydrothermal reaction kettle and is sealed, carry out 8h insulation reaction at 180 DEG C, after question response finishes, naturally cool to room temperature.Adopt deionized water and dehydrated alcohol repeatedly to wash and centrifugation gained white precipitate product, rotating speed is 3000rpm, and the time is 10min, ensures that remaining ion and organic solvent all wash to the greatest extent; Under 50 ~ 80 DEG C of conditions, carry out 12 ~ 24h drying and processing, obtain sodium columbate (NaNbO
3) nano wire powder.
Embodiment tri-
In 50ml ethylene glycol solvent, add 3.3328g NaOH, heated and stirred 20 ~ 30min; After it fully mixes, continue to add 0.5g raw material Nb
2o
5, heated and stirred 15 ~ 20min, evenly mixes it, forms milky mixing solutions.Gained mixing solutions is transferred in polytetrafluoroethyllining lining, then liner is positioned in stainless steel hydrothermal reaction kettle and is sealed, carry out 4h insulation reaction at 200 DEG C, after question response finishes, naturally cool to room temperature.Adopt deionized water and dehydrated alcohol repeatedly to wash and centrifugation gained white precipitate product, rotating speed is 3000rpm, and the time is 10min, ensures that remaining ion and organic solvent all wash to the greatest extent; Under 50 ~ 80 DEG C of conditions, carry out 12 ~ 24h drying and processing, obtain sodium columbate (NaNbO3) nano wire powder.
Claims (3)
1.
onethe synthetic method of planting sodium niobate nano line, is characterized in that, comprises the following steps:
Step 1: add NaOH powder according to the concentration ratio of 0.5 ~ 1.0mol/L in organic solvent, heat and stir 20 ~ 30min and obtain the mixing solutions of NaOH and organic solvent; After it fully mixes, in above-mentioned mixing solutions, add 0.5 ~ 1.5g raw material Nb
2o
5, heated and stirred 15 ~ 20min, evenly mixes it, forms milky mixing solutions;
Step 2: the mixing solutions of step 1 gained is transferred in polytetrafluoroethyllining lining, then liner is positioned in stainless steel hydrothermal reaction kettle and is sealed, carry out 4 ~ 16h insulation reaction at 120 ~ 200 DEG C, after question response finishes, naturally cool to room temperature and obtain white depositions;
Step 3: adopt respectively deionized water and dehydrated alcohol repeatedly to wash and centrifugation gained white precipitate product, rotating speed is 1000 ~ 3000rpm, and the time is 5 ~ 30min, all washes remaining ion and organic solvent to the greatest extent;
Step 4: carry out drying and processing under 50 ~ 80 DEG C of conditions, the time is 12 ~ 24h, obtains sodium niobate nano line powder.
2. a kind of synthetic method of sodium niobate nano line as described in claim 1, is characterized in that: the organic solvents such as selected reaction solvent is ethylene glycol.
3. a kind of synthetic method of sodium niobate nano line as described in claim 1, is characterized in that: ensure NaOH and Nb
2o
5the ratio of amount of substance be greater than 1, temperature of reaction is 120 ~ 200 DEG C, the reaction times is 4 ~ 16h.
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Cited By (7)
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|---|---|---|---|---|
| CN105110791A (en) * | 2015-09-17 | 2015-12-02 | 白杉 | Method for synthesizing niobate sheet-shaped formwork powder |
| CN105399418A (en) * | 2015-12-08 | 2016-03-16 | 南京航空航天大学 | Preparation method of high-performance sodium niobate dielectric ceramic powder |
| CN106076312A (en) * | 2016-06-02 | 2016-11-09 | 河南理工大学 | A kind of Nb (OH)5nano wire/redox graphene composite photo-catalyst and preparation method and application |
| CN107640788A (en) * | 2017-09-25 | 2018-01-30 | 清华大学深圳研究生院 | Niobic acid salt material and preparation method thereof |
| CN107758743A (en) * | 2017-11-17 | 2018-03-06 | 北京工业大学 | A kind of method that cation exchange approach prepares sodium niobate nano line |
| CN108910947A (en) * | 2018-07-17 | 2018-11-30 | 天津城建大学 | A kind of micro-nano (K, Na) NbO of thin slice3Crystal and preparation method thereof |
| CN110474029A (en) * | 2019-07-11 | 2019-11-19 | 江苏师范大学 | A kind of anode composite material of lithium sulfur battery and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105110791A (en) * | 2015-09-17 | 2015-12-02 | 白杉 | Method for synthesizing niobate sheet-shaped formwork powder |
| CN105399418A (en) * | 2015-12-08 | 2016-03-16 | 南京航空航天大学 | Preparation method of high-performance sodium niobate dielectric ceramic powder |
| CN106076312A (en) * | 2016-06-02 | 2016-11-09 | 河南理工大学 | A kind of Nb (OH)5nano wire/redox graphene composite photo-catalyst and preparation method and application |
| CN107640788A (en) * | 2017-09-25 | 2018-01-30 | 清华大学深圳研究生院 | Niobic acid salt material and preparation method thereof |
| CN107758743A (en) * | 2017-11-17 | 2018-03-06 | 北京工业大学 | A kind of method that cation exchange approach prepares sodium niobate nano line |
| CN108910947A (en) * | 2018-07-17 | 2018-11-30 | 天津城建大学 | A kind of micro-nano (K, Na) NbO of thin slice3Crystal and preparation method thereof |
| CN108910947B (en) * | 2018-07-17 | 2020-11-03 | 天津城建大学 | Thin-sheet micro-nano (K, Na) NbO3Crystal and method for producing same |
| CN110474029A (en) * | 2019-07-11 | 2019-11-19 | 江苏师范大学 | A kind of anode composite material of lithium sulfur battery and preparation method thereof |
| CN110474029B (en) * | 2019-07-11 | 2022-06-10 | 江苏师范大学 | Lithium-sulfur battery positive electrode composite material and preparation method thereof |
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