CN104030358A - Method for preparing sodium niobate fiber by combining hydrothermal method and later thermal treatment process - Google Patents
Method for preparing sodium niobate fiber by combining hydrothermal method and later thermal treatment process Download PDFInfo
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- CN104030358A CN104030358A CN201410261991.9A CN201410261991A CN104030358A CN 104030358 A CN104030358 A CN 104030358A CN 201410261991 A CN201410261991 A CN 201410261991A CN 104030358 A CN104030358 A CN 104030358A
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Abstract
The invention discloses a method for preparing sodium niobate fiber by combining a hydrothermal method and a later thermal treatment process. The method is characterized in that sodium hydroxide and niobium oxide are used as raw materials, sodium hydroxide is simultaneously used as a hydrothermal reaction mineralizing agent, and deionized water is used as a hydrothermal reaction solvent. The method comprises the steps of preparing an initial product under the conditions that the concentration of sodium hydroxide is 10mol/L, the concentration of niobium oxide is 0.0125mol/L, the hydrothermal temperature is 160 DEG C and the reaction time is 6-8h; and then, placing the initial product into a muffle furnace, and keeping the temperature of 400-650 DEG C for 1-3h to obtain a final product, i.e., the sodium niobate fiber with the diameter of 300-900nm and the length of 100-150mu m. The fiber as the final product is very obvious in characteristic, relatively good in dispersibility and perfected in growth and development. The method disclosed by the invention has the advantages that the raw materials are easy to obtain and low in price, experimental equipment is simple, the process flow is easy to control, and the prepared sodium niobate fiber has relatively good development prospect on the aspects such as preparation and application of antiferroelectric sodium niobate, texturing research on potassium sodium niobate based leadless piezoelectric ceramics and the like.
Description
Technical field
The present invention relates to a kind of preparation method of one dimension sodium columbate material.
Background technology
Sodium columbate is antiferroelectric when room temperature, has very high specific inductivity during Curie temperature, in the application aspect of piezoelectric device and acoustic sensor, has potential value.Sodium columbate, as antiferroelectric, can also form with the ferroelectrics of various structures the solid solution ceramic of different qualities.Sodium columbate based leadless piezoelectric ceramics has unique physical properties: low density, high acoustic velocity, specific inductivity, mechanical quality factor and piezoelectric constant span are wider etc.Because sodium columbate based solid solution has excellent piezoelectricity and electro-optical properties, be widely used in the fields such as electrical condenser and posistor.
In recent years, many methods comprise that sol-gel method, coprecipitation method and Pechini s method are widely used in preparing base metal niobate powder and film.Hydrothermal method synthesizing ceramic powder shows more traditional solid phase reaction method and other certain methods advantage as distinctive in wet chemistry method, and hydrothermal synthesis method reaction conditions is gentle, does not need expensive presoma and equipment, can generate uniform crystallization phases powder.Yet, up to the present not yet relevant for sodium columbate fiber preparation method's report.
Summary of the invention
The object of this invention is to provide a kind of hydrothermal method and in conjunction with later stage thermal treatment process, prepare the method for sodium columbate fiber.
Hydrothermal method of the present invention is prepared sodium columbate fiber process in conjunction with later stage thermal treatment process, it is characterized in that take that sodium hydroxide, niobium oxides are raw material, and sodium hydroxide serves as the mineralizer of hydro-thermal reaction simultaneously, take deionized water as hydro-thermal reaction solvent.When naoh concentration is 10mol/L, niobium oxides concentration is 0.0125mol/L, hydrothermal temperature is 160 ℃, reaction times is 6 ~ 8h, obtain initial product, then initial product is put at 400 ~ 650 ℃ of temperature of retort furnace and is incubated 1 ~ 3h, obtain final product sodium columbate fiber, diameter 300 ~ 900nm, length 100 ~ 150 μ m.Final product fiber properties is fairly obvious, better dispersed, grows perfect.This inventive method raw material is easy to get and is cheap, experimental installation is simple, technical process is easy to control, and the sodium columbate fiber of preparation is in preparation and the application of antiferroelectric sodium columbate, and there is good development prospect the aspects such as potassium niobate sodium-based leadless piezoelectric ceramic texturing research.
Hydrothermal method of the present invention is prepared sodium columbate fiber process in conjunction with later stage thermal treatment process and can be taked following technical measures to solve:
1. according to naoh concentration, be 10mol/L, niobium oxides concentration be 0.0125mol/L require weighing sodium hydroxide and niobium oxides, raw material is added in the beaker that 60ml deionized water is housed, slurries precipitate without obvious solid particulate until mixing solutions is white in color at 60 ℃ of temperature lower magnetic forces, to stir 2h.
2. the white slurries that obtain after stirring being poured into volume is in 100 ~ 200ml teflon-lined hydrothermal reaction kettle, in reactor, add a stirrer simultaneously, after sealing, put into the 160 ℃ of reaction 6 ~ 8h of oil bath pan with magnetic stirring function, reaction process remains magnetic agitation, and stir speed (S.S.) is 0 ~ 120r/min.
3. after reaction finishes, will obtain white depositions and filter, and use deionized water repetitive scrubbing, in air dry oven, 110 ℃ of freeze-day with constant temperature 12h, obtain initial product.
4. the initial product of acquisition is put into 400 ~ 650 ℃ of insulation 1 ~ 3h of retort furnace, cooled to the furnace room temperature, obtaining final product is fibrous sodium columbate.
Hydrothermal method of the present invention is prepared sodium columbate fiber process in conjunction with later stage thermal treatment process and is had the following advantages:
Hydrothermal method of the present invention is prepared sodium columbate fiber process at lower temperature in conjunction with later stage thermal treatment process, do not need expensive raw material and equipment, by changing hydrothermal condition, obtain initial product, again initial product is carried out at relatively low temperature to later stage thermal treatment and obtain sodium columbate fiber, final product fiber properties is fairly obvious, better dispersed, grow perfect.
Accompanying drawing explanation
Fig. 1 embodiment 1 hydrothermal method is prepared 5 μ m SEM figure of sodium columbate fiber in conjunction with later stage thermal treatment process;
Fig. 2 embodiment 1 hydrothermal method is prepared 100 μ m SEM figure of sodium columbate fiber in conjunction with later stage thermal treatment process;
Fig. 3 embodiment 2 hydrothermal methods are prepared 5 μ m SEM figure of sodium columbate fiber in conjunction with later stage thermal treatment process;
Fig. 4 embodiment 2 hydrothermal methods are prepared 50 μ m SEM figure of sodium columbate fiber in conjunction with later stage thermal treatment process;
Fig. 5 embodiment 3 hydrothermal methods are prepared 5 μ m SEM figure of sodium columbate fiber in conjunction with later stage thermal treatment process;
Fig. 6 embodiment 3 hydrothermal methods are prepared 50 μ m SEM figure of sodium columbate fiber in conjunction with later stage thermal treatment process.
Embodiment
embodiment 1:
1, weighing sodium hydroxide 24g and niobium oxides 0.2g, add two kinds of raw materials in the beaker that fills 60ml deionized water, 60 ℃ of temperature lower magnetic forces stir 2h until mixing solutions is white in color slurries and without obvious solid particulate precipitation.
2, the white slurries that obtain after stirring being poured into volume is in 100ml teflon-lined hydrothermal reaction kettle, in reactor, add a magnetic stir bar simultaneously, after sealing, put into the 160 ℃ of reaction 6h of oil bath pan with magnetic stirring function, reaction process remains magnetic agitation, and speed is 60r/min.
3, after reaction finishes, will obtain white depositions and filter, use deionized water repetitive scrubbing, 110 ℃ of freeze-day with constant temperature 12h in air dry oven.
4, the initial product of acquisition is put into 400 ℃ of heating and thermal insulation 2h of retort furnace, cooled to the furnace room temperature, obtaining final product is fibrous sodium columbate.The sodium columbate fiber of acquisition is weighed, and its weight is about 0.05g, the about 400nm of scanning electronic microscope (SEM) display fibers mean diameter, length 150 μ m(are shown in Fig. 1, Fig. 2).
embodiment 2:
1, weighing sodium hydroxide 48g and niobium oxides 0.4g, add two kinds of raw materials in the beaker that fills 120ml deionized water, 60 ℃ of temperature lower magnetic forces stir 2h until mixing solutions is white in color slurries and without obvious solid particulate precipitation.
2, the white slurries that obtain after stirring being poured into volume is in 200ml teflon-lined hydrothermal reaction kettle, in reactor, add a magnetic stir bar simultaneously, after sealing, put into the 160 ℃ of reaction 6h of oil bath pan with magnetic stirring function, reaction process remains magnetic agitation, and stir speed (S.S.) is 120r/min.
3, after reaction finishes, will obtain white depositions and filter, use deionized water repetitive scrubbing, 110 ℃ of freeze-day with constant temperature 12h in air dry oven.
4, the initial product of acquisition is put into 450 ℃ of heating and thermal insulation 2h of retort furnace, cool to room temperature with the furnace, obtaining final product is fibrous sodium columbate, the sodium columbate fiber of acquisition is weighed, its weight is about 0.1g, the about 300nm of scanning electronic microscope (SEM) average fibre diameter, mean length 100 μ m(are shown in Fig. 3, Fig. 4).
embodiment 3:
1, weighing sodium hydroxide 24g and niobium oxides 0.2g, add two kinds of raw materials in the beaker that fills 60ml deionized water, 60 ℃ of temperature lower magnetic forces stir 2h until mixing solutions is white in color slurries and without obvious solid particulate precipitation.
2, the white slurries that obtain after stirring being poured into volume is in 100ml teflon-lined hydrothermal reaction kettle, puts into 160 ℃ of reaction 6h of oil bath pan after sealing simultaneously, in reaction process, does not stir.
3, after reaction finishes, will obtain white depositions and filter, use deionized water repetitive scrubbing, 110 ℃ of freeze-day with constant temperature 12h in air dry oven.
4, the initial product of acquisition is put into 650 ℃ of heating and thermal insulation 2h of muffle furnace, cool to room temperature with the furnace, obtaining final product is fibrous sodium columbate, the sodium columbate fiber of acquisition is weighed, its weight is about 0.05g, the about 800nm of scanning electronic microscope (SEM) average fibre diameter, mean length 120 μ m(are shown in Fig. 5, Fig. 6).
Claims (3)
1. hydrothermal method is prepared a method for sodium columbate fiber in conjunction with later stage thermal treatment process, and take sodium hydroxide, niobium oxides is raw material, take deionized water as hydro-thermal reaction solvent; Raw material adds in the hydrothermal reaction kettle of 100 ~ 200ml volume, 160 ℃ of hydrothermal temperatures, reaction times is 6 ~ 8h, in hydrothermal reaction process, keep magnetic agitation, stir speed (S.S.) is 0 ~ 120r/min, obtains initial product dry, subsequently initial product is put into retort furnace, at 400 ~ 650 ℃ of temperature, be incubated 2h, obtain final product sodium columbate fiber.
2. the method for preparing sodium columbate fiber according to claim 1, is characterized in that: experiment is 10mol/L with ionized water preparation naoh concentration, and niobium oxides concentration is 0.0125mol/L.
3. the sodium columbate fiber process of preparing according to claim 1, is characterized in that: final product sodium columbate fiber single " fiber " length 100 ~ 150 μ m, diameter 300 ~ 900nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105817231A (en) * | 2016-04-12 | 2016-08-03 | 河海大学 | Preparation method of iron-loaded NaNbO3 perovskite photocatalyst |
| CN108660544A (en) * | 2018-03-30 | 2018-10-16 | 常州大学 | A kind of preparation method of semiconductor nano fiber |
| CN115924970A (en) * | 2022-09-19 | 2023-04-07 | 济南大学 | Potassium niobate nanowire and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101391815A (en) * | 2008-10-24 | 2009-03-25 | 哈尔滨工业大学 | Method for preparing niobate one-dimensional nano material |
| CN101696035A (en) * | 2009-11-03 | 2010-04-21 | 陕西科技大学 | Method for preparing sodium niobate powder |
-
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101391815A (en) * | 2008-10-24 | 2009-03-25 | 哈尔滨工业大学 | Method for preparing niobate one-dimensional nano material |
| CN101696035A (en) * | 2009-11-03 | 2010-04-21 | 陕西科技大学 | Method for preparing sodium niobate powder |
Non-Patent Citations (2)
| Title |
|---|
| DEQING ZHANG ET AL.: "Preparation and characterization of orthorhombic NaNbO3 Long Bar", 《CERAMICS INTERNATIONAL》, vol. 40, 11 June 2014 (2014-06-11), pages 14279 - 14285, XP029017765, DOI: 10.1016/j.ceramint.2014.06.018 * |
| 甄玉花等: "铌酸钾钠基无铅压电材料的水热法制备和结构调控", 《硅酸盐学报》, vol. 42, no. 4, 30 April 2014 (2014-04-30), pages 432 - 436 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105817231A (en) * | 2016-04-12 | 2016-08-03 | 河海大学 | Preparation method of iron-loaded NaNbO3 perovskite photocatalyst |
| CN105817231B (en) * | 2016-04-12 | 2019-05-28 | 河海大学 | A kind of NaNbO of iron load3The preparation method of perovskite type photocatalyst |
| CN108660544A (en) * | 2018-03-30 | 2018-10-16 | 常州大学 | A kind of preparation method of semiconductor nano fiber |
| CN108660544B (en) * | 2018-03-30 | 2020-10-02 | 常州大学 | Preparation method of semiconductor nano-fiber |
| CN115924970A (en) * | 2022-09-19 | 2023-04-07 | 济南大学 | Potassium niobate nanowire and preparation method thereof |
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Application publication date: 20140910 |