CN104986795A - Method for obtaining Na0.5Bi0.5TiO3 and Na-Ti-O nanowire in hydrothermal condition by virtue of phase separation method - Google Patents
Method for obtaining Na0.5Bi0.5TiO3 and Na-Ti-O nanowire in hydrothermal condition by virtue of phase separation method Download PDFInfo
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Abstract
A method for obtaining Na0.5Bi0.5TiO3 and a Na-Ti-O nanowire in a hydrothermal condition by virtue of a phase separation method belongs to the technical field of preparation of a novel functional material. According to the method provided by the invention, Na0.5Bi0.5TiO3 and a Na-Ti-O one-dimensional nanostructure are generated simultaneously through concentration control over reaction raw materials; the Na0.5Bi0.5TiO3 and the Na-Ti-O one-dimensional nanostructure are successfully separated by virtue of a phase separation technology for the first time, so that simplification, and structure and performance research on a target product and an intermediate product are facilitated, and substantial development of a hydrothermal technique is promoted. The method disclosed by the invention comprises the steps: fully grinding bismuth nitrate in a mortar into fine powder; weighing titanium dioxide powder according to a stoichiometric relationship that the molar ratio of Bi toTi being 1:2; adding the titanium dioxide powder into a prepared sodium hydroxide solution and carrying out reaction for 60-70 hours at 200-220 DEG C; after reaction, cooling the solution to room temperature at a rate of 10 DEG C/h, wherein reactants are separated as a result of different densities; carrying out centrifugation and washing drying on the reactants to obtain the pure Na-Ti-O nanowire and Na0.5Bi0.5TiO3 nanopowder.
Description
Technical field:
The hydrothermal synthesis method of nano-powder, belongs to the preparing technical field of new function material.
Background technology:
High Temperature High Pressure hydro-thermal method prepares the important chemical synthesis process of nano-powder, and the pattern of its product and composition depend on the control of pH value and multiple factor such as pressure, temperature of reaction and time, reactant concn etc. in water-heat process.Compared with some traditional preparation means, have many advantages, as being relatively easy to component regulation and control, the diameter of particle of acquisition is little, narrowly distributing, and pattern is rich and varied; Some thing phase, low temperature isomr etc. that additive method is difficult to prepare can be prepared, be easy to retain metastable state, the intermediate state in water-heat process, explore new thing phase.
At present direct mixing, washing is all adopted to the post-processed of hydrothermal product, not yet have the method and report that target product and intermediate product are successfully separated.Thus the metastable state catching, obtain in hydrothermal product, especially some intermediate products, often with the mixed state powder of target product, are difficult to obtain single product.This can have influence on purity and the performance of target product on the one hand, is unfavorable for that the structure of generated metastable state intermediate product and character are probed on the other hand.
The present invention, in hydrothermal system, is controlled by reaction raw materials concentration, generates Na simultaneously
0.5bi
0.5tiO
3and Na-Ti-O one dimension Nano structure; And utilize thing phase detachment technique first, successfully the two is separated, obtains relatively pure Na
0.5bi
0.5tiO
3powder and Na-Ti-O nano wire; And further study optical property and the mechanical property of Na-Ti-O nanoscale; The developing of this technique is conducive to simplification and the properity research of target product and intermediate product, has promoted the substance development of hydrothermal technique.
Summary of the invention
Obtain Na under the invention provides a kind of high pressure water thermal rection condition simultaneously
0.5bi
0.5tiO
3and Na-Ti-O two kinds of products, and utilize thing phase detachment technique successfully by the method for two kinds of nano-powders separation.
Phase detachment technique under hydrothermal condition of the present invention, comprises following processing step:
Be separated under hydrothermal condition and obtain Na
0.5bi
4.5tiO
3and the method for Na-Ti-O nano wire, it is characterized in that, comprise the following steps:
1) take a certain amount of five water Bismuth trinitrates, and the amount of Bismuth trinitrate is 0.03-0.05mol/50ml water heating kettle; Bismuth trinitrate is fully ground to form thin powder in mortar; Be the stoichiometric relation of Bi:Ti=1:2 in molar ratio, take titanium dioxide powder;
2) sodium hydroxide solution of 12-24mol/L is configured;
3) by taking ground Bismuth trinitrate and titania powder, joining in the sodium hydroxide solution prepared, fully stirring, make it mix;
4) transfer in the reactor of tetrafluoroethylene by mixing solutions, compactedness is between 80%--85%; Then reactor is sealed in the hydro-thermal tank of steel, by hydro-thermal tank global transfer in Reaktionsofen, at 200-220 DEG C of temperature, reaction 60-70h;
5) after reaction terminates, be down to room temperature with the speed of 10 DEG C/h, obtain upper liquid and bottom solid product because density difference is separated;
6) outwell upper liquid, the white foam that bottom solid product is divided into upper strata loose and the muffin shape that lower floor compacts fine and closely woven, by two-layer stripping, be dispensed in different centrifuge tubes;
7) by centrifugal for the above-mentioned two kinds of powder deionized waters be obtained by reacting, washing drying, Na-Ti-O nano wire and Na is obtained respectively
0.5bi
4.5tiO
3nano powder.
By centrifugal for the above-mentioned powder deionized water be obtained by reacting, washing several, until final centrifuge tube liquid pH value is 7; Then dry, obtain dry pure nano-powder.
Beneficial effect of the present invention is:
The present invention utilizes simple equipment and technology controlling and process cleverly, and hydro-thermal reaction Midst density different two kinds of products are separated, and solves the difficulty that hydro-thermal reaction product in a lot of situation mixes.And obtain relatively pure Na-Ti-O nano wire and Na by one step hydro thermal method separation simultaneously first
0.5bi
0.5tiO
3nano powder.
Accompanying drawing explanation
The Na that Fig. 1 embodiment 1 obtains
0.5bi
0.5tiO
3and Na-Ti-O mixes the scanning electron microscope (SEM) photograph of nanometer product
The Na that Fig. 2 embodiment 2 thing phase separation method obtains
0.5bi
0.5tiO
3scanning electron microscope (SEM) photograph
The Na that Fig. 3 embodiment 2 thing phase separation method obtains
0.5bi
0.5tiO
3composition analysis
The scanning electron microscope (SEM) photograph of the Na-Ti-O nano wire that Fig. 4 embodiment 2 obtains
The transmission electron microscope picture of the Na-Ti-O nano wire that Fig. 5 embodiment 2 obtains
The composition analysis of the Na-Ti-O nano wire that Fig. 6 embodiment 2 obtains
Mechanics property analysis--the load-displacement curves of the Na-Ti-O nano wire obtained in Fig. 7 embodiment 2
Embodiment
Illustrate substantive distinguishing features of the present invention further below by embodiment, but the present invention is never only confined to following examples.Arranging of significant parameter involved in embodiment is as shown in the table:
Wherein temperature of reaction is selected at 200-220 DEG C, reactor compactedness 80-85%, to ensure when not damaging tetrafluoroethylene material reactor, one-tenth phase temperature necessary in reactor and pressure conditions.Reaction times is 60-70h, makes reaction raw materials under the growth in situ mechanism and dissolving crystallized machine-processed acting in conjunction of crystal, fully reacts.Mineralizer concentration can affect the solubleness of reactant, only when the effective concentration of reactant is greater than a corresponding minimum degree of supersaturation, just can cause nucleation and the growth of crystal, and affect nucleation rate and crystal morphology.Choose NaOH in the present invention simultaneously as Na source and mineralizer, under 12-24mol/L condition, resultant has good morphology controllable.The amount of Bismuth trinitrate is 0.03-0.05mol/50ml water heating kettle (Bi:Ti=1:2), Na-Ti-O one dimension Nano structure and Na within the scope of this
0.5bi
0.5tiO
3generate simultaneously.
The instrument that powder x-ray diffraction (XRD) collection of illustrative plates of product adopts be Bruker D-8Advance powder diffractometer (Cu K α radiation,
); Scanning electron microscope instrument is Hitachi S-3500 type scanning electronic microscope; Electron diffraction pattern and energy spectrometer spectrum instrument are JEM-2010 type transmission electron microscope and EDS annex thereof; Mechanics property analysis instrument is atomic force microscope.
Embodiment 1
Embodiment 1 does not adopt phase separation method, is the comparative example of embodiment 2.Take 0.04mol five water Bismuth trinitrate, Bismuth trinitrate is fully ground to form thin powder in mortar.Be the stoichiometric relation of Bi:Ti=1:2 in molar ratio, take titanium dioxide powder.The sodium hydroxide solution of preparation 16mol/L utilizes magnetic stirring apparatus to make it fully dissolve.By taking ground Bismuth trinitrate and titania powder, joining in the sodium hydroxide solution prepared, fully stirring, make it mix.Transferred to by mixing solutions in the reactor of the tetrafluoroethylene of 50ml, compactedness is 80%.Then reactor is sealed in the hydro-thermal tank of steel, ensures that it is in high-pressure sealed state.By hydro-thermal tank global transfer in Reaktionsofen, at 200 DEG C of temperature, reaction 60h.After reaching the reaction times, hydro-thermal tank is taken out from Reaktionsofen, by neutral to pH value for the solid-liquid mix products deionized water centrifuge washing obtained after room temperature cooling, dry, obtain Na-Ti-O nano wire and Na that impurity is less than 5%
0.5bi
0.5tiO
3the mix products of nano powder.
Embodiment 2
Take 0.04mol five water Bismuth trinitrate, Bismuth trinitrate is fully ground to form thin powder in mortar.Be the stoichiometric relation of Bi:Ti=1:2 in molar ratio, take titanium dioxide powder.The sodium hydroxide solution of preparation 16mol/L utilizes magnetic stirring apparatus to make it fully dissolve.By taking ground Bismuth trinitrate and titania powder, joining in the sodium hydroxide solution prepared, fully stirring, make it mix.Transferred to by mixing solutions in the reactor of the tetrafluoroethylene of 50ml, compactedness is 80%.Then reactor is sealed in the hydro-thermal tank of steel, ensures that it is in high-pressure sealed state.By hydro-thermal tank global transfer in Reaktionsofen, at 200 DEG C of temperature, reaction 60h.After reaction terminates, lower the temperature with the rate of temperature fall of 10 DEG C/h.After reaction terminates, outwell upper liquid, bottom solid product is divided into upper strata white foam and lower floor to compact fine and closely woven Na
0.5bi
0.5tiO
3nano powder, carefully by two-layer stripping, is dispensed in different centrifuge tubes.By centrifugal for the above-mentioned powder deionized water be obtained by reacting, wash to pH value neutral, dry, obtain pure Na-Ti-O nano wire and Na
0.5bi
0.5tiO
3nano powder.Compared with usual way, the Na-Ti-O nano wire that phase separation method obtains has better dispersiveness.
Embodiment 3
Take 0.03mol five water Bismuth trinitrate, Bismuth trinitrate is fully ground to form thin powder in mortar.Be the stoichiometric relation of Bi:Ti=1:2 in molar ratio, take titanium dioxide powder.The sodium hydroxide solution of preparation 12mol/L utilizes magnetic stirring apparatus to make it fully dissolve.By taking ground Bismuth trinitrate and titania powder, joining in the sodium hydroxide solution prepared, fully stirring, make it mix.Transferred to by mixing solutions in the reactor of the tetrafluoroethylene of 50ml, compactedness is 85%.Then reactor is sealed in the hydro-thermal tank of steel, ensures that it is in high-pressure sealed state.By hydro-thermal tank global transfer in Reaktionsofen, at 200 DEG C of temperature, reaction 60h.After reaction terminates, lower the temperature with the rate of temperature fall of 10 DEG C/h.After reaction terminates, outwell upper liquid, bottom solid product is divided into the fine and closely woven nano powder of upper strata white foam and lower floor, carefully by two-layer stripping, is dispensed in different centrifuge tubes.By centrifugal for the above-mentioned powder deionized water be obtained by reacting, wash to pH value neutral, dry, obtain pure Na-Ti-O nano wire and Na
0.5bi
0.5tiO
3nano powder.
Embodiment 4
Take 0.05mol five water Bismuth trinitrate, Bismuth trinitrate is fully ground to form thin powder in mortar.Be the stoichiometric relation of Bi:Ti=1:2 in molar ratio, take titanium dioxide powder.The sodium hydroxide solution of preparation 20mol/L utilizes magnetic stirring apparatus to make it fully dissolve.By taking ground Bismuth trinitrate and titania powder, joining in the sodium hydroxide solution prepared, fully stirring, make it mix.Transferred to by mixing solutions in the reactor of the tetrafluoroethylene of 50ml, compactedness is 80%.Then reactor is sealed in the hydro-thermal tank of steel, ensures that it is in high-pressure sealed state.By hydro-thermal tank global transfer in Reaktionsofen, at 220 DEG C of temperature, reaction 60h.After reaction terminates, lower the temperature with the rate of temperature fall of 10 DEG C/h.After reaction terminates, outwell upper liquid, bottom solid product is divided into the fine and closely woven nano powder of upper and lower two-layer white foam and lower floor, carefully by two-layer stripping, is dispensed in different centrifuge tubes.By centrifugal for the above-mentioned powder deionized water be obtained by reacting, wash to pH value neutral, dry, obtain pure Na-Ti-O nano wire and Na
0.5bi
0.5tiO
3nano powder.
Claims (1)
1. be separated under hydrothermal condition and obtain Na
0.5bi
4.5tiO
3and the method for Na-Ti-O nano wire, it is characterized in that, comprise the following steps:
1) take a certain amount of five water Bismuth trinitrates, and the amount of Bismuth trinitrate is 0.03-0.05mol/50ml water heating kettle; Bismuth trinitrate is fully ground to form thin powder in mortar; Be the stoichiometric relation of Bi:Ti=1:2 in molar ratio, take titanium dioxide powder;
2) sodium hydroxide solution of 12-24mol/L is configured;
3) by taking ground Bismuth trinitrate and titania powder, joining in the sodium hydroxide solution prepared, fully stirring, make it mix;
4) transfer in the reactor of tetrafluoroethylene by mixing solutions, compactedness is between 80%--85%; Then reactor is sealed in the hydro-thermal tank of steel, by hydro-thermal tank global transfer in Reaktionsofen, at 200-220 DEG C of temperature, reaction 60-70h;
5) after reaction terminates, be down to room temperature with the speed of 10 DEG C/h, obtain upper liquid and bottom solid product because density difference is separated;
6) outwell upper liquid, the white foam that bottom solid product is divided into upper strata loose and the muffin shape that lower floor compacts fine and closely woven, by two-layer stripping, be dispensed in different centrifuge tubes;
7) by centrifugal for the above-mentioned two kinds of powder deionized waters be obtained by reacting, washing drying, Na-Ti-O nano wire and Na is obtained respectively
0.5bi
4.5tiO
3nano powder.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105561966A (en) * | 2016-01-11 | 2016-05-11 | 黄冈师范学院 | Mesoporous zinc aluminate nanocrystalline catalyst, preparation method, and application thereof in phenol hydroxylation |
| CN107431200A (en) * | 2015-02-25 | 2017-12-01 | 新加坡国立大学 | Sodium-ion battery anode |
| CN109160540A (en) * | 2018-08-14 | 2019-01-08 | 沈阳工业大学 | A kind of method that two one-step hydrothermals prepares bismuth-sodium titanate spherical powder |
| CN109553127A (en) * | 2018-12-29 | 2019-04-02 | 陕西科技大学 | A kind of bismuth sodium titanate nanometer line and preparation method thereof of hydro-thermal method preparation |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101244933A (en) * | 2008-03-18 | 2008-08-20 | 中国科学院上海硅酸盐研究所 | Sheet bismuth sodium titanate mould plate grain and manufacture method thereof |
| CN102757220A (en) * | 2012-07-13 | 2012-10-31 | 北京工业大学 | Bi0.5, Na0.5 and TiO3 based ternary-system lead-free piezoelectric ceramic and preparation thereof |
-
2015
- 2015-07-19 CN CN201510425326.3A patent/CN104986795B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101244933A (en) * | 2008-03-18 | 2008-08-20 | 中国科学院上海硅酸盐研究所 | Sheet bismuth sodium titanate mould plate grain and manufacture method thereof |
| CN102757220A (en) * | 2012-07-13 | 2012-10-31 | 北京工业大学 | Bi0.5, Na0.5 and TiO3 based ternary-system lead-free piezoelectric ceramic and preparation thereof |
Non-Patent Citations (3)
| Title |
|---|
| 侯磊等: "水热法合成K0.5Bi0.5TiO3纳米陶瓷粉体", 《无机化学学报》, vol. 22, no. 3, 31 March 2006 (2006-03-31), pages 563 - 566 * |
| 徐明珠等: "二步水热法制备钛酸铋钠粉体的研究", 《压电与声光》, vol. 37, no. 1, 28 February 2015 (2015-02-28), pages 92 - 95 * |
| 苗鸿雁等: "水热法制备纳米Na0.5Bi0.5TiO3粉体", 《电子元件与材料》, vol. 23, no. 11, 30 November 2004 (2004-11-30), pages 16 - 19 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107431200A (en) * | 2015-02-25 | 2017-12-01 | 新加坡国立大学 | Sodium-ion battery anode |
| CN105561966A (en) * | 2016-01-11 | 2016-05-11 | 黄冈师范学院 | Mesoporous zinc aluminate nanocrystalline catalyst, preparation method, and application thereof in phenol hydroxylation |
| CN105561966B (en) * | 2016-01-11 | 2018-02-13 | 黄冈师范学院 | Mesoporous zinc aluminate nanocrystalline catalyst and its preparation method and the application in catalysis of phenol hydroxylating |
| CN109160540A (en) * | 2018-08-14 | 2019-01-08 | 沈阳工业大学 | A kind of method that two one-step hydrothermals prepares bismuth-sodium titanate spherical powder |
| CN109553127A (en) * | 2018-12-29 | 2019-04-02 | 陕西科技大学 | A kind of bismuth sodium titanate nanometer line and preparation method thereof of hydro-thermal method preparation |
| CN109553127B (en) * | 2018-12-29 | 2021-06-29 | 陕西科技大学 | Sodium bismuth titanate nanowire prepared by hydrothermal method and preparation method thereof |
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