CN105271419A - Preparation method of tungstic oxide nanosheet self-assembled micro-nano flower-balls - Google Patents
Preparation method of tungstic oxide nanosheet self-assembled micro-nano flower-balls Download PDFInfo
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Abstract
The invention discloses a controllable preparation method of tungstic oxide nanosheet self-assembled micro-nano flower-balls. Tungstic oxide is an n-type wide-gap semiconductor oxide, has unique physical and chemical properties and is widely applied in fields of electrochromism, intelligent display, chemical sensing, supercapacitor and the like. By a hydro-thermal method, a tungsten source, an alcohols solvent and a surfactant react under a mild condition to synthesize high-purity cubic-phase ultrathin two-dimensional tungsten oxide nanosheet, and the nanosheet is further self-assmbled to obtain three-dimensional structured tungsten oxide micro-nano flower-balls with controllable dimension and uniform morphology. In comparison with existing preparation methods of tungsten oxide nanosheets and nanometer flower-balls, the method of the invention has advantages of mild experimental condition, low cost, simple preparation technology, good repeatability and the like.
Description
Technical field
The present invention relates to metal oxide semiconductor nano-material preparing technical field, particularly a kind of can be applicable to electrochromism, photochromic, intelligent display, chemical sensitisation and ultracapacitor tungstic oxide nano-sheets be self-assembled into the preparation method of micro-nano bouquet.
Background technology
Tungstic oxide crystalline structure belongs to ReO
3type, with uhligite ABO
3structure is very similar, and its desired crystal structure can be regarded as and be formed tungsten oxygen octahedra [WO by the W atom at center and 6 the O atoms be centered around around W atom
6] be formed by connecting through being total to summit, there are many spaces between octahedron, define various passage, and WO
6w in octahedron
6+ion usually departs from center and causes structure to deform, and has multiple crystalline phase.Tungstic oxide is a kind of N-shaped wide bandgap semiconductor oxide compound (energy gap is about 2.8eV), there is unique process based prediction model and be widely used, can be used as photocatalyst catalysis pollutent to decompose, as using gas sensor obnoxious flavour, as off-color material for the preparation of electrochromic device and photochromic device.
Low-dimension nano material attracts wide attention with performances such as the physics of its uniqueness, chemistry, electronics and mechanics, low-dimensional nano structure Tungsten oxide 99.999 (as nanometer rod, nano belt, nanotube, nanometer sheet etc.) is a kind of very important functional materials, and its performance and application and its microtexture and pattern have very large association.In recent years, owing to there is higher specific surface area and in electrochemistry and the potential application prospect of sensory field, the aspect such as preparation, performance and application of low-dimensional nanometer tungsten oxide obtains extensive research, and successfully prepares the nanostructure of various ways.Tungsten powder is oxidized to gaseous oxidation tungsten by the people such as Cao (JournalofMaterialsChemistry, 2009,19,2323-2327) under 1000 DEG C of high temperature, is then deposited on silicon chip, obtains the one dimension WO of oriented growth
3nano wire.(the SergeZhuiykov such as Balendhran, EugeneKats, BenjaminCarey, SivacarendranBalendhran, Nanoscale, 2014,6,15029 – 15036) with sodium wolframate, hydrogen peroxide, polythene PE G, nitric acid and perchloric acid for source material has prepared two dimensional oxidation tungsten nanometer sheet, this nanometer sheet carrier mobility reaches 319cm
2v
-1s
-1, and can be used for field-effect transistor.Chinese patent (201210377609.1) discloses a kind of method that thermal oxidation method prepares tungstic trioxide nano-slice; do not adopt any catalyzer; directly tungsten heating raw materials is incubated to certain temperature, under protection of inert gas, obtains tungstic trioxide nano-slice.
In recent years, Nanoscale assemblies system more and more receives publicity, and monodispersed metal or semi-conductor zero-dimensional quantum dots are assembled into the own comparative maturity of superstructure, and the assembling of current one dimension or two-dimensional nanostructure unit becomes the new focus of nano materials research just gradually.One dimension or two-dimensional nanostructure unit are assembled into three-dimensional even more senior structure in an orderly manner, can more effectively prepare function nano electron device.Chinese patent (201110110143.4) discloses a kind of tungstic oxide nano-sheets self-assembly microspheres and its preparation method and application, this technology adopts ultrasonic method successfully to prepare tungstic oxide nano-sheets under relatively mild condition, and is self-assembled into microballoon nitrogen peroxide to highly sensitive detection.But have not yet to see adopt hydrothermal method prepare tungstic oxide nano-sheets and be self-assembled into the report of micro-nano bouquet.
Summary of the invention
A kind of tungstic trioxide nano-slice is the object of the present invention is to provide to be self-assembled into the preparation method of micro-nano bouquet.
The technical solution realizing the object of the invention is: a kind of tungstic trioxide nano-slice is self-assembled into the preparation method of micro-nano bouquet, utilize hydrothermal method, with tungsten source, alcoholic solvent, tensio-active agent for raw material, by changing reaction times, temperature of reaction, reactant concn, obtain the two dimensional oxidation tungsten nanometer sheet of different size and thickness, nanometer sheet forms further by self-assembly the micro-nano bouquet of three-dimensional structure Tungsten oxide 99.999 that size is controlled and pattern is homogeneous, specifically comprises the following steps:
Step 1, in reaction vessel, add alcoholic solvent and tensio-active agent, mix to tensio-active agent and dissolve completely.The tensio-active agent added is pluronic F127 or pluronic P123, and the alcoholic solvent added is ethanol or methyl alcohol, and tensio-active agent and alcoholic solvent mass ratio are 1:150 ~ 1:30, mix and blend 15 ~ 20min.
Step 2, in reaction vessel, add tungsten source, deionized water mixes to solution and to turn yellow completely look, forms the colloid of stable homogeneous.The tungsten source added is WCl
6, the mass ratio of tungsten source and alcoholic solvent is 1:150 ~ 1:30, and the mass ratio of tungsten source and deionized water is 1:5 ~ 1:3, mix and blend 15 ~ 20min.
Step 3, the precursor solution in reaction vessel is transferred in reactor is warming up to design temperature, and be incubated.Reaction design temperature is 110 ~ 220 DEG C, and soaking time is 60 ~ 600min.
After step 4, reaction terminate, cool to room temperature with the furnace.
Step 5, removal reactor clear liquid at the middle and upper levels, repeatedly clean centrifugal by reactor bottoms organic solvent, be precipitated, the micro-nano bouquet that described precipitation is tungstic trioxide nano-slice self-assembly and is formed.Cleaning organic solvent used is ethanol or methyl alcohol, and centrifugal rotational speed is 7000 ~ 10000r/min, and centrifugation time is 2 ~ 4min, and cleaning centrifugal number of times is 3 ~ 6 times.
Compared with prior art, its remarkable advantage is in the present invention: the hydrothermal method that the present invention adopts has experiment condition gentleness, with low cost, and preparation technology is simple, easily control, reproducible, is easy to promote.The tungstic oxide nano-sheets size that the present invention obtains and pattern is homogeneous, size adjustable, the micro-nano bouquet size that nanometer sheet is assembled into is controlled, pattern is homogeneous.
Accompanying drawing explanation
Fig. 1 is the SEM figure of product tungsten trioxide nano bouquet prepared by invention example 1.
Fig. 2 is the TEM figure of product tungsten trioxide nano bouquet prepared by invention example 1.
Fig. 3 is the XRD figure of product tungsten trioxide nano bouquet prepared by invention example 1.
Fig. 4 is the SEM figure of product tungsten trioxide nano bouquet prepared by invention example 2.
Fig. 5 is the XRD figure of product tungsten trioxide nano bouquet prepared by invention example 2.
Fig. 6 is the SEM figure of product tungsten trioxide nano bouquet prepared by invention example 3.
Fig. 7 is the XRD figure of product tungsten trioxide nano bouquet prepared by invention example 3.
Fig. 8 is the SEM figure of product tungsten trioxide nano bouquet prepared by invention example 4.
Fig. 9 is the XRD figure of product tungsten trioxide nano bouquet prepared by invention example 4.
Figure 10 is the SEM figure of product tungsten trioxide nano bouquet prepared by invention example 5.
Figure 11 is the XRD figure of product tungsten trioxide nano bouquet prepared by invention example 5.
Figure 12 is the SEM figure of product tungsten trioxide nano bouquet prepared by invention example 6.
Figure 13 is the XRD figure of product tungsten trioxide nano bouquet prepared by invention example 6.
Embodiment
The preparation method that tungstic trioxide nano-slice of the present invention is self-assembled into micro-nano bouquet specifically adopts hydrothermal method, with tungsten source, alcoholic solvent, tensio-active agent for raw material, by changing reaction times, temperature of reaction, reactant concn, obtain the two dimensional oxidation tungsten nanometer sheet of different size and thickness, nanometer sheet forms further by self-assembly the micro-nano bouquet of three-dimensional structure Tungsten oxide 99.999 that size is controlled and pattern is homogeneous, specifically comprises the following steps:
Step 1, in reaction vessel, add alcoholic solvent and tensio-active agent, mix to tensio-active agent and dissolve completely; The tensio-active agent added is pluronic F127 or pluronic P123, and the alcoholic solvent added is ethanol or methyl alcohol, and tensio-active agent and alcoholic solvent mass ratio are 1:150 ~ 1:30, mix and blend 15 ~ 20min.
Step 2, in reaction vessel, add tungsten source, deionized water mixes to solution and to turn yellow completely look, forms the colloid of stable homogeneous; The tungsten source added is WCl
6, the mass ratio of tungsten source and alcoholic solvent is 1:150 ~ 1:30, and the mass ratio of tungsten source and deionized water is 1:5 ~ 1:3, mix and blend 15 ~ 20min.
Step 3, the precursor solution in reaction vessel is transferred in reactor is warming up to design temperature, and be incubated; Reaction design temperature is 110 ~ 220 DEG C, and soaking time is 60 ~ 600min.
After step 4, reaction terminate, reaction system cools to room temperature with the furnace;
Step 5, removal reactor clear liquid at the middle and upper levels, repeatedly clean centrifugal by reactor bottoms organic solvent, be precipitated, the micro-nano bouquet that described precipitation is tungstic trioxide nano-slice self-assembly and is formed.Cleaning organic solvent used is ethanol or methyl alcohol, and centrifugal rotational speed is 7000 ~ 10000r/min, and centrifugation time is 2 ~ 4min, and cleaning centrifugal number of times is 3 ~ 6 times.
Be described in more detail below in conjunction with embodiment:
Embodiment 1:
Adopt hydrothermal method, with tungsten source, alcoholic solvent and tensio-active agent for raw material, Reactive Synthesis Emission in Cubic, ultra-thin two-dimension tungstic oxide nano-sheets under the comparatively mild conditions, and be self-assembled into the homogeneous micro-nano bouquet of three-dimensional structure Tungsten oxide 99.999 of pattern further, concrete steps are as follows:
Step 1, in container, add 15g ethanol and 0.1g pluronic F127, mix to pluronic F127 and dissolve completely, solution is water white transparency.
Step 2, in container, add 0.2gWCl
6, 0.6g deionized water mixes to solution and becomes yellow, forms the tungstic oxide colloid of stable homogeneous.
Step 3, the precursor solution in reaction vessel is transferred in reactor is warming up to 110 DEG C, and be incubated 120min.
After step 4, reaction terminate, cool to room temperature with the furnace.
Step 5, removal supernatant liquid, by centrifugal for reactor bottoms ethanol purge 6 times, centrifugal rotational speed 7000r/min, centrifugation time 2min, is precipitated, and described precipitation is the nanometer bouquet of tungstic trioxide nano-slice self-assembly.
Phenetic analysis is carried out to the product of preparation, as shown in Figure 1, Figure 2, Figure 3 shows.Result shows the processing parameter according to embodiment 1, can obtain the Emission in Cubic WO that pattern is even, diameter is about 200-250nm
3nanometer bouquet; As can be seen from TEM, WO
3nanometer bouquet is formed by ultra-thin tungstic oxide nano-sheets self-assembly; Its diffraction peak and Emission in Cubic WO can be found out by XRD
3diffraction peak meet, there is higher purity and crystallinity.
Embodiment 2:
Adopt hydrothermal method, with tungsten source, alcoholic solvent and tensio-active agent for raw material, Reactive Synthesis Emission in Cubic, ultra-thin two-dimension tungstic oxide nano-sheets under the comparatively mild conditions, and be self-assembled into the homogeneous micro-nano bouquet of three-dimensional structure Tungsten oxide 99.999 of pattern further, concrete steps are as follows:
Step 1, in container, add 15g ethanol and 0.4g pluronic F127, mix to pluronic F127 and dissolve completely, solution is water white transparency.
Step 2, in container, add 0.2gWCl
6, 0.7g deionized water mixes to solution and becomes yellow, forms the tungstic oxide colloid of stable homogeneous.
Step 3, the precursor solution in reaction vessel is transferred in reactor is warming up to 110 DEG C, and be incubated 120min.
After step 4, reaction terminate, cool to room temperature with the furnace.
Step 5, removal supernatant liquid, by centrifugal for reactor bottoms ethanol purge 6 times, centrifugal rotational speed 7000r/min, centrifugation time 2min, is precipitated, and described precipitation is tungstic trioxide nano-slice self-assembled nanometer bouquet.
Phenetic analysis is carried out to the product of preparation, as shown in Figure 4, Figure 5.Result shows the processing parameter according to embodiment 2, can obtain the Emission in Cubic WO that pattern is even, size is homogeneous, diameter is about 300-350nm
3nanometer bouquet; Its diffraction peak and Emission in Cubic WO can be found out by XRD
3diffraction peak meet, there is higher purity and crystallinity.
Embodiment 3:
Adopt hydrothermal method, with tungsten source, alcoholic solvent and tensio-active agent for raw material, Reactive Synthesis Emission in Cubic, ultra-thin two-dimension tungstic oxide nano-sheets under the comparatively mild conditions, and be self-assembled into the homogeneous micro-nano bouquet of three-dimensional structure Tungsten oxide 99.999 of pattern further, concrete steps are as follows:
Step 1, in container, add 15g ethanol and 0.2g pluronic P123, mix to pluronic P123 and dissolve completely, solution is water white transparency.
Step 2, in container, add 0.2gWCl
6, 0.7g deionized water mixes to solution and becomes yellow, forms the tungstic oxide colloid of stable homogeneous.
Step 3, the precursor solution in reaction vessel is transferred in reactor is warming up to 220 DEG C, and be incubated 300min.
After step 4, reaction terminate, cool to room temperature with the furnace.
Step 5, removal supernatant liquid, by centrifugal for reactor bottoms ethanol purge 5 times, centrifugal rotational speed 8000r/min, centrifugation time 4min, is precipitated, and described precipitation is tungstic trioxide nano-slice self-assembled nanometer bouquet.
Phenetic analysis is carried out to the product of preparation, as shown in Figure 6, Figure 7.Result shows the processing parameter according to embodiment 3, can obtain the Emission in Cubic WO that pattern is even, size is homogeneous, diameter is about 220-250nm
3nanometer bouquet; Its diffraction peak and Emission in Cubic WO can be found out by XRD
3diffraction peak meet, there is higher purity and crystallinity.
Embodiment 4:
Adopt hydrothermal method, with tungsten source, alcoholic solvent and tensio-active agent for raw material, Reactive Synthesis Emission in Cubic, ultra-thin two-dimension tungstic oxide nano-sheets under the comparatively mild conditions, and be self-assembled into the homogeneous micro-nano bouquet of three-dimensional structure Tungsten oxide 99.999 of pattern further, concrete steps are as follows:
Step 1, in container, add 15g ethanol and 0.4g pluronic P123, mix to pluronic P123 and dissolve completely, solution is water white transparency.
Step 2, in container, add 0.2gWCl
6, 0.9g deionized water mixes to solution and becomes yellow, forms the tungstic oxide colloid of stable homogeneous.
Step 3, the precursor solution in reaction vessel is transferred in reactor is warming up to 160 DEG C, and be incubated 60min.
After step 4, reaction terminate, cool to room temperature with the furnace.
Step 5, removal supernatant liquid, by centrifugal for reactor bottoms ethanol purge 4 times, centrifugal rotational speed 10000r/min, centrifugation time 3min, is precipitated, and described precipitation is tungstic trioxide nano-slice self-assembled nanometer bouquet.
Phenetic analysis is carried out to the product of preparation, as shown in Figure 8, Figure 9.Result shows the processing parameter according to embodiment 4, can obtain the Emission in Cubic WO that pattern is even, size is homogeneous, diameter is about 140-160nm
3nanometer bouquet; Its diffraction peak and Emission in Cubic WO can be found out by XRD
3diffraction peak meet, there is higher purity and crystallinity.
Embodiment 5:
Adopt hydrothermal method, with tungsten source, alcoholic solvent and tensio-active agent for raw material, Reactive Synthesis Emission in Cubic, ultra-thin two-dimension tungstic oxide nano-sheets under the comparatively mild conditions, and be self-assembled into the homogeneous micro-nano bouquet of three-dimensional structure Tungsten oxide 99.999 of pattern further, concrete steps are as follows:
Step 1, in container, add 15g ethanol and 0.2g pluronic F127, mix to pluronic F127 and dissolve completely, solution is water white transparency.
Step 2, in container, add 0.2gWCl
6, 1.0g deionized water mixes to solution and becomes yellow, forms the tungstic oxide colloid of stable homogeneous.
Step 3, the precursor solution in reaction vessel is transferred in reactor is warming up to 110 DEG C, and be incubated 600min.
After step 4, reaction terminate, cool to room temperature with the furnace.
Step 5, removal supernatant liquid, by centrifugal for reactor bottoms ethanol purge 6 times, centrifugal rotational speed 8000r/min, centrifugation time 3min, is precipitated, and described precipitation is tungstic trioxide nano-slice self-assembled nanometer bouquet.
Phenetic analysis is carried out to the product of preparation, as shown in Figure 10, Figure 11.Result shows the processing parameter according to embodiment 5, can obtain the Emission in Cubic WO that pattern is even, size is homogeneous, diameter is about 120-150nm
3nanometer bouquet; Its diffraction peak and Emission in Cubic WO can be found out by XRD
3diffraction peak meet, there is higher purity and crystallinity.
Embodiment 6:
Adopt hydrothermal method, with tungsten source, alcoholic solvent and tensio-active agent for raw material, Reactive Synthesis Emission in Cubic, ultra-thin two-dimension tungstic oxide nano-sheets under the comparatively mild conditions, and be self-assembled into the homogeneous micro-nano bouquet of three-dimensional structure Tungsten oxide 99.999 of pattern further, concrete steps are as follows:
Step 1, in container, add 13g methyl alcohol and 0.1g pluronic F127, mix to pluronic F127 and dissolve completely, solution is water white transparency.
Step 2, in container, add 0.2gWCl
6, 0.6g deionized water mixes to solution and becomes yellow, forms the tungstic oxide colloid of stable homogeneous.
Step 3, the precursor solution in reaction vessel is transferred in reactor is warming up to 110 DEG C, and be incubated 120min.
After step 4, reaction terminate, cool to room temperature with the furnace.
Step 5, removal supernatant liquid, by centrifugal 6 times of product with methylalcohol cleaning bottom reactor, centrifugal rotational speed 7000r/min, centrifugation time 2min, is precipitated, and described precipitation is the nanometer bouquet of tungstic trioxide nano-slice self-assembly.
Phenetic analysis is carried out to the product of preparation, as shown in Figure 12 and Figure 13.Result shows the processing parameter according to embodiment 6, can obtain the Emission in Cubic WO that pattern is even, diameter is about 100-200nm
3nanometer bouquet; Its diffraction peak and Emission in Cubic WO can be found out by XRD
3diffraction peak meet, there is higher purity and crystallinity.
Embodiment 7 ~ 16:
Adopt hydrothermal method, with tungsten source, alcoholic solvent and tensio-active agent for raw material, Reactive Synthesis Emission in Cubic, ultra-thin two-dimension tungstic oxide nano-sheets under the comparatively mild conditions, and be self-assembled into the homogeneous micro-nano bouquet of three-dimensional structure Tungsten oxide 99.999 of pattern further, adopt the experimental procedure similar with example 1, change the parameters such as tungsten source addition, F127 addition, alcoholic solvent amount, amount of deionized water, soaking time, holding temperature, prepare the micro-nano bouquet of Tungsten oxide 99.999 of different size.Specific experiment parameter is as shown in the table.
Claims (5)
1. tungstic trioxide nano-slice is self-assembled into a preparation method for micro-nano bouquet, it is characterized in that, comprises the following steps:
Step 1, in reaction vessel, add alcoholic solvent and tensio-active agent, mix to tensio-active agent and dissolve completely;
Step 2, in reaction vessel, add tungsten source, deionized water, mix to solution and to turn yellow completely look, form the colloid of stable homogeneous;
Step 3, the precursor solution in reaction vessel is transferred in reactor is warming up to design temperature, and be incubated;
After step 4, reaction terminate, reaction system cools to room temperature with the furnace;
Step 5, removal reactor clear liquid at the middle and upper levels, by centrifugal for the cleaning of reactor bottoms organic solvent, be precipitated, the micro-nano bouquet that described precipitation is tungstic trioxide nano-slice self-assembly and is formed.
2. tungstic trioxide nano-slice according to claim 1 is self-assembled into the preparation method of micro-nano bouquet, it is characterized in that, the tensio-active agent added in step 1 is pluronic F127 or pluronic P123, the alcoholic solvent added is ethanol or methyl alcohol, tensio-active agent and alcoholic solvent mass ratio are 1:150 ~ 1:30, mix and blend 15 ~ 20min.
3. tungstic trioxide nano-slice according to claim 1 is self-assembled into the preparation method of micro-nano bouquet, it is characterized in that, the tungsten source added in step 2 is WCl
6, the mass ratio of tungsten source and alcoholic solvent is 1:150 ~ 1:30, and the mass ratio of tungsten source and deionized water is 1:5 ~ 1:3, mix and blend 15 ~ 20min.
4. tungstic trioxide nano-slice according to claim 1 is self-assembled into the preparation method of micro-nano bouquet, it is characterized in that, reacting design temperature in step 3 is 110 ~ 220 DEG C, and soaking time is 60 ~ 600min.
5. tungstic trioxide nano-slice according to claim 1 is self-assembled into the preparation method of micro-nano bouquet, it is characterized in that, cleaning organic solvent used in step 5 is ethanol or methyl alcohol, and centrifugal rotational speed is 7000 ~ 10000r/min, centrifugation time is 2 ~ 4min, and cleaning centrifugal number of times is 3 ~ 6 times.
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| CN107088407A (en) * | 2017-04-24 | 2017-08-25 | 陕西科技大学 | A kind of nano-sheet tungstic acid high efficiency photocatalyst and preparation method thereof |
| CN107482183A (en) * | 2017-07-14 | 2017-12-15 | 昆明理工大学 | A kind of preparation method of nano flower-like lithium ion battery negative material |
| CN107482183B (en) * | 2017-07-14 | 2020-04-07 | 昆明理工大学 | Preparation method of nanometer flower-shaped lithium ion battery negative electrode material |
| CN108859334A (en) * | 2018-06-08 | 2018-11-23 | 佛山市南海区佳妍内衣有限公司 | A kind of underwear with far-infrared functional |
| CN110282661A (en) * | 2019-07-09 | 2019-09-27 | 王干 | One kind being used for the classifying porous W of gas detection18O49Nanometer piece preparation method |
| CN111994957A (en) * | 2020-08-20 | 2020-11-27 | 临沂大学 | WO (WO)3Gas-sensitive material and preparation method and application thereof |
| CN112421007A (en) * | 2020-11-20 | 2021-02-26 | 贵州梅岭电源有限公司 | Preparation method of tungsten oxide/carbon flower-ball-shaped lithium battery composite negative electrode material |
| CN112421007B (en) * | 2020-11-20 | 2022-06-14 | 贵州梅岭电源有限公司 | Preparation method of tungsten oxide/carbon flower-ball-shaped lithium battery composite negative electrode material |
| CN112951608A (en) * | 2021-02-04 | 2021-06-11 | 山东大学 | Ultrathin leaf type WO3Preparation method of nanosheet array photoanode |
| CN113184912A (en) * | 2021-04-02 | 2021-07-30 | 北京工业大学 | Method for preparing hierarchical tungsten trioxide under assistance of microwaves |
| CN113184912B (en) * | 2021-04-02 | 2022-10-04 | 北京工业大学 | Method for preparing hierarchical tungsten trioxide with assistance of microwaves |
| CN113860374A (en) * | 2021-09-30 | 2021-12-31 | 郑州轻工业大学 | In-situ free-growing flower-shaped nano WO3Gas-sensitive material and preparation method and application thereof |
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