CN103539205A - Method for preparing controllable-morphology-and-size mixed-valence tungsten-based nanoparticles - Google Patents
Method for preparing controllable-morphology-and-size mixed-valence tungsten-based nanoparticles Download PDFInfo
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Abstract
The invention relates to a method for preparing controllable-morphology-and-size mixed-valence tungsten-based nanoparticles, belonging to the field of the preparation of inorganic oxide materials. The method comprises the steps of dissolving a tungsten source into organic straight-chain alcohol, mixing uniformly under magnetic stirring, then, transferring a solution to a reactor for crystallization reaction, and carrying out centrifugation, washing and vacuum drying on a powder sample after reaction, thereby obtaining a powder sample. According to the method, the synthesis steps are simple, and the obtained particles are uniform, are controllable in morphology and size and have excellent and stable near-infrared ray absorbing performance. According to the sample prepared by the method, the sample is a monoclinic-phase W18O49 nanocrystal, the size can be regulated and controlled between 50nm and 2,000nm, the form is uniform, the morphology can be nanowires, nanospheres, fusiform nanoparticles and columnar nanoparticles, and the chemical valence is of the coexistence of +4, +5 and +6. In addition, the sample prepared by the method has relatively strong near-infrared ray absorbing capacity.
Description
Technical field
The invention belongs to the preparation field of inorganic oxide material, relate to the preparation method of a kind of pattern and size adjustable mixed valence tungsten base nanoparticle.
Background technology
The tungsten base nanoparticle of mixed valence, is mainly reduction-state Tungsten oxide 99.999 (WO
3-x, x=0～0.375).Because tungsten ion in this compounds is with mixed valence (W
6+, W
5+and W
4+) form exist, therefore possess special electronic structure and photoelectric properties, this also makes this compounds have a wide range of applications, as field emission performance, electronics and ionic semiconductor, variable color components and parts, chemistry, biosensor, hot line protection and bio-light heat cure etc.In above-claimed cpd, W
18o
49it is the unique low oxygen value Tungsten oxide 99.999 compound can pure state existing being in the news.According to the literature, existing several different methods can be for the synthesis of W
18o
49nano-powder, but product pattern is one-dimensional material, as nano wire, nanotube etc.Meanwhile, synthesis step relates to pyroprocess more and uses chemical toxicity, expensive organic reagent that corrodibility is stronger.In recent years bibliographical information the synthetic W of hydrothermal method
18o
49nanoparticle, but synthetic method is divided into two steps, comprises Hydrothermal Synthesis and product is carried out to follow-up reduction processing, and this class methods complexity and product size are larger.Therefore, seek that the low temperature method that is easy to get directly obtains pattern, the controlled mixed valence tungsten of size base nanoparticle becomes very important.
Summary of the invention
For the problems referred to above, the invention provides the synthetic method of a kind of directly synthetic pattern, the controlled mixed valence tungsten of size base nanoparticle.
In synthetic method provided by the invention, reduction-state Tungsten oxide 99.999 W
18o
49(be WO
2.72) under solvent thermal condition, utilize organic alcohols for reductive agent, by controlling the kind of tungsten source, organic alcohols reductive agent and volumetric molar concentration, directly obtaining all controlled mixed valence tungsten base nanoparticles of pattern, size, concrete steps are as follows:
(1) tungsten source is dissolved in organic straight chain alcohol, controlling tungsten source concentration is 1～50mmol/L, after then mixing under magnetic agitation, move in reactor, 120～350 ℃ of crystallizations 1～48 hour, after reaction, powder sample is centrifugal, washing, vacuum-drying, obtains powder sample.
(2) adopt respectively the x-ray diffractometer (D/max-rB 12KW) of Rigaku Co., Ltd., 8 degrees/min of sweep velocitys, analytic sample crystalline structure and phase; Adopt the field transmission electron microscope (Tecnai G2F30 type) of U.S. FEI company, observe the microscopic appearance of nanoparticle; Adopt x-ray photoelectron power spectrum (XPS, Perkin Elmer PHI 5600), the surface composition of assay products and W4f bond energy; Adopt FDAC ultraviolet/Vis/NIR instrument (U-4100), analytic sample is in ultraviolet-visible-near infrared absorptive character.
In the present invention, described Organic Alcohol is ethanol, propyl alcohol or butanols.
In the present invention, described tungsten source is tungsten hexachloride, tungsten tetrachloride, ethanol tungsten (V) or ethanol tungsten (VI).
In the present invention, described reactor is hydrothermal reaction kettle or supercritical reaction still.
In the present invention, described vacuum-drying temperature is 20～150 ℃.
In the present invention, the valence state of tungsten ion with+4 ,+5 ,+6 coexist.
The significant advantage of above method is that its synthesis step is simple, the particle that obtains even, pattern and size are controlled, and possess excellence, stable near infrared ray absorbing energy.As shown in Fig. 1-14, sample prepared by the present invention is monoclinic phase W
18o
49nanocrystal, size can regulate and control between 50～2000 nm, form is even, pattern can be nano wire, nanometer ball, fusiformis nanoparticle, columnar nanometer particle, chemical valence state for+4 ,+5 ,+6 coexist.In addition, the prepared sample of the present invention has stronger near-infrared absorbing ability, and powder sample can effectively sponge the most of infrared light within the scope of 780～2500nm.
Accompanying drawing explanation
Fig. 1 is W
18o
49x-ray diffraction spectrogram;
Fig. 2 is the transmission electron microscope figure of fusiformis nanoparticle in embodiment 1;
Fig. 3 is the transmission electron microscope figure of flake nano particle in embodiment 2;
Fig. 4 is the transmission electron microscope figure of spherical nanoparticle in embodiment 3;
Fig. 5 is the transmission electron microscope figure of spherical nanoparticle in embodiment 4;
Fig. 6 is the transmission electron microscope figure of spherical nanoparticle in embodiment 5;
Fig. 7 is the transmission electron microscope figure of sea urchin type nanoparticle in embodiment 6;
Fig. 8 is the transmission electron microscope figure of nano wire in embodiment 7;
Fig. 9 is the transmission electron microscope figure of column nanometer brush in embodiment 8;
Figure 10 is the transmission electron microscope figure of barbed nanometer ball in embodiment 9;
Figure 11 is the transmission electron microscope figure of barbed nanometer ball in embodiment 10;
Figure 12 is the transmission electron microscope figure of barbed nanometer ball in embodiment 11;
Figure 13 is W
18o
49x-ray photoelectron energy spectrogram;
Figure 14 is W in embodiment 1
18o
49optical absorption spectrogram.
Embodiment
Below in conjunction with accompanying drawing, technical scheme of the present invention is further described; but be not limited to this; every technical solution of the present invention is modified or is equal to replacement, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
embodiment 1:
In this example, adopting tungsten hexachloride is tungsten source, and concentration is 15 mmol/L, and n-propyl alcohol is reductive agent, and concrete preparation process is as follows:
In 100 ml hydrothermal reaction kettles, add after 50 ml n-propyl alcohols, add 0.2976 g tungsten hexachloride powder, be at room temperature uniformly mixed, after solution mixes completely, sealed reactor, 200 ℃ of standing crystallization 22 h in baking oven.Centrifugation after cool to room temperature, successively with deionized water and alternately washing of dehydrated alcohol, after vacuum-drying, obtains mixed valence tungsten base nanoparticle powder.As shown in Figure 2, sample prepared by the present embodiment is fusiformis nanoparticle, and it is about 450 nm, middle part diameter 180 nm.
embodiment 2:
In this example, adopt ethanol tungsten (V) for tungsten source, concentration is 4.4 mmol/L, and ethanol is reductive agent, and concrete preparation process is as follows:
In 100 ml hydrothermal reaction kettles, add after 50ml dehydrated alcohol, be added dropwise to 0.09 g ethanol tungsten (V), be at room temperature uniformly mixed, after solution mixes completely, sealed reactor, 200 ℃ of standing crystallization 22 h in baking oven.Centrifugation after cool to room temperature, uses deionized water and absolute ethanol washing successively, after vacuum-drying, obtains mixed valence tungsten base nanoparticle powder.As shown in Figure 3, sample prepared by the present embodiment is flake nano particle, and its length and width is approximately 30 nm all.
embodiment 3:
In this example, adopt ethanol tungsten (V) for tungsten source, concentration is 10 mmol/L, and ethanol is reductive agent, and concrete preparation process is as follows:
In 100ml hydrothermal reaction kettle, add after 50ml dehydrated alcohol, be added dropwise to 0.2047 g ethanol tungsten (V), be at room temperature uniformly mixed, after solution mixes completely, sealed reactor, 200 ℃ of standing crystallization 22 h in baking oven.Centrifugation after cool to room temperature, uses deionized water and absolute ethanol washing successively, after vacuum-drying, obtains mixed valence tungsten base nanoparticle powder.As shown in Figure 4, sample prepared by the present embodiment is spherical nanoparticle, its diameter 130 nm.
embodiment 4:
In this example, adopt ethanol tungsten (V) for tungsten source, concentration is 15 mmol/L, and ethanol is reductive agent, and concrete preparation process is as follows:
In 100ml hydrothermal reaction kettle, add after 50ml dehydrated alcohol, be added dropwise to 0.3071 g ethanol tungsten (V), be at room temperature uniformly mixed, after solution mixes completely, sealed reactor, 200 ℃ of standing crystallization 22 h in baking oven.Centrifugation after cool to room temperature, uses deionized water and absolute ethanol washing successively, after vacuum-drying, obtains mixed valence tungsten base nanoparticle powder.As shown in Figure 5, sample prepared by the present embodiment is spherical nanoparticle, its diameter 180 nm.
embodiment 5:
In 100ml hydrothermal reaction kettle, add after 50ml dehydrated alcohol, be added dropwise to 0.8189 g ethanol tungsten (V), be at room temperature uniformly mixed, after solution mixes completely, sealed reactor, 200 ℃ of standing crystallization 22 h in baking oven.Centrifugation after cool to room temperature, uses deionized water and absolute ethanol washing successively, after vacuum-drying, obtains mixed valence tungsten base nanoparticle powder.As shown in Figure 6, sample prepared by the present embodiment is spherical nanoparticle, its diameter 550 nm.
embodiment 6:
In this example, adopting tungsten tetrachloride is tungsten source, and concentration is 4.4 mmol/L, and reductive agent is ethanol, and concrete preparation process is as follows:
In 100ml hydrothermal reaction kettle, add after 50ml dehydrated alcohol, add 0.0717 g tungsten tetrachloride, be at room temperature uniformly mixed, after solution mixes completely, sealed reactor, 200 ℃ of standing crystallization 22 h in baking oven.Centrifugation after cool to room temperature, uses deionized water and absolute ethanol washing successively, after vacuum-drying, obtains mixed valence tungsten base nanoparticle powder.As shown in Figure 7, sample prepared by the present embodiment is sea urchin type nanoparticle, its central diameter approximately 130 nm, peripheral diameter approximately 300 nm.
embodiment 7:
In this example, adopting tungsten tetrachloride is tungsten source, and concentration is 4.4 mmol/L, and reductive agent is n-propyl alcohol, and concrete preparation process is as follows:
In 100ml hydrothermal reaction kettle, add after 50ml n-propyl alcohol, add 0.0717 g tungsten tetrachloride, be at room temperature uniformly mixed, after solution mixes completely, sealed reactor, 200 ℃ of standing crystallization 22 h in baking oven.Centrifugation after cool to room temperature, uses deionized water and absolute ethanol washing successively, after vacuum-drying, obtains mixed valence tungsten base nanoparticle powder.As shown in Figure 8, sample prepared by the present embodiment is nano wire, and it is about 2 μ m, diameter 25 nm.
embodiment 8:
In this example, adopting tungsten tetrachloride is tungsten source, and concentration is 10 mmol/L, and reductive agent is n-propyl alcohol, and concrete preparation process is as follows:
In 100ml hydrothermal reaction kettle, add after 50ml n-propyl alcohol, add 0.1630 g tungsten tetrachloride, be at room temperature uniformly mixed, after solution mixes completely, sealed reactor, 200 ℃ of standing crystallization 22 h in baking oven.Centrifugation after cool to room temperature, uses deionized water and absolute ethanol washing successively, after vacuum-drying, obtains mixed valence tungsten base nanoparticle powder.As shown in Figure 9, sample prepared by the present embodiment is columnar nanometer brush, its diameter 200 nm, high approximately 500 nm.
embodiment 9:
In this example, adopting tungsten tetrachloride is tungsten source, and concentration is 15 mmol/L, and reductive agent is n-propyl alcohol,, concrete preparation process is as follows:
In 100ml hydrothermal reaction kettle, add after 50ml n-propyl alcohol, add 0.2444 g tungsten tetrachloride, be at room temperature uniformly mixed, after solution mixes completely, sealed reactor, 200 ℃ of standing crystallization 22 h in baking oven.Centrifugation after cool to room temperature, uses deionized water and absolute ethanol washing successively, after vacuum-drying, obtains mixed valence tungsten base nanoparticle powder.As shown in figure 10, sample prepared by the present embodiment is barbed nanometer ball, its diameter 250 nm.
embodiment 10:
In this example, adopt ethanol tungsten (VI) for tungsten source, concentration is 4.4 mmol/L, and reductive agent is dehydrated alcohol, and concrete preparation process is as follows:
In 100ml hydrothermal reaction kettle, add after 50ml dehydrated alcohol, add 0.1 g ethanol tungsten (VI), 60 ℃ of water-baths, be uniformly mixed approximately 15 minutes, after solution mixes completely, sealed reactor, 200 ℃ of standing crystallization 22 h in baking oven.Centrifugation after cool to room temperature, uses deionized water and absolute ethanol washing successively, after vacuum-drying, obtains mixed valence tungsten base nanoparticle powder.As shown in figure 11, sample prepared by the present embodiment is barbed nanometer ball, its diameter 80 nm.
embodiment 11:
In this example, adopt ethanol tungsten (VI) for tungsten source, concentration is 2.2 mmol/L, and reductive agent is dehydrated alcohol, and concrete preparation process is as follows:
In 100ml hydrothermal reaction kettle, add after 50ml dehydrated alcohol, add 0.05 g ethanol tungsten (VI), 60 ℃ of water-baths, be uniformly mixed approximately 15 minutes, after solution mixes completely, sealed reactor, 200 ℃ of standing crystallization 22 h in baking oven.Centrifugation after cool to room temperature, uses deionized water and absolute ethanol washing successively, after vacuum-drying, obtains mixed valence tungsten base nanoparticle powder.As shown in figure 12, sample prepared by the present embodiment is barbed nanometer ball, its diameter 50 nm.
embodiment 12:
In 100 ml hydrothermal reaction kettles, add after 50 ml propyl carbinols, add 0.2976 g tungsten hexachloride powder, be at room temperature uniformly mixed, after solution mixes completely, sealed reactor, 200 ℃ of standing crystallization 22 h in baking oven.Centrifugation after cool to room temperature, uses deionized water and absolute ethanol washing successively, after vacuum-drying, obtains mixed valence tungsten base nanoparticle powder.Sample prepared by the present embodiment is fusiformis nanoparticle, and it is about 500nm, middle part diameter 200 nm.
embodiment 13:
In 20 ml supercritical reaction stills, add after 10 ml propyl carbinols, add 0.1 g tungsten hexachloride powder, be at room temperature uniformly mixed, after solution mixes completely, sealed reactor, reactor heating to 350 ℃ crystallization 1 h.Centrifugation after cool to room temperature, uses deionized water and absolute ethanol washing successively, after vacuum-drying, obtains mixed valence tungsten base nanoparticle powder.Sample prepared by the present embodiment is rod-like nano particle, and it is about 50nm, middle part diameter 15 nm.
embodiment 14:
In this example, adopt ethanol tungsten (VI) for tungsten source, concentration is 50 mmol/L, and reductive agent is dehydrated alcohol, and concrete preparation process is as follows:
In 100 ml hydrothermal reaction kettles, add after 50 ml ethanol, add 1.1363 g tungsten hexachloride powders, be at room temperature uniformly mixed, after solution mixes completely, sealed reactor, 200 ℃ of standing crystallization 22 h in baking oven.Centrifugation after cool to room temperature, uses deionized water and absolute ethanol washing successively, after vacuum-drying, obtains mixed valence tungsten base nanoparticle powder.Sample prepared by the present embodiment is that diameter is the spherical particle of 2 μ m.
embodiment 15:
This example is W
18o
49the near-infrared absorbing aptitude tests of nano-powder, selected sample is fusiformis nanoparticle in example 1.The optical absorption curve (Figure 14) of measuring from UV-Vis-NIR spectrophotometer can find out, the nanoparticle of this compounds can produce stronger absorption to ultraviolet and most of near infrared light, and absorption value will be apparently higher than the absorption to visible region.
Claims (8)
1. the preparation method of the controlled mixed valence tungsten of pattern and size base nanoparticle, it is characterized in that described method steps is as follows: tungsten source is dissolved in organic straight chain alcohol, then after mixing under magnetic agitation, move in reactor, 120～350 ℃ of crystallizations 1～48 hour, after reaction, powder sample is centrifugal, washing, vacuum-drying, obtains mixed valence tungsten base nanoparticle.
2. the preparation method of the controlled mixed valence tungsten of pattern according to claim 1 and size base nanoparticle, is characterized in that described Organic Alcohol is ethanol, propyl alcohol or butanols.
3. the preparation method of the controlled mixed valence tungsten of pattern according to claim 1 and size base nanoparticle, is characterized in that described tungsten source is tungsten hexachloride, tungsten tetrachloride, ethanol tungsten or ethanol tungsten.
4. the preparation method of the controlled mixed valence tungsten of pattern according to claim 1 and size base nanoparticle, is characterized in that the size of described mixed valence tungsten base nanoparticle is between 50～2000 nm.
5. the preparation method of the controlled mixed valence tungsten of pattern according to claim 1 and size base nanoparticle, the pattern that it is characterized in that described mixed valence tungsten base nanoparticle is nano wire, nanometer ball, fusiformis nanoparticle or columnar nanometer particle.
6. the preparation method of the controlled mixed valence tungsten of pattern according to claim 1 and size base nanoparticle, is characterized in that described reactor is hydrothermal reaction kettle or supercritical reaction still.
7. the preparation method of the controlled mixed valence tungsten of pattern according to claim 1 and size base nanoparticle, is characterized in that described tungsten source concentration is 1～50mmol/L.
8. the preparation method of the controlled mixed valence tungsten of pattern according to claim 1 and size base nanoparticle, is characterized in that described vacuum-drying temperature is 20～150 ℃.
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| CN103818964A (en) * | 2014-02-27 | 2014-05-28 | 盐城工学院 | Preparation method for W18O49 ultrafine nanowire |
| CN103977789A (en) * | 2014-05-23 | 2014-08-13 | 福州大学 | W18O49 nanosphere peroxidase analogue and application thereof |
| CN105236491A (en) * | 2015-08-27 | 2016-01-13 | 陕西科技大学 | Preparation method of filament-like W18O49 material |
| CN105271421A (en) * | 2015-11-02 | 2016-01-27 | 哈尔滨工业大学 | Preparation method of tungsten-based nanosphere particle powder |
| CN105621488A (en) * | 2014-10-14 | 2016-06-01 | 台虹科技股份有限公司 | Method for producing infrared absorbing powder |
| CN106082344A (en) * | 2016-06-15 | 2016-11-09 | 中国科学技术大学 | A kind of preparation method of the defect state Tungstic anhydride. for photocatalysis aerobic coupling |
| CN106770494A (en) * | 2016-11-29 | 2017-05-31 | 中华人民共和国龙岩出入境检验检疫局 | A kind of novel acetone sensor with ultra-fine tungsten oxide nano wire as sensitive material |
| CN106745273A (en) * | 2016-11-22 | 2017-05-31 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of multilist planar defect tungsten oxide nanometer gas sensitive and preparation and application |
| CN107055618A (en) * | 2016-12-23 | 2017-08-18 | 青岛大学 | Method for simultaneously preparing tungsten oxide quantum dots and tungsten oxide nanowires |
| CN107831194A (en) * | 2017-10-30 | 2018-03-23 | 中国石油大学(华东) | A kind of nano line cluster WO sensitive to ammonia3‑W18O49Hetero-junction thin-film |
| CN110563042A (en) * | 2019-09-17 | 2019-12-13 | 西南交通大学 | Preparation method of oxygen-deficient tungsten oxide |
| CN111702902A (en) * | 2020-06-24 | 2020-09-25 | 王怀远 | Preparation method of wood-based selective near-infrared absorbing material |
| CN112588286A (en) * | 2020-12-11 | 2021-04-02 | 江苏大学 | Preparation method and application of carbon nanotube modified molybdenum-doped tungsten oxide catalyst |
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| CN103818964A (en) * | 2014-02-27 | 2014-05-28 | 盐城工学院 | Preparation method for W18O49 ultrafine nanowire |
| CN103977789A (en) * | 2014-05-23 | 2014-08-13 | 福州大学 | W18O49 nanosphere peroxidase analogue and application thereof |
| CN103977789B (en) * | 2014-05-23 | 2016-06-01 | 福州大学 | A kind of W18O49Nanometer ball peroxidase and application thereof |
| CN105621488B (en) * | 2014-10-14 | 2017-08-25 | 台虹科技股份有限公司 | Method for producing infrared absorbing powder |
| CN105621488A (en) * | 2014-10-14 | 2016-06-01 | 台虹科技股份有限公司 | Method for producing infrared absorbing powder |
| CN105236491A (en) * | 2015-08-27 | 2016-01-13 | 陕西科技大学 | Preparation method of filament-like W18O49 material |
| CN105271421A (en) * | 2015-11-02 | 2016-01-27 | 哈尔滨工业大学 | Preparation method of tungsten-based nanosphere particle powder |
| CN106082344A (en) * | 2016-06-15 | 2016-11-09 | 中国科学技术大学 | A kind of preparation method of the defect state Tungstic anhydride. for photocatalysis aerobic coupling |
| CN106082344B (en) * | 2016-06-15 | 2017-10-31 | 中国科学技术大学 | A kind of preparation method of defect state tungstic acid for the aerobic coupling of photocatalysis |
| CN106745273A (en) * | 2016-11-22 | 2017-05-31 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of multilist planar defect tungsten oxide nanometer gas sensitive and preparation and application |
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| CN107055618A (en) * | 2016-12-23 | 2017-08-18 | 青岛大学 | Method for simultaneously preparing tungsten oxide quantum dots and tungsten oxide nanowires |
| CN107055618B (en) * | 2016-12-23 | 2018-05-29 | 青岛大学 | Method for simultaneously preparing tungsten oxide quantum dots and tungsten oxide nanowires |
| CN107831194A (en) * | 2017-10-30 | 2018-03-23 | 中国石油大学(华东) | A kind of nano line cluster WO sensitive to ammonia3‑W18O49Hetero-junction thin-film |
| CN110563042A (en) * | 2019-09-17 | 2019-12-13 | 西南交通大学 | Preparation method of oxygen-deficient tungsten oxide |
| CN111702902A (en) * | 2020-06-24 | 2020-09-25 | 王怀远 | Preparation method of wood-based selective near-infrared absorbing material |
| CN112588286A (en) * | 2020-12-11 | 2021-04-02 | 江苏大学 | Preparation method and application of carbon nanotube modified molybdenum-doped tungsten oxide catalyst |
| CN112588286B (en) * | 2020-12-11 | 2023-07-18 | 江苏大学 | Preparation method and application of carbon nanotube modified molybdenum doped tungsten oxide catalyst |
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