CN102874875A - Nano-porous WO3 with ordered macroscopic structure and preparation method thereof - Google Patents
Nano-porous WO3 with ordered macroscopic structure and preparation method thereof Download PDFInfo
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- CN102874875A CN102874875A CN2012103751770A CN201210375177A CN102874875A CN 102874875 A CN102874875 A CN 102874875A CN 2012103751770 A CN2012103751770 A CN 2012103751770A CN 201210375177 A CN201210375177 A CN 201210375177A CN 102874875 A CN102874875 A CN 102874875A
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Abstract
The invention discloses nano-porous WO3 with ordered macroscopic structure and a preparation method thereof. Carbon nanofiber is synthesized based on macroscopic base material with ordered structure by chemical vapor deposition, and the synthetized carbon nanofiber is used as a template for synthetizing nano-porous WO3 with ordered macroscopic structure. The WO3 is 60-80wt% in bearing capacity and about 300-350nm in average grain size. The obtained nano-porous WO3 with ordered macroscopic structure has the advantages of fine orientation, and controllability in feature and structure. The preparation process is simple. The selected raw material sources are wide and low in cost. Therefore, production cost of the nano-porous WO3 with ordered macroscopic structure is reduced greatly.
Description
Technical field
This invention relates to a kind of nanoporous WO with orderly macrostructure
3And preparation method thereof, belong to field of inorganic materials.
Background technology
Tungstic oxide (WO
3) be a transition metal oxide that is widely studied, have the characteristics such as unique electrochromism, photochromic, gas-discoloration and catalysis because of it, can be applicable to flat-panel monitor, erasable Optical devices, smart windows, sensor and the fields such as energy storage and microwave material.In addition, WO
3Base and doped mixture also has katalysis.In recent years, relevant nanostructure WO
3Design and the report increase year after year of control growth aspect, synthesized at present WO
3Nanoparticle, nano wire, nanometer rod and mesoporous WO
3, its intermediary hole WO
3Be expected to bring into play more effective effect in above Application Areas.
About mesoporous WO
3Preparation, domestic and international more existing relevant reports.Its preparation method can be divided into two classes: a class is as template take the long-chain organism, tungsten hexachloride is the tungsten source, in ethanol, remove organic formwork agent by calcining or solvent extraction after the gelation and prepare the Tungsten oxide 99.999 mesoporous material, very easily cave in but Tungsten oxide 99.999 is mesoporous during high-temperature calcination, extract when removing organic formwork and utilize, need repeatedly extraction and very obstinate, simultaneous oxidation tungsten is difficult to sufficient crystallising, so these class methods finally are difficult to obtain preferably Tungsten oxide 99.999 mesoporous material of structure; Another kind of is hard template method, is template with mesoporous silicon oxide namely, makes Tungsten oxide 99.999 remove template with HF behind its mesoporous middle high temperature crystallization, and these class methods condition when removing template is gentle, and template is removed more thorough.And in recent years, towards application-specific, develop a kind of ordered structure oriented growth nanometer WO
3Technology of preparing,, favorable orientation a large amount of in the hope of obtaining, pattern and the controlled sample of structure then more and more receive numerous investigators' concern.
Carbon nano fiber is as a kind of novel carbon material, not only possesses excellent physics and chemistry stability, has also simultaneously that defects count is few, specific surface area large concurrently, advantages such as high ratio modulus, high specific strength, high conductivity and compact structure.In addition, carbon nano fiber is compared with carbon nanotube on cost and output and is had absolute advantage.Carbon nano fiber has been widely applied in fields such as aerospace, sports and amusement product, civil construction and communications and transportation at present.In addition, carbon nano fiber also has broad application prospects at aspects such as storage medium, electrode materials, support of the catalyst, high-efficiency adsorbent and matrix materials.Especially in recent years carbon nano fiber is as a kind of emerging mould material, and its application prospect is very wide.
Summary of the invention
One of purpose of this invention provides a kind of nanoporous WO with orderly macrostructure
3, namely adopt the regulation and control of carbon nano fiber mould plate technique to prepare nanoporous WO
3, simultaneously with nanometer WO
3Be solidificated on macroscopical body material of various ordered structures, and by optimizing preparation condition, finally can obtain the compound porous material of high quality ordered structure macroscopic view matrix and microscopic particles, have not yet to see the report of relevant this respect work.
Two of purpose of the present invention provides above-mentioned a kind of nanoporous WO with orderly macrostructure
3Concrete preparation method.
Technical scheme of the present invention
A kind of nanoporous WO with orderly macrostructure
3, be a kind of macroscopical matrix nano-porous materials mutually compound with microscopic particulate, WO
3Loading be 60-80 wt%, average grain size is about 300-350 nm, namely adopt chemical Vapor deposition process synthesis of nano carbon fiber on macroscopical body material of ordered structure, then make the synthetic nanoporous WO with orderly macrostructure of template with synthetic carbon nano fiber
3
Macroscopical body material of described ordered structure is rod-like fibre, honeycomb ceramic body or porous anodic alumina films (AAO) etc., and described rod-like fibre is preferably SiO
2Fiber.
Above-mentioned a kind of nanoporous WO with orderly macrostructure
3The preparation method, specifically comprise the steps:
(1), synthesis of nano carbon fiber template on macroscopical body material of ordered structure;
1., adopt pickling process to prepare macroscopical matrix integer catalyzer of NiO/ ordered structure:
0.2-0.5g macroscopic view body material is immersed in the Ni (NO of the 0.3moL/L take acetone as solvent
3)
2.6H
210min in the O solution, then vacuum filtration is in order to remove its surface excess solution, and cool to room temperature obtains macroscopical matrix integer catalyzer of NiO/ ordered structure after 300 ℃ of roastings;
In macroscopical matrix integer catalyzer of described NiO/ ordered structure the content of active ingredient Ni be ordered structure macroscopical body material 1%;
2., adopt vapour deposition process to prepare the carbon nano fiber template:
With step 1. in macroscopical matrix integer catalyzer of NiO/ ordered structure of gained put into the crystal reaction tube of the flat-temperature zone that places the chemical vapour deposition reaction device; pass into nitrogen protection reaction system is risen to 550～600 ℃ by room temperature, then pass into the CH that flow is 20-30 mL/min under the condition of normal pressure
4, C
2H
4Or CO gas carries out carbon nano fiber growth 2-3h, thereby is cooled to the carbon nano fiber template on macroscopical body material that room temperature obtains being solidificated in ordered structure after growth finishes under nitrogen atmosphere;
(2), the nanoporous WO that has orderly macrostructure
3Synthetic
It is the silicotungstic acid of 0.2-0.4moL/L or the C of tungsten chloride that carbon nano fiber template on the resulting macroscopical body material that is solidificated in ordered structure of step (1) is immersed in concentration
2H
510min is through vacuum filtration and 300 ℃ of drying treatment in the OH solution;
Repeat above-mentioned dipping, suction filtration and drying treatment process 3-4 time;
At last, the control temperature is that 600～650 ℃ of lower roastings are solidificated in the carbon nano fiber template on macroscopical body material of ordered structure with removal in air, finally obtains the nanoporous WO on a kind of macroscopical body material that is solidificated in ordered structure
3, the nanoporous WO that namely has orderly macrostructure
3
A kind of nanoporous WO with orderly macrostructure that the present invention obtains
3, be expected to bring into play more effective effect at its suitable application area.
Beneficial effect of the present invention
A kind of nanoporous WO with orderly macrostructure of the present invention
3Be a kind of macroscopical matrix porous material mutually compound with microscopic particulate, and have the controlled advantage of favorable orientation, pattern and structure, can be towards application-specific.
A kind of nanoporous WO with orderly macrostructure of the present invention
3Owing to adopt chemical Vapor deposition process (CVD) synthesis of nano carbon fiber template, its preparation technology is simple, with low cost and repeated high, condition by the control chemical vapour deposition can be regulated and control the formation of carbon nano fiber template effectively, therefore a kind of nanoporous WO with orderly macrostructure of the present invention
3The preparation method, it is simple to have preparation technology, selected starting material wide material sources, with low cost, so decrease its production cost.
Further, by the optimal preparation technology condition, finally can obtain high-quality a kind of nanoporous WO with orderly macrostructure
3, and have potential application prospect.
Description of drawings
Fig. 1 a, be solidificated in macroscopical body material SiO of ordered structure
2The scanning electron microscope diagram (amplifying 5000 times) of the carbon nano fiber on the fiber;
Fig. 1 b, be solidificated in macroscopical body material SiO of ordered structure
2The scanning electron microscope diagram (amplifying 30000 times) of the carbon nano fiber on the fiber;
Fig. 2, be solidificated in macroscopical body material SiO of ordered structure
2The X-ray powder diffraction of the carbon nano fiber on the fiber (XRD) diagram;
Fig. 3 a, be solidificated in macroscopical body material SiO of ordered structure
2Nanoporous WO on the fiber
3Scanning electron microscope diagram (amplifying 5000 times);
Fig. 3 b, be solidificated in macroscopical body material SiO of ordered structure
2Nanoporous WO on the fiber
3Scanning electron microscope diagram (amplifying 30000 times);
Fig. 4, be solidificated in macroscopical body material SiO of ordered structure
2Nanoporous WO on the fiber
3X-ray powder diffraction (XRD) diagram.
Embodiment
Below by embodiment and a kind of nanoporous WO with orderly macrostructure of by reference to the accompanying drawings this invention being provided
3Be described further, but do not limit the present invention.
The X-ray powder diffraction instrument that the present invention is used, model TG8120, Rigaku Co., Ltd.;
The field emission electron flying-spot microscope that the present invention is used, model JSM-7400, Japanese JEOL;
It is pure that the used all ingredients of the present invention is reagent, is Japanese Taihei, and Sangyo provides.
Embodiment 1
A kind of nanoporous WO with orderly macrostructure
3, namely at macroscopical body material SiO of ordered structure
2Loaded with nano porous WO on the fiber
3, nanoporous WO wherein
3Macroscopical body material SiO in ordered structure
2Loading is 80 wt% on the fiber, and average grain size is about 350 nm.
Above-mentioned a kind of nanoporous WO with orderly macrostructure
3The preparation method, specifically comprise the steps:
(1), at macroscopical body material SiO of ordered structure
2Synthesis of nano carbon fiber on the fiber;
1., at first adopt pickling process to prepare NiO/SiO
2The fabric integer catalyzer
Macroscopical body material SiO with the 0.2g ordered structure
2Fiber impregnation is at the Ni (NO of 0.3 moL/L take acetone as solvent
3)
2.6H
210min in the O solution, then vacuum filtration is in order to remove its surface excess solution, and cool to room temperature obtains NiO/SiO after 300 ℃ of roastings
2The fabric integer catalyzer;
2., secondly adopt chemical Vapor deposition process to prepare the carbon nano fiber template
With the NiO/SiO that obtains in 1.
2The fabric integer catalyzer is put into the crystal reaction tube of the flat-temperature zone that places the chemical vapour deposition reaction device, passes into nitrogen protection and reaction system is risen to 550 ℃ by room temperature, then passes into the CH that the 2h flow is 20 mL/min under the condition of normal pressure
4Gas carries out the carbon nano fiber growth, and the final reaction system is cooled to room temperature under nitrogen atmosphere, thereby obtains being solidificated in macroscopical body material SiO of ordered structure
2Carbon nano fiber template on the fiber;
The macroscopical body material SiO that is solidificated in ordered structure of gained
2The scanning electron microscope (SEM) photograph of the carbon nano fiber template on the fiber can find out respectively that from Fig. 1 a and Fig. 1 b the carbon nano fiber that adopts chemical Vapor deposition process to prepare can be in a large number and be solidificated in uniformly macroscopical body material SiO of ordered structure shown in Fig. 1 a and Fig. 1 b
2On the fiber, its diameter Distribution is between 40-70 nm.
The macroscopical body material SiO that is solidificated in ordered structure of gained
2The X-ray powder diffraction figure (XRD) of the carbon nano fiber template on the fiber as shown in Figure 2, can find out and very strong graphite master characteristic diffraction peak (corresponding (002) crystal face) near 2 θ=26.5 °, occur, and weak graphite characteristic diffraction peak (corresponding (101) crystal face) has appearred near 2 θ=43.1 °, this has confirmed that carbon nano fiber mainly exists with graphite carbon.In addition, ° have the characteristic diffraction peak (corresponding (111) crystal face) of simple substance Ni in 2 θ=44.8, this is because at the macroscopical body material SiO that adopts chemical Vapor deposition process in ordered structure
2In the process of synthesis of nano carbon fiber, the Ni catalyzer is not separated on the fiber, is present in the top of carbon nano fiber always;
(2), nanoporous WO
3At SiO
2Curing on the fiber-based material
Take by weighing the tungsten hexachloride of certain amount of substance and it is dissolved in C
2H
5Among the OH, preparation obtains tungsten hexachloride-C that tungsten ion concentration is 0.3 moL/L
2H
5OH solution;
The macroscopical body material SiO that is solidificated in ordered structure that step (1) is obtained
2The concentration that carbon nano fiber template on the fiber is immersed in above-mentioned gained is tungsten hexachloride-C of 0.3 moL/L
2H
510 min in the OH solution, then suction filtration is in order to removing its surface excess solution, after successively through 120 ℃ of dry 0.5h, 300 ℃ of dry 0.5h;
Repeat above-mentioned dipping, suction filtration and drying process 3 times;
Last in air 650 ℃ of lower roasting 5h be solidificated in macroscopical body material SiO of ordered structure in order to removal
2Carbon nano fiber template on the fiber namely obtains being solidificated in macroscopical body material SiO of ordered structure
2Nanoporous WO on the fiber
3, i.e. a kind of nanoporous WO with orderly macrostructure
3
The macroscopical body material SiO that is solidificated in ordered structure of gained
2Nanoporous WO on the fiber
3Scanning electron microscope (SEM) photograph shown in Fig. 3 a and Fig. 3 b, from Fig. 3 a and Fig. 3 b, can find out nanoporous WO respectively
3Also uniform coating load is at macroscopical body material SiO of ordered structure in a large number
2On the fiber, thereby obtain macroscopical matrix porous material mutually compound with microscopic particulate, (loading is 80 wt%).After the result shows that simultaneously the carbon nano fiber template is removed, the nanoporous WO that generates
3Have the pattern similar to the carbon nano fiber template, i.e. the pattern of copying nano carbon fiber template.
Measure the macroscopical body material SiO that is solidificated in ordered structure of (model TG8120, Rigaku Co., Ltd.) above-mentioned gained by X-ray powder instrument
2Nanoporous WO on the fiber
3, its X-ray powder diffraction pattern (XRD) can be found out and adopt the macroscopical body material SiO that is solidificated in ordered structure as shown in Figure 4
2The macroscopical body material SiO that is solidificated in ordered structure that carbon nano fiber template synthesis on the fiber obtains
2Nanoporous WO on the fiber
3WO has clearly appearred in the XRD spectra of sample
3Monoclinic crystal characteristic peak, and relatively purity is very high, this shows that the carbon nano fiber mould plate technique that adopts the macroscopical body material that is solidificated in ordered structure can prepare the nanoporous WO on the high-quality macroscopical body material that is solidificated in ordered structure
3
And by Scherrer formula (D=R λ/β cos θ, wherein D is particle dia, R is Scherrer constant (0.89), λ is incident X-ray wavelength (0.15406 nm), θ be diffraction angle (°), β is the peak width at half height of diffraction peak) further calculate and show, be solidificated in the nanoporous WO on macroscopical body material of ordered structure
3Average grain size is about 350 nm.
Embodiment 2
A kind of nanoporous WO with orderly macrostructure
3, namely at the upper loaded with nano porous WO of macroscopical body material porous anodic alumina films (AAO) of ordered structure
3, nanoporous WO wherein
3Loading on macroscopical body material porous anodic alumina films of ordered structure is 60 wt%, and average grain size is about 300nm.
Above-mentioned a kind of nanoporous WO with orderly macrostructure
3The preparation method, specifically may further comprise the steps:
(1), at the upper synthesis of nano carbon fiber of macroscopical body material porous anodic alumina films (AAO) of ordered structure;
1., at first adopt pickling process to prepare the NiO/AAO integer catalyzer
Macroscopical body material AAO of 0.3g ordered structure is immersed in the Ni (NO of 0.3 moL/L take acetone as solvent
3)
2.6H
210 min in the O solution, then vacuum filtration is in order to remove its surface excess solution, and cool to room temperature obtains the NiO/AAO integer catalyzer after 300 ℃ of roastings;
2., secondly adopt chemical Vapor deposition process to prepare the carbon nano fiber template
NiO/AAO integer catalyzer obtained above is put into the crystal reaction tube of the flat-temperature zone that places the chemical vapour deposition reaction device, pass into nitrogen protection reaction system is risen to 600 ℃ by room temperature, then pass into the C that the 2h flow is 25mL/min under the condition of normal pressure
2H
4Gas carries out carbon nano fiber growth, thereby the final reaction system is cooled to the carbon nano fiber template on macroscopical body material AAO that room temperature obtains being solidificated in ordered structure under nitrogen atmosphere;
(2), nanoporous WO
3Curing on macroscopical body material AAO of ordered structure
Take by weighing the tungsten hexachloride of certain amount of substance and it is dissolved in C
2H
5Among the OH, preparation obtains tungsten hexachloride-C that tungsten ion concentration is 0.2 moL/L
2H
5OH solution;
1. the carbon nano fiber template on the macroscopical body material AAO that is solidificated in ordered structure that obtains is immersed in the tungsten hexachloride-C of above-mentioned gained
2 H
510 min in the OH solution, then suction filtration is in order to removing its surface excess solution, after successively through 120 ℃ of dry 0.5h, 300 ℃ of dry 0.5h;
Repeat above-mentioned dipping, suction filtration and drying process 3 times;
Last in air 650 ℃ of lower roasting 5h be solidificated in carbon nano fiber template on macroscopical body material AAO of ordered structure in order to removal, obtain being solidificated in the nanoporous WO on macroscopical body material AAO of ordered structure
3, i.e. a kind of nanoporous WO with orderly macrostructure
3
Embodiment 3
A kind of nanoporous WO with orderly macrostructure
3, this material is the nanoporous WO of load on macroscopical body material honeycomb ceramic body of ordered structure
3, nanoporous WO wherein
3Loading on macroscopical body material honeycomb ceramic body of ordered structure is 70 wt%, and average grain size is about 320nm.
Above-mentioned a kind of nanoporous WO with orderly macrostructure
3The preparation method, specifically may further comprise the steps:
(1), synthesis of nano carbon fiber on macroscopical body material honeycomb ceramic body of ordered structure;
1., at first adopt pickling process to prepare NiO/ honeycomb ceramic body integer catalyzer
Macroscopical body material honeycomb ceramic body of 0.5g ordered structure is immersed in the Ni (NO of the 0.3moL/L take acetone as solvent
3)
2.6H
210 min in the O solution, then vacuum filtration is in order to remove its surface excess solution, and cool to room temperature obtains NiO/ honeycomb ceramic body integer catalyzer after 300 ℃ of roastings;
2., secondly adopt chemical Vapor deposition process to prepare the carbon nano fiber template
1. the NiO/ ceramic honey comb body catalyst that obtains is put into the crystal reaction tube of the flat-temperature zone that places the chemical vapour deposition reaction device, pass into nitrogen protection and reaction system is risen to 550 ℃ by room temperature, then the CO gas that passes into the 2h flow under the condition of normal pressure and be 30mL/min carries out the carbon nano fiber growth, thereby the final reaction system is cooled to the carbon nano fiber template on macroscopical body material honeycomb ceramic body that room temperature obtains being solidificated in ordered structure under nitrogen atmosphere;
(2), nanoporous WO
3Curing on the honeycomb ceramic body body material
Take by weighing the tungsten hexachloride of certain amount of substance and it is dissolved in C
2H
5Among the OH, preparation obtains tungsten hexachloride-C that tungsten ion concentration is 0.4moL/L
2H
5OH solution;
Carbon nano fiber template on the macroscopical body material honeycomb ceramic body that is solidificated in ordered structure that step (1) is obtained is immersed in tungsten hexachloride-C obtained above
2H
5OH solution 10 min, then suction filtration is in order to removing its surface excess solution, after successively through 120 ℃ of dry 0.5h, 300 ℃ of dry 0.5h;
Repeat above-mentioned dipping, suction filtration and drying process 3 times;
Last in air 650 ℃ of lower roasting 5h be solidificated in carbon nano fiber template on macroscopical body material honeycomb ceramic body of ordered structure in order to removal, obtain being solidificated in the nanoporous WO on macroscopical body material honeycomb ceramic body of ordered structure
3, i.e. a kind of nanoporous WO with orderly macrostructure
3
Can find out by above-described embodiment, adopt the macroscopical body material carbon nano fiber mould plate technique be solidificated in ordered structure can be with nanoporous WO
3Be solidificated on macroscopical body material of ordered structure.By optimizing preparation condition, finally can obtain the compound porous material of high quality ordered structure macroscopic view matrix and microscopic particles, such material has potential application prospect.
In addition, this invention equipment is simple, operational condition is easy to control, repeatability is high, with low cost, economic results in society are remarkable, is conducive to it and applies.
The above only is giving an example of embodiments of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.
Claims (3)
1. nanoporous WO with orderly macrostructure
3, it is characterized in that namely adopting chemical Vapor deposition process synthesis of nano carbon fiber on macroscopical body material of ordered structure, then make the synthetic nanoporous WO with orderly macrostructure of template with synthetic carbon nano fiber
3
Macroscopical body material of described ordered structure is rod-like fibre, honeycomb ceramic body or porous anodic alumina films (AAO);
Described nanoporous WO with orderly macrostructure
3, nanoporous WO
3Loading be 60-80wt%, average grain size is about 300-350nm.
2. a kind of nanoporous WO with orderly macrostructure as claimed in claim 1
3, it is characterized in that described rod-like fibre is SiO
2Fiber.
3. a kind of nanoporous WO with orderly macrostructure as claimed in claim 1 or 2
3The preparation method, it is characterized in that specifically comprising the steps:
(1), synthesis of nano carbon fiber template on macroscopical body material of ordered structure;
1., adopt pickling process to prepare macroscopical matrix integer catalyzer of NiO/ ordered structure:
0.2-0.5g macroscopic view body material is immersed in the Ni (NO of 0.3 moL/L take acetone as solvent
3)
2.6H
210 min in the O solution, vacuum filtration then, cool to room temperature after 300 ℃ of roastings obtains macroscopical matrix integer catalyzer of NiO/ ordered structure;
In macroscopical matrix integer catalyzer of described NiO/ ordered structure the content of active ingredient Ni be ordered structure macroscopical body material 1%;
2., adopt vapour deposition process to prepare the carbon nano fiber template:
With step 1. in macroscopical matrix integer catalyzer of NiO/ ordered structure of gained put into the crystal reaction tube of the flat-temperature zone that places the chemical vapour deposition reaction device; pass into nitrogen protection and reaction system is risen to 550～600 ℃ by room temperature, then pass into the CH that flow is 20-30 mL/min under the condition of normal pressure
4, C
2H
4Or CO gas 2-3h, under nitrogen atmosphere, be cooled to room temperature, namely get the carbon nano fiber template on the macroscopical body material that is solidificated in ordered structure;
(2), the nanoporous WO that has orderly macrostructure
3Synthetic
Carbon nano fiber template on the resulting macroscopical body material that is solidificated in ordered structure of step (1) is immersed in the C that concentration is 0.2-0.4 moL/L silicotungstic acid or tungsten chloride
2H
510 min in the OH solution are through vacuum filtration and 300 ℃ of drying treatment;
Repeat above-mentioned dipping, suction filtration and drying treatment process 3-4 time;
At last, 600～650 ℃ of lower roastings in air finally obtain being solidificated in the nanoporous WO on macroscopical body material of ordered structure
3, i.e. a kind of nanoporous WO with orderly macrostructure
3
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| CN104198531A (en) * | 2014-09-01 | 2014-12-10 | 郑州大学 | Composite gas sensitive material with multilevel structure and preparation method thereof |
| CN109975327A (en) * | 2019-04-04 | 2019-07-05 | 王琮 | Lung cancer early diagnosis microwave respiration transducer and preparation method thereof based on semiconductor microactuator processing technology |
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| CN104198531A (en) * | 2014-09-01 | 2014-12-10 | 郑州大学 | Composite gas sensitive material with multilevel structure and preparation method thereof |
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| CN109975327A (en) * | 2019-04-04 | 2019-07-05 | 王琮 | Lung cancer early diagnosis microwave respiration transducer and preparation method thereof based on semiconductor microactuator processing technology |
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