CN103896338A - Method for preparing tungsten trioxide with regular hexagonal flaky morphology by using template method and application thereof - Google Patents
Method for preparing tungsten trioxide with regular hexagonal flaky morphology by using template method and application thereof Download PDFInfo
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- CN103896338A CN103896338A CN201410110388.0A CN201410110388A CN103896338A CN 103896338 A CN103896338 A CN 103896338A CN 201410110388 A CN201410110388 A CN 201410110388A CN 103896338 A CN103896338 A CN 103896338A
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Abstract
The invention relates to a method for preparing tungsten trioxide with regular hexagonal flaky morphology by using a template method. The material exhibits excellent gas sensing property on a hydrogen sulfide (H2S) gas. The invention belongs to the technical field of sensitive materials and gas sensors. According to the method provided by the invention, with an amino-functionalized NH2-SBA-15 with regular hexagonal flaky morphology as a template, hexagonal flaky tungsten trioxide with regular morphology is prepared. The prepared flaky tungsten trioxide exhibits excellent gas sensing property on the hydrogen sulfide (H2S) gas, the prepared hydrogen sulfide sensor has the advantages of high sensitivity, high selectivity, short response/recovery time and good repeatability. Meanwhile, by virtue of adjustable degeneration composed of a plurality of acids, the method can also be used for preparing nanometer metal oxides with other regular morphologies, thereby having positive significance on control of the growth of nanometer materials.
Description
Technical field
The present invention relates to a kind of method of utilizing template synthesis to there is the tungstic oxide of regular hexagonal flake pattern.This material is to hydrogen sulfide (H
2s) gas table reveals good gas-sensitive property.Belong to sensitive material and gas sensor technical field.
Technical background
The controllable growth of nano material, especially for preparation and the assembling of special appearance nano material, is focus and the difficult point of nano materials research in recent years.Due to its specific form and size, make them there is unique catalysis, nonlinear optics, semi-conductor and magnetic behavior, in various application, show unique advantage.Therefore, the nanocrystalline material of synthetic specific dimensions and pattern is all to have great significance aspect basic science or applied research.As important wide band gap semiconducter, tungstic oxide (WO
3) because of its unique physical properties and chemical property, be applicable to gas sensor, electrochromic device, the application such as photochemical catalysis and photoelectric device, are paid close attention to widely.WO
3complex structure own, thing is mutually various, to nano level WO
3the research of controlledly synthesis has caused people's broad interest, even to this day, such as nano wire, nanometer rod, the WO of the various patterns such as nanotube
3all be synthesized out.Prepare the WO of special appearance
3nano material method a lot, as chemical vapour deposition, electrochemical deposition, electrochemical anodic oxidation, collosol and gel and template etc.Template is a kind of important nanomaterial assembly method, its main thought is to adopt the material with certain pattern or pore passage structure as template, the nanoparticle of target material or presoma are covered in to the surface of template or insert the inner host-guest composite material that forms of template by there is certain interaction with template, under certain condition, nanoparticle or precursor are cross-linked with each other, after forming external phase, remove template, there is the pattern of the template of copying or the target material of pore passage structure thereby obtain.Template is as a kind of effective ways of preparing nano material, its principal feature is template no matter be the chemical reaction occurring in liquid phase or in gas phase, its reaction is all to carry out in the region of effectively controlling, the key distinction of template that Here it is and usual way.Template nano materials has plurality of advantages compared with directly synthesizing, and is mainly manifested in: size and dimension, structure and the character of 1. accurately controlling nano material taking template as carrier; 2. realize nano material and synthesize and being assembled into one, can solve the dispersion stabilization problem of nano material simultaneously; 3. building-up process is relatively simple, and a lot of methods are applicable to batch production [16].Utilize the duct of the regular arrangement of mesoporous nano material with being " microreactor " and carrier, aspect synthetic nanometer ball, cake, line and the block materials coming in every shape, there is unique advantage.
Based on above-mentioned thought, we are to have the amino functional NH of regular hexagonal flake pattern
2-SBA-15 is template, prepares the hexagonal flake tungstic oxide with regular morphology.Prepared sheet tungstic oxide is to hydrogen sulfide (H
2the advantages such as S) gas table reveals good gas-sensitive property, and prepared hydrogen sulfide sensor has highly sensitive, and selectivity is good, and response/time of recovery is short, reproducible.Utilize the adjustable sex change of polyacid composition, this method also may be used to prepare the nano-metal-oxide of other regular morphologies simultaneously, has positive effect for controlling nano material growth.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing template synthesis to there is the tungstic oxide of regular hexagonal flake pattern.Another object of the present invention is to provide a kind of to hydrogen sulfide (H
2s) gas table reveals the sensitive material of good gas-sensitive property.
The present invention is a kind of method based on template synthesis with the tungstic oxide of regular hexagonal flake pattern, it is characterized in that having following technological process and step:
A. hexagonal flake WO
3the preparation of presoma: the hexagonal flake mesoporous material silicon-dioxide SBA-15 after calcining vacuumizes heating 3 h at 180 DEG C, then above-mentioned 1～5mg SBA-15 is dispersed in the anhydrous toluene solution of the γ-aminopropyltrimethoxysilane (APTMS) that 15 ml concentration are 2-5%, reflux after 24 h sample is taken out, suction filtration, with dry toluene or alcohol solvent washing, then 60～85 DEG C of placement 1～3 h in baking oven, dry rear for subsequent use, this sample is designated as APTMS/SBA-15; In 10～20 mg APTMS/SBA-15, add 1～5 ml to contain 0.1 × 10
-3mol H
3pW
12o
40the alcoholic solution of (phospho-molybdic acid), 60 DEG C continue to stir after suction filtrations, and by a large amount of washing with alcohol three times, be then dried 30 h at 50 DEG C, obtain H
3pW
12o
40/ APTMS/SBA-15;
B. hexagonal flake WO
3the preparation of material: the H that above-mentioned reaction is obtained
3pW
12o
40/ APTMS/SBA-15 is heated to 500 DEG C from room temperature with temperature programming in retort furnace, and keeps 3 h in 500 DEG C of air, and the sample that obtains is designated as WO
3/ SBA-15; By WO
3/ SBA-15 dissolves in the HF aqueous solution, removes SBA-15 silicon oxide and obtains the pure jade-green WO that is
3.
The well-regulated hexagonal flake WO of a kind of template synthesis tool of the present invention
3purposes and application-manufacture H thereof
2s gas sensor; Its manufacture method is as follows: the WO that inserts a little above-mentioned preparation in agate mortar
3nanometer sheet, then splashes into a small amount of tamanori, is evenly applied to the vitrified pipe outside of gas sensor after furnishing pasty state, will scribble WO
3after the vitrified pipe of sensitive material is placed under infrared lamp and dries, in retort furnace, 300 ° of C calcine 3 h, for subsequent use after naturally cooling.Finally its 4 wire electrodes are welded on base, the element welding is placed on special agingtable, aging 240 h, make H
2s gas sensor.
The advantage and disadvantage of the QCM (Quartz Crystal Microbalance) formaldehyde sensor that the inventive method makes is as described below:
(1) use hexagonal flake SBA-15 as material of main part, carry out amino functional modification, be beneficial to diffusion and the transmission of guest materials APTMS in duct, avoided guest materials skewness, the too low problem of grafting amount in duct.Amino based on amino functional material surface can be with polyacid in conjunction with forming strong ionic linkage.Therefore can be by polyacid and the fixing synthetic WO of amino effect strong interaction
3presoma H
3pW
12o
40, so just can realize dispersed on carrier of presoma, the nanostructure of composite structure rule is laid a good foundation.Template NH used in this experimentation
2the well-regulated pattern of-SBA-15 tool and uniformly duct, make WO
3nanoparticle growth is subject to certain restrictions and along certain direction growth, finally in thermal decomposition process, has formed the WO of hexagonal flake
3.Utilize the adjustable sex change of polyacid composition, this method also may be used to prepare the nano-metal-oxide of other regular morphologies.
(2) prepared sheet tungstic oxide is to hydrogen sulfide (H
2the advantages such as S) gas table reveals good gas-sensitive property, and prepared hydrogen sulfide sensor has highly sensitive, and selectivity is good, and response/time of recovery is short, reproducible.
Brief description of the drawings
Fig. 1 be embodiment 1 hexagonal flake mesoporous material SBA-15 used the TEM photo of transmission electron microscope;
Fig. 2 is by the nitrogen adsorption desorption curve of SBA-15 after the mesoporous material SBA-15 of using in embodiment 1 and modification;
Fig. 3 is by mesoporous material SBA-15 used in embodiment 1 and modifies rear infared spectrum;
Fig. 4 is the hexagonal flake WO preparing by following embodiment 1
3the photo of transmission electron microscope and the photo of scanning electronic microscope;
Fig. 5 is the hexagonal flake WO preparing in embodiment 1
3the cyclic curve figure of sensitive material under hydrogen sulfide different concns.
Embodiment
Specific embodiments of the invention are as follows.
Embodiment mono-
Hexagonal flake WO
3and gas sensor preparation method, its process and step are as follows:
(1) hexagonal flake WO
3preparation: the hexagonal flake SBA-15 after calcining vacuumizes heating 1 h at 180 DEG C and removes wherein the moisture of absorption, then at its finishing γ-aminopropyltrimethoxysilane (APTMS); 5 mg SBA-15 are dispersed in the anhydrous toluene solution of 15ml (APTMS that concentration is 2-5%), after 24 h that reflux, sample are taken out to suction filtration, wash with anhydrous ethanol solvent, then 70 DEG C of placement 2 h in baking oven, to be dried rear for subsequent use, this sample is designated as APTMS/SBA-15; In 10 mg APTMS/SBA-15, add 2ml to contain 0.1 × 10
-3mol H
3pW
12o
40the alcoholic solution of (phospho-molybdic acid), continues to stir 28 h at 60 DEG C, and inclining and suction filtration, and with a large amount of alcohol washings three times, removes the polyacid of not grafting, is then dried 30 h at 50 DEG C, obtains H
3pW
12o
40/ APTMS/SBA-15.(2) hexagonal flake WO
3the preparation of material: the H that reaction is obtained
3pW
12o
40/ APTMS/SBA-15 is heated to 500 DEG C from room temperature with temperature programming in retort furnace, and keeps 3 h, and the sample that obtains is designated as WO
3/ SBA-15; By WO
3/ SBA-15 dissolves in the 5 ml HF aqueous solution, removes SBA-15 silicon oxide and obtains pure WO
3.Centrifugation after fully dissolving, by a large amount of methyl alcohol and washed with de-ionized water, finally obtains the pure jade-green WO that is
3.
Application-the H of product of the present invention
2the preparation of S gas sensor
In agate mortar, insert WO prepared by embodiment 1
3nanometer sheet, splashes into a small amount of tamanori after grinding evenly, after furnishing pasty state, is evenly applied to the vitrified pipe outside with Pt lead-in wire with bamboo let, scribbles WO
3after the vitrified pipe of sensitive material stands on and is placed in ceramic Noah's ark and dries under infrared lamp, in retort furnace, 300 ° of C calcining 1～6 h, to remove tamanori used in material, for subsequent use after naturally cooling.4 wire electrodes of the vitrified pipe that scribbles sensitive material are welded on base, then heater strip are passed from vitrified pipe and its two ends are also welded on base, make gas sensor.In order to improve the performance of device, increase the stability of element, the element welding is placed on special agingtable to aging 240 h.
To the detection of gained sample in above-described embodiment and the result of experiment referring to Fig. 1～5 in accompanying drawing.
Referring to Fig. 1, Fig. 1 is the transmission electron microscope photo of the SBA-15 of the present invention's hexagonal flake pattern used, can find out that from TEM the SBA-15 using this experiment all has hexagonal flake regular morphology, and homogeneous grain size.High-resolution TEM result shows that this sample has the hexagonal hole road structure of even rule.
Referring to accompanying drawing 2, as can be seen from the figure the SBA-15 before and after modifying all has IV type adsorption curve, prove that this material has typical linear pattern pore structure, illustrates that mesoporous material SBA-15 used has the duct of uniform and ordered, and before and after modifying, the duct of mesoporous material keeps good, and just its aperture and specific surface area diminish.
Referring to accompanying drawing 3, be SBA-15, APTMS/SBA-15 and WO
3the infrared spectrum of/SBA-15.As can be seen from the figure after functional amido, as shown in the figure, 1076 cm
-1with 803 cm
-1the absorption peak at place is to be caused by the stretching vibration of the Si-O-Si key of SBA-15 skeleton, 460 cm
-1the flexural vibration of the corresponding Si-O-Si key of absorption peak at place, 939 cm
-1the absorption peak at place is to be caused by the stretching vibration of terminal hydroxy group Si-OH.In sample, the absorption peak of c h bond appears at 2927 cm
-1place ,-NH
2the absorption peak of functional group appears at 1590 cm
-1with 1480 cm
-1place.Above result shows that the successful grafting of APTMS is to mesoporous material SBA-15.At WO
3in the infrared spectrum of/SBA-15 at 600 ~ 1000 cm
-1there is the absorption peak corresponding to W-O-W, meanwhile, at 1590 cm
-1with 1480 cm
-1place is corresponding to-NH
2the absorption peak of functional group disappears, and illustrates that phospho-wolframic acid has formed WO in calcination process in SBA-15 template
3.
Referring to accompanying drawing 4, be TEM photo and the XRD figure spectrum of synthetic sample, as can be seen from the figure, the WO as can be seen from the figure obtaining in this experiment
3with the capable looks of the well-regulated hexagonal flake of the same tool of template amino functional SBA-15 used, and homogeneous grain size.The peak of all XRD diffraction peaks that mark in figure and standard diagram (JCPDS No. 46-1096, a=7.521) is the consistent WO that belongs to Emission in Cubic completely
3.In figure, without obviously other impurity peaks appearance, interpret sample is single WO
3phase.
Referring to accompanying drawing 5, be WO
3the graph of a relation that the voltage of gas sensor prepared by nanometer sheet changes with concentration of hydrogen sulfide.As seen from the figure based on WO
3the voltage of gas sensor prepared by nanometer sheet increases with concentration of hydrogen sulfide, i.e. WO
3nanometer sheet raises along with the increase of concentration of hydrogen sulfide to the response of alcohol, almost linear.And from figure, it can also be seen that WO
3nanometer sheet is also relatively good to the repeatability of hydrogen sulfide response, and the response-recovery time is also very short.It responds and is respectively time of recovery 8 s and 11 s.
Claims (2)
1. template synthesis has a method for the tungstic oxide of regular hexagonal flake pattern, it is characterized in that having following process and step:
A. hexagonal flake WO
3the preparation of presoma: the hexagonal flake mesoporous material silicon-dioxide SBA-15 after calcining vacuumizes heating 3 h at 180 DEG C, then above-mentioned 1～5mg SBA-15 is dispersed in the anhydrous toluene solution of the γ-aminopropyltrimethoxysilane (APTMS) that 15 ml concentration are 2～5%, reflux after 24 h sample is taken out, suction filtration, with dry toluene or alcohol solvent washing, then 60～85 DEG C of placement 1～3 h in baking oven, dry rear for subsequent use, this sample is designated as APTMS/SBA-15; In 10～20 mg APTMS/SBA-15, add 1～5 ml to contain 0.1 × 10
-3mol H
3pW
12o
40the alcoholic solution of (phospho-molybdic acid), 60 DEG C continue to stir after suction filtrations, and by a large amount of washing with alcohol three times, be then dried 30 h at 50 DEG C, obtain H
3pW
12o
40/ APTMS/SBA-15;
B. hexagonal flake WO
3the preparation of material: the H that above-mentioned reaction is obtained
3pW
12o
40/ APTMS/SBA-15 is heated to 500 DEG C from room temperature with temperature programming in retort furnace, and keeps 3 h in 500 DEG C of air, and the sample that obtains is designated as WO
3/ SBA-15; By WO
3/ SBA-15 dissolves in the HF aqueous solution, removes SBA-15 silicon oxide and obtains the pure jade-green WO that is
3.
2. a template synthesis has regular hexagonal flake WO
3application-manufacture H
2s gas sensor; Its manufacture method is as follows: the WO that inserts a little above-mentioned preparation in agate mortar
3nanometer sheet, then splashes into a small amount of tamanori, is evenly applied to the vitrified pipe outside of gas sensor after furnishing pasty state, will scribble WO
3after the vitrified pipe of sensitive material is placed under infrared lamp and dries, in retort furnace, 300 ° of C calcine 3 h, for subsequent use after naturally cooling; Finally its 4 wire electrodes are welded on base, the element welding is placed on special agingtable, aging 240 h, make H
2s gas sensor.
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Cited By (6)
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|---|---|---|---|---|
| CN105004765A (en) * | 2015-07-02 | 2015-10-28 | 吉林大学 | Mesoporous CuO/SnO2 adsorption enhanced sensor, and detection method |
| CN105668638A (en) * | 2016-01-18 | 2016-06-15 | 郑州轻工业学院 | Nano-material and preparation method and application thereof |
| CN109809372A (en) * | 2019-03-26 | 2019-05-28 | 湘潭大学 | A method of two tungsten selenide nanobelt of single layer is prepared based on space confinement strategy |
| CN110743584A (en) * | 2019-10-14 | 2020-02-04 | 东北大学秦皇岛分校 | WO (WO)3Preparation and application of modified BiPO4 photocatalyst |
| CN111701590A (en) * | 2020-05-08 | 2020-09-25 | 广州大学 | Au (gold)xCubic WO3Photocatalyst and application thereof in preparing formaldehyde by photocatalysis of methane |
| CN112098473A (en) * | 2020-08-18 | 2020-12-18 | 国网河北省电力有限公司电力科学研究院 | Preparation method and evaluation method of sphere-like tungsten trioxide sensitive material and sulfur dioxide gas sensor |
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| CN105004765A (en) * | 2015-07-02 | 2015-10-28 | 吉林大学 | Mesoporous CuO/SnO2 adsorption enhanced sensor, and detection method |
| CN105004765B (en) * | 2015-07-02 | 2017-09-26 | 吉林大学 | Mesoporous CuO/SnO2Absorption sensitizing type sensor and detection method |
| CN105668638A (en) * | 2016-01-18 | 2016-06-15 | 郑州轻工业学院 | Nano-material and preparation method and application thereof |
| CN109809372A (en) * | 2019-03-26 | 2019-05-28 | 湘潭大学 | A method of two tungsten selenide nanobelt of single layer is prepared based on space confinement strategy |
| CN109809372B (en) * | 2019-03-26 | 2022-05-03 | 湘潭大学 | Method for preparing single-layer tungsten diselenide nanobelt based on space confinement strategy |
| CN110743584A (en) * | 2019-10-14 | 2020-02-04 | 东北大学秦皇岛分校 | WO (WO)3Preparation and application of modified BiPO4 photocatalyst |
| CN110743584B (en) * | 2019-10-14 | 2022-03-29 | 东北大学秦皇岛分校 | WO (WO)3Modified BiPO4Preparation method and application of photocatalyst |
| CN111701590A (en) * | 2020-05-08 | 2020-09-25 | 广州大学 | Au (gold)xCubic WO3Photocatalyst and application thereof in preparing formaldehyde by photocatalysis of methane |
| CN111701590B (en) * | 2020-05-08 | 2022-04-19 | 广州大学 | Au (gold)xCubic WO3Photocatalyst and application thereof in preparing formaldehyde by photocatalysis of methane |
| CN112098473A (en) * | 2020-08-18 | 2020-12-18 | 国网河北省电力有限公司电力科学研究院 | Preparation method and evaluation method of sphere-like tungsten trioxide sensitive material and sulfur dioxide gas sensor |
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Application publication date: 20140702 |