CN110282661A - One kind being used for the classifying porous W of gas detection18O49Nanometer piece preparation method - Google Patents
One kind being used for the classifying porous W of gas detection18O49Nanometer piece preparation method Download PDFInfo
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- CN110282661A CN110282661A CN201910616647.XA CN201910616647A CN110282661A CN 110282661 A CN110282661 A CN 110282661A CN 201910616647 A CN201910616647 A CN 201910616647A CN 110282661 A CN110282661 A CN 110282661A
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- classifying porous
- nanometer sheet
- gas detection
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/02—Oxides; Hydroxides
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
Abstract
A kind of classifying porous W for gas detection18O49Block copolymer micropore template P123: being first dispersed in dehydrated alcohol by the preparation method of nanometer sheet, step are as follows: S1 under strong agitation, and charcoal ball of the addition partial size in 20-50nm is several, continues to stir, until being uniformly dispersed；S2: preparing the mixed solution of dehydrated alcohol and deionized water with the ratio of volume ratio 1:0.1-0.2, and tungsten source and Surfactant CTAB are added thereto, and later, which is continued stirring 0.5 hour or more；S3: the mixed templates prepared in step S1 are added slowly in the precursor solution in step S2, hydrothermal reaction kettle is transferred to, react 10-18h at 100-140 DEG C；After reaction, reaction product separated, washed, dried；Later, product is laid in corundum crucible, heats up in air atmosphere and product is sintered, remove template therein, product can be obtained.
Description
Technical field
The present invention relates to a kind of field of functional materials, specifically a kind of material preparation and application neck for gas detection
Domain.
Background technique
Gas sensitive is a kind of functional material in industrial and agricultural production with important value, normal to its evaluation index
Including sensitivity, cyclical stability, selectivity, responsiveness and repeatability etc..Metal oxide semiconductor is as gas sensitive
One kind having huge potentiality, and cardinal principle is absorption-desorption and catalysis by sensor material surface gas molecule
The chemical action on reaction process, realization gas molecule and its surface will lead to the variation of conductivity, so as to cause electrical signal
The detection of pernicious gas molecule is realized in variation.In numerous metal oxide semiconductors, studying more has zinc oxide, oxygen
Change iron, titanium oxide and tungsten oxide etc., wherein tungsten oxide is a kind of important n-type semiconductor, is commonly used for the inspection of multiple gases
It surveys, such as detects indoor air pollutants, detect toxic, the inflammable or explosive gas in mine, other application further includes medicine
Diagnosis, such as the research to exhalation acetone.
Sizable effort has been made in research for tungsten oxide, researcher.However, traditional synthetic method, such as
Chemical vapor deposition, spray pyrolysis and precipitation reaction, it will usually the nano particle with defect sturcture, small surface area is generated,
It is highly detrimental to air-sensitive application in this way.Soft template synthetic method is using surfactant or amphipathic nature block polymer as template and pore-forming
Agent, and the mesoporous material with heterogeneity is developed accordingly.It is this to have both multi-functional and flexible supramolecular assembly device, make
Aperture, pore structure, hole connectivity etc. can flexibly be efficiently controlled by obtaining this method.
W18O49It is a kind of novel tungsten oxide nanometer material, there is unique fault of construction and pattern, in air-sensitive, electroluminescent
The fields such as discoloration and infrared absorption have huge application potential.As Jianwei Liu et al. people sends out on " Nano Letters "
Article " the ultrathin W of table18O49Nanowire assemblies for electrochromic devices " is open
A kind of W of ultra-fine overlength18O49The preparation method of nano wire, and single thin film is obtained by the method that LB is assembled and is answered
For electrochromic devices, preferable effect is realized.And the paper of Gu Lingjun " is based on W18O49Surface-enhanced Raman dissipate
Penetrate performance and mechanism study ", W is prepared by hydro-thermal method18O49And its SERS performance is studied as substrate, it tests not
With the SERS spectra of the R6G of concentration, discovery is reduced with R6G concentration, and enhancement factor is gradually increased, and finally found that W18O49To R6G
Detectable limit concentration reach 10-7M illustrates W18O49There is very strong SERS effect as R6G of the substrate to low concentration.Also
For example Shaanxi Tech Univ Huang Jianfeng et al. discloses a kind of W in patent document CN109731580A18O49/ NF self-supporting electricity
Catalysis material obtains solution A by the way that tungsten source to be added in mixed alcohol；The pure ethylenediamine of analysis is added into solution A and cycloheptylamine obtains
To solution B；Solution B is poured into polytetrafluoroethyllining lining autoclave, then nickel foam is put into poly- four containing solution B
Hydro-thermal reaction is carried out in vinyl fluoride reaction kettle, is cooled to room temperature after reaction, and the centrifugation of end reaction object dehydrated alcohol is washed
It washs, W is dried to obtain to the substance after centrifuge washing18O49/ NF self-supporting electrocatalysis material.Up to now, also few researchs
Personnel are to W18O49Nano material carries out organizational structure design, to be applied to field of gas detection.
Summary of the invention
Based on the above issues, it is an object of the invention to propose a kind of completely new synthetic route by change reaction process,
To W18O49The structure of nanometer sheet carries out original design, can show preferably to examine to be applied to field of gas detection
Survey performance.
For metal oxide semiconductor, tungsten oxide for gas detection cardinal principle also or by receiving and losing electrons from
And cause the resistor-type gas sensitive of resistance variations.Therefore, increase transmission speed and contact of the gas molecule in gas sensitive
Area is a kind of feasible thinking to improve air-sensitive responsiveness, for this purpose, the present invention, according to the thinking, spy proposes a kind of following use
In the classifying porous W of gas detection18O49The preparation method of nanometer sheet, mainly comprises the steps that
S1: mixed templates are prepared: being first dispersed in block copolymer micropore template P123 in dehydrated alcohol under strong agitation, so
The charcoal ball that partial size is added afterwards in 20-50nm is several, continues to stir, until being uniformly dispersed；
S2: W is prepared18O49The precursor solution of nanometer sheet: firstly, with the ratio of volume ratio 1:0.1-0.2 prepare dehydrated alcohol and
The mixed solution of deionized water, tungsten source and Surfactant CTAB, the use of the surfactant is then added thereto again to be had
Conducive to the formation and dispersion of control nanometer sheet, later, which is continued stirring 0.5 hour or more；
S3: classifying porous W18O49The preparation of nanometer sheet: the mixed templates prepared in step S1 are added slowly in step S2
Precursor solution in, be then transferred to hydrothermal reaction kettle, react 10-18h at 100-140 DEG C；After reaction, reaction is produced
Object carries out conventional separation, washing, drying；Later, the reaction product after grinding, is laid in corundum crucible, then exists
Heating is sintered product under air atmosphere, removes template therein, the W with graded porous structure can be obtained18O49
Nanometer sheet.
Preferably, the mass ratio of P123 and charcoal ball is 0.01-0.2:1 in step S1.
Preferably, mixing time is 2-4h in step S1.
Preferably, tungsten source is the chloride of tungsten, preferably tungsten hexachloride in step S2, if we are in reality using tungstates
The nanometer sheet pattern for testing middle discovery preparation is very poor, is all with the presence of the irregular forms such as bulk, the formation of nanometer sheet and chlorine mostly
The corrasion of ion has substantial connection.
Preferably, the mass ratio of tungsten source and CTAB are 1:0.5-0.8 in step S2.
Preferably, temperature program is to be warming up to 350-400 DEG C with the heating rate of 1-3 DEG C/min and keep the temperature 2- in step S3
5h。
Preferably, the graded porous structure in the present invention refers to W18O49Nanometer sheet has mesoporous and micropore cellular structure.
Preferably, the classifying porous W in the present invention18O49Nanometer sheet can be used for field of gas detection.
Preferably, the classifying porous W in the present invention18O49Nanometer sheet has selectivity well, detection to alcohol gas
Lower limit can achieve 20ppb.
The content illustrated is not known for other, is all ordinary skill in the art means, then this is not necessarily to illustrate one by one.
The experimental method of gas test:
Before test, by classifying porous W18O49Nanometer sheet sample grinds and disperses to be formed in ethanol paste, then applies again
It overlays on alumina tube.The device dry 2 h at 100 DEG C.Using steady-state gas distribution method, tests gas and use ethyl alcohol, third
Ketone, nitrogen dioxide and methanol by one closed chamber of injection and mix with air.Sensor gas response be defined as S=
Rg/Ra, wherein Ra and Rg is the sensor resistance in air and test gas respectively.Response or recovery time are calculated by sensor
To apply or closing after gas the time for reaching 90% and 10% saturation degree and original value.All gas sensing measurement humidity about
To carry out in 45% air environment, laboratory temperature is about 28 DEG C.
The present invention has following advantageous effects:
1) by changing reaction process, classifying porous W is realized18O49The successful preparation of nanometer sheet；
2) by W18O49The structure of nanometer sheet designs, it is made to have excellent reaction sensitivity to the detection of ethanol molecule；
3) W that the present invention obtains18O49Nanometer sheet goes out good cyclical stability and detection pole to the detected representation of ethanol molecule
Limit, so that this product has good market value.
Detailed description of the invention
Fig. 1 classifying porous W prepared by the present invention18O49Detection line of response of the nanometer sheet to ethyl alcohol.
Specific embodiment
The contents of the present invention are further illustrated below by specific embodiment.It should be noted that specific implementation is real
The range that example is not intended to restrict the invention, under conditions of the contribution of no substantial technological content, the routine of those skilled in the art
Transformation is also considered as enforceable range of the invention, within the scope of protection required by the present invention.
A kind of classifying porous W for gas detection18O49The preparation method of nanometer sheet, mainly comprises the steps that
S1: mixed templates are prepared: being first dispersed in block copolymer micropore template P123 in dehydrated alcohol under strong agitation, so
The charcoal ball that partial size is added afterwards in 20-50nm is several, continues to stir, until being uniformly dispersed；
S2: W is prepared18O49The precursor solution of nanometer sheet: firstly, with the ratio of volume ratio 1:0.1-0.2 prepare dehydrated alcohol and
The mixed solution of deionized water, tungsten source and Surfactant CTAB, the use of the surfactant is then added thereto again to be had
Conducive to the formation and dispersion of control nanometer sheet, later, which is continued stirring 0.5 hour or more；
S3: classifying porous W18O49The preparation of nanometer sheet: the mixed templates prepared in step S1 are added slowly in step S2
Precursor solution in, be then transferred to hydrothermal reaction kettle, react 10-18h at 100-140 DEG C；After reaction, reaction is produced
Object carries out conventional separation, washing, drying；Later, the reaction product after grinding, is laid in corundum crucible, then exists
Heating is sintered product under air atmosphere, removes template therein, the W with graded porous structure can be obtained18O49
Nanometer sheet.
Embodiment 1
It is the charcoal ball of 20nm that 0.05:1 in mass ratio, which weighs P123 and diameter, it is successively dispersed in dehydrated alcohol, at stirring
Manage 2h；Later, the tungsten hexachloride and CTAB that mass ratio is 1:0.5 are being weighed, is being allowed to molten in the alcohol water mixing that volume ratio is 1:0.1
It is fully dispersed in liquid；Then dropper is used, hybrid template agent solution is added to by W with 30 drops/min drop rate18O49Nanometer
In piece precursor solution, continue to stir 1h；Finally, the mixed solution is transferred in hydrothermal reaction kettle and is reacted at 140 DEG C
12h successively by centrifugation, washing and drying, is laid in corundum crucible after grinding and is put into Muffle furnace after reaction
400 DEG C are warming up under air atmosphere with the heating rate of 2 DEG C/min to be roasted and keep the temperature 2h.
Embodiment 2
It is the charcoal ball of 50nm that 0.05:1 in mass ratio, which weighs P123 and diameter, it is successively dispersed in dehydrated alcohol, at stirring
Manage 2h；Later, the tungsten hexachloride and CTAB that mass ratio is 1:0.6 are being weighed, is being allowed to molten in the alcohol water mixing that volume ratio is 1:0.1
It is fully dispersed in liquid；Then dropper is used, hybrid template agent solution is added to by W with 30 drops/min drop rate18O49Nanometer
In piece precursor solution, continue to stir 1h；Finally, the mixed solution is transferred in hydrothermal reaction kettle and is reacted at 140 DEG C
12h successively by centrifugation, washing and drying, is laid in corundum crucible after grinding and is put into Muffle furnace after reaction
400 DEG C are warming up under air atmosphere with the heating rate of 2 DEG C/min to be roasted and keep the temperature 2h.
Embodiment 3
It is the charcoal ball of 20nm that 0.1:1 in mass ratio, which weighs P123 and diameter, it is successively dispersed in dehydrated alcohol, stir process
2h；Later, the tungsten hexachloride and CTAB that mass ratio is 1:0.6 are being weighed, be allowed in the alcohol water mixed solution that volume ratio is 1:0.2
In it is fully dispersed；Then dropper is used, hybrid template agent solution is added to by W with 20 drops/min drop rate18O49Nanometer sheet
In precursor solution, continue to stir 1h；Finally, the mixed solution is transferred in hydrothermal reaction kettle and is reacted at 140 DEG C
12h successively by centrifugation, washing and drying, is laid in corundum crucible after grinding and is put into Muffle furnace after reaction
360 DEG C are warming up under air atmosphere with the heating rate of 1 DEG C/min to be roasted and keep the temperature 5h.
Embodiment 4
It is the charcoal ball of 40nm that 0.1:1 in mass ratio, which weighs P123 and diameter, it is successively dispersed in dehydrated alcohol, stir process
2h；Later, the tungsten hexachloride and CTAB that mass ratio is 1:0.8 are being weighed, is being allowed to molten in the alcohol water mixing that volume ratio is 1:0.15
It is fully dispersed in liquid；Then dropper is used, hybrid template agent solution is added to by W with 20 drops/min drop rate18O49Nanometer
In piece precursor solution, continue to stir 1h；Finally, the mixed solution is transferred in hydrothermal reaction kettle and is reacted at 100 DEG C
18h successively by centrifugation, washing and drying, is laid in corundum crucible after grinding and is put into Muffle furnace after reaction
360 DEG C are warming up under air atmosphere with the heating rate of 1 DEG C/min to be roasted and keep the temperature 5h.
Embodiment 5
It is the charcoal ball of 30nm that 0.2:1 in mass ratio, which weighs P123 and diameter, it is successively dispersed in dehydrated alcohol, stir process
2h；Later, the tungsten hexachloride and CTAB that mass ratio is 1:0.8 are being weighed, is being allowed to molten in the alcohol water mixing that volume ratio is 1:0.15
It is fully dispersed in liquid；Then dropper is used, hybrid template agent solution is added to by W with 20 drops/min drop rate18O49Nanometer
In piece precursor solution, continue to stir 1h；Finally, the mixed solution is transferred in hydrothermal reaction kettle and is reacted at 100 DEG C
18h successively by centrifugation, washing and drying, is laid in corundum crucible after grinding and is put into Muffle furnace after reaction
390 DEG C are warming up under air atmosphere with the heating rate of 3 DEG C/min to be roasted and keep the temperature 4h.
Claims (8)
1. one kind is used for the classifying porous W of gas detection18O49Nanometer piece preparation method, which is characterized in that mainly comprise the steps that
S1: mixed templates are prepared: being first dispersed in block copolymer micropore template P123 in dehydrated alcohol under strong agitation, so
The charcoal ball that partial size is added afterwards in 20-50nm is several, continues to stir, until being uniformly dispersed；
S2: W is prepared18O49The precursor solution of nanometer sheet: firstly, with the ratio of volume ratio 1:0.1-0.2 prepare dehydrated alcohol and
The mixed solution of deionized water, tungsten source and Surfactant CTAB, the use of the surfactant is then added thereto again to be had
Conducive to the formation and dispersion of control nanometer sheet, later, which is continued stirring 0.5 hour or more；
S3: classifying porous W18O49The preparation of nanometer sheet: the mixed templates prepared in step S1 are added slowly in step S2
Precursor solution in, be then transferred to hydrothermal reaction kettle, react 10-18h at 100-140 DEG C；After reaction, reaction is produced
Object carries out conventional separation, washing, drying；Later, the reaction product after grinding, is laid in corundum crucible, then exists
Heating is sintered product under air atmosphere, removes template therein, the W with graded porous structure can be obtained18O49
Nanometer sheet.
2. according to claim 1 a kind of for the classifying porous W of gas detection18O49Nanometer piece preparation method, feature exist
In the mass ratio of P123 and charcoal ball is 0.01-0.2:1 in step S1.
3. according to claim 1 a kind of for the classifying porous W of gas detection18O49Nanometer piece preparation method, feature exist
In mixing time is 2-4h in step S1.
4. according to claim 1 a kind of for the classifying porous W of gas detection18O49Nanometer piece preparation method, feature exist
In tungsten source is the chloride of tungsten, preferably tungsten hexachloride in step S2.
5. according to claim 1 a kind of for the classifying porous W of gas detection18O49Nanometer piece preparation method, feature exist
In the mass ratio of tungsten source and CTAB are 1:0.5-0.8 in step S2.
6. according to claim 1 a kind of for the classifying porous W of gas detection18O49The preparation method of nanometer sheet, feature
It is, temperature program is to be warming up to 350-400 DEG C with the heating rate of 1-3 DEG C/min and keep the temperature 2-5h in step S3.
7. the classifying porous W that any one of -6 preparation methods are prepared according to claim 118O49Nanometer sheet.
8. classifying porous W according to claim 718O49Nanometer sheet is applied to gas detection, especially has to ethanol molecule
There is very high selectivity, Monitoring lower-cut reaches 20ppb.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111589460A (en) * | 2020-06-03 | 2020-08-28 | 哈尔滨理工大学 | W18O49BiOX composite photocatalytic material and preparation method thereof |
| CN112490435A (en) * | 2020-11-26 | 2021-03-12 | 陕西科技大学 | W for lithium-sulfur battery electrode18O49Nano-rod-carbon composite material and preparation method thereof |
| CN113943018A (en) * | 2021-10-25 | 2022-01-18 | 昆明理工大学 | Sea urchin-shaped W growing on foamed nickel in situ18O49Method for preparing micron array |
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| CN112490435A (en) * | 2020-11-26 | 2021-03-12 | 陕西科技大学 | W for lithium-sulfur battery electrode18O49Nano-rod-carbon composite material and preparation method thereof |
| CN112490435B (en) * | 2020-11-26 | 2022-06-10 | 陕西科技大学 | W for lithium-sulfur battery electrode18O49Nano-rod-carbon composite material and preparation method thereof |
| CN113943018A (en) * | 2021-10-25 | 2022-01-18 | 昆明理工大学 | Sea urchin-shaped W growing on foamed nickel in situ18O49Method for preparing micron array |
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