CN109650454A - A kind of Microwave-assisted synthesis W18O49The method of nano material - Google Patents

A kind of Microwave-assisted synthesis W18O49The method of nano material Download PDF

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CN109650454A
CN109650454A CN201910152289.1A CN201910152289A CN109650454A CN 109650454 A CN109650454 A CN 109650454A CN 201910152289 A CN201910152289 A CN 201910152289A CN 109650454 A CN109650454 A CN 109650454A
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microwave
nano material
solution
reaction
alcohol
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黄剑锋
海国娟
冯亮亮
曹丽云
介燕妮
杨佳
付常乐
吴建鹏
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Shaanxi University of Science and Technology
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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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM

Abstract

A kind of Microwave-assisted synthesis W18O49The method of nano material, by analytically pure (NH4)10W12O41·5H2O is added in alcohol and is configured to solution A；Enuatrol and n-propylamine are added in solution A and obtain mixed solution B；Mixed solution B is fitted into microwave hydrothermal reaction kettle, hydro-thermal reaction is carried out using microwave hydrothermal instrument；End reaction object deionized water and dehydrated alcohol are distinguished centrifuge washing, the substance after centrifuge washing are dried to obtain pure phase W by cooled to room temperature after reaction18O49Nano material.The present invention uses microwave assisted techniques, using microwave as heating tool,, it can be achieved that stirring on molecular level, has heating speed fast compared with traditional preparation methods, homogeneous heating, without temperature gradient, no hysteresis effect overcomes hydro-thermal container and heats non-uniform disadvantage, the reaction time is shortened, is improved work efficiency.

Description

A kind of Microwave-assisted synthesis W18O49The method of nano material
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to a kind of Microwave-assisted synthesis W18O49Nano material Method.
Background technique
Tungsten oxide has a variety of existing forms and crystal structure, and existing forms include having stoichiometric ratio WO3With it is non- The W of stoichiometric ratio18O49(WO2.72)、W5O14(WO2.8)、W24O68(WO2.83) and W20O58(WO2.9), general chemical formula For WO3-x(x=0~1).Non-stoichiometry WO3-xColor is in yellow green with the difference of oxygen content, is a kind of important more function Energy N-shaped broad stopband (2.5~3.6eV) semiconductor, shows many unique properties and has potential application range, for example, The electrochromism that has due to tungsten oxide, photochromic and gas-discoloration characteristic thus can be widely applied to flat-panel monitor, The fields such as smart window and various sensors.
Wherein W18O49It is known uniquely with non-stoichiometric existing for pure form with the maximum amount of oxygen defect WOx.Recent studies have indicated that the material other than with good air-sensitive, discoloration and catalytic performance, shows infrared light good Precious metal ion can be generated metallic particles in its surface in situ by the week reduction of good absorption-heat-convertibility energy, the material.From From [ZHU Y Q, HU W B, HSU W K, TERRONES M, GROBERT N, the HARE J P.Tungsten oxide such as ZHU Tree-like structures [J] .Chemical Physics Letters, 1999,309 (5/6): 327-334.] for the first time W has been obtained by broken micron dendrite18O49Since nano wire, researchers utilize a variety of methods such as heat treatment, vapor phase growth The W of different-shape is synthesized18O49Nanostructure, and detailed characterization has been carried out to its structure and performance.LI etc. [LI Y B, BANDO Y S,GOLBERG D.Quasi-aligned single-crystalline W18O49nanotubes and Nanowires nanowires [J] .Advanced Materials, 2003,15 (15): 1294-1296.] pass through irradiation heating Tungsten foil obtains W in Ta substrate18O49Nano wire and W18O49Nanotube；[ZHOU Jun, GONG Li, the DENG Shao- such as ZHOU zhi,CHEN Jun,SHEJun-cong,XU Ning-sheng.Growth and field-emission property of tungsten oxide nanotip arrays[J].Applied Physics Letters,2005,87(22):31081- 31083.] nano-wire array with cone structure has been prepared by two step hydatogenesiss.SU and LIN [SU C Y, LIN H C.Direct route to tungsten oxide nanorod bundles:Microstructures and electro- optical properties[J].The Journal of Physical Chemistry C,2009,113(10):4042- 4046.] tungsten block is evaporated directly in the environment of anoxic, has obtained W18O49Pencil nanometer rods.[the Zhen-Feng such as HUANG Huang,Jiajia Song,MesoporousW18O49hollow spheres as highly active Photocatalysts [J] .The Royal Society of Chemistry, 2014,50,10959-10962] pass through adjusting The content of acid has been prepared with mesoporous chondritic.The nano wire for improving yield, simplifying preparation process and preparing Pattern and size are the targets that researcher pursues.
The preparation method of the purple tungsten proposed both at home and abroad at present includes solid-phase synthesis and Moist chemical synthesis method.Synthesis in solid state side Method sintering temperature is higher, and soaking time is longer, and product purity is not high.Wet process mainly utilizes homogeneous reaction instrument by product certain Related reaction is carried out under temperature and pressure.
Summary of the invention
The purpose of the present invention is to provide one kind can shorten the reaction time, improves the Microwave-assisted synthesis of working efficiency W18O49The method of nano material, pure phase W obtained18O49Nano material crystal property is good, purity is high, and morphology and size is controllable.
In order to achieve the above objectives, the technical solution adopted by the present invention is that:
1) analytically pure (NH is taken4)10W12O41·5H2The solution A for being configured to 0.01~0.2mol/L is added in alcohol in O；
2) enuatrol and n-propylamine are added in solution A, magnetic agitation waits for that solution gradually becomes blue from yellow, obtains The mixed solution B that concentrations of sodium oleate is 0.01~0.08mol/L, n-propylamine concentration is 0.01~0.05mol/L；
3) mixed solution B is fitted into microwave hydrothermal reaction kettle, uses heating power for the microwave hydrothermal instrument of 300~400W Reactor temperature is risen to 130~160 DEG C from room temperature with the heating rate of 10 DEG C/min, reacts 60~90min；
4) cooled to room temperature after reaction, end reaction object deionized water and dehydrated alcohol are centrifuged respectively and washed It washs, the substance after centrifuge washing is dried to obtain pure phase W18O49Nano material.
The alcohol of the step 1) uses: dehydrated alcohol, isopropanol, n-butanol or volume ratio is dehydrated alcohols: isopropanol= 1:(1~3), dehydrated alcohol: isopropanol: n-butanol=1:(0.5~1): the mixed alcohol of (0.5~1).
The solution A that the step 1) is prepared is sealed up for safekeeping with preservative film in time.
The packing ratio that step 3) the mixed solution B is packed into microwave hydrothermal reaction kettle is 20%~40%.
Step 3) the microwave hydrothermal instrument uses MDS-8 microwave hydrothermal instrument.
The drying of the step 4) is using 40~60 DEG C of vacuum drying ovens or the dry 5~8h of freeze drying box.
The present invention use microwave assisted techniques, using microwave as heating tool, compared with traditional preparation methods, it can be achieved that Stirring on molecular level has heating speed fast, homogeneous heating, no temperature gradient, and no hysteresis effect overcomes hydro-thermal container Non-uniform disadvantage is heated, the reaction time is shortened, is improved work efficiency.
The beneficial effects of the present invention are embodied in:
1. the method that the present invention uses solvent heat, by selecting different solvents and introducing anionic surfactant, control The concentration of proportion, surfactant between different solvents, reaction temperature, reaction time prepare various structures W18O49Material.
2. preparation method of the present invention is simple, material composition is few, cost is relatively low, and reaction temperature and time are in larger control Range, and product does not need later period Crystallizing treatment, avoids the crystal grain that may cause during Post isothermal treatment to a certain extent The defects of growing up, be roughened or crimping.
3. the W prepared using method of the invention18O49Pattern multiplicity, there is one-dimensional, 2 and 3 dimensional organization.
4. the W for the different-shape that the present invention synthesizes18O49Material possesses preferable absorption and Photocatalytic Degradation Property, for There is potential explore to be worth in the fields such as other performances, such as photoelectrocatalysis.
Detailed description of the invention
Fig. 1 is W prepared by the embodiment of the present invention 118O49XRD spectrum.
Fig. 2 is W prepared by the embodiment of the present invention 118O49SEM photograph.
Specific embodiment
Embodiment 1:
1) analytically pure (NH is taken4)10W12O41·5H2O is added to absolute ethanol the solution A for being configured to 0.05mol/L, and and When sealed up for safekeeping and avoid pollution with preservative film；
2) enuatrol and n-propylamine are added in solution A, magnetic agitation waits for that solution gradually becomes blue from yellow, obtains The mixed solution B that concentrations of sodium oleate is 0.05mol/L, n-propylamine concentration is 0.05mol/L；
3) mixed solution B is fitted into microwave hydrothermal reaction kettle by 40% packing ratio, is set using MDS-8 microwave hydrothermal instrument Determining heating power is 300W, and reactor temperature is risen to 150 DEG C from room temperature with the heating rate of 10 DEG C/min, reacts 60min；
4) cooled to room temperature after reaction, end reaction object deionized water and dehydrated alcohol are centrifuged respectively and washed It washs, the substance after centrifuge washing is obtained into pure phase W in 50 DEG C of vacuum drying ovens or the dry 5h of freeze drying box18O49Nano material.
Nanometer sheet self assembly W obtained by this example18O49Material.Product prepared by the present invention is pure phase as seen from Figure 1 W18O49Material.
The nanometer sheet self-assembled structures W that the present invention obtains as seen from Figure 218O49。
Embodiment 2:
1) analytically pure (NH is taken4)10W12O41·5H2The solution A for being configured to 0.01mol/L is added in isopropanol in O, and in time It is sealed up for safekeeping and is avoided pollution with preservative film；
2) enuatrol and n-propylamine are added in solution A, magnetic agitation waits for that solution gradually becomes blue from yellow, obtains The mixed solution B that concentrations of sodium oleate is 0.03mol/L, n-propylamine concentration is 0.03mol/L；
3) mixed solution B is fitted into microwave hydrothermal reaction kettle by 30% packing ratio, is set using MDS-8 microwave hydrothermal instrument Determining heating power is 400W, and reactor temperature is risen to 160 DEG C from room temperature with the heating rate of 10 DEG C/min, reacts 80min；
4) cooled to room temperature after reaction, end reaction object deionized water and dehydrated alcohol are centrifuged respectively and washed It washs, the substance after centrifuge washing is obtained into pure phase W in 60 DEG C of vacuum drying ovens or the dry 6h of freeze drying box18O49Nano material.
Nano bar-shape W obtained by this example18O49Material.
Embodiment 3:
1) analytically pure (NH is taken4)10W12O41·5H2The solution A for being configured to 0.2mol/L is added in n-butanol in O, and in time It is sealed up for safekeeping and is avoided pollution with preservative film；
2) enuatrol and n-propylamine are added in solution A, magnetic agitation waits for that solution gradually becomes blue from yellow, obtains The mixed solution B that concentrations of sodium oleate is 0.04mol/L, n-propylamine concentration is 0.02mol/L；
3) mixed solution B is fitted into microwave hydrothermal reaction kettle by 40% packing ratio, is set using MDS-8 microwave hydrothermal instrument Determining heating power is 400W, and reactor temperature is risen to 140 DEG C from room temperature with the heating rate of 10 DEG C/min, reacts 70min；
4) cooled to room temperature after reaction, end reaction object deionized water and dehydrated alcohol are centrifuged respectively and washed It washs, the substance after centrifuge washing is obtained into pure phase W in 50 DEG C of vacuum drying ovens or the dry 6h of freeze drying box18O49Nano material.
The W of the distribution of nanometer pencil obtained by this example18O49Nano material.
Embodiment 4:
1) analytically pure (NH is taken4)10W12O41·5H2It is dehydrated alcohol: isopropanol=1:1 mixed alcohol that volume ratio, which is added, in O In be configured to the solution A of 0.12mol/L, and sealed up for safekeeping avoid pollution with preservative film in time；
2) enuatrol and n-propylamine are added in solution A, magnetic agitation waits for that solution gradually becomes blue from yellow, obtains The mixed solution B that concentrations of sodium oleate is 0.05mol/L, n-propylamine concentration is 0.01mol/L；
3) mixed solution B is fitted into microwave hydrothermal reaction kettle by 40% packing ratio, is set using MDS-8 microwave hydrothermal instrument Determining heating power is 300W, and reactor temperature is risen to 150 DEG C from room temperature with the heating rate of 10 DEG C/min, reacts 65min；
4) cooled to room temperature after reaction, end reaction object deionized water and dehydrated alcohol are centrifuged respectively and washed It washs, the substance after centrifuge washing is obtained into pure phase W in 50 DEG C of vacuum drying ovens or the dry 5h of freeze drying box18O49Nano material.
Three-dimensional flower-shaped W obtained by this example18O49Nano material.
Embodiment 5:
1) analytically pure (NH is taken4)10W12O41·5H2It is dehydrated alcohol: isopropanol=1:2 mixed alcohol that volume ratio, which is added, in O In be configured to the solution A of 0.03mol/L, and sealed up for safekeeping avoid pollution with preservative film in time；
2) enuatrol and n-propylamine are added in solution A, magnetic agitation waits for that solution gradually becomes blue from yellow, obtains The mixed solution B that concentrations of sodium oleate is 0.02mol/L, n-propylamine concentration is 0.04mol/L；
3) mixed solution B is fitted into microwave hydrothermal reaction kettle by 20% packing ratio, is set using MDS-8 microwave hydrothermal instrument Determining heating power is 400W, and reactor temperature is risen to 130 DEG C from room temperature with the heating rate of 10 DEG C/min, reacts 90min；
4) cooled to room temperature after reaction, end reaction object deionized water and dehydrated alcohol are centrifuged respectively and washed It washs, the substance after centrifuge washing is obtained into pure phase W in 40 DEG C of vacuum drying ovens or the dry 8h of freeze drying box18O49Nano material.
Embodiment 6:
1) analytically pure (NH is taken4)10W12O41·5H2It is dehydrated alcohol: isopropanol=1:3 mixed alcohol that volume ratio, which is added, in O In be configured to the solution A of 0.15mol/L, and sealed up for safekeeping avoid pollution with preservative film in time；
2) enuatrol and n-propylamine are added in solution A, magnetic agitation waits for that solution gradually becomes blue from yellow, obtains The mixed solution B that concentrations of sodium oleate is 0.06mol/L, n-propylamine concentration is 0.03mol/L；
3) mixed solution B is fitted into microwave hydrothermal reaction kettle by 26% packing ratio, is set using MDS-8 microwave hydrothermal instrument Determining heating power is 360W, and reactor temperature is risen to 150 DEG C from room temperature with the heating rate of 10 DEG C/min, reacts 80min；
4) cooled to room temperature after reaction, end reaction object deionized water and dehydrated alcohol are centrifuged respectively and washed It washs, the substance after centrifuge washing is obtained into pure phase W in 50 DEG C of vacuum drying ovens or the dry 7h of freeze drying box18O49Nano material.
Embodiment 7:
1) analytically pure (NH is taken4)10W12O41·5H2It is dehydrated alcohol: isopropanol: n-butanol=1 that volume ratio, which is added, in O: It is configured to the solution A of 0.05mol/L in the mixed alcohol of 0.5:0.8, and is sealed up for safekeeping avoid pollution with preservative film in time；
2) enuatrol and n-propylamine are added in solution A, magnetic agitation waits for that solution gradually becomes blue from yellow, obtains The mixed solution B that concentrations of sodium oleate is 0.01mol/L, n-propylamine concentration is 0.01mol/L；
3) mixed solution B is fitted into microwave hydrothermal reaction kettle by 32% packing ratio, is set using MDS-8 microwave hydrothermal instrument Determining heating power is 380W, and reactor temperature is risen to 140 DEG C from room temperature with the heating rate of 10 DEG C/min, reacts 70min；
4) cooled to room temperature after reaction, end reaction object deionized water and dehydrated alcohol are centrifuged respectively and washed It washs, the substance after centrifuge washing is obtained into pure phase W in 55 DEG C of vacuum drying ovens or the dry 6h of freeze drying box18O49Nano material.
Embodiment 8:
1) analytically pure (NH is taken4)10W12O41·5H2It is dehydrated alcohol: isopropanol: n-butanol=1 that volume ratio, which is added, in O: It is configured to the solution A of 0.18mol/L in the mixed alcohol of 0.8:1, and is sealed up for safekeeping avoid pollution with preservative film in time；
2) enuatrol and n-propylamine are added in solution A, magnetic agitation waits for that solution gradually becomes blue from yellow, obtains The mixed solution B that concentrations of sodium oleate is 0.08mol/L, n-propylamine concentration is 0.05mol/L；
3) mixed solution B is fitted into microwave hydrothermal reaction kettle by 38% packing ratio, is set using MDS-8 microwave hydrothermal instrument Determining heating power is 350W, and reactor temperature is risen to 160 DEG C from room temperature with the heating rate of 10 DEG C/min, reacts 60min；
4) cooled to room temperature after reaction, end reaction object deionized water and dehydrated alcohol are centrifuged respectively and washed It washs, the substance after centrifuge washing is obtained into pure phase W in 45 DEG C of vacuum drying ovens or the dry 5h of freeze drying box18O49Nano material.
Embodiment 9:
1) analytically pure (NH is taken4)10W12O41·5H2It is dehydrated alcohol: isopropanol: n-butanol=1:1 that volume ratio, which is added, in O: It is configured to the solution A of 0.13mol/L in 0.5 mixed alcohol, and is sealed up for safekeeping avoid pollution with preservative film in time；
2) enuatrol and n-propylamine are added in solution A, magnetic agitation waits for that solution gradually becomes blue from yellow, obtains The mixed solution B that concentrations of sodium oleate is 0.07mol/L, n-propylamine concentration is 0.04mol/L；
3) mixed solution B is fitted into microwave hydrothermal reaction kettle by 25% packing ratio, is set using MDS-8 microwave hydrothermal instrument Determining heating power is 400W, and reactor temperature is risen to 130 DEG C from room temperature with the heating rate of 10 DEG C/min, reacts 80min；
4) cooled to room temperature after reaction, end reaction object deionized water and dehydrated alcohol are centrifuged respectively and washed It washs, the substance after centrifuge washing is obtained into pure phase W in 50 DEG C of vacuum drying ovens or the dry 8h of freeze drying box18O49Nano material.

Claims (6)

1. a kind of Microwave-assisted synthesis W18O49The method of nano material, it is characterised in that the following steps are included:
1) analytically pure (NH is taken4)10W12O41·5H2The solution A for being configured to 0.01~0.2mol/L is added in alcohol in O；
2) enuatrol and n-propylamine are added in solution A, magnetic agitation waits for that solution gradually becomes blue from yellow, obtains oleic acid The mixed solution B that na concn is 0.01~0.08mol/L, n-propylamine concentration is 0.01~0.05mol/L；
3) mixed solution B is fitted into microwave hydrothermal reaction kettle, uses the microwave hydrothermal instrument that heating power is 300~400W with 10 DEG C/reactor temperature rises to 130~160 DEG C from room temperature by the heating rate of min, react 60~90min；
4) end reaction object deionized water and dehydrated alcohol are distinguished centrifuge washing by cooled to room temperature after reaction, Substance after centrifuge washing is dried to obtain pure phase W18O49Nano material.
2. Microwave-assisted synthesis W according to claim 118O49The method of nano material, it is characterised in that: the step 1) Alcohol use: dehydrated alcohol, isopropanol, n-butanol or volume ratio is dehydrated alcohols: isopropanol=1:(1~3), dehydrated alcohol: Isopropanol: n-butanol=1:(0.5~1): the mixed alcohol of (0.5~1).
3. Microwave-assisted synthesis W according to claim 118O49The method of nano material, it is characterised in that: the step 1) The solution A of preparation is sealed up for safekeeping with preservative film in time.
4. Microwave-assisted synthesis W according to claim 118O49The method of nano material, it is characterised in that: the step 3) The packing ratio that mixed solution B is packed into microwave hydrothermal reaction kettle is 20%~40%.
5. Microwave-assisted synthesis W according to claim 118O49The method of nano material, it is characterised in that: the step 3) Microwave hydrothermal instrument uses MDS-8 microwave hydrothermal instrument.
6. Microwave-assisted synthesis W according to claim 118O49The method of nano material, it is characterised in that: the step 4) Drying using the dry 5~8h of 40~60 DEG C of vacuum drying ovens or freeze drying box.
CN201910152289.1A 2019-02-28 2019-02-28 A kind of Microwave-assisted synthesis W18O49The method of nano material Pending CN109650454A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111393658A (en) * 2019-11-20 2020-07-10 济南大学 Preparation method of manganese-based nanowire
CN111393659A (en) * 2019-11-20 2020-07-10 济南大学 Preparation method of cobalt-based one-dimensional nano material
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
CN113511683A (en) * 2020-04-10 2021-10-19 中国石油化工股份有限公司 WO3Nanowire, preparation method thereof and gas sensor

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Publication number Priority date Publication date Assignee Title
CN105036196A (en) * 2015-08-27 2015-11-11 陕西科技大学 Preparation method of multi-dimensional pure-phase W18O49
CN107604635A (en) * 2017-07-21 2018-01-19 西北大学 A kind of W18O49Coat carbon fibre composite and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105036196A (en) * 2015-08-27 2015-11-11 陕西科技大学 Preparation method of multi-dimensional pure-phase W18O49
CN107604635A (en) * 2017-07-21 2018-01-19 西北大学 A kind of W18O49Coat carbon fibre composite and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111393658A (en) * 2019-11-20 2020-07-10 济南大学 Preparation method of manganese-based nanowire
CN111393659A (en) * 2019-11-20 2020-07-10 济南大学 Preparation method of cobalt-based one-dimensional nano material
CN113511683A (en) * 2020-04-10 2021-10-19 中国石油化工股份有限公司 WO3Nanowire, preparation method thereof and gas sensor
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

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