CN104909409A - Preparation method of one-dimensional Euphorbia-milii-shaped WO3 microcrystal - Google Patents
Preparation method of one-dimensional Euphorbia-milii-shaped WO3 microcrystal Download PDFInfo
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Abstract
The invention provides a preparation method of a one-dimensional Euphorbia-milii-shaped WO3 microcrystal, which comprises the following steps: adding WCl6 into an isopropanol-distilled water mixed solvent, adding a polyoxyethylene-polyoxypropylene block copolymer into the solution to obtain a precursor solution, pouring the precursor solution into a hydrothermal kettle, and reacting while controlling the temperature at 80-240 DEG C under the pressure of 2-16 MPa for 4-36 hours, wherein the hydrothermal kettle is fixed in an homogeneous reaction instrument, and rotates around a fixed axis at the rate of 20-70 r/min in the insulating process; and taking out the product, washing and drying. The prepared one-dimensional Euphorbia-milii-shaped WO3 microcrystal has the advantages of high purity, favorable crystallinity, favorable dispersity, uniform size, uniform shape and obvious oriented growth.
Description
Technical field
The present invention relates to one and prepare one dimension euphorbia milii shape WO
3the method of crystallite, particularly the hot legal system of a kind of homogeneous phase nonionic surface active agent secondary solvent is for one dimension euphorbia milii shape WO
3the method of crystallite.
Background technology
Tungstic oxide (WO
3) normally a kind of yellow powder, water insoluble, be dissolved in alkali lye, be slightly soluble in acid.For high-meltiing alloy processed and Wimet, tungsten filament processed and fire-retardant material etc.Significantly distil when temperature reaches 850 DEG C, hardly with the inorganic acid reaction except hydrofluoric acid, ammoniacal liquor or concentrated alkali solution can be dissolved in slowly.Generate oxychloride with chlorine reacting by heating, but can not with bromine, Iod R.WO
3crystalline structure depend on temperature: it more than 740 DEG C for tetragonal system, 330-740 DEG C be rhombic system, 17-330 DEG C for oblique system ,-50-17 DEG C be triclinic(crystalline)system.Monoclinic phase is the most common, and its spacer is P21/n.
WO
3it is a kind of critical function material.As transition metal oxide, it belongs to n-type semiconductor, and its energy gap is 2.8eV.Except there is excellent gas-sensitive property (to NO
x, H
2s, NH
3very responsive etc. multiple gases), good electrochromism and photocatalytic activity, or a kind of photocatalyst of energy-efficient, cleanliness without any pollution.It also has very strong receptivity to hertzian wave, and the utilization of sun power can be used as excellent absorbing material.Militarily can be used as important stealth material.It also has excellent chemical property simultaneously, is paid close attention to widely.In recent years, one dimension transition metal oxide nano-material (nanotube, nanometer rod, nano wire and nano belt etc.) is with its special physical property and the potential application in nano-device.Especially nanometer WO
3in smart window, display device, light shutter device and secondary cell etc., there is good application prospect, become one of oxide electrode material of primary study in recent years.
WO
3the most steady oxide of tungsten under normal temperature, environmental friendliness, cheap, the high (693mAhg of theoretical specific capacity
-1), be a kind of lithium ion battery negative material having development potentiality.But, block WO
3specific conductivity low, in charge and discharge process, volume change is large, cause its high rate performance and cyclical stability poor.One of improve one's methods at present is control the WO that synthesis has various pattern
3nano material, improves the storage lithium dynamic performance of material with this.
The nanometer WO reported at present
3correlative study have: microemulsion method has prepared particulate state nanometer WO
3[Hou Changjun, Diao Xianzhen, Tang Yike, Huo Danqun, Wei Lifan. microreactor method nanometer WO
3the synthesis and characterization [J] of powder. Rare Metals Materials and engineering, 2007,36 (3): 60-63]; Hydrothermal method has prepared WO
3[Song Xuchun, Zheng loses all nanometer rod, Wang Yun, Cao Guangsheng, the good brave .Na of Yin
3pO
4assisted hydrothermal synthesis WO
3nanometer rod [J]. Journal of Inorganic Materials, 2006,2 (6): 1472-1476] and [Tianming Li, Wen Zeng, Bin Miao, Shuoqing Zhao, Yanqiong Li, He Zhang.Urchinlike hex-WO
3microspheres:Hydrothermal synthesis and gas-sensing properties [J] .Materials Letters, 2015,144:106 – 109] and hydrothermal method prepared hexagonal flower ball-shaped WO
3[Li Jiayin, Huang Jianfeng, Wu Jianpeng, Cao Liyun, Kazumichi Yanagisawa.Morphology-controlled synthesis of tungsten oxide hydrates crystallites via a facile, additive-free hydrothermal process [J] .Ceramics International, 2012,38:4495 – 4500]; Tungsten powder and hydrogen peroxide peroxide gather wolframic acid legal system for nanometer WO
3[Ye Ailing, He Yunqiu. Tungsten oxide 99.999 and hydrate photocatalysis property research [J] .2014 thereof, 12 (45): 12042-12046] and [Huang Jianfeng, Li Jiayin, Cao Liyun, Hu Baoyun, Wu Jianpeng. a kind of hexagon snow shaped WO
3preparation method [P] .ZL 200910218869.2 of nanometer plate]; Spraying dry-heat treating process has prepared hollow mesoporous WO
3ball [Liu Baixiong, Wang Jinshu, Li Hongyi, Wu Junshu, Li Zhifei. hollow mesoporous WO
3the preparation of ball and photocatalysis performance [J]. Chinese Journal of Inorganic Chemistry, 2012,28 (3): 465-470]; Acid precipitation method [Chong Wang, Xin Li, Changhao Feng, Yanfeng Sun, Geyu L.Nanosheets assembled hierarchical flower-like WO
3nanostructures:Synthesis, characterization and their gas sensing properties [J] .Sensors and Actuators B, 2015,210:75 – 81]; Chemical Vapor deposition process (CVD) [Jianzhe Liu, Mianzeng Zhong, Jingbo Li, Anlian Pan, Xiaoli Zhu.Few-layer WO
3nanosheets for high-performance UV-photodetectors [J] .Materials Letters, 2015,148:184 – 187] and template duplicating technology [Katherine Villa, Sebasti á n Murcia-L ó pez, Teresa Andreu, Joan Ram ó n Morante.Mesoporous WO
3photocatalyst for the partial oxidation of methane to methanol using electron scavengers [J] .Applied Catalysis B:Environmental, 2015,163:150 – 155].In addition, the hot legal system of microwave-assisted solvent is also had for flower-shaped WO
3[Zhenyu Wang, Peng Sun, Tianlin Yang, Yuan Gao, Xiaowei Li, Geyu Lu, Yu Du.Flower-like WO
3architectures synthesized via a microwave-assisted method and their gas sensing properties [J] .Sensors and Actuators B, 2013,186:734 – 740] and sol-gel method prepared WO
3film [N.Naseri, S.Yousefzadeh, E.Daryaei, A.Z.Moshfegh.Photoresponse and H
2production of topographically controlled PEG assisted Sol-gel WO
3nanocrystalline thin films [J] .International journal of hydrogenenergy, 2011,36:13461-13472].Microemulsion method, spray-drying process and acid precipitation method all need to synthesize WO under high-temperature calcination condition
3, powder is easily reunited and processing condition and structure design are difficult to control, to preparation WO
3the utilization ratio of required raw material is very little, is difficult to the monodimension nanometer material obtaining oriented growth; And template duplicating technology and sol-gel method also need Post isothermal treatment crystallization process, also can cause nanocrystalline reunion, abnormal grain growth, the microtexture of material is difficult to regulation and control.Meanwhile, to equipment requirements, the high and proportioning of reactant is difficult to control chemical Vapor deposition process, prepared WO
3easily impurity is introduced in nano material.In addition, hydrothermal method can only react in water medium, by controlling the polarity of reaction solvent, and then cannot control crystallization and the pattern of product; Microwave-assisted solvent thermal reaction rate is fast, and nucleation-growth velocity is fast, is difficult to the oriented growth controlling product.
Summary of the invention
The object of the present invention is to provide a kind of one dimension euphorbia milii shape WO
3the preparation method of crystallite.
For achieving the above object, present invention employs following technical scheme:
Step one: by WCl
6add in the mixed solvent of Virahol and distilled water, and be constantly stirred to WCl
6dissolve, obtain W
6+concentration is the solution of 0.005 ~ 3.0mol/L, and in mixed solvent, the volume ratio of Virahol and distilled water is (1 ~ 4): (1 ~ 4);
Step 2: add polyoxyethylene polyoxypropylene block copolymer again in above-mentioned solution, and 35 ~ 50 DEG C of stirrings, polyoxyethylene polyoxypropylene block copolymer is fully dissolved, obtain precursor aqueous solution, the concentration controlling polyoxyethylene polyoxypropylene block copolymer in precursor aqueous solution is 5 ~ 50g/L;
Step 3: precursor aqueous solution is poured in water heating kettle, control the compactedness of water heating kettle 40 ~ 70%, then water heating kettle is sealed, water heating kettle after sealing is put into and is fixed on homogeneous reactor, controlling temperature of reaction is 80 ~ 240 DEG C, and pressure is 2 ~ 16MPa, and the reaction times is 4 ~ 36h, the rotating speed that in reaction process, water heating kettle rotates around stationary shaft in homogeneous reactor is 20 ~ 70r/min, naturally cools to room temperature after reaction terminates;
Step 4: after step 3, opens water heating kettle, and take out product, product is yellow mercury oxide, namely obtains one dimension euphorbia milii shape WO after adopting deionized water and dehydrated alcohol repeated washing product 4 ~ 6 times successively in 40 ~ 80 DEG C of dryings
3crystallite.
The WO of gained
3crystallite is six side's phases, and the length of rod is 20 ~ 200 μm, and diameter is 2 ~ 30 μm.
In described step one and step 2, stir the magnetic stirring apparatus that the model adopting Mettler-Toledo Instrument (Shanghai) Co., Ltd. to produce is RCT B S25.
In described step 3, the model that homogeneous reactor adopts Yantai Ke Li Chemical Equipment Co., Ltd. to manufacture: KLJX-8A.
In described step 4, the dry DZ-3BC II type vacuum drying oven adopting Tianjin Stettlen instrument to have company to manufacture, time of drying is 3 ~ 6h.
Beneficial effect of the present invention is embodied in:
Because the present invention prepares one dimension euphorbia milii shape WO
3the reaction of crystallite once completes in the liquid phase and processing unit is simple, does not need the crystallization and thermal treatment in later stage, thus avoids prepared WO
3the defects such as impurity are introduced in the reunion that bar-shaped crystallite may cause in heat treatment process, grain coarsening and atmosphere reaction.Meanwhile, reunion degree is comparatively light, more cheap raw material can be used to obtain crystallinity better, uniform crystal particles and the single euphorbia milii shape WO of pattern
3crystallite.The more important thing is, owing to the present invention is based on the hot method of mixed solvent, the equipment of requirement and instrument are more simple and more effectively can to prepare crystallinity better, and oriented growth pattern is single, and particle diameter is less and be evenly distributed, the crystallite that purity is higher.Adopt Virahol to mix by a certain percentage as solvent with distilled water, adopt nonionic surface active agent F127 as template, green, clean, harmless and be more conducive to WO
3oriented growth, generate one dimension euphorbia milii club shaped structure, so more efficient, economical, feasible.In addition, under solvent thermal environment, high pressure easily obtains, and is conducive to rapid diffusion mass transfer, can nucleation-oriented growth at short notice, finally realizes one dimension euphorbia milii shape WO
3the controlledly synthesis of crystallite.In a word, utilize the hot method of tensio-active agent secondary solvent than hydrothermal method and microwave solvothermal method efficiently more economical, morphology controllable, feasibility is strong and more can be conducive to WO
3the oriented growth of micro crystal material.
Accompanying drawing explanation
Fig. 1 is one dimension WO prepared by the embodiment of the present invention 4
3the XRD figure of crystallite;
Fig. 2 is the one dimension WO prepared by the embodiment of the present invention 4
3the SEM figure of crystallite.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
Embodiment 1:
Step one: by analytical pure WCl
6add in the mixed solvent of Virahol and distilled water, the volume ratio controlling solvent Virahol and distilled water is V
virahol: V
water=1: 1, and be constantly stirred to WCl
6dissolve, obtained W
6+concentration is the solution of 0.06mol/L;
Step 2: add analytically pure polyoxyethylene polyoxypropylene block copolymer (F127) again in above-mentioned solution, the add-on controlling polyoxyethylene polyoxypropylene block copolymer is 20g/L, and 45 DEG C of heated and stirred, described polyoxyethylene polyoxypropylene block copolymer is fully dissolved, obtain precursor aqueous solution;
Step 3: precursor aqueous solution is poured in water heating kettle, compactedness controls 60%, then water heating kettle is sealed, water heating kettle after sealing is put into and is fixed on homogeneous reactor, controlling solvent thermal temperature is 160 DEG C, and rotating speed is 40r/min (water heating kettle rotates around stationary shaft in insulating process), and pressure is 8MPa, reaction 12h, naturally cools to room temperature after reaction terminates;
Step 4: open water heating kettle, takes out product, and namely the vacuum drying oven inner drying 4h adopting deionized water and dehydrated alcohol repeated washing to be placed on 60 DEG C for 6 times successively obtains one dimension euphorbia milii shape WO
3crystallite.
The WO of gained
3crystallite is six side's phases, and the length of rod is 100 μm, and diameter is 20 μm.
Embodiment 2:
Step one: by analytical pure WCl
6add in the mixed solvent of Virahol and distilled water, the volume ratio controlling solvent Virahol and distilled water is V
virahol: V
water=3: 2, be constantly stirred to WCl
6dissolve, obtained W
6+concentration is the solution of 0.01mol/L;
Step 2: add analytically pure polyoxyethylene polyoxypropylene block copolymer (F127) again in above-mentioned solution, the add-on controlling polyoxyethylene polyoxypropylene block copolymer is 15g/L, and 40 DEG C of heated and stirred, described polyoxyethylene polyoxypropylene block copolymer is fully dissolved, obtain precursor aqueous solution;
Step 3: precursor aqueous solution is poured in water heating kettle, compactedness controls 65%, then water heating kettle is sealed, water heating kettle after sealing is put into and is fixed on homogeneous reactor, controlling solvent thermal temperature is 140 DEG C, and rotating speed is 30r/min (water heating kettle rotates around stationary shaft in insulating process), and pressure is 6MPa, reaction 10h, naturally cools to room temperature after reaction terminates;
Step 4: open water heating kettle, takes out product, and namely the vacuum drying oven inner drying 5h adopting deionized water and dehydrated alcohol repeated washing to be placed on 50 DEG C for 5 times successively obtains one dimension euphorbia milii shape WO
3crystallite.
The WO of gained
3crystallite is six side's phases, and the length of rod is 50 μm, and diameter is 10 μm.
Embodiment 3:
Step one: by analytical pure WCl
6add in the mixed solvent of Virahol and distilled water, the volume ratio controlling solvent Virahol and distilled water is V
virahol: V
water=4: 1, be constantly stirred to WCl
6dissolve, obtained W
6+concentration is the solution of 0.005mol/L;
Step 2: add analytically pure polyoxyethylene polyoxypropylene block copolymer (F127) again in above-mentioned solution, the add-on controlling polyoxyethylene polyoxypropylene block copolymer is 5g/L, and 35 DEG C of heated and stirred, described polyoxyethylene polyoxypropylene block copolymer is fully dissolved, obtain precursor aqueous solution;
Step 3: precursor aqueous solution is poured in water heating kettle, compactedness controls 70%, then water heating kettle is sealed, water heating kettle after sealing is put into and is fixed on homogeneous reactor, controlling solvent thermal temperature is 120 DEG C, and rotating speed is 20r/min (water heating kettle rotates around stationary shaft in insulating process), and pressure is 4MPa, reaction 8h, naturally cools to room temperature after reaction terminates;
Step 4: open water heating kettle, takes out product, and namely the vacuum drying oven inner drying 6h adopting deionized water and dehydrated alcohol repeated washing to be placed on 40 DEG C for 4 times successively obtains one dimension euphorbia milii shape WO
3crystallite.
The WO of gained
3crystallite is six side's phases, and the length of rod is 20 μm, and diameter is 2 μm.
Embodiment 4:
Step one: by analytical pure WCl
6add in the mixed solvent of Virahol and distilled water, the volume ratio controlling solvent Virahol and distilled water is V
virahol: V
water=1: 4, and be constantly stirred to WCl
6dissolve, obtained W
6+concentration is the solution of 3.0mol/L;
Step 2: add analytically pure polyoxyethylene polyoxypropylene block copolymer (F127) again in above-mentioned solution, the add-on controlling polyoxyethylene polyoxypropylene block copolymer is 30g/L, and 50 DEG C of heated and stirred, described polyoxyethylene polyoxypropylene block copolymer is fully dissolved, obtain precursor aqueous solution;
Step 3: precursor aqueous solution is poured in water heating kettle, compactedness controls 50%, then water heating kettle is sealed, water heating kettle after sealing is put into and is fixed on homogeneous reactor, controlling solvent thermal temperature is 220 DEG C, and rotating speed is 60r/min (water heating kettle rotates around stationary shaft in insulating process), and pressure is 12MPa, reaction 24h, naturally cools to room temperature after reaction terminates;
Step 4: open water heating kettle, takes out product, and namely the vacuum drying oven inner drying 3h adopting deionized water and dehydrated alcohol repeated washing to be placed on 80 DEG C for 5 times successively obtains one dimension euphorbia milii shape WO
3crystallite.
WO as seen from Figure 1 prepared by embodiment 4
3crystallite purity is high, and diffraction peak is comparatively sharp-pointed, and is six single side phase WO
3, with the PDF 85-2460WO of standard
3card matches.
WO as seen from Figure 2 prepared by embodiment 4
3crystallite dimension is evenly distributed, and length is about 200 μm, and diameter is about 30 μm, without obviously reuniting, presents euphorbia milii club shaped structure (see Fig. 2 upper left corner).
The one dimension euphorbia milii shape WO that the present invention is prepared under the hot liquid-phase condition of template secondary solvent
3crystallite presents one-dimensional rod-like structure, and rat is more, increases the specific surface area of material self with this, is conducive to materials adsorption electrolytic solution, reacts.In addition, bar-shaped crystallite is more conducive to shaping, forms porous material after assembled formation, so have good using value in lithium ion battery negative material field.Its structure is changeable simultaneously, surface relief, is conducive to alleviating the volume change of negative material in charge and discharge process.
In a word, the nonionic surface active agent secondary solvent thermal technology that the present invention proposes a kind of lesser temps prepares one dimension euphorbia milii shape WO
3the method of crystallite.The method is simply effective, prepares that product structure is controlled, purity is high and specific surface area large, and can by controlling the regulation and control product structures such as the polarity of solvent and template, and it is lower than hydrothermal method temperature, hyperbaric environment easily obtains, and material morphology is controlled, and oriented growth is more obvious; Lower than microwave solvothermal equipment requirements, synthesis rate is low, and oriented growth easily controls.By the one dimension euphorbia milii shape WO prepared by low temperature nonionic type tensio-active agent secondary solvent thermal technology of the present invention
3crystallite purity is high, and crystallinity is better, good dispersity, size uniform, and pattern is homogeneous, and orientation growth obviously.
Claims (3)
1. an one dimension euphorbia milii shape WO
3the preparation method of crystallite, is characterized in that: comprise the following steps:
Step one: by WCl
6add in the mixed solvent of Virahol and distilled water, and be constantly stirred to WCl
6dissolve, obtain W
6+concentration is the solution of 0.005 ~ 3.0mol/L, and in mixed solvent, the volume ratio of Virahol and distilled water is (1 ~ 4): (1 ~ 4);
Step 2: add polyoxyethylene polyoxypropylene block copolymer again in above-mentioned solution, and 35 ~ 50 DEG C of stirrings, polyoxyethylene polyoxypropylene block copolymer is fully dissolved, obtain precursor aqueous solution, the concentration controlling polyoxyethylene polyoxypropylene block copolymer in precursor aqueous solution is 5 ~ 50g/L;
Step 3: precursor aqueous solution is poured in water heating kettle, control the compactedness of water heating kettle 40 ~ 70%, then water heating kettle is sealed, water heating kettle after sealing is put into and is fixed on homogeneous reactor, controlling temperature of reaction is 80 ~ 240 DEG C, and pressure is 2 ~ 16MPa, and the reaction times is 4 ~ 36h, the rotating speed that in reaction process, water heating kettle rotates around stationary shaft in homogeneous reactor is 20 ~ 70r/min, naturally cools to room temperature after reaction terminates;
Step 4: after step 3, opens water heating kettle, takes out product, namely obtains one dimension euphorbia milii shape WO after adopting deionized water and absolute ethanol washing successively in 40 ~ 80 DEG C of dryings
3crystallite.
2. a kind of one dimension euphorbia milii shape WO according to claim 1
3the preparation method of crystallite, is characterized in that: in described step one and step 2, stirs and adopts magnetic stirring apparatus.
3. a kind of one dimension euphorbia milii shape WO according to claim 1
3the preparation method of crystallite, is characterized in that: in described step 4, and dry employing vacuum drying oven, time of drying is 3 ~ 6h.
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Cited By (4)
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| CN105271419A (en) * | 2015-09-30 | 2016-01-27 | 南京理工大学 | Preparation method of tungstic oxide nanosheet self-assembled micro-nano flower-balls |
| CN106865997A (en) * | 2017-02-21 | 2017-06-20 | 上海第二工业大学 | A kind of method that tungsten oxide film is directly grown on electro-conductive glass |
| CN112421007A (en) * | 2020-11-20 | 2021-02-26 | 贵州梅岭电源有限公司 | Preparation method of tungsten oxide/carbon flower-ball-shaped lithium battery composite negative electrode material |
| CN115124067A (en) * | 2022-07-18 | 2022-09-30 | 东北电力大学 | For H 2 S detected CuO/WO 3 Method for preparing composite material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271419A (en) * | 2015-09-30 | 2016-01-27 | 南京理工大学 | Preparation method of tungstic oxide nanosheet self-assembled micro-nano flower-balls |
| CN106865997A (en) * | 2017-02-21 | 2017-06-20 | 上海第二工业大学 | A kind of method that tungsten oxide film is directly grown on electro-conductive glass |
| CN106865997B (en) * | 2017-02-21 | 2019-06-07 | 上海第二工业大学 | A method of growing tungsten oxide film directly on electro-conductive glass |
| CN112421007A (en) * | 2020-11-20 | 2021-02-26 | 贵州梅岭电源有限公司 | Preparation method of tungsten oxide/carbon flower-ball-shaped lithium battery composite negative electrode material |
| CN112421007B (en) * | 2020-11-20 | 2022-06-14 | 贵州梅岭电源有限公司 | Preparation method of tungsten oxide/carbon flower-ball-shaped lithium battery composite negative electrode material |
| CN115124067A (en) * | 2022-07-18 | 2022-09-30 | 东北电力大学 | For H 2 S detected CuO/WO 3 Method for preparing composite material |
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Effective date of registration: 20201202 Address after: 233000 Room 1402, Ziyang Building, Pearl Plaza, Huaishang District, Bengbu City, Anhui Province Patentee after: Anhui Hanbang Technology Consulting Co., Ltd Address before: 710021 Shaanxi province Xi'an Weiyang University Park No. 1 Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY |