CN107604635A - A kind of W18O49Coat carbon fibre composite and preparation method thereof - Google Patents

A kind of W18O49Coat carbon fibre composite and preparation method thereof Download PDF

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Publication number
CN107604635A
CN107604635A CN201710602202.7A CN201710602202A CN107604635A CN 107604635 A CN107604635 A CN 107604635A CN 201710602202 A CN201710602202 A CN 201710602202A CN 107604635 A CN107604635 A CN 107604635A
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carbon
microwave radiation
fibre composite
radiation technology
preparation
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CN107604635B (en
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闫军锋
许曼章
贾仕隆
贠江妮
刘成
陈诚
张志勇
赵武
翟春雪
任晓瀛
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Northwest University
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Northwest University
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Abstract

The invention discloses a kind of W18O49Carbon fibre composite and preparation method thereof is coated, is included in carbon fiber surface and uses microwave radiation technology solvent thermal growth W18O49Nano material, without any template and catalyst during microwave radiation technology solvent hot preparation, technique is simple, and yield is high, and cost is cheap, is adapted to batch production;The direct growth W on carbon cloth18O49Nano material, prepared nano composite material form is homogeneous, cladding is close, can be used as photocatalysis, electro-catalysis, solar cell, flexible sensor, Flied emission and lithium ion battery negative material.

Description

A kind of W18O49Coat carbon fibre composite and preparation method thereof
Technical field
The invention belongs to field of nanometer material technology, is related to a kind of W18O49Coat carbon fibre composite and preparation method thereof.
Background technology
With the continuous development of science and technology, electronic product and smart machine start constantly to miniaturization, lightweight direction to develop, Flexible electronic product has been applied to the every field of people's life, such as wearable electronic, flexible display device.Carbon is fine Denapon is with good pliability, can be formed by weaving to form carbon cloth, can be widely used in as flexible electrode various The fields such as battery, ultracapacitor.W18O49It is to contain defective tungsten oxide, is a kind of important semiconductor functional material, W18O49 Nano material is widely used as solar cell, lithium ion battery display device, Sensitive Apparatus, photoelectric device, photocatalysis material Material, electrocatalysis material etc..By carbon cloth and W18O49Nano material carries out compound composition W18O49Carbon cloth composite is coated, it is more single Material is compared, and is all increased significantly in photocatalysis, lithium electricity, ultracapacitor etc., therefore by regulating and controlling W18O49Nanometer material The growth of material can obtain quality it is good and tool clad structure nano composite material, it is significant in above-mentioned application.At present There is researcher to be engaged in carbon fiber with aoxidizing the preparation of composite tungsten material and achieving certain achievement, such as Chinese patent CN106423144A discloses a kind of carbon fiber@tungsten oxide nanoparticles core-shell structures and preparation method thereof, using true In empty stove, in the presence of carrier gas, first WO was soaked with high-temperature heating3The carbon fiber of suspension, then at low temperature, moved back in air Fire obtains composite, and its preparation process is relatively cumbersome, and the reaction time, length was, it is necessary to which hot environment, obtained tungsten oxide are nanometer Brilliant particle, does not accomplish oriented growth, limits property and the application of material.
The content of the invention
For in the prior art the defects of and deficiency, the invention provides a kind of W18O49Coat carbon fibre composite and Its preparation method, its process is simple, and reaction temperature is low, and W prepared by the present invention18O49Nano material morphology is homogeneous, neat Be grown in carbon cloth surfaces, be advantageous to improve material property.
To solve the above problems, the technical scheme that the present invention takes is:
A kind of W18O49Carbon fibre composite is coated, including carbon fiber and the use hot method of microwave radiation technology solvent are coated on carbon The W of fiber surface18O49Nano material.
A kind of possible form, the appearance form of described carbon fiber are carbon cloth, the model WOS1002 of carbon cloth.
A kind of W18O49The preparation method of carbon fibre composite is coated, using the hot method of microwave radiation technology solvent in carbon fiber surface Look unfamiliar long W18O49Nano material.
Specifically, W is grown in carbon fiber surface using the hot method of microwave radiation technology solvent18O49Nano material includes:With containing tungsten The alcoholic solution of compound is precursor solution, and carbon fiber carries out microwave radiation technology solvent thermal response as reaction source, and microwave power is 400W, reaction temperature are 160~200 DEG C, and the reaction time is 5~60min.
Or W is grown in carbon fiber surface using the hot method of microwave radiation technology solvent18O49Nano material includes:With tungstenic chemical combination The alcoholic solution of thing is precursor solution, and carbon cloth carries out microwave radiation technology solvent thermal response as reaction source, microwave power 400W, instead It is 160~200 DEG C to answer temperature, and the reaction time is 5~60min.
Preferably, W is grown in carbon cloth surfaces using the hot method of microwave radiation technology solvent18O49Nano material includes:With tungstenic chemical combination The alcoholic solution of thing is growth solution, and carbon cloth carries out microwave radiation technology solvent thermal response, microwave power 400W, reaction as reaction source Temperature is 160 DEG C, reaction time 5min.
Preferably, W is grown in carbon cloth surfaces using the hot method of microwave radiation technology solvent18O49Nano material includes:With tungstenic chemical combination The alcoholic solution of thing is growth solution, and carbon cloth carries out microwave radiation technology solvent thermal response, microwave power 400W, reaction as reaction source Temperature is 180 DEG C, reaction time 30min.
Preferably, W is grown in carbon cloth surfaces using the hot method of microwave radiation technology solvent18O49Nano material includes:With tungstenic chemical combination The alcoholic solution of thing is growth solution, and carbon cloth carries out microwave radiation technology solvent thermal response, microwave power 400W, reaction as reaction source Temperature is 200 DEG C, reaction time 60min.
Specifically, described Tungstenic compound is WCl6, the alcoholic solution concentration of Tungstenic compound is 4g/L~12g/L.
More specifically, the alcoholic solution of described Tungstenic compound is the ethanol solution of Tungstenic compound.
Advantages of the present invention is:
(1) W prepared by the present invention18O49Cladding carbon fibre composite is the grown on carbon fibers at a diameter of 10 μm W18O49Nano material, W18O49Nano material cladding carbon fiber structural density height, composition and morphology controllable, can be straight after preparation Connect use, without post-processing, from microstructure, W18O49Cladding carbon fibre composite has very big specific surface area, can To be used as flexible sensor, W18O49Cladding carbon cloth composite is because carbon material is present such that electronics can be passed rapidly Lead, photo-generated carrier recombination probability reduces, and electron hole pair efficiently separates, dense so as to add the life-span of carrier and carrier Degree so that W18O49Cladding carbon cloth composite has excellent photocatalysis performance.
(2) present invention is preparing W18O49When coating carbon fibre composite, using the hot method of microwave radiation technology solvent on carbon cloth Cladding growth W18O49Nano material, without any template and catalyst in microwave radiation technology solvent thermal process reactor, technique is simple, Speed is fast, yield is high, and cost is cheap, is adapted to batch production;
(3) the directly cladding growth W on carbon cloth18O49Nano material, prepared nano composite material form is homogeneous, bag Cover close.
Brief description of the drawings
Fig. 1 is the XRD spectrum of embodiment 1 in the present invention;
Fig. 2 is the XRD spectrum of embodiment 2 in the present invention;
Fig. 3 is the XRD spectrum of embodiment 3 in the present invention;
Fig. 4 is the SEM photograph of embodiment 1 in the present invention;
Fig. 5 is the SEM photograph of embodiment 1 in the present invention;
Fig. 6 is the SEM photograph of embodiment 2 in the present invention;
Fig. 7 is the SEM photograph of embodiment 2 in the present invention;
Fig. 8 is the SEM photograph of embodiment 3 in the present invention;
Fig. 9 is the SEM photograph of embodiment 3 in the present invention;
The present invention is illustrated below in conjunction with specification drawings and specific embodiments.
Embodiment
W prepared by the present invention18O49Carbon fibre composite is coated, using the simple hot template-free method of microwave radiation technology solvent The cladding growth W directly on carbon fiber18O49Nano material.
The preparation method of the present invention can grow W on the surface of all carbon fibers18O49Nano material, in order to prepare Journey is convenient, the uniform diameter of carbon fiber, and the present invention uses appearance form of the carbon cloth as carbon fiber in R&D process, used Carbon cloth (CarbonFiberCloth), the i.e. abbreviation of carbon cloth, the fabric of carbon fiber, are knitted by the polyacrylonitrile fibre pre-oxidized Thing through charing or carbon fiber through being formed by weaving, also known as carbon fiber sheet, carbon fiber cloth, carbon cloth, carbon fibre fabric, carbon fiber tape or Carbon fiber plate (prepreg cloth) etc..All carbon cloths can realize the solution of the present invention in principle, in an embodiment of the present invention The carbon cloth used is directly buys in Ce Tech Co., Ltd companies, model WOS1002, forms the individual carbon fibers of carbon cloth A diameter of 10 μm.
The present invention mainly use the hot method of microwave radiation technology solvent, by control the concentration of tungsten salt in reaction system, reaction temperature, The factors such as reaction time obtain a kind of W18O49Cladding carbon fibre composite and the method for preparing the material, microwave-assistant sol Without any template and catalyst in agent thermal process reactor, technique is simple, and yield is high, and cost is cheap, is adapted to batch production;Carbon Fiber directly coats growth W as trunk structure18O49Nano material, prepared W18O49Nano material form is homogeneous, in carbon fiber On be evenly coated.
In order that objects and advantages of the present invention are more clearly understood, the present invention is carried out below in conjunction with drawings and examples It is further described.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit The present invention.
Embodiment one:
Will Ce Tech Co., Ltd companies buy WOS1002 model carbon cloth punchings into a diameter of 12mm circular base Piece, it is put into concentrated nitric acid solution and 1h is handled at 100 DEG C, then cleaned repeatedly with deionized water, dries, be put into the reaction of TFM liners It is standby in kettle (reactor volume 100ml).By 0.12g (4g/L) WCl6It is added in 30ml absolute ethyl alcohols, carries out abundant Stirring, works as WCl6Yellow transparent precursor solution is formed after being completely dissolved, precursor solution is moved into the reactor containing carbon cloth In, it is placed under 400W microwave power, 160 DEG C of reaction 5min, after question response terminates, carbon cloth is taken out, and by deionization Water cleaning is multiple, and then carbon cloth is placed at 60 DEG C and dried, obtains W18O49Coat carbon fibre composite.
Fig. 1 illustrates the product W of embodiment one18O49/ carbon fibre composite, Fig. 4 illustrate the product W of embodiment one18O49Receive Rice material coats highly uniform, W on whole carbon fiber18O49In villiform, Fig. 5 illustrates that the product of embodiment one is tied for cladding Structure.
Embodiment two:
Will Ce Tech Co., Ltd companies buy WOS1002 model carbon cloth punchings into a diameter of 12mm circular base Piece, it is put into concentrated nitric acid solution and 1h is handled at 100 DEG C, then cleaned repeatedly with deionized water, dries, be put into the reaction of TFM liners It is standby in kettle (reactor volume 100ml).By 0.24g (8g/L) WCl6It is added in 30ml absolute ethyl alcohols, carries out abundant Stirring, works as WCl6Yellow transparent precursor solution is formed after being completely dissolved, precursor solution is moved into the reactor containing carbon cloth In, it is placed under 400W microwave power, 180 DEG C of reaction 30min, after question response terminates, carbon cloth is taken out, and by deionization Water cleaning is multiple, and then carbon cloth is placed at 60 DEG C and dried, obtains W18O49Coat carbon fibre composite.
Fig. 2 illustrates the product W of embodiment two18O49/ carbon fibre composite, Fig. 6 illustrate the product W of embodiment two18O49Receive Rice material coats highly uniform, W on whole carbon fiber18O49In wire, Fig. 7 illustrates that the product of embodiment two is clad structure.
Embodiment three:
Will Ce Tech Co., Ltd companies buy WOS1002 model carbon cloth punchings into a diameter of 12mm circular base Piece, it is put into concentrated nitric acid solution and 1h is handled at 100 DEG C, then cleaned repeatedly with deionized water, dries, be put into the reaction of TFM liners It is standby in kettle (reactor volume 100ml).By 0.36g (12g/L) WCl6It is added in 30ml absolute ethyl alcohols, carries out abundant Stirring, works as WCl6Yellow transparent precursor solution is formed after being completely dissolved, precursor solution is moved into the reactor containing carbon cloth In, it is placed under 400W microwave power, 200 DEG C of reaction 60min, after question response terminates, carbon cloth is taken out, and by deionization Water cleaning is multiple, and then carbon cloth is placed at 60 DEG C and dried, obtains W18O49Coat carbon fibre composite.
Fig. 3 illustrates the product W of embodiment three18O49/ carbon fibre composite, Fig. 8 illustrate the product W of embodiment three18O49Receive Rice material coats highly uniform, W on whole carbon fiber18O49In the form of sheets, Fig. 9 illustrates that the product of embodiment three is clad structure.
In summary, the present invention relates to a kind of W18O49Carbon fibre composite and preparation method thereof is coated, it is used micro- The hot method preparation process of ripple secondary solvent is simple, and controllability is strong, and yield is high, and cost is cheap, is adapted to batch production.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should It is considered as protection scope of the present invention.

Claims (10)

  1. A kind of 1. W18O49Coat carbon fibre composite, it is characterised in that including carbon fiber and use the hot method of microwave radiation technology solvent It is coated on the W of carbon fiber surface18O49Nano material.
  2. 2. W as claimed in claim 118O49Coat carbon fibre composite, it is characterised in that the presentation shape of described carbon fiber Formula is carbon cloth, the model WOS1002 of carbon cloth.
  3. A kind of 3. W18O49Coat the preparation method of carbon fibre composite, it is characterised in that exist using the hot method of microwave radiation technology solvent Carbon fiber surface grows W18O49Nano material.
  4. 4. the W described in claim 318O49Coat the preparation method of carbon fibre composite, it is characterised in that using microwave radiation technology Solvent-thermal method grows W in carbon fiber surface18O49Nano material includes:Using the alcoholic solution of Tungstenic compound as precursor solution, carbon Fiber carries out microwave radiation technology solvent thermal response, microwave power 400W as reaction source, and reaction temperature is 160~200 DEG C, reaction Time is 5~60min.
  5. 5. the W described in claim 318O49Coat the preparation method of carbon fibre composite, it is characterised in that using microwave radiation technology Solvent-thermal method grows W in carbon fiber surface18O49Nano material includes:Using the alcoholic solution of Tungstenic compound as precursor solution, carbon Cloth carries out microwave radiation technology solvent thermal response as reaction source, and microwave power 400W, reaction temperature is 160~200 DEG C, during reaction Between be 5~60min.
  6. 6. the W described in claim 318O49Coat the preparation method of carbon fibre composite, it is characterised in that using microwave radiation technology Solvent-thermal method grows W in carbon cloth surfaces18O49Nano material includes:Using the alcoholic solution of Tungstenic compound as growth solution, carbon cloth is made Microwave radiation technology solvent thermal response, microwave power 400W are carried out for reaction source, reaction temperature is 160 DEG C, reaction time 5min.
  7. 7. the W described in claim 318O49Coat the preparation method of carbon fibre composite, it is characterised in that using microwave radiation technology Solvent-thermal method grows W in carbon cloth surfaces18O49Nano material includes:Using the alcoholic solution of Tungstenic compound as growth solution, carbon cloth is made Microwave radiation technology solvent thermal response, microwave power 400W are carried out for reaction source, reaction temperature is 180 DEG C, and the reaction time is 30min。
  8. 8. the W described in claim 318O49Coat the preparation method of carbon fibre composite, it is characterised in that using microwave radiation technology Solvent-thermal method grows W in carbon cloth surfaces18O49Nano material includes:Using the alcoholic solution of Tungstenic compound as growth solution, carbon cloth is made Microwave radiation technology solvent thermal response, microwave power 400W are carried out for reaction source, reaction temperature is 200 DEG C, and the reaction time is 60min。
  9. 9. the W as described in claim 4,5,6,7 or 818O49Coat the preparation method of carbon fibre composite, it is characterised in that Described Tungstenic compound is WCl6, the alcoholic solution concentration of Tungstenic compound is 4g/L~12g/L.
  10. 10. the W as described in claim 4,5,6,7 or 818O49Coat the preparation method of carbon fibre composite, it is characterised in that The alcoholic solution of described Tungstenic compound is the ethanol solution of Tungstenic compound.
CN201710602202.7A 2017-07-21 2017-07-21 W18O49Coated carbon fiber composite material and preparation method thereof Expired - Fee Related CN107604635B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109650454A (en) * 2019-02-28 2019-04-19 陕西科技大学 A kind of Microwave-assisted synthesis W18O49The method of nano material
CN109731580A (en) * 2019-02-28 2019-05-10 陕西科技大学 A kind of W18O49The preparation method of/NF self-supporting electrocatalysis material

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105355875A (en) * 2015-11-05 2016-02-24 盐城工学院 Tungsten oxide nanowire wound composite material, preparation method and application
CN105749912A (en) * 2016-03-14 2016-07-13 中国海洋大学 Multi-morphology metal-doped W18O49 electrocatalyst and application thereof to hydrogen production by water electrolysis
JP2017025348A (en) * 2015-07-15 2017-02-02 三菱マテリアル株式会社 Mo-W OXIDE SPUTTERING TARGET, AND MANUFACTURING METHOD OF Mo-W OXIDE SPUTTERING TARGET
CN106423144A (en) * 2016-11-17 2017-02-22 中国地质大学(北京) Carbon fiber@tungsten oxide nano-particle core-shell composite structure and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2017025348A (en) * 2015-07-15 2017-02-02 三菱マテリアル株式会社 Mo-W OXIDE SPUTTERING TARGET, AND MANUFACTURING METHOD OF Mo-W OXIDE SPUTTERING TARGET
CN105355875A (en) * 2015-11-05 2016-02-24 盐城工学院 Tungsten oxide nanowire wound composite material, preparation method and application
CN105749912A (en) * 2016-03-14 2016-07-13 中国海洋大学 Multi-morphology metal-doped W18O49 electrocatalyst and application thereof to hydrogen production by water electrolysis
CN106423144A (en) * 2016-11-17 2017-02-22 中国地质大学(北京) Carbon fiber@tungsten oxide nano-particle core-shell composite structure and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109650454A (en) * 2019-02-28 2019-04-19 陕西科技大学 A kind of Microwave-assisted synthesis W18O49The method of nano material
CN109731580A (en) * 2019-02-28 2019-05-10 陕西科技大学 A kind of W18O49The preparation method of/NF self-supporting electrocatalysis material
CN109731580B (en) * 2019-02-28 2021-07-06 陕西科技大学 W18O49Preparation method of/NF self-supporting electrocatalytic material

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