CN114455586B - W (W) 2 Rapid preparation method of C nano-particles - Google Patents
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000002238 carbon nanotube film Substances 0.000 claims abstract description 32
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 31
- 108010005939 Ciliary Neurotrophic Factor Proteins 0.000 claims description 75
- 102100031614 Ciliary neurotrophic factor Human genes 0.000 claims description 75
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 27
- 238000010438 heat treatment Methods 0.000 claims description 16
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 13
- 229910052709 silver Inorganic materials 0.000 claims description 13
- 239000004332 silver Substances 0.000 claims description 13
- 239000000853 adhesive Substances 0.000 claims description 12
- 230000001070 adhesive effect Effects 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 239000010937 tungsten Substances 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 3
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- 238000000034 method Methods 0.000 abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 13
- 229910052799 carbon Inorganic materials 0.000 abstract description 11
- 230000015572 biosynthetic process Effects 0.000 abstract description 10
- 238000003786 synthesis reaction Methods 0.000 abstract description 10
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- 238000011065 in-situ storage Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 4
- 239000007791 liquid phase Substances 0.000 abstract description 2
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 abstract 1
- 238000007747 plating Methods 0.000 abstract 1
- 238000005478 sputtering type Methods 0.000 abstract 1
- 229910001930 tungsten oxide Inorganic materials 0.000 abstract 1
- 238000000967 suction filtration Methods 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
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- 235000019441 ethanol Nutrition 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000002041 carbon nanotube Substances 0.000 description 3
- 238000007740 vapor deposition Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000002134 carbon nanofiber Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
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- 239000004744 fabric Substances 0.000 description 1
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- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
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- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- -1 sites ACS omega Chemical compound 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/949—Tungsten or molybdenum carbides
-
- 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
-
- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The invention discloses a W 2 A rapid preparation method of C nano-particles. The method utilizes joule heat generated by electrifying a carbon nanotube film (CNTF) to evaporate tungsten powder at high temperature, and loads tungsten oxide (WOx) on the surface of the film; further quickly reducing WOx by in-situ Joule heat in a mode of consuming framework carbon to obtain W 2 C nanoparticles. The invention replaces the traditional resistive and sputtering type film plating process, the liquid phase method and other W by using CNTF with rapid temperature rise and drop characteristics to generate Joule heat 2 The C synthesis mode has the characteristics of low cost, low energy consumption and high efficiency, and can realize W in a few seconds 2 The ultra-fast preparation of the C nano-particles has important commercial application prospect.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to an ultra-rapid preparation method of tungsten carbide nanoparticles.
Background
W 2 C has the characteristics of high melting point, better heat conductivity, excellent mechanical property and the like. The method has wide application in the fields of material processing, aerospace and catalysis. Wherein in the aspects of electrocatalytic hydrogen evolution, hydrogen production and the like, W 2 The catalytic yield of C is outstanding in non-noble metal catalysts; meanwhile, the catalyst has the advantage of being not easy to be poisoned by CO and the like, and has great potential for replacing noble metal catalysts Pt, ru and the like.
In view of the above advantages, many researchers struggle to explore W 2 The method for synthesizing the C nano-particles is efficient, but is generally limited to the traditional vapor deposition synthesis. For example, xia et al report a method for vapor deposition synthesis of tunable carbon nanotube-tungsten carbide nanoparticle heterostructures (Xia, et al Tunable carbon nanotube-tungsten carbide nanoparticles heterostructures by vapor deposition Journal of Applied Physics, 2014, 115 (18)). The method first involves mixing 0.5gW (CO) 6 The powder was charged to the bottom of an alumina crucible and covered with 0.034g of purified α -CNTs, and the crucible was then covered. Prior to deposition, the furnace was vacuum cleaned and high purity hydrogen gas was introduced at a rate of 400 sccm (standard cubic centimeters per minute). The deposition temperature was raised to 400 and 900 ℃ at 5 ℃/min, respectively, and after 1h incubation was cooled to room temperature. Annealing at 2200 ℃ for 30 minutes under argon atmosphere to obtain W 2 C. Although this way the CNTs are uniformly loaded with W 2 C nano particles still have certain WC and other impurities mixed in, and have long time consumption, high energy consumption and low efficiency, and hydrogen is needed in experiments, so that the danger in the preparation process is increased. In addition, takafumi et al reported a single step synthesis of W 2 Method of C nanoparticles (Takafumi, et al Single-step synthesis of W) 2 C nanomarticle-dispersed carbon electrocatalysts for hydrogen evolution reactions utilizing phosphate groups on carbon edge sites ACS omega, 2016, 1 (4)). They developed the selective synthesis of W from phosphotungstic acid 2 One step protocol for C nanoparticles. The method is compared with the prior W 2 The synthesis method of the C nano particles is simple, but the synthesis process still needs high-temperature calcination treatment for several hours, and has high energy consumption and low efficiency. In addition, the process utilizes a mechanism of selective synthesis, W 2 The presence of phase C is not stable.
Disclosure of Invention
The invention provides a W for solving the short plate in the prior art 2 A rapid preparation method of C nano-particles.
The invention solves the technical problems by the following scheme:
w (W) 2 Method for rapidly preparing C nano-particles by electrifying one carbon nano-tube filmCarrying out WOx loading on the other carbon nano tube film by using the generated Joule heat, and then quickly and in-situ reducing WOx by using the Joule heat high temperature of CNTF and the self carbon skeleton as a carbon source to prepare the target W 2 C nanoparticles.
The joule heat source includes, but is not limited to, carbon nanotube film, graphene, carbon nanofiber film or fabric.
W (W) 2 The rapid preparation method of the C nano-particles comprises the following steps:
(1) Pretreatment of a carbon nanotube film: cutting a carbon nano tube film with the specification of 2 multiplied by 4cm and the thickness of 20 micrometers, and soaking for 6 hours by using concentrated hydrochloric acid to remove metal impurities such as a catalyst and the like;
(2) Loading of WOx particles: uniformly dispersing tungsten powder in absolute ethyl alcohol, and then carrying out suction filtration on the tungsten powder to obtain CNTF deposited with a tungsten powder layer; then the tungsten-containing powder of the CNTF faces upwards, two ends of the tungsten-containing powder are adhered to a sample frame in a Joule heating furnace by utilizing conductive silver adhesive, and another CNTF with the same thickness specification is placed on the sample frame at intervals. The furnace chamber is further pumped to a certain vacuum degree and is connected with a direct current power supply. The tungsten powder on the upper surface of the CNTF of the lower layer is partially evaporated and oxidized by controlling the voltage and the electrifying time, and is deposited on the lower surface of the CNTF of the upper layer.
（3）W 2 Fast joule heating preparation of C nanoparticles: coating a layer of PVP solution on the surface of the CNTF loaded with WOx particles, drying in a blast drying oven, and taking out; and (3) adhering the two ends of the sample rack in the Joule heating furnace by using conductive silver adhesive, and pumping the furnace chamber to a certain vacuum degree. The target W is prepared by controlling the voltage and the power-on time and quickly reducing WOx at high temperature by utilizing the Joule heat of CNTF 2 C nanoparticles.
Wherein the oxidation and evaporation temperatures in the step (2) are 700-1000 ℃.
As a preferable technical scheme, the specific flow of the step (2) is as follows: uniformly dispersing 0.2g of tungsten powder in 20ml of absolute ethyl alcohol, carrying out ultrasonic treatment for 10 minutes, and taking 2ml of solution to carry out suction filtration on a carbon nano tube film to obtain CNTF uniformly coated with tungsten powder; then followThe surface of the CNTF containing tungsten powder faces upwards, two ends of the CNTF are adhered to a sample frame in a Joule heating furnace by using conductive silver adhesive, and a CNTF with the same thickness specification is placed at a distance of 5 mm. Further draw the furnace chamber to 10 -1 Pa vacuum degree, and connecting DC power supply to both ends of CNTF. At 13V constant pressure, the CNTF surface reached 800 ℃. And maintaining the constant pressure for 1s to partially oxidize tungsten powder on the upper surface of the CNTF of the lower layer, and quickly evaporating WOx particles on the lower surface of the CNTF of the upper layer.
As a preferable technical scheme, the specific flow of the step (2) is as follows: uniformly dispersing 0.2g of tungsten powder in 20ml of absolute ethyl alcohol, carrying out ultrasonic treatment for 10 minutes, and taking 2ml of solution to carry out suction filtration on a carbon nano tube film to obtain CNTF uniformly coated with tungsten powder; then the surface of the CNTF containing tungsten powder faces upwards, two ends of the CNTF are adhered to a sample frame in a Joule heating furnace by using conductive silver adhesive, and a CNTF with the same thickness specification is placed at a distance of 5 mm. Further draw the furnace chamber to 10 -1 Pa vacuum degree, and connecting DC power supply to both ends of CNTF. At a constant pressure of 14V, the CNTF surface reached 850 ℃. And maintaining the constant pressure for 1s, so that tungsten powder on the upper surface of the CNTF of the lower layer is partially oxidized, and WOx particles are uniformly evaporated to the lower surface of the CNTF of the upper layer.
The specific flow of the step (3) is as follows: 0.2g PVP was added to 20ml ethanol, sonicated and dispersed for 1h. Uniformly coating 1ml of PVP-ethanol solution on the surface of the CNTF loaded with WOx, and drying the PVP-ethanol solution in a blast drying oven at 60 ℃ for 0.5h. Further using conductive silver adhesive to adhere two ends of the film to a sample holder in a Joule heating furnace, and pumping the furnace chamber to 10 -2 Pa vacuum degree and direct current power supply. At a constant pressure of 35V, the surface of CNTF reached 1100 ℃. At the moment, the skeleton carbon of CNTF and PVP synergistically reduce WOx to obtain target W uniformly distributed on the surface of CNTF 2 C nanoparticles.
The beneficial technology which can be realized by the invention at least comprises: the CNTF with rapid temperature rise and drop characteristics is electrified to generate Joule heat to replace the traditional resistive and sputtering coating processes, and the W method 2 The C synthesis mode has the characteristics of low cost, low energy consumption and high efficiency, and can realize W in a few seconds 2 The ultra-fast preparation of the C nano-particles has important commercial application prospect.
Drawings
FIG. 1 is a graph showing the preparation of nano-W on the surface of a carbon nanotube film using ultra-fast Joule thermal temperature response in the present invention 2 Schematic of the process of C.
FIG. 2 is a nano-W prepared on the surface of a carbon nanotube film in example 1 of the present invention 2 C scanning electron microscope photograph.
FIG. 3 is a nano-W prepared on the surface of a carbon nanotube film in example 1 of the present invention 2 C scanning electron microscope photograph.
FIG. 4 is a nano-W prepared on the surface of a carbon nanotube film in example 1 of the present invention 2 X-ray diffraction pattern of C.
FIG. 5 is a nano-W prepared on the surface of a carbon nanotube film in example 1 of the present invention 2 Transmission electron microscope photograph of C particles.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It is apparent that the described embodiments are only some, but not all, examples of the invention. Based on the embodiments of the present invention, other embodiments that may be obtained by those of ordinary skill in the art without making any inventive effort are within the scope of the present invention.
Example 1
W (W) 2 The fast preparation process of C nanometer particle includes first utilizing the Joule heat produced by energizing the carbon nanotube film to load WOx onto the carbon nanotube film, and subsequent fast in-situ reduction of WOx with the Joule heat in high temperature to prepare target W on the surface of the carbon nanotube film 2 C nanoparticles.
W (W) 2 The rapid preparation method of the C nano-particles specifically comprises the following steps:
a carbon nanotube film with the thickness of 20 micrometers and the specification of 2X 4cm is cut, and is soaked for 6 hours by concentrated hydrochloric acid to remove metal impurities such as the contained catalyst and the like.
Further, willUniformly dispersing 0.2g of tungsten powder in 20ml of absolute ethyl alcohol, carrying out ultrasonic treatment for 10 minutes, taking 2ml of solution, and carrying out suction filtration on the solution onto a carbon nano tube film to obtain CNTF uniformly coated with tungsten powder; then the surface of the CNTF containing tungsten powder faces upwards, two ends of the CNTF are adhered to a sample frame in a Joule heating furnace by using conductive silver adhesive, and a CNTF with the same thickness specification is placed at a distance of 5 mm. Further draw the furnace chamber to 10 -1 Pa vacuum degree, and connecting DC power supply to both ends of CNTF. At a constant pressure of 12V, the CNTF surface reached 750 ℃. And maintaining the constant pressure for 1s, so that tungsten powder on the upper surface of the CNTF of the lower layer is partially oxidized, and WOx particles are uniformly evaporated to the lower surface of the CNTF of the upper layer.
Further, 0.2g PVP was added to 20ml ethanol, and sonicated and dispersed for 1h. Uniformly coating 1ml of PVP-ethanol solution on the surface of the CNTF loaded with WOx, and drying the PVP-ethanol solution in a blast drying oven at 60 ℃ for 0.5h. Further using conductive silver adhesive to adhere two ends of the film to a sample holder in a Joule heating furnace, and pumping the furnace chamber to 10 -2 Pa vacuum degree and direct current power supply. Under constant pressure of 32V, the surface of CNTF reaches 1000 ℃, at this time, the skeleton carbon of CNTF and PVP will jointly reduce WOx to obtain target W uniformly distributed on the surface of CNTF 2 C nanoparticles.
Example 2
W (W) 2 The fast preparation process of C nanometer particle includes first utilizing the Joule heat produced by energizing the carbon nanotube film to load WOx onto the carbon nanotube film, and subsequent fast in-situ reduction of WOx with the Joule heat in high temperature to prepare target W on the surface of the carbon nanotube film 2 C nanoparticles.
W (W) 2 The rapid preparation method of the C nano-particles specifically comprises the following steps:
a carbon nanotube film with the thickness of 20 micrometers and the specification of 2X 4cm is cut, and is soaked for 6 hours by concentrated hydrochloric acid to remove metal impurities such as the contained catalyst and the like.
Further, uniformly dispersing 0.2g of tungsten powder in 20ml of absolute ethyl alcohol, carrying out ultrasonic treatment for 10 minutes, and taking 2ml of solution to carry out suction filtration on a carbon nano tube film to obtain CNTF uniformly coated with tungsten powder; then the CNTF contains tungsten powder with one side facing upwardsThe two ends of the sample are adhered to a sample holder in a Joule heating furnace by using conductive silver adhesive, and a CNTF with the same thickness specification is placed at a distance of 5mm on the sample holder. Further draw the furnace chamber to 10 -1 Pa vacuum degree, and connecting DC power supply to both ends of CNTF. At 13V constant pressure, the CNTF surface reached 800 ℃. And maintaining the constant pressure for 1s to partially oxidize tungsten powder on the upper surface of the CNTF of the lower layer, and quickly evaporating WOx particles on the lower surface of the CNTF of the upper layer.
Further, 0.2g PVP was added to 20ml ethanol, and sonicated and dispersed for 1h. Uniformly coating 1ml of PVP-ethanol solution on the surface of the CNTF loaded with WOx, and drying the PVP-ethanol solution in a blast drying oven at 60 ℃ for 0.5h. Further using conductive silver adhesive to adhere two ends of the film to a sample holder in a Joule heating furnace, and pumping the furnace chamber to 10 -2 Pa vacuum degree and direct current power supply. At a constant pressure of 35V, the surface of CNTF reached 1100 ℃. At the moment, the skeleton carbon of CNTF and PVP jointly reduce WOx to obtain target W uniformly distributed on the surface of CNTF 2 C nanoparticles.
Example 3
W (W) 2 A rapid preparation method of C nano-particles. The invention uses the Joule heat generated by electrifying the carbon nano tube film to carry out WOx load on the carbon nano tube film, and continuously uses the Joule heat high temperature of the film to quickly reduce WOx in situ, and then prepares the target W on the surface of the carbon nano tube film 2 C nanoparticles.
W (W) 2 The rapid preparation method of the C nano-particles specifically comprises the following steps:
a carbon nanotube film with the thickness of 20 micrometers and the specification of 2X 4cm is cut, and is soaked for 6 hours by concentrated hydrochloric acid to remove metal impurities such as the contained catalyst and the like.
Further, uniformly dispersing 0.2g of tungsten powder in 20ml of absolute ethyl alcohol, carrying out ultrasonic treatment for 10 minutes, and taking 2ml of solution to carry out suction filtration on a carbon nano tube film to obtain CNTF uniformly coated with tungsten powder; then the surface of the CNTF containing tungsten powder faces upwards, two ends of the CNTF are adhered to a sample frame in a Joule heating furnace by using conductive silver adhesive, and a CNTF with the same thickness specification is placed at a distance of 5 mm. Further draw the furnace chamber to 10 -1 The degree of vacuum of Pa,and the two ends of the CNTF are connected with a direct current power supply. At a constant pressure of 14V, the CNTF surface reached 850 ℃. And maintaining the constant pressure for 1s to partially oxidize tungsten powder on the upper surface of the CNTF of the lower layer, and quickly evaporating WOx particles on the lower surface of the CNTF of the upper layer.
Further, 0.2g PVP was added to 20ml ethanol, and sonicated and dispersed for 1h. Uniformly coating 1ml of PVP-ethanol solution on the surface of the CNTF loaded with WOx, and drying the PVP-ethanol solution in a blast drying oven at 60 ℃ for 0.5h. Further using conductive silver adhesive to adhere two ends of the film to a sample holder in a Joule heating furnace, and pumping the furnace chamber to 10 -2 Pa vacuum degree and direct current power supply. At a constant pressure of 46V, the surface of CNTF reached 1300 ℃. At the moment, the skeleton carbon of CNTF and PVP jointly reduce WOx to obtain target W uniformly distributed on the surface of CNTF 2 C nanoparticles.
Relative to other W 2 Preparation method of C nano-particles, W is described in the invention 2 The fast preparation method of the C nano particles replaces the traditional resistive and sputtering coating processes, and W such as a liquid phase method and the like by using CNTF with fast heating and cooling characteristics to generate Joule heat through electrifying 2 The C synthesis mode has the characteristics of low cost, low energy consumption and high efficiency, and can realize W in a few seconds 2 The ultra-fast preparation of the C nano-particles has important commercial application prospect.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (1)
1. W (W) 2 The rapid preparation method of the C nano-particles is characterized by comprising the following steps: mainly comprises the following steps:
pretreatment of a carbon nanotube film: cutting a carbon nano tube film with the specification of 2 multiplied by 4cm and the thickness of 20 micrometers, and soaking for 6 hours by using concentrated hydrochloric acid to remove metal impurities of the contained catalyst;
WO x loading of particles: uniformly dispersing tungsten powderIn absolute ethyl alcohol, then suction-filtering the solution onto a carbon nano tube film to obtain CNTF deposited with a tungsten powder layer; then the tungsten-containing powder of the CNTF faces upwards, the two ends of the CNTF are adhered to a sample frame in a Joule heating furnace by using conductive silver colloid, and another CNTF with the same thickness specification is placed at a distance of 5mm above the sample frame, and the furnace chamber is further pumped to 10 -1 The Pa vacuum degree is connected with a direct current power supply, the CNTF surface reaches 750-850 ℃ under 13V constant pressure, and the constant pressure is kept for 1s, so that tungsten powder on the upper surface of the lower CNTF is partially evaporated and oxidized, and is deposited on the lower surface of the upper CNTF;
（3）W 2 fast joule heating preparation of C nanoparticles: in a load of WO x Coating a layer of PVP solution on the surface of the CNTF of the particles, drying in a blast drying oven at 60 ℃ for 0.5h, and taking out; the two ends of the conductive silver adhesive are adhered to a sample frame in a Joule heating furnace, and the furnace chamber is pumped to 10 -2 Pa vacuum degree, and switching in DC power supply, under constant voltage of 35V, when CNTF surface reaches 1000deg.C, 1100 deg.C or 1300 deg.C, high temperature rapid reduction of WO by using CNTF joule heat x Obtaining the target W 2 C nanoparticles.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015021177A1 (en) * | 2013-08-06 | 2015-02-12 | Massachusetts Institute Of Technology | Production of non-sintered transition metal carbide nanoparticles |
| CN107176604A (en) * | 2016-03-10 | 2017-09-19 | 中国科学院金属研究所 | A kind of method that carbon materials surface in situ generates nano-carbide coating |
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