CN115155482A - Device and method for preparing graphene loaded nano metal particles by pulse discharge flash - Google Patents
Device and method for preparing graphene loaded nano metal particles by pulse discharge flash Download PDFInfo
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- CN115155482A CN115155482A CN202210875695.2A CN202210875695A CN115155482A CN 115155482 A CN115155482 A CN 115155482A CN 202210875695 A CN202210875695 A CN 202210875695A CN 115155482 A CN115155482 A CN 115155482A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 138
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 59
- 239000002923 metal particle Substances 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 31
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 250
- 229910052802 copper Inorganic materials 0.000 claims abstract description 210
- 239000010949 copper Substances 0.000 claims abstract description 210
- 238000006243 chemical reaction Methods 0.000 claims abstract description 186
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 72
- 239000000843 powder Substances 0.000 claims abstract description 48
- 239000002184 metal Substances 0.000 claims abstract description 41
- 229910052751 metal Inorganic materials 0.000 claims abstract description 41
- 239000011812 mixed powder Substances 0.000 claims abstract description 28
- 238000000926 separation method Methods 0.000 claims abstract description 22
- 238000002360 preparation method Methods 0.000 claims abstract description 17
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 7
- 238000007599 discharging Methods 0.000 claims abstract description 5
- 239000002082 metal nanoparticle Substances 0.000 claims abstract description 5
- 238000005336 cracking Methods 0.000 claims abstract description 4
- 230000007246 mechanism Effects 0.000 claims description 27
- 238000001514 detection method Methods 0.000 claims description 26
- 239000007789 gas Substances 0.000 claims description 20
- 239000003990 capacitor Substances 0.000 claims description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 230000001681 protective effect Effects 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 5
- 239000004033 plastic Substances 0.000 claims description 4
- 229920003023 plastic Polymers 0.000 claims description 4
- 239000005060 rubber Substances 0.000 claims description 4
- 239000002699 waste material Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000002023 wood Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000003054 catalyst Substances 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 4
- 238000011068 loading method Methods 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 description 4
- 239000003245 coal Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- -1 alcohol compound Chemical class 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000005192 partition Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000002134 carbon nanofiber Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002723 waste plastics and rubber Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
- B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/72—Copper
-
- B01J35/23—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/342—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electric, magnetic or electromagnetic fields, e.g. for magnetic separation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention discloses a device and a method for preparing graphene-loaded nano metal particles by pulse discharge flash in the field of nano metal catalyst preparation.A separation net is used for separating two reaction cavities, mixed powder of metal and carbon is added into a space between two copper electrode plates in a first reaction cavity, carbon source powder is added into a space between two copper electrode plates in a second reaction cavity, four electric telescopic rods correspondingly connected with the four copper electrode plates work simultaneously, and the mixed powder and the compressed carbon source powder are compressed; discharging by a second pulse discharge circuit, and cracking carbon source powder into carbon atoms to generate graphene; then the first pulse discharge circuit discharges to gasify the metal powder into gaseous metal nano particles, and the gaseous nano metal particles diffuse into the second reaction cavity through the separation net, are condensed and deposit on the graphene; the invention combines the production preparation of graphene and the loading of nano metal particles, and realizes high efficiency, high yield and industrial production.
Description
Technical Field
The invention relates to the field of preparation of nano metal catalysts, in particular to a device and a method for preparing graphene loaded with nano metal particles by using pulse discharge action.
Background
Carbon materials such as graphene, carbon black, activated carbon, CNTs, carbon nanofibers, and the like have been widely used as carriers of catalysts, wherein graphene has a regular two-dimensional surface structure, good stability, excellent mechanical properties, and the like, and can be used as a good template to carry catalysts. For example, the nano Pt particles are loaded on graphene, and the nano Pt particles are applied to an anode material of a proton exchange membrane fuel cell, and have higher electrocatalytic activity and stability for electrocatalytic reduction of oxygen. For another example, the nano Au particles are loaded on the graphene, so that the graphene has good catalytic performance on the oxidation of the alcohol compound into the corresponding aldehyde ketone compound. The problems of agglomeration and reduction of catalytic activity of the nano metal particles are solved by loading the nano metal particles on the graphene. Two key problems that need to be solved most for the preparation of graphene and graphene-supported metal particles are: on one hand, the preparation efficiency and the yield are improved, and on the other hand, the preparation method and the preparation device are easy to realize industrial production.
The existing method for preparing graphene and graphene-loaded nano metal particles with high efficiency comprises the following steps: joule heat generated by pulse discharge of the capacitor is used for carrying out high-temperature impact on a carbon source and cracking and recombining the carbon source into graphene. For example, the preparation method disclosed in the document of chinese patent application No. 202110704452.8 entitled "a preparation method of coal-based porous carbon" is to prepare a coal-based porous material by a pulse discharge method; the preparation method disclosed in the document with the Chinese patent application number of 202110704558.8 and the name of "a method for preparing metal particles loaded with coal-based graphene through high-temperature thermal shock" is also to prepare the graphene-loaded iron, cobalt, nickel and other nano metal particles by using a pulse discharge method. Compared with the traditional method for loading nano metal particles on graphene, such as a traditional chemical reduction method, an electrochemical deposition method and the like, the preparation methods have higher efficiency, but the methods can only be used for production in a small-batch laboratory, have no large-scale forming production device, need manual regulation and control, and cannot solve the problems of large-batch, high-efficiency and industrial production.
Disclosure of Invention
The invention provides a device and a method for preparing graphene-loaded nano metal particles by pulse discharge flash aiming at the problems that the existing process for preparing the graphene-loaded nano metal particles by pulse discharge can only realize small-batch production and needs manual regulation and control, and the like, so that the composite material of the graphene-loaded nano metal particles is produced with high efficiency and high yield in an industrialized mode.
The device for preparing the graphene loaded nano metal particles by the pulse discharge flash adopts the following technical scheme: the device is provided with a first reaction cavity and a second reaction cavity which are arranged side by side and are the same, and the two reaction cavities are separated by a separation net; a first copper electrode plate and a second copper electrode plate which are identical in structure and are arranged face to face are arranged in the first reaction cavity, mixed powder of metal and carbon is filled between the first copper electrode plate and the second copper electrode plate, a third copper electrode plate and a fourth copper electrode plate which are identical in structure and are arranged face to face are arranged in the second reaction cavity, and carbon source powder is filled between the third copper electrode plate and the fourth copper electrode plate; each copper electrode plate is connected with a corresponding electric telescopic rod; a first pulse discharge series circuit and a first resistance detection series circuit are connected between the first copper electrode plate and the second copper electrode plate, and a second pulse discharge series circuit and a second resistance detection series circuit are connected between the third copper electrode plate and the fourth copper electrode plate; the top and the bottom of the first reaction cavity and the second reaction cavity are both provided with openings, and the openings at the top and the bottom are respectively connected with a movable cover plate through a polished rod screw-nut mechanism to drive the movable cover plate at the top or the bottom to open or close the openings.
Furthermore, each copper electrode plate is formed by connecting a flat cuboid and a long and thin cylinder, the long and thin cylinder is connected to the center of the flat cuboid and perpendicular to the flat cuboid, the flat cuboid is positioned inside the corresponding reaction cavity and perpendicular to the separation net and the bottom surface of the reaction cavity, the long and thin cylinder penetrates through the side wall of the reaction cavity and extends out, an insulating connector is coaxially and fixedly connected between the long and thin cylinder outside the reaction cavity and the output end of the electric telescopic rod, a copper ring electrode is tightly sleeved outside the long and thin cylinder, and an electric telescopic rod outer sleeve is tightly sleeved outside the copper ring electrode, the insulating connector and the output end of the electric telescopic rod; each copper electrode plate is connected to the corresponding pulse discharge series circuit and the resistance detection series circuit through the corresponding copper ring electrode.
Further, every polished rod lead screw nut mechanism all includes polished rod, polished rod bearing frame, lead screw nut bearing frame and step motor, and the lead screw is opposite at the polished rod, and lead screw and polished rod parallel with electric telescopic handle, cup joint the lead screw nut bearing frame on the lead screw, and the cover has the polished rod bearing frame on the polished rod, and lead screw and polished rod all run through the upper end lateral wall and the copper plate electrode of the reaction cavity that correspond with clearance, and the tip of lead screw is with axle center fixed connection step motor, removal apron and polished rod bearing frame and the equal fixed connection of lead screw nut bearing frame.
Furthermore, each pulse discharge series circuit is formed by connecting a corresponding high-voltage direct-current power supply, a capacitor, a current transformer, two copper ring electrodes, two copper electrode plates and a relay; each resistance detection series circuit is formed by connecting a corresponding resistance detector, two copper ring electrodes and two copper electrode plates.
Furthermore, an oscilloscope is connected with a current transformer and is connected in parallel with the corresponding pulse discharge series circuit, a relay and a resistance detector in the first pulse discharge series circuit are both connected with a first main control center, and the first main control center is also respectively connected with two electric telescopic rods connected with the first copper electrode plate and the second copper electrode plate through control lines; a relay and a resistance detector in the second pulse discharge series circuit are both connected with a second control center, and the second control center is also respectively connected with two electric telescopic rods connected with a third copper electrode plate and a fourth copper electrode plate through control lines; the first main control center is connected with the second secondary control center to control the second secondary control center.
The method for preparing the graphene loaded nano metal particles by the pulse discharge flash adopts the technical scheme that:
step 1): crushing a carbon source into carbon source powder, and mixing the carbon powder and metal powder to be loaded into mixed powder of metal and carbon;
step 2): the top polished rod screw nut mechanisms of the first reaction cavity and the second reaction cavity work, two movable cover plates at the tops are opened, mixed powder of metal and carbon is added into a space between the first copper electrode plate and the second copper electrode plate, carbon source powder is added into a space between the third copper electrode plate and the fourth copper electrode plate, meshes of the separation net are smaller than the mixed powder of the metal and the carbon and the size of the carbon source powder, and the two movable cover plates are closed;
step 3): the four electric telescopic rods correspondingly connected with the four copper electrode plates work simultaneously to drive the first copper electrode plate and the second copper electrode plate to move towards the opposite direction to compress mixed powder of metal and carbon, and the third copper electrode plate and the fourth copper electrode plate to move towards the opposite direction to compress carbon source powder;
step 4): the two resistance detection series circuits work simultaneously to detect the resistance between the first copper electrode plate and the mixed powder of the metal and the carbon, and the resistance between the third copper electrode plate and the carbon source powder, and the resistance between the fourth copper electrode plate and the carbon source powder, when the detected resistance values meet the requirements, the metal and carbon mixed powder and the carbon source powder are compressed compactly, and the two resistance detection series circuits stop working;
and step 5): discharging by a second pulse discharge circuit, and cracking carbon source powder into carbon atoms to generate graphene; then the first pulse discharge circuit discharges to gasify the metal powder into gaseous metal nano-particles; and the gaseous nano metal particles diffuse into the second reaction cavity through the separation net, are condensed and deposited on the graphene, and generate the graphene-loaded nano metal particles.
Further, in the processes of the steps 3) -5), argon gas is output from the protective gas supply device, enters the first reaction cavity, sequentially passes through the space between the first copper electrode plate and the second copper electrode plate, the separation net and the space between the third copper electrode plate and the fourth copper electrode plate, and finally comes out from the second reaction cavity.
Furthermore, the voltage of the first pulse discharge series circuit is 500-1000V, the current is 20-30A, and the discharge period is 50-100ms; the discharge voltage of the second pulse discharge series circuit is 1000-1500V, the current is 20-30A, and the discharge period is 50-100ms; the time interval of the pulse discharge of the two pulse discharge series circuits is 100-150ms.
The innovation and superiority of the invention after adopting the technical scheme are as follows:
1. compared with the problem that the graphene-loaded nano metal particles can be produced only in small batches in a laboratory in the existing process of producing and preparing the graphene-loaded nano metal particles by using high temperature generated by pulse discharge, the method provided by the invention realizes high-efficiency, high-yield and industrialized production of the composite material for preparing the graphene-loaded nano metal particles.
2. The preparation of the graphene utilizes polymers with higher carbon content such as waste plastics, rubber and the like as carbon sources, is favorable for pulse discharge to instantly generate ultrahigh temperature, and the carbon sources are cracked into carbon atoms and recombined into the graphene. Is beneficial to the recovery and reutilization of waste plastics, rubber and the like, and is green and environment-friendly.
3. The method combines the production and preparation of the graphene and the loading of the nano metal particles, has simple process and is easy to realize industrial production.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for flash preparation of graphene loaded with nano-metal particles by pulse discharge according to the present invention;
FIG. 2 is an enlarged isometric view of FIG. 1 with two upper removable cover plates removed;
FIG. 3 is an enlarged connection view of the copper electrode plate and the electric telescopic rod in FIG. 1;
FIG. 4 is a connection diagram of a control circuit for the four copper electrode plates of FIG. 2;
fig. 5 is a schematic diagram of the generation of the metal nanoparticles supported by graphene.
In the figure: 1: a first electric telescopic rod; 101: a first resistance detector energization slot; 102: a first copper ring electrode; 103, a first pulse discharge circuit electrifying groove; 104: a first electric telescopic rod driving motor; 105: a telescopic rod body of the first electric telescopic rod; 106: the first electric telescopic rod is sleeved with: 107: a first insulating connector; 2: a shielding gas supply device; 3: a shielding gas line; 4: a cover plate is moved on the first reaction cavity; 5: a second electric telescopic rod; 6: a cover plate is moved on the second reaction cavity; 7: a third electric telescopic rod; 8: a shielding gas outlet; 9: a collection box; 10: a fourth electric telescopic rod; 11: a stepping motor is arranged on the second reaction cavity; 12: a stepping motor is arranged on the first reaction cavity; 13: a first reaction chamber; 14: a first copper electrode plate; 15: a second copper electrode plate; 16: a polished rod bearing seat; 17: a polish rod; 18: a lead screw nut bearing seat; 19: a lead screw; 20: a third copper electrode plate; 21: a fourth copper electrode plate; 22: a second reaction chamber; 23: separating the net; 24: a first capacitor; 25: a first relay; 26: a first current transformer; 27: a second current transformer; 28: a second relay; 29: a second capacitor; 30: a second high voltage DC power supply; 31: a second control center; 32: a second oscilloscope; 33: a second resistance detector; 34: a first resistance detector; 35: a first oscilloscope; 36: a first master control center; 37: the first high-voltage direct current power supply.
Detailed Description
Referring to fig. 1 and 2, the apparatus for preparing graphene-loaded nano metal particles by pulse discharge flash according to the present invention includes two reaction chambers, namely a first reaction chamber 13 and a second reaction chamber 22, wherein the first reaction chamber 13 and the second reaction chamber 22 are chambers having the same size and shape and are disposed side by side. The invention adopts a first reaction cavity 13 and a second reaction cavity 22 which are cuboid, and the inner cavities of the two reaction cavities are also cuboid. The two reaction cavities are separated by a rectangular separation net 23, the separation net 23 is vertical to the bottoms of the two reaction cavities, and the two reaction cavities are communicated after penetrating through the separation net 23.
Two racks are fixed below the bottom of the first reaction cavity 13, the two racks are perpendicular to the bottom of the first reaction cavity 13, the two racks are fixed below the bottom of the second reaction cavity 22, the two racks are perpendicular to the bottom of the second reaction cavity 22, the four racks are positioned at four corners of the two reaction cavities, the four racks are fixedly supported on a horizontal ground and have a certain height from the horizontal ground, a collecting box 9 is conveniently placed under the bottom of the second reaction cavity 22, and the collecting box 9 is placed on the horizontal ground. The first reaction chamber 13, the separation net 23 and the second reaction chamber 22 are fixed in space.
The top and the bottom of the first reaction cavity 13 are both open openings, the opening at the top is covered with the movable cover plate 4 on the first reaction cavity, and the size and the shape of the movable cover plate 4 on the first reaction cavity are consistent with the top opening of the first reaction cavity 13. A first reaction chamber lower movable cover plate (not shown) is covered at the bottom opening, and the size and shape of the first reaction chamber lower movable cover plate are consistent with the bottom opening of the first reaction chamber 13. Similarly, the top and the bottom of the second reaction chamber 22 are also open, the top opening of the second reaction chamber 22 is covered with the upper movable cover plate 6 of the second reaction chamber, the bottom opening is covered with the lower movable cover plate (not shown in the figure) of the second reaction chamber, and the size and the shape of the lower movable cover plate of the second reaction chamber are consistent with the bottom opening of the second reaction chamber 13.
The top and the bottom of the first reaction cavity 13 and the second reaction cavity 22 are respectively connected with a corresponding movable cover plate through a polished rod lead screw nut mechanism, and the movable cover plates are driven by the polished rod lead screw nut mechanism to open or close the opening, so that four polished rod lead screw nut mechanisms with the same structure are provided, and two upper movable cover plates and two lower movable cover plates are correspondingly driven.
The first reaction chamber 13 is taken as an example as follows:
the top of the first reaction cavity 13 is provided with a first polished rod lead screw nut mechanism, and the first polished rod lead screw nut mechanism is connected between the first reaction cavity 13 and the movable cover plate 4 on the first reaction cavity and is used for driving the movable cover plate 4 on the first reaction cavity to move, so that the top opening of the first reaction cavity 13 is opened or the top opening of the first reaction cavity 13 is closed. The first polished rod lead screw nut mechanism comprises a polished rod 17, a polished rod bearing block 16, a lead screw 19, a lead screw nut bearing block 18 and a stepping motor 12 on a first reaction cavity. The direction of the lead screw 19 is consistent with the first electric telescopic rod 1 and the second electric telescopic rod 5 and is parallel to the first electric telescopic rod 1 and the second electric telescopic rod 5. The lead screw 19 is matched and sleeved with the lead screw nut bearing seat 18, and the lead screw and the nut bearing seat are connected through threads. The lead screw 19 penetrates through the upper end side wall of the first reaction cavity 13, the first copper electrode plate 14 and the second copper electrode plate 15 with a gap, the end part of the lead screw 19 is fixedly connected with the stepping motor 12 on the first reaction cavity, and the stepping motor 12 on the first reaction cavity is coaxially and fixedly connected with the lead screw 19 and can drive the lead screw 19 to rotate. A polish rod 17 is arranged opposite to the lead screw 19 at the same height, the polish rod 17 is parallel to the lead screw 19, and the polish rod 17 also penetrates through the upper end side wall of the first reaction cavity 13, the first copper electrode plate 14 and the second copper electrode plate 15 with gaps. A polish rod bearing seat 16 is sleeved on the polish rod 17, and two axial ends of the polish rod 17 are fixed on the side wall of the first reaction cavity 13. The bottom of the movable cover plate 4 on the first reaction cavity is welded with a polished rod bearing seat 16 and a lead screw nut bearing seat 18 and fixed together. When the stepping motor 12 works on the first reaction cavity, the matched polished rod bearing seat 16 and the lead screw nut bearing seat 18 drive the movable cover plate 4 on the first reaction cavity to horizontally move through the first lead screw nut mechanism.
Similarly, a second polished rod lead screw nut mechanism is arranged at the bottom of the first reaction cavity 13, a third polished rod lead screw nut mechanism is arranged at the top of the second reaction cavity 22, the third polished rod lead screw nut mechanism is a stepping motor 11 on the second reaction cavity, and the stepping motor 11 on the second reaction cavity drives the cover plate 6 on the second reaction cavity to move. The bottom of the second reaction chamber 22 is provided with a fourth polished rod lead screw nut mechanism. Four stepping motors in the four polished rod lead screw nut mechanisms are arranged outside the first reaction cavity 13 and the second reaction cavity 22 and are positioned at two sides close to the separation net 23, and the two sides of the separation net 23 are arranged at four square corners.
The first reaction cavity 13 is internally provided with a first copper electrode plate 14 and a second copper electrode plate 15 which have the same structure and are arranged face to face and are symmetrical relative to the center of the first reaction cavity 13. Inside two copper electrode boards of first reaction cavity 13 all respectively are connected by flat cuboid and slender cylinder and are formed, and flat cuboid is located inside first reaction cavity 13, and slender cylinder runs through first reaction cavity 13 lateral wall and stretches out to first reaction cavity 13 outside. The elongated cylinder is connected at the center of the flat cuboid, perpendicular to the flat cuboid, and parallel to the ground. The flat cuboids of the two copper electrode plates are vertically arranged and are perpendicular to the bottom surface of the first reaction cavity 13. A certain space is left between the first copper electrode plate 14 and the second copper electrode plate 15 in the first reaction chamber 13, and during operation, the mixed powder of metal and carbon is filled between the first copper electrode plate 14 and the second copper electrode plate 15.
Outside the first reaction cavity 13, the slender cylinder of the first copper electrode plate 14 is connected with the first electric telescopic handle 1, the central axis of the first electric telescopic handle 1 is collinear with the central axis of the slender cylinder of the first copper electrode plate 14, and the first electric telescopic handle 1 can drive the first copper electrode plate 14 to move horizontally and move towards or away from the opposite second copper electrode plate 15. The first electric telescopic rod 1 is fixed in space. Outside the first reaction cavity 13, the slender cylinder of the second copper electrode plate 15 is connected with the second electric telescopic rod 5, the central axis of the second electric telescopic rod 5 is collinear with the central axis of the slender cylinder of the second copper electrode plate 15, and the second electric telescopic rod 5 can drive the second copper electrode plate 15 to move horizontally, and is close to or far away from the opposite first copper electrode plate 14. The second electric telescopic bar 5 is fixed in space. The first electric telescopic rod 1 and the second electric telescopic rod 5 have the same structure and are symmetrically arranged relative to the center of the first reaction cavity 13.
The internal structure of the second reaction cavity 22 is completely consistent with the internal structure of the first reaction cavity 13, and the internal structure of the second reaction cavity 22 is symmetrical to the internal structure of the first reaction cavity 13 about the separation net 23. A third copper electrode plate 20 and a fourth copper electrode plate 21 are arranged in the second reaction cavity 22, and the structures of the third copper electrode plate 20 and the fourth copper electrode plate 21 and the arrangement mode in the second reaction cavity 22 are completely the same as those of the first copper electrode plate 14 and the second copper electrode plate 15. A certain space is left between the third copper electrode plate 20 and the fourth copper electrode plate 21 in the second reaction cavity 22, and during operation, carbon source powder is filled between the third copper electrode plate 20 and the fourth copper electrode plate 21, and between the third copper electrode plate 20 and the fourth copper electrode plate 21.
. Outside the second reaction cavity 22, the third electric telescopic rod 7 is coaxially connected with the third copper electrode plate 20, and drives the third copper electrode plate 20 to move towards or away from the opposite fourth copper electrode plate 21. In the same way, the fourth electric telescopic rod 10 is coaxially connected with the fourth copper electrode plate 21, and drives the fourth copper electrode plate 2 to move towards the direction of the third copper electrode plate 20 close to or far away from the opposite side 1. The third electric telescopic rod 7 and the fourth electric telescopic rod 10 are fixed in space. Symmetrically arranged with respect to the center of the second reaction chamber 22.
The first reaction chamber 13 is connected to a shielding gas supply device 2 through a gas pipeline 3, and the shielding gas supply device 2 is fixed in space outside the first reaction chamber 13. The first reaction chamber 13 is communicated with the space between the first copper electrode plate 14 and the second copper electrode plate 15 through the gas pipeline 3. The second reaction chamber 22 is provided with a shielding gas outlet 8, and the shielding gas outlet 8 is communicated with the space between the third copper electrode plate 20 and the fourth copper electrode plate 21.
The collection box 9 is fixed on the ground right below the second reaction cavity 22, the top of the collection box 9 is open, and the size of the top opening of the collection box 9 is consistent with the size and the shape of the bottom opening of the second reaction cavity 22.
Referring to fig. 3, the four copper electrode plates, i.e., the first copper electrode plate 14, the second copper electrode plate 15, the third copper electrode plate 20, and the fourth copper electrode plate 21, have the same structure. The internal parts and the structures of the second electric telescopic rod 5, the third electric telescopic rod 7, the fourth electric telescopic rod 10 and the first electric telescopic rod 1 are completely the same. Taking the first copper electrode plate 14 as an example:
the first insulating connector 107 is coaxially and fixedly connected between the elongated cylindrical body of the first copper electrode plate 14 and the first electric telescopic rod 1. The output end of the first electric telescopic rod 1 is a first electric telescopic rod body 105, the first insulation connector 107 is a cylinder, the outer diameter of the first electric telescopic rod body is the same as that of the first electric telescopic rod body 105, and the slender cylinder of the first copper electrode plate 14 is fixedly connected with the first insulation connector 107 and the first electric telescopic rod body 105 in sequence with the same axle center. A first copper ring electrode 102 is closely sleeved outside the elongated cylinder of the first copper electrode plate 14. The outer diameter of the first copper ring electrode 102 is the same as the outer diameter of the first telescopic rod 105 and the first insulating connector 107. A first telescopic electric pole sheath 106 is tightly fitted over the first copper ring electrode 102, the first telescopic electric pole body 105 and the first insulating connector 107. The central axes of the first copper ring electrode 102, the first electric telescopic rod body 105 and the first insulating connector 107 are combined into a whole in a collinear way and can move together along the horizontal direction.
A first resistance detector electrifying groove 101 and a first pulse discharging circuit electrifying groove 103 are formed in a first electric telescopic rod outer sleeve 106 outside a first copper ring electrode 102, the first resistance detector electrifying groove 101 and the first pulse discharging circuit electrifying groove 103 are both formed in the diameter direction and penetrate through the side wall of the first electric telescopic rod outer sleeve 106, and the two electrifying grooves are both in contact with the first copper ring electrode 102. The first electric telescopic rod driving motor 104 of the first electric telescopic rod 1 is located below the first electric telescopic rod body 105 at the output end and is fixed in space. When the first electric telescopic rod driving motor 104 works, it drives the first electric telescopic rod body 105 to move horizontally, so that the first insulating connector 107, the first copper ring electrode 102 and the first copper electrode plate 14 move integrally and simultaneously.
Similarly, the other three copper electrode plates, i.e., the second electrode plate 15, the third copper electrode plate 20 and the fourth copper electrode plate 21, are respectively and tightly sleeved with a copper ring electrode outside the elongated cylinder of each copper electrode plate, and are respectively and fixedly connected with the output ends of the corresponding electric telescopic rods through an insulating connector, i.e., are respectively and fixedly connected with the output ends of the second electric telescopic rod 5, the third electric telescopic rod 7 and the fourth electric telescopic rod 10 through an insulating connector.
Referring to fig. 4, a pulse discharge series circuit and a resistance detection series circuit respectively connected to the first copper electrode plate 14, the second copper electrode plate 15, the third copper electrode plate 20 and the fourth copper electrode plate 21 are disposed outside the first reaction chamber 13 and the second reaction chamber 22. The two pulse discharge series circuits are completely the same in form and control connection mode, and the two resistance detection series circuits are completely the same in form and control connection mode. The first copper electrode plate 14 and the second copper electrode plate 15 are connected to the first pulse discharge series circuit and the second resistance detection series circuit, and the third copper electrode plate 20 and the fourth copper electrode plate 21 are connected to the second pulse discharge series circuit and the resistance detection series circuit. The method comprises the following steps:
the first pulse discharge series circuit and the resistance detection series circuit comprise: the high-voltage direct-current power supply comprises a first high-voltage direct-current power supply 37, a first capacitor 24, a first relay 25, a first current transformer 26, a first resistance detector 34, a first oscilloscope 35 and a first main control center 36. The first high-voltage direct-current power supply 37, the first capacitor 24, the first current transformer 26, the second copper ring electrode, the second copper electrode plate 15, the first copper electrode plate 14, the first copper ring electrode and the first relay 25 form a first pulse discharge series circuit. A first oscilloscope 35 is connected to the first current transformer 26 and connected in parallel to the first pulse discharge series circuit integrally formed. The first resistance detector 34, the second copper ring electrode, the second copper electrode plate 15, the first copper electrode plate 14 and the first copper ring electrode 102 form a first resistance detection series circuit.
The first main control center 36 is connected to the first relay 25 for controlling the voltage and current and the discharge period when the first pulse discharge circuit is discharged. The first main control center 36 is connected to the first resistance detector 34 for detecting the resistance between the first copper electrode plate 14 and the second copper electrode plate 15. The first main control center 36 is further connected with the first electric telescopic rod 1 and the second electric telescopic rod 5 through control lines respectively, and is used for controlling the telescopic distance of the first copper electrode plate 14 and the second copper electrode plate 15. The first main control center 36 is further connected to the first reaction chamber upper step motor 12 and the first reaction chamber lower step motor via control lines, respectively, for controlling the first reaction chamber upper movable cover plate 4 and the first reaction chamber lower movable cover plate.
A second pulse discharge series circuit and a second resistance detection series circuit are connected between the third copper electrode plate 20 and the fourth copper electrode plate 21, and the second pulse discharge series circuit and the second resistance detection series circuit include: a second high voltage direct current power supply 30, a second capacitor 24, a second relay 28, a second current transformer 27, a second resistance detector 33, a second oscilloscope 32 and a second secondary control center 32. The second high-voltage dc power supply 30, the second capacitor 24, the second current transformer 27, the fourth copper ring electrode, the fourth copper electrode plate 21, the third copper electrode plate 20, the third copper ring electrode and the second relay 28 form a second pulse discharge series circuit. A second oscilloscope 32 is connected to the second current transformer 27 and connected in parallel to the second pulse discharge series circuit formed integrally. The second resistance detector 33, the fourth copper ring electrode, the fourth copper electrode plate 21, the third copper electrode plate 20, and the third copper ring electrode form a second resistance detection series circuit.
The second control center 32 is connected to the second relay 28 for controlling the voltage and current and the discharge period of the second pulse discharge circuit during discharge. The second sub-control center 32 is connected to a second resistance detector 33 for detecting the resistance between the third copper electrode plate 20 and the fourth copper electrode plate 21. The second control center 32 is also connected to the third electric telescopic rod 7 and the fourth electric telescopic rod 10 via control lines, respectively, for controlling the telescopic distance of the first copper electrode plate 14 and the second copper electrode plate 15. The second control center 32 is further connected to the second reaction chamber upper step motor 11 and the second reaction chamber lower step motor through control lines, respectively, for controlling the second reaction chamber upper moving cover plate 6 and the second reaction chamber lower moving cover plate.
In the two resistance detection series circuits, when the copper ring electrodes are connected, the connection line passes through the corresponding resistance detector energization groove, for example, when the first copper ring electrode 102 is connected, the connection line passes through the first resistance detector energization groove 101. In the pulse discharge series circuit, when the copper ring electrodes are connected, the connection line passes through the corresponding pulse discharge circuit conducting groove, for example, when the first copper ring electrode 102 is connected, the connection line passes through the first pulse discharge circuit conducting groove 103.
The second sub-control center 32 is connected to a first main control center 36, which connects two identical pulse discharge series circuits and two resistance detection series circuits, and the first main control center 36 as a main control center can control the second sub-control center 31.
Referring to fig. 1-4 in combination with fig. 5, when graphene-loaded nano metal particles are prepared by the pulse discharge flash method, polymers with high carbon content, such as waste plastics and rubber, are used as a carbon source of graphene, metal powder is used as a raw material of the nano metal particles, and an ultrahigh temperature is generated by successive instantaneous pulse discharge, so that the carbon source is cracked, carbon atoms are recombined to generate graphene, and then the metal powder is gasified. Through the expansion and condensation of the gaseous metal, the gaseous nano metal particles are condensed into solid nano metal particles to be loaded on graphene, and finally the graphene loaded nano metal particle composite material is generated, as shown in fig. 5.
The method comprises the following specific steps:
the method comprises the following steps: the recovered waste plastic, rubber or wood and other articles with high carbon content are screened and fully crushed into powder to be used as a carbon source for generating graphene.
Step two: the metal powder and the carbon powder to be loaded are fully mixed to form mixed powder of the metal and the carbon. The metal powder and the carbon powder in the invention are mixed according to the volume ratio of 5:1 and mixing. The purpose of the carbon powder is to reduce the mutual contact between the metal powders. Prevent the final pulse discharge from sintering the metal powder and better realize the gasification of the metal powder.
Step three: the first main control center 36 controls the polished rod screw nut mechanism at the top of the first reaction cavity 13 to work, and simultaneously the first main control center 36 controls the polished rod screw nut mechanism at the top of the second reaction cavity 22 to work through the second control center 31, namely, the stepping motor 12 on the first reaction cavity and the stepping motor 11 on the second reaction cavity are started simultaneously, the stepping motor 12 on the first reaction cavity drives the corresponding screw 19, the screw nut bearing seat 18 is matched with the polished rod bearing seat 16 to drive the movable cover plate 4 on the first reaction cavity to move away, so that the first reaction cavity 13 is completely opened; similarly, the upper cover plate of the second reaction chamber moves horizontally backwards, the top opening of the second reaction chamber 22 is completely opened, and then the two polished rod screw nut mechanisms stop working, i.e. the stepper motor 12 on the first reaction chamber and the stepper motor 11 on the second reaction chamber are turned off.
Step four: a mixed powder of metal and carbon is quantitatively added to a space between the first copper electrode plate 14 and the second copper electrode plate 15 in the first reaction chamber 13, and the added amount of the mixed powder is smaller in volume than the volume between the first copper electrode plate 14 and the second copper electrode plate 15. Meanwhile, carbon source powder is also quantitatively added to the space between the third copper electrode plate 20 and the fourth copper electrode plate 21 in the second reaction chamber 22, and the volume of the added carbon source powder is smaller than the volume between the third copper electrode plate 20 and the fourth copper electrode plate 21.
The mesh size of the partition net 23 is smaller than the size of the mixed powder of the metal and the carbon, and also smaller than the size of the carbon source powder, so that the mixed powder in the first reaction chamber 13 and the carbon source powder in the second reaction chamber 22 are separated from each other by the partition net 23.
Step five: and starting the polish rod screw nut mechanisms at the tops of the first reaction cavity 13 and the second reaction cavity 22 in a reverse direction, and enabling the movable cover plate 4 on the first reaction cavity to completely close the top opening of the first reaction cavity 13 and the movable cover plate 6 on the second reaction cavity to completely close the top opening of the second reaction cavity 22. After the completion, two polished rod lead screw nut mechanisms stop working.
Step six: starting the protective gas supply device 2 and keeping the protective gas supply device open in the whole process, wherein argon is selected as the gas, the flow speed of the gas is 2m/s, and the argon is discharged from the protective gas supply device 2. The protective gas supply device 2 outputs argon, the argon firstly enters the first reaction cavity 13, passes through the protective gas pipeline 3, reaches a space formed between the first copper electrode plate 14 and the second copper electrode plate 15, passes through the separation net 23, reaches a space formed between the third copper electrode plate 20 and the fourth copper electrode plate 21, and finally comes out through the protective gas outlet 8 to reach the atmosphere, and the whole first reaction cavity 13 and the whole second reaction cavity 22 are both in the protective atmosphere of the argon.
Step seven: the first main control center 36 is always in a working state, and the first main control center 36 controls and starts the first electric telescopic rod 1 and the second electric telescopic rod 5 to work simultaneously, so that the first electric telescopic rod 1 and the second electric telescopic rod 5 extend towards each other, and the first copper electrode plate 14 and the second copper electrode plate 15 are driven to move towards each other, and the purpose is to compress the mixed powder of metal and carbon between the first copper electrode plate 14 and the second copper electrode plate 15.
In order to ensure the compactness of the metal and carbon mixed powder, the resistance detection series circuit works, the first resistance detector 34 is always in a working state, and the working circuit of the resistance detection series circuit is formed by the first resistance detector 34, the first copper ring electrode 102, the first copper electrode plate 14, the metal and carbon mixed powder, the second copper electrode plate 15 and the second copper ring electrode. The first resistance detector 34 can detect the magnitude of resistance formed between the first copper electrode plate 14, the second copper electrode plate 15, and the metal and carbon mixed powder in real time. The first resistance detector 34 transmits the magnitude of the resistance value to the first main control center 36 in real time, and when the detected resistance value is 50-100 Ω, that is, the resistance value meets the requirement, which indicates that the mixed powder of metal and carbon is compressed and compacted, the first main control center 36 controls and stops the operation of the first electric telescopic rod 1 and the second electric telescopic rod 5.
Meanwhile, the second control center 31 is always in a working state, and the second control center 31 controls and starts the third electric telescopic rod 7 and the fourth electric telescopic rod 10 to work, so as to drive the third copper electrode plate 20 and the fourth copper electrode plate 21 to move towards opposite directions, so as to compress the carbon source powder.
In order to ensure the compactness of the carbon source powder, the second resistance detector 33 between the third copper electrode plate 20 and the fourth copper electrode plate 21 is always in a working state, and a resistance detection series circuit where the second resistance detector 33 is located is formed by the second resistance detector 33, the third copper ring electrode, the third copper electrode plate 20, the carbon source powder, the fourth copper electrode plate 21 and the fourth copper ring electrode. The second resistance detector 33 can detect the magnitude of the resistance formed between the third copper electrode plate 20, the fourth copper electrode plate 21 and the carbon source powder in real time, and transmit the magnitude of the resistance value to the second control center 31 in real time, when the detected resistance value is 1000-1500 Ω, that is, the resistance value meets the requirement, it indicates that the carbon source powder is compressed and compacted, and then the second control center 31 controls and stops the third electric telescopic rod 7 and the fourth electric telescopic rod 10.
Step eight: the second pulse discharge series circuit discharges: the second high voltage dc power supply 30 is started, the second high voltage dc power supply 30 charges the second capacitor 29, and the second high voltage dc power supply 30 is turned off after the charging is completed. The second relay 28 is controlled by the second control center 31, the second relay 28 controls the second capacitor 29 to discharge in a pulse mode, the released voltage is 1000-1500V, the released current is 20-30A, and the discharge period is 50-100ms. Pulse discharge is formed between the third copper electrode plate 20 and the fourth copper electrode plate 21, ultra-high temperature is generated, carbon source powder between the third copper electrode plate 20 and the fourth copper electrode plate 21 is cracked into carbon atoms, and the carbon atoms are quickly recombined to form graphene.
Meanwhile, the first current transformer 27 monitors the current of the whole line in real time, the second oscilloscope 32 monitors the voltage of the whole line, and the first current transformer 27 and the second oscilloscope 32 only play a role in real-time monitoring and only enable a worker operating the equipment to see the current and the current voltage at any time. The trend of the current is as follows: a second capacitor 29, a second relay 28, a fourth copper ring electrode, a fourth copper electrode plate 21, carbon source powder, a third copper electrode plate 20, a third copper ring electrode, a first current transformer 27 to the second capacitor 29.
Step nine: the first pulse discharge series circuit discharges: the first high voltage dc power supply 37 is started and the first high voltage dc power supply 37 charges the first capacitor 24 and the first high voltage dc power supply 37 is turned off after the charging is completed. The first main control center 36 controls the first relay 25, the first relay 25 controls the first capacitor 24 to discharge in pulse, the released voltage is 500-1000V, the released current is 20-30A, and the discharge period is 50-100ms. Pulse discharge is formed between the first copper electrode plate 14 and the second copper electrode plate 15, ultra-high temperature is generated, and metal powder between the first copper electrode plate 14 and the second copper electrode plate 15 is gasified into gaseous metal nanoparticles.
The first current transformer 26 monitors the current of the whole line in real time, the first oscilloscope 35 monitors the voltage of the whole line, and the first current transformer 26 and the first oscilloscope 35 only play a real-time monitoring role and only see the current and the current voltage at any time for workers who operate the equipment conveniently. The trend of the current is as follows: a first capacitor 24, a first relay 25, a first copper ring electrode 102, a first copper electrode plate 14, a mixed powder of metal and carbon, a second copper electrode plate 15, a second copper ring electrode, a first current transformer 26 to the first capacitor 24. In order to protect the entire first electric telescopic rod 1 by allowing the electric current to flow from the first copper ring electrode 102 to the first copper electrode plate 14 instead of to the first electric telescopic rod body 105, a first insulating connector 107 is used to connect between the elongated cylindrical body of the first copper electrode plate 14 and the first electric telescopic rod body 105.
In the eighth step and the ninth step, there is a time interval between the discharge of the second pulse discharge circuit and the discharge of the first pulse discharge circuit, the time is about 100-150ms, and the specific control time mode is that the first main control center 36 controls the second control center 31, so that the time for the second control center 31 to issue the control command to the second relay 28 is prior to the time for the first control center to issue the control command to the first relay 25, and the time interval between the two pulse discharges is ensured to be 100-150ms. Namely, graphene needs to be generated in the second reaction cavity 22, and then gaseous nano metal particles are generated in the first reaction cavity 13, and since graphene is generated first, the generated graphene can be cooled in advance, and subsequent gaseous nano metal particles are guaranteed to be better loaded on the graphene.
Step ten: in the first reaction cavity 13, the gasified nano metal particles horizontally move to the second reaction cavity 22 by thermal expansion, and rapidly diffuse into the second reaction cavity 22 through the separation net 23, and finally condense and deposit on the graphene generated in the second reaction cavity 22 to form a composite nano structure in which the nano metal particles are loaded on the graphene, that is, the graphene loaded nano metal particles. The whole flow direction of the gaseous nano-metal particles is as follows: a first reaction cavity 13, a separation net 23 and a second reaction cavity 22.
Step eleven: the first main control center 36 controls the work of the polish rod screw nut mechanism at the bottom of the second reaction cavity 22 through the second control center 31, and the stepping motor under the second reaction cavity is started to drive the moving cover plate under the second reaction cavity to move, so that the bottom opening of the second reaction cavity 22 is completely opened, and the stepping motor under the second reaction cavity stops working. And the product of the graphene loaded with the nano metal particles generated by the reaction freely falls into the collecting box 9 positioned right below the second reaction cavity 22, and after the product is collected, the polish rod screw nut mechanism at the bottom of the second reaction cavity 22 is reversely started, and the bottom opening of the second reaction cavity 22 is closed.
When residues in the first reaction cavity 13 need to be cleaned, the first main control center 36 controls the polish rod screw nut mechanism at the bottom opening of the first reaction cavity 13 to work, and opens the bottom opening of the first reaction cavity 13, so that the inside of the first reaction cavity 13 is cleaned.
Claims (10)
1. A device for preparing graphene loaded nano metal particles by pulse discharge flash is characterized in that: the reaction device is provided with a first reaction cavity (13) and a second reaction cavity (22) which are arranged side by side and are the same, and the two reaction cavities are separated by a separation net (23); a first copper electrode plate (14) and a second copper electrode plate (15) which are identical in structure and are arranged face to face are arranged in the first reaction cavity (13), mixed powder of metal and carbon is filled between the first copper electrode plate (14) and the second copper electrode plate (15), a third copper electrode plate (20) and a fourth copper electrode plate (21) which are identical in structure and are arranged face to face are arranged in the second reaction cavity (22), and carbon source powder is filled between the third copper electrode plate (20) and the fourth copper electrode plate (21); each copper electrode plate is connected with a corresponding electric telescopic rod; a first pulse discharge series circuit and a first resistance detection series circuit are connected between the first copper electrode plate (14) and the second copper electrode plate (15), and a second pulse discharge series circuit and a second resistance detection series circuit are connected between the third copper electrode plate (20) and the fourth copper electrode plate (21); the top and the bottom of the first reaction cavity (13) and the second reaction cavity (22) are both provided with openings, and the openings at the top and the bottom are respectively connected with a movable cover plate through a polished rod screw nut mechanism to drive the movable cover plate at the top or the bottom to open or close the openings.
2. The apparatus for flash preparation of graphene-supported nano-metal particles by pulse discharge according to claim 1, wherein: each copper electrode plate is formed by connecting a flat cuboid and a long and thin cylinder, the long and thin cylinder is connected to the center of the flat cuboid and perpendicular to the flat cuboid, the flat cuboid is positioned inside the corresponding reaction cavity and perpendicular to the separation net (23) and the bottom surface of the reaction cavity, the long and thin cylinder penetrates through the side wall of the reaction cavity and extends out, an insulating connector is coaxially and fixedly connected between the long and thin cylinder outside the reaction cavity and the output end of the electric telescopic rod, a copper ring electrode is tightly sleeved outside the long and thin cylinder, and an electric telescopic rod outer sleeve is tightly sleeved outside the copper ring electrode, the insulating connector and the output end of the electric telescopic rod; each copper electrode plate is connected to the corresponding pulse discharge series circuit and the resistance detection series circuit through the corresponding copper ring electrode.
3. The apparatus for flash preparation of graphene-supported nano-metal particles by pulse discharge according to claim 1, wherein: each polished rod lead screw nut mechanism comprises a polished rod, a polished rod bearing seat, a lead screw nut bearing seat and a stepping motor, wherein the lead screw is opposite to the polished rod, the lead screw and the polished rod are parallel to an electric telescopic rod, the lead screw nut bearing seat is sleeved on the lead screw, the polished rod is sleeved with the polished rod bearing seat, the lead screw and the polished rod penetrate through the upper end side wall of the corresponding reaction cavity and the copper electrode plate at intervals, the end part of the lead screw is fixedly connected with the stepping motor through the same axle center, and the movable cover plate is fixedly connected with the polished rod bearing seat and the lead screw nut bearing seat.
4. The apparatus for flash preparing graphene-supported nano metal particles by pulse discharge according to claim 3, wherein: each pulse discharge series circuit is formed by connecting a corresponding high-voltage direct-current power supply, a capacitor, a current transformer, two copper ring electrodes, two copper electrode plates and a relay; each resistance detection series circuit is formed by connecting a corresponding resistance detector, two copper ring electrodes and two copper electrode plates.
5. The apparatus for flash preparation of graphene loaded with nano-metal particles by pulse discharge according to claim 4, wherein: an oscilloscope is connected with a current transformer and is connected in parallel with a corresponding pulse discharge series circuit, a relay and a resistance detector in the first pulse discharge series circuit are both connected with a first main control center (36), and the first main control center (36) is also respectively connected with two electric telescopic rods connected with a first copper electrode plate (14) and a second copper electrode plate (15) through control lines; a relay and a resistance detector in the second pulse discharge series circuit are both connected with a second control center (32), and the second control center (32) is also respectively connected with two electric telescopic rods connected with a third copper electrode plate (20) and a fourth copper electrode plate (21) through control lines; the first main control center (36) is connected with the second sub-control center (32) to control the second sub-control center (31).
6. A method for preparing graphene-supported nano metal particles by using the apparatus of claim 1, wherein the method comprises the following steps:
step 1): crushing a carbon source into carbon source powder, and mixing the carbon powder and metal powder to be loaded into mixed powder of metal and carbon;
step 2): the top polished rod lead screw nut mechanisms of the first reaction cavity (13) and the second reaction cavity (22) work, two movable cover plates on the top are opened, mixed powder of metal and carbon is added into a space between the first copper electrode plate (14) and the second copper electrode plate (15), carbon source powder is added into a space between the third copper electrode plate (20) and the fourth copper electrode plate (21), and meshes of the separation net (23) are smaller than the size of the mixed powder of the metal and the carbon and the size of the carbon source powder, and the two movable cover plates are closed;
and step 3): the four electric telescopic rods correspondingly connected with the four copper electrode plates work simultaneously to drive the first copper electrode plate (14) and the second copper electrode plate (15) to move towards the opposite side to compress mixed powder of metal and carbon, and the third copper electrode plate (20) and the fourth copper electrode plate (21) to move towards the opposite side to compress carbon source powder;
step 4): the two resistance detection series circuits work simultaneously to detect the resistance between the first copper electrode plate (14), the second copper electrode plate (15) and the mixed powder of metal and carbon, and the resistance between the third copper electrode plate (20), the fourth copper electrode plate (21) and the carbon source powder, when the detected resistance values meet the requirements, the mixed powder of metal and carbon and the carbon source powder are compressed compactly, and the two resistance detection series circuits stop working;
step 5): discharging by a second pulse discharge circuit, and cracking carbon source powder into carbon atoms to generate graphene; then the first pulse discharge circuit discharges to gasify the metal powder into gaseous metal nano particles; and the gaseous nano metal particles are diffused into the second reaction cavity (22) through the separation net (23), condensed and deposited on the graphene to generate the graphene-loaded nano metal particles.
7. The method of claim 6, wherein: in the processes of the steps 3) to 5), argon is output from the protective gas supply device, enters the first reaction cavity (13), sequentially passes through the space between the first copper electrode plate (14) and the second copper electrode plate (15), the separation net (23), the space between the third copper electrode plate (20) and the fourth copper electrode plate (21), and finally comes out from the second reaction cavity (22).
8. The method of claim 6, wherein: the voltage of the first pulse discharge series circuit is 500-1000V, the current is 20-30A, and the discharge period is 50-100ms; the discharge voltage of the second pulse discharge series circuit is 1000-1500V, the current is 20-30A, and the discharge period is 50-100ms; the time interval of the pulse discharge of the two pulse discharge series circuits is 100-150ms.
9. The method of claim 6, wherein: a collecting box (9) is placed under the bottom of the second reaction cavity (22), after the graphene loaded nano metal particles are generated in the step 5), the polished rod screw nut mechanism with the opening in the bottom of the second reaction cavity (22) works to open the bottom movable cover plate, and the graphene loaded nano metal particles fall into the collecting box (9).
10. The method of claim 6, wherein: in the step 1), waste plastics, rubber or wood with carbon content are crushed into powder as carbon source powder.
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| KR20050000667A (en) * | 2003-06-24 | 2005-01-06 | 한국원자력연구소 | Equipment for production of metal, alloy and ceramic nano powders by simultaneous wire feeding of electrical explosion of wire and it's method |
| CN108318543A (en) * | 2018-01-30 | 2018-07-24 | 河海大学常州校区 | A kind of heavy metal ion sensor and its operating method based on grapheme material |
| CN112280540A (en) * | 2019-07-22 | 2021-01-29 | 天津大学 | Preparation method of high-thermal-conductivity graphene-metal particle composite material |
| CN113333773A (en) * | 2021-06-24 | 2021-09-03 | 中国矿业大学 | Method for preparing metal particle-loaded coal-based graphene through high-temperature thermal shock |
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| KR20050000667A (en) * | 2003-06-24 | 2005-01-06 | 한국원자력연구소 | Equipment for production of metal, alloy and ceramic nano powders by simultaneous wire feeding of electrical explosion of wire and it's method |
| CN108318543A (en) * | 2018-01-30 | 2018-07-24 | 河海大学常州校区 | A kind of heavy metal ion sensor and its operating method based on grapheme material |
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