CN110526237B - Device and method for preparing noble metal/graphene composite nano material - Google Patents
Device and method for preparing noble metal/graphene composite nano material Download PDFInfo
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- CN110526237B CN110526237B CN201910828407.6A CN201910828407A CN110526237B CN 110526237 B CN110526237 B CN 110526237B CN 201910828407 A CN201910828407 A CN 201910828407A CN 110526237 B CN110526237 B CN 110526237B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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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
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention discloses a device and a method for preparing a noble metal/graphene composite nano material, wherein the device comprises a reaction cavity, a cooling device, a high-voltage electrode, a grounding electrode, a temperature sensor, a pH sensor, a grounding wire, a high-voltage probe, a current coil, a high-voltage power output wire, a high-voltage power supply, a power grounding wire and a power supply controller; the preparation method comprises the following steps: cleaning the reaction cavity by deionized water; the distance between the two electrodes is regulated to be 1mm-10mm; preparing a precursor with a certain concentration; adding a certain amount of reaction liquid into the reaction cavity, and switching on a cooling device; adjusting a high-voltage power supply switch and adjusting high-voltage power supply parameters; opening an oscilloscope, and connecting a high-voltage probe and a current coil; starting a timer, and controlling the reaction time to be 5-60 min, wherein the generated noble metal/graphene composite material is dispersed in the reaction cavity. The invention has the beneficial effects that the reaction efficiency is improved, and the noble metal nano particles on the composite material matrix are distributed more uniformly under the action of arc discharge.
Description
Technical Field
The invention relates to a device and a method for preparing a noble metal/graphene composite nano material, and belongs to the field of composite material preparation.
Background
Graphene (Graphene) is a two-dimensional carbon nanomaterial with hexagonal honeycomb lattice formed by carbon atoms in sp2 hybridized orbits, has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materialization, micro-nano processing, energy sources, biomedicine, drug delivery and the like, and is considered as a material revolutionary in the future. The interlayer acting force of the graphite is weak, and the graphite is easy to peel off each other, so that a thin graphite sheet is formed. In addition, the specific surface area of the graphene is large, a large amount of metal can be loaded, and the performance of the graphene is synergistically enhanced. There is a strong interaction between electrons in graphene and between electrons and the honeycomb grid. The noble metal with nanometer scale has become one of the most active branch subjects in the nano technology field due to its outstanding catalytic performance, electrical performance, magnetic performance and optical performance. The noble metal nano particles are adopted to modify the graphene, so that the excellent performance of the noble metal nano particles can be exerted, and the defect that the active noble metal nano particles are easy to agglomerate and oxidize can be overcome. Thus, the composite material attracts attention of many researchers.
However, graphene or graphene oxide is used as a raw material for preparing the graphene-based precious metal nanoparticle composite material at the present stage, precious metal ions loaded on the graphene material are reduced into precious metal nanoparticles by using a reducing agent, residual oxygen-containing functional groups on the graphene material are removed, and finally the graphene-based precious metal nanoparticle composite material can be obtained. Therefore, the high-risk chemical reagent (the most commonly used reducing agent is the highly toxic hydrazine hydrate) is generally required to be added in the preparation method for reducing the noble metal nano particles at the present stage, so that the method is not beneficial to environmental protection. Due to the existence of the problem, the industrialization progress of the graphene-based precious metal nanoparticle composite material is restricted.
Chinese patent CN109594068A describes a method of simultaneously reducing graphite oxide and heavy metal ions by irradiation to produce a noble metal/graphene composite. The method can cause uneven phenomenon to influence the quality of the composite material due to the fact that irradiation is used for processing the material. Chinese patent CN10974615a describes a method for rapidly preparing graphene-based composite materials by performing intermittent or continuous treatment of graphene using microwaves, and performing graphene perforation, doping and compounding in one step during the reaction. Chinese patent CN109181175a describes a composite material of graphene and bi-metallic nanowires and a method for preparing the same, which is produced by a substitution reaction. The method has slower reaction rate and insufficient reaction degree. Chinese patent CN106442464a describes a preparation method for controlling gold nanostructures on the surface of graphene oxide/polymer brush composites by pyrrole gas phase polymerization and finally forming reduced graphene/gold composites. Although this method can produce noble metal nanoparticles of a specific shape, it produces a composite material with poor uniformity.
Disclosure of Invention
Aiming at the problems, the invention provides a device and a method for preparing a noble metal/graphene composite nanomaterial. And the high-voltage power supply is used for exciting the graphite electrode to generate arc discharge so as to peel off the graphene, and meanwhile, high-energy electrons and free radicals generated by plasma discharge, hydrogen peroxide generated in the solution and other substances reduce metal particles, so that nano gold and nano silver are prepared and attached to the graphene, and a supporting effect is provided for the graphene. The method has the advantages of simple structure, easy operation, short reaction time and better uniformity of the compound degree of the experimental product.
The aim of the invention can be achieved by the following technical scheme: the device for preparing the noble metal/graphene composite nano material mainly comprises a reaction cavity, a cooling device, a high-voltage electrode, a grounding electrode, a temperature sensor, a pH sensor, a grounding wire, a high-voltage probe, a current coil, a high-voltage power output wire, a high-voltage power supply, a power supply grounding wire and a power supply controller; the voltage output end of the high-voltage pulse power supply is connected with the high-voltage electrode of the reaction cavity, and the ground electrode is connected with the ground wire. The high-voltage electrode is connected with a high-voltage probe, and the grounding wire passes through the induction current coil, so that the input power in the reaction cavity can be known in time, and different parameters can be controlled by adjusting the high-voltage power control panel, so that composite nano materials with different specifications can be produced. The quartz tube is sleeved outside the electrode to avoid the reaction between the electrode and the mixed solution.
Furthermore, the high-voltage power supply is a microsecond pulse power supply, a nanosecond pulse power supply or a direct-current power supply, an arc is generated between the two electrodes through high-voltage discharge, and the alternating-current high-voltage power supply is not suitable for the discharge mode. The voltage range of the high-voltage power supply is 2kV-20kV.
Furthermore, the high-voltage power supply is connected to the oscilloscope through the high-voltage probe and is used for measuring the voltage value of the circuit.
Further, the grounding electrode is connected to the digital oscilloscope through a current sensor and used for measuring the current value of the circuit.
Furthermore, the cooling device is connected with circulating water, so that the experimental device can be cooled at high temperature, and the reaction solution is kept at normal temperature.
Furthermore, the reaction cavity is made of non-conductive quartz, glass, polytetrafluoroethylene and the like, but is not limited to the above materials, and can be cylindrical or square, and the area is designed according to the size and the spacing of the electrodes.
Further, the temperature sensor and the pH sensor are positioned at the bottom of the reaction cavity, and the positions of the temperature sensor and the pH sensor are longitudinally symmetrical.
Further, the high-voltage electrode is opposite to the electrode, the high-voltage electrode is made of graphite, the outer diameter is 3mm-1cm, and the length is 50mm-300mm;
further, the electrode is made of tungsten bars, copper, aluminum and other metal materials, the outer diameter of the electrode is 3mm-1cm, the length of the electrode is 50mm-300mm, and the electrode is a solid cylinder.
The device for preparing the noble metal/graphene composite nanomaterial provided by the invention is utilized, and the method for preparing the noble metal graphene composite nanomaterial by utilizing the underwater discharge plasma comprises the following steps:
step 1, cleaning a reaction cavity by deionized water;
step 2, adjusting the distance between the two electrodes to be 1mm-10mm;
step 3, preparing a precursor with a certain concentration, wherein when nano gold is prepared, chloroauric acid solution is used as the precursor, and when nano silver is prepared, silver chloride is used as the precursor;
step 4, adding a certain amount of reaction liquid into the reaction cavity, and connecting a cooling device;
step 5, adjusting a high-voltage power supply switch and adjusting high-voltage power supply parameters;
step 6, opening an oscilloscope, and connecting a high-voltage probe and a current coil;
and 7, starting a timer, and controlling the reaction time to be 5-60 min, wherein the generated noble metal/graphene composite material is dispersed in the reaction cavity.
The invention has the advantages of reducing the long time required by the preparation of the noble metal composite nano particles, improving the reaction efficiency and enhancing the reaction effect. Meanwhile, under the action of arc discharge, noble metal nano particles on the composite material matrix are distributed more uniformly. The invention has strong operability and is easy to realize. The problems of long time consumption, uneven reaction and the like in the conventional reaction can be effectively avoided.
Drawings
FIG. 1 is a schematic diagram of an apparatus for preparing a noble metal/graphene composite nanomaterial in accordance with the present invention, wherein the apparatus is a low-temperature plasma apparatus for preparing a noble metal/composite nanomaterial;
in the figure: the device comprises a 1-reaction cavity, a 2-cooling device, a 3-high-voltage electrode, a 4-grounding electrode, a 5-temperature sensor, a 6-pH sensor, a 7-grounding wire, an 8-high-voltage probe, a 9-current coil, a 10-oscilloscope, a 11-high-voltage power supply output wire, a 12-high-voltage power supply, a 13-power supply grounding wire, a 14-power supply controller and a 15-noble metal/graphene composite material.
Detailed Description
The invention relates to a device for preparing a noble metal/graphene composite nano material, which is shown in fig. 1 and comprises a reaction cavity 1, a cooling device 2, a high-voltage electrode 3, a grounding electrode 4, a temperature sensor 5, a pH sensor 6, a grounding wire 7, a high-voltage probe 8, a current coil 9, an oscilloscope 10, a high-voltage power output line 11, a high-voltage power supply 12, a power grounding wire 13 and a power controller 14. The steps of the specific embodiment for preparing the noble metal/graphene composite nanomaterial 15 by adopting the device are as follows:
step 1, cleaning a reaction cavity by deionized water;
step 2, adjusting the distance between the two electrodes to be 1mm-10mm;
step 3, preparing a precursor with a certain concentration, wherein when nano gold is prepared, chloroauric acid solution is used as the precursor, and when nano silver is prepared, silver chloride is used as the precursor; 1ml of 1.214mM chloroauric acid solution and 3ml of 34mM sodium citrate solution were prepared and mixed;
step 4, adding a certain amount of reaction liquid into the reaction cavity, and connecting a cooling device; adjusting the reaction device to a preset position, and connecting an experimental device;
step 5, adjusting a high-voltage power supply switch and adjusting high-voltage power supply parameters;
the graphite electrode is excited by a direct current power supply, the voltage is 5kV during breakdown, the maintenance voltage is 400V after discharge breakdown, the discharge current is 2A, and the discharge time is 30min.
Step 6, opening an oscilloscope, and connecting a high-voltage probe and a current coil;
adopting cylindrical graphite electrodes, wherein the diameter of each electrode is 2mm, adjusting the distance between the two electrodes to be 10mm, and placing the prepared solution into a reaction cavity 1; the current coil 9 and the high-voltage probe 8 are connected with the oscilloscope 10 well; the cooling device is switched on.
And 7, starting a timer, and controlling the reaction time to be 5-60 min, wherein the generated noble metal/graphene composite material is dispersed in the reaction cavity.
And (3) adopting a high-speed centrifuge, setting the rotating speed to be 1 ten thousand rpm, collecting the nano material after 10min, and carrying out ultraviolet and visible spectrum measurement, SEM, TEM and other characterization on the nano material.
Claims (8)
1. The device for preparing the noble metal/graphene composite nanomaterial is characterized in that: the device mainly comprises a reaction cavity, a cooling device, a high-voltage electrode, a grounding electrode, a temperature sensor, a pH sensor, a grounding wire, a high-voltage probe, a current coil, an oscilloscope, a high-voltage power output wire, a high-voltage power supply, a power grounding wire and a power supply controller; the voltage output end of the high-voltage pulse power supply is connected with the high-voltage electrode of the reaction cavity, and the grounding electrode is connected with the grounding wire; the high-voltage electrode is connected with a high-voltage probe, and the grounding wire passes through the induction current coil, so that the input power in the reaction cavity is known in time, and different parameters are controlled by adjusting the high-voltage power control panel to produce composite nano materials with different specifications; the quartz tube is sleeved outside the electrode to prevent the electrode from reacting with the mixed solution, the high-voltage power supply is a microsecond pulse power supply, a nanosecond pulse power supply or a direct-current power supply, an electric arc is generated between the two electrodes through high-voltage discharge, the voltage range of the high-voltage power supply is 2kV-20kV, the high-voltage electrode is in butt joint with the grounding electrode, the outer diameter of the high-voltage electrode is 3mm-1cm, and the length of the high-voltage electrode is 50mm-300mm; and the high-voltage power supply is used for exciting the graphite electrode to generate arc discharge so as to peel off the graphene, and simultaneously, high-energy electrons and free radicals generated by plasma discharge and hydrogen peroxide substances generated in the solution reduce metal ions, so that nano gold and nano silver are prepared and attached to the graphene, and a supporting effect is provided for the graphene.
2. The apparatus for preparing a noble metal/graphene composite nanomaterial according to claim 1, wherein: the high-voltage power supply is connected to the oscilloscope through the high-voltage probe and is used for measuring the voltage value of the circuit; the grounding electrode is connected to the digital oscilloscope through the current sensor and is used for measuring the current value of the circuit.
3. The apparatus for preparing a noble metal/graphene composite nanomaterial according to claim 1, wherein: the cooling device is connected with circulating water; the reaction cavity is made of non-conductive quartz, glass or polytetrafluoroethylene, and is cylindrical or square.
4. The apparatus for preparing a noble metal/graphene composite nanomaterial according to claim 1, wherein: the temperature sensor and the pH sensor are positioned at the bottom of the reaction cavity, and the positions of the temperature sensor and the pH sensor are longitudinally symmetrical.
5. The apparatus for preparing a noble metal/graphene composite nanomaterial according to claim 1, wherein: the grounding electrode is made of tungsten bars, copper and aluminum metal materials, the outer diameter of the grounding electrode is 3mm-1cm, the grounding electrode is a solid cylinder, and the length of the grounding electrode is 50mm-300mm.
6. A method for preparing a noble metal/graphene composite nanomaterial using the apparatus for preparing a noble metal/graphene composite nanomaterial of claim 1, characterized in that: the method comprises the following steps:
step 1, cleaning a reaction cavity by deionized water
Step 2, adjusting the distance between the two electrodes to be 1mm-10mm;
step 3, preparing a precursor with a certain concentration, wherein when nano gold is prepared, chloroauric acid solution is used as the precursor, and when nano silver is prepared, silver chloride is used as the precursor;
step 4, adding a certain amount of reaction liquid into the reaction cavity, and connecting a cooling device;
step 5, adjusting a high-voltage power supply switch and adjusting high-voltage power supply parameters;
step 6, opening an oscilloscope, and connecting a high-voltage probe and a current coil;
and 7, starting a timer, and controlling the reaction time to be 5-60 min, wherein the generated noble metal/graphene composite material is dispersed in the reaction cavity.
7. The method for preparing the noble metal/graphene composite nanomaterial according to claim 6, wherein: 1ml of 1.214mM chloroauric acid solution and 3ml of 34mM sodium citrate solution were prepared and mixed using chloroauric acid solution as a precursor.
8. The method for preparing the noble metal/graphene composite nanomaterial according to claim 6, wherein: exciting a graphite electrode by adopting a direct current power supply, wherein the voltage is 5kV during breakdown, the maintenance voltage is 400V after discharge breakdown, the discharge current is 2A, and the discharge time is 30min; cylindrical graphite electrodes were used, the diameter of the electrodes being 2mm.
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| CN111722723B (en) * | 2020-06-29 | 2021-07-13 | 北京化工大学 | Bidirectional bending flexible sensor, sign language recognition system and method |
| CN113333773B (en) * | 2021-06-24 | 2022-10-21 | 中国矿业大学 | Method for preparing metal particle-loaded coal-based graphene through high-temperature thermal shock |
| CN113695588B (en) * | 2021-08-30 | 2023-12-26 | 炭索未来(广东)生态环境科技有限公司 | High-activity zero-valent iron composite material and preparation method and application thereof |
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