CN110526237A - It is a kind of to prepare noble metal/graphene composite nano material device and method - Google Patents
It is a kind of to prepare noble metal/graphene composite nano material device and method Download PDFInfo
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- CN110526237A CN110526237A CN201910828407.6A CN201910828407A CN110526237A CN 110526237 A CN110526237 A CN 110526237A CN 201910828407 A CN201910828407 A CN 201910828407A CN 110526237 A CN110526237 A CN 110526237A
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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
- 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
- C01B32/184—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 present invention disclose it is a kind of prepare noble metal/graphene composite nano material device and method, which is made of reaction chamber, cooling device, high-field electrode, grounding electrode, temperature sensor, pH sensor, ground line, high-voltage probe, current coil, high voltage power supply output line, high voltage power supply, power ground line and power-supply controller of electric；Preparation step includes: to be cleaned with deionized water to reaction chamber；Regulating two interelectrode spacing is 1mm-10mm；Configure good certain density presoma；A certain amount of reaction liquid is added in reaction cavity, cooling device is connected；High-voltage electric switch is adjusted, high voltage power supply parameter is adjusted；Oscillograph is opened, high-voltage probe and current coil are connected；Timer is opened, reaction time 5min-60min is controlled, noble metal/graphene composite material of generation is dispersed in reaction cavity.Present invention has the advantages that improving reaction efficiency, under arc discharge effect, the noble metal nano particles distribution on matrices of composite material is more uniform.
Description
Technical field
Noble metal/graphene composite nano material device and method is prepared the present invention relates to a kind of, belongs to composite material
Preparation field.
Background technique
Graphene (Graphene) is a kind of two dimension for forming hexangle type in honeycomb lattice with sp2 hybridized orbit by carbon atom
Carbon nanomaterial has excellent optics, electricity, mechanical characteristic, in materialogy, micro-nano technology, the energy, biomedicine and drug
Transmitting etc. is with important application prospects, it is considered to be a kind of future revolutionary material.The interlaminar action power of graphite compared with
It is weak, it is easy to which that removing mutually forms very thin graphite flake.In addition, the large specific surface area of graphene, can a large amount of carried metals,
The performance of collaboration enhancing graphene.There is strong phase interactions between electronics and between electronics and honeycomb grid in graphene
With.And the noble metal of nanoscale has become and receives because of its catalytic performance, electric property, magnetic property and optical property outstanding
Most dynamic one of subdiscipline in rice sciemtifec and technical sphere.It, not only can be with using noble metal nano particles come grapheme modified
Play the excellent properties of noble metal nano particles, moreover it is possible to overcome active noble metals nano particle easy to reunite and it is oxidizable not
Foot.Therefore, which causes the concern of many researchers.
But prepare at this stage graphene-based noble metal nano particles composite material using graphene or graphene oxide as
The precious metal ion being supported on grapheme material is reduced into noble metal nano particles with reducing agent, then removes stone by raw material
Remaining oxygen-containing functional group on black alkene material, finally can just obtain graphene-based nano-noble metal composite material.It can be seen that
Preparation method reduction noble metal nano particles at this stage generally need to be added high-risk chemical reagent, and (most common reducing agent is play
The hydrazine hydrate of poison), it is unfavorable for environmental protection.Due to the presence of the problem, so that graphene-based noble metal nano particles composite material
Process of industrialization receives restriction.
Chinese patent CN109594068A describe a kind of method by irradiation simultaneously to graphite oxide and heavy metal from
Son is restored, and noble metal/graphene composite material is generated.This method is because will appear unevenly material processing using irradiation
The quality of phenomena impair composite material.Chinese patent CN10974615A describe it is a kind of by using microwave take it is intermittent or
Continous way handles graphene, and a step realizes graphene punching, doping and recombination process during the reaction, is quickly made
The method of graphene-based composite material.Chinese patent CN109181175A describes answering for a kind of graphene and bimetal nano line
Condensation material and preparation method thereof is reacted by displacement and generates composite material.This method reaction rate is slower, and the extent of reaction is not enough filled
Point.Chinese patent CN106442464A describes a kind of multiple in graphene oxide/polymer brush using pyrroles's gas phase polymerization process
Condensation material surface regulation gold nano structure simultaneously ultimately forms reduced graphene/metal/composite material preparation method.Although this method
It can produce the noble metal nano particles of specific shape, but its generation composite material uniformity is poor.
Summary of the invention
In view of the above problems, the present invention provides and a kind of prepares noble metal/graphene composite nano material device and method.
Graphite electrode is motivated to generate arc discharge by high voltage power supply, so that graphene is removed, meanwhile, what plasma discharge generated
The substances such as high energy electron, free radical and the hydrogen peroxide that generates in the solution restore metallic, to prepare nanometer
Gold and nano silver are attached on graphene, are provided a supporting role for graphene.This method structure is simple, easily operated and reaction
Required time is shorter, and experimental product Compound Degree uniformity is more preferable.
The purpose of the present invention can be achieved through the following technical solutions: a kind of to prepare noble metal/graphene composite Nano
The device of material mainly includes reaction chamber, cooling device, high-field electrode, grounding electrode, temperature sensor, pH sensor, ground connection
Line, high-voltage probe, current coil, high voltage power supply output line, high voltage power supply, power ground line and power-supply controller of electric are constituted；High pressure
The pulse power, voltage output end access at reaction chamber high-field electrode, ground electrode connection ground line.Height is connected at high-field electrode
Pressure probe, while ground line being made to pass through adjusting by induced current coil to understand the input power size in reaction chamber in time
High voltage power supply control panel can control different parameters, produce the composite nano materials of different size.Stone is cased on the outside of electrode
English pipe can avoid electrode and react with mixed solution.
Further, the high voltage power supply is microsecond pulse power supply, nanosecond pulse power supply, DC power supply, is pressed by height
Electricity generates electric arc between two electrodes, and ac high voltage source is not suitable for this discharge type.High-voltage power voltage range is 2kV-20kV.
Further, the high voltage power supply accesses oscillograph by high-voltage probe, the voltage value for measuring circuit.
Further, grounding electrode accesses the digital oscilloscope by current inductor, the electric current for measuring circuit
Value.
Further, cooling device accesses recirculated water, can carry out High-temperature cooling to experimental provision, be maintained at reaction solution
Normal temperature state.
Further, the reaction cavity material is nonconducting quartz, glass, polytetrafluoroethylene (PTFE) etc., but is not limited to
The above material, reaction cavity can be to be cylindrical or rectangular, and area is designed according to electrode size and spacing.
Further, the temperature sensor and pH sensor are located at the bottom of reaction chamber, and the position of the two is longitudinally asymmetric.
Further, to the heart, high-field electrode material is graphite for the high-field electrode and ground electrode, and outer diameter 3mm-1cm is real
Stem body, length 50mm-300mm；
Further, the ground electrode is the metal materials such as tungsten bar, copper, aluminium, outer diameter 3mm-1cm, solid cylinder, length
Degree is 50mm-300mm.
Using it is of the present invention it is a kind of prepare noble metal/graphene composite nano material device, utilize the water
The method that lower discharge plasma prepares noble metal graphene composite nano material, comprising the following steps:
Step 1, reaction chamber is cleaned with deionized water；
Step 2, regulating two interelectrode spacing is 1mm-10mm；
Step 3, good certain density presoma is configured, wherein when preparing nanogold, using chlorauric acid solution as forerunner
Body, when preparing nano silver, using silver chlorate as presoma；
Step 4, a certain amount of reaction liquid is added in reaction cavity, connects cooling device；
Step 5, high-voltage electric switch is adjusted, high voltage power supply parameter is adjusted；
Step 6, oscillograph is opened, high-voltage probe and current coil are connected；
Step 7, timer is opened, reaction time 5min-60min, noble metal/graphene composite material point of generation are controlled
It is dispersed in reaction cavity.
The invention has the advantages that reducing longer time needed for prepared by previous noble metal composite nanometer particle, mention
High reaction efficiency, enhances reaction effect.Meanwhile under the action of arc discharge, the noble metal on matrices of composite material is received
Rice grain distribution is more uniform.Strong operability of the present invention, it is easy to accomplish.It can effectively avoid in popular response that time-consuming, anti-
Answer the problems such as uneven.
Detailed description of the invention
Fig. 1, which is that the present invention is a kind of, prepares noble metal/graphene composite nano material device, and low temperature plasma prepares expensive
Metal/composite material schematic device；
In figure: 1- reaction chamber, 2- cooling device, 3- high-field electrode, 4- grounding electrode, 5- temperature sensor, 6-pH sensing
Device, 7- ground line, 8- high-voltage probe, 9- current coil, 10- oscillograph, 11- high voltage power supply output line, 12- high voltage power supply, 13-
Power ground line, 14- power-supply controller of electric, 15- noble metal/graphene composite material.
Specific embodiment
The present invention is a kind of to prepare noble metal/graphene composite nano material device, as shown in Figure 1, by reaction chamber 1, cold
But device 2, high-field electrode 3, grounding electrode 4, temperature sensor 5, pH sensor 6, ground line 7, high-voltage probe 8, current coil
9, oscillograph 10, high voltage power supply output line 11, high voltage power supply 12, power ground line 13 and power-supply controller of electric 14 form.Using this
Device prepares specifically applying example steps are as follows for noble metal/graphene composite nano material 15:
Step 1, reaction chamber is cleaned with deionized water；
Step 2, regulating two interelectrode spacing is 1mm-10mm；
Step 3, good certain density presoma is configured, wherein when preparing nanogold, using chlorauric acid solution as forerunner
Body, when preparing nano silver, using silver chlorate as presoma；Configure 1.214mM chlorauric acid solution 1ml and 34mM sodium citrate solution
3ml is mixed；
Step 4, a certain amount of reaction liquid is added in reaction cavity, connects cooling device；Reaction unit is adjusted to pre-
Positioning is set, and connects experimental provision；
Step 5, high-voltage electric switch is adjusted, high voltage power supply parameter is adjusted；
Graphite electrode is motivated using DC power supply, voltage is 5kV when breakdown, and maintenance voltage is 400V after discharge breakdown, is put
Electric current is 2A, discharge time 30min.
Step 6, oscillograph is opened, high-voltage probe and current coil are connected；
Using cylindric graphite electrode, electrode diameter 2mm, regulating two interelectrode spacing is 10mm, will be configured
Solution is put into reaction chamber 1；Current coil 9 and high-voltage probe 8 and oscillograph 10 are connected intact；Connect cooling device.
Step 7, timer is opened, reaction time 5min-60min, noble metal/graphene composite material point of generation are controlled
It is dispersed in reaction cavity.
Using supercentrifuge, it is 10,000 revs/min that revolving speed, which is arranged, nano material is collected after 10min, and carry out purple to it
The characterization such as outer visible spectrum measurement, SEM, TEM.
Claims (10)
1. a kind of prepare noble metal/graphene composite nano material device, it is characterised in that: mainly include reaction chamber, cooling
Device, high-field electrode, grounding electrode, temperature sensor, pH sensor, ground line, high-voltage probe, current coil, high voltage power supply
Output line, high voltage power supply, power ground line and power-supply controller of electric are constituted；High-voltage pulse power source, voltage output end access reaction
At chamber high-field electrode, ground electrode connection ground line；It is connected to high-voltage probe at high-field electrode, while ground line being made to pass through induced electricity
Streamline circle can control different ginsengs by adjusting high voltage power supply control panel to understand the input power size in reaction chamber in time
Number, produces the composite nano materials of different size；Quartz ampoule is cased on the outside of electrode can avoid electrode and mixed solution generation
Reaction.
2. a kind of noble metal/graphene composite nano material device is prepared according to claim 1, it is characterised in that:
High voltage power supply is microsecond pulse power supply, nanosecond pulse power supply or DC power supply, generates electric arc between two electrodes by electrion,
High-voltage power voltage range is 2kV-20kV.
3. a kind of noble metal/graphene composite nano material device is prepared according to claim 1, it is characterised in that:
High voltage power supply accesses oscillograph by high-voltage probe, the voltage value for measuring circuit；Grounding electrode is connect by current inductor
Enter the digital oscilloscope, the current value for measuring circuit.
4. a kind of noble metal/graphene composite nano material device is prepared according to claim 1, it is characterised in that:
Cooling device accesses recirculated water；Reaction cavity material is that nonconducting quartz, glass or polytetrafluoroethylene (PTFE), reaction cavity can be
It is cylindrical or rectangular.
5. a kind of noble metal/graphene composite nano material device is prepared according to claim 1, it is characterised in that:
Temperature sensor and pH sensor are located at the bottom of reaction chamber, and the position of the two is longitudinally asymmetric.
6. a kind of noble metal/graphene composite nano material device is prepared according to claim 1, it is characterised in that:
To the heart, high-field electrode material is graphite, outer diameter 3mm-1cm, solid cylinder, length 50mm- for high-field electrode and ground electrode
300mm。
7. a kind of noble metal/graphene composite nano material device is prepared according to claim 1, it is characterised in that:
Ground electrode is the metal materials such as tungsten bar, copper, aluminium, outer diameter 3mm-1cm, solid cylinder, length 50mm-300mm.
8. a kind of prepare noble metal/graphene composite nano material method, it is characterised in that: the following steps are included:
Step 1, reaction chamber is cleaned with deionized water；
Step 2, regulating two interelectrode spacing is 1mm-10mm；
Step 3, good certain density presoma is configured, wherein when preparing nanogold, using chlorauric acid solution as presoma, system
When standby nano silver, using silver chlorate as presoma；
Step 4, a certain amount of reaction liquid is added in reaction cavity, connects cooling device；
Step 5, high-voltage electric switch is adjusted, high voltage power supply parameter is adjusted；
Step 6, oscillograph is opened, high-voltage probe and current coil are connected；
Step 7, timer is opened, reaction time 5min-60min is controlled, noble metal/graphene composite material of generation is dispersed in
In reaction cavity.
9. a kind of noble metal/graphene composite nano material method is prepared according to claim 8, it is characterised in that:
Using chlorauric acid solution as presoma, configures 1.214mM chlorauric acid solution 1ml and 34mM sodium citrate solution 3ml and mixed
It closes.
10. a kind of noble metal/graphene composite nano material method is prepared according to claim 8, it is characterised in that:
Graphite electrode is motivated using DC power supply, voltage is 5kV when breakdown, and maintenance voltage is 400V after discharge breakdown, and discharge current is
2A, discharge time 30min；Using cylindric graphite electrode, electrode diameter 2mm.
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Cited By (3)
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| 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 |
| CN113695588A (en) * | 2021-08-30 | 2021-11-26 | 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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