CN104047017B - A kind of method and apparatus utilizing microplasma to prepare nano cuprous oxide - Google Patents
A kind of method and apparatus utilizing microplasma to prepare nano cuprous oxide Download PDFInfo
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- CN104047017B CN104047017B CN201410314189.1A CN201410314189A CN104047017B CN 104047017 B CN104047017 B CN 104047017B CN 201410314189 A CN201410314189 A CN 201410314189A CN 104047017 B CN104047017 B CN 104047017B
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Abstract
The invention discloses a kind of method and apparatus utilizing microplasma to prepare nano cuprous oxide, concrete steps will containing NaCl, NaOH and NaNO3Electrolyte solution pour microplasma reactor into；Open argon bottle, regulate effusion meter and control gas flow, DC high-voltage power supply is opened after steady air current, when voltage arrives about 2000V, the gas between solution and stainless steel tube is breakdown, produces bright microplasma, immediately regulating voltage makes discharge stability run, nano cuprous oxide preparation starts, discharge process reaction 5～20min, completes the preparation of nano cuprous oxide.The preparation process of nano cupric oxide can be completed according to actual requirement, simple, low cost, prepare nano oxidized copper product efficiently.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, particularly relate to a kind of method and apparatus utilizing microplasma to prepare nano cuprous oxide.
Background technology
Nano material causes the extensive concern of not industry because it has special performance and broad prospect of application.Red copper oxide (Cu2O) it is a kind of important P-type semiconductor material, can be widely applied for the numerous areas such as electrode material, solar energy conversion, sensor, catalysis and environment, specifically, being greatly the cuprous nano material of loose structure for those specific surface areas, they can as adsorbent by the organic pollution selective removal in waste water.It addition, Red copper oxide has, source is wide, production cost preparation low, nontoxic, easy and the feature such as environmentally friendly, thus causes people to study interest greatly.
At present, the method preparing different-shape and structure cuprous nano material is a lot, such as solid phase method, hydro-thermal method, electrochemical method, chemical vapour deposition (CVD), solvent-thermal process method and sonochemistry method etc., these methods have respective limitation, yield as right in solid phase method is very big, preparation technology is simple, but reaction power consumption is too high, pollutes more serious.Therefore, economical, prepare nano cuprous oxide efficiently, except improving existing technology, new technology need be developed.
Summary of the invention
For solving the problems referred to above, the present invention proposes a kind of method and apparatus utilizing microplasma to prepare nano cuprous oxide.The method and device can be applied to prepare cuprous oxide nano particle, and advantage is in that simple, efficient, energy consumption and gas consumption are low, has potential development prospect.
The present invention, for reaching object above, is realized by following technical scheme:
A kind of method utilizing microplasma to prepare nano cuprous oxide is provided, 1) will containing NaCl, NaOH and NaNO3Electrolyte solution pour microplasma reactor into；2) argon bottle is opened, regulate effusion meter and control gas flow, DC high-voltage power supply is opened after steady air current, when voltage arrives about 2000V, the gas between solution and stainless steel tube is breakdown, produces bright microplasma, immediately regulating voltage makes discharge stability run, nano cuprous oxide preparation starts, discharge process reaction 5～20min, completes the preparation of nano cuprous oxide.
The present invention prepares the principle of nano cuprous oxide: the present invention does negative electrode with microplasma, itself and anode copper sheet connect and compose microplasma electrochemical system by electrolytic medium, after gas breakdown produces microplasma, a large amount of high energy electrons that microplasma carries enter reaction medium, and following reaction occurs:
Cathode chamber is reacted:
2H2O+2e-=H2↑+2OH-
Anode region is reacted:
The redox reaction occurred in solution:
Therefore, overall reaction equation is:
2Cu+H2O=H2↑+Cu2O
There is provided a kind of device utilizing microplasma to prepare nano cuprous oxide, including microplasma reactor, the DC high-voltage power supply (1) powered to microplasma reactor and the argon bottle (9) giving microplasma reactor supply；Microplasma reactor adopts glass reactor (5), solution stirring adopts magnetic stirring apparatus (8), cathode body is capillary stainless steel tube (3), and argon injects in stainless steel electrode body until reactor from argon bottle through glass rotameter；Stainless steel electrode is vertically arranged in above reaction solution, electrode outlet side distance solution surface 2mm；Anode is copper sheet (4)；Copper sheet is connected with the earth terminal of DC high-voltage power supply by series ballast resistance (2)；After starting DC high-voltage power supply, between stainless steel electrode and liquid level, produce microplasma (6), System forming path.
The present invention can complete the preparation process of nano cupric oxide according to actual requirement, simple, low cost, prepares nano oxidized copper product efficiently.
Accompanying drawing explanation
Fig. 1 is the device schematic diagram of the inventive method.
In figure: 1 DC high-voltage power supply, 2 steady resistances, 3 stainless steel tubes, 4 copper sheets, 5 glass reactors, 6 microplasmas, 7 magnetic stirring apparatuss, 8 glass rotameters, 9 argon bottles.
Fig. 2 is that microplasma electric discharge in different electrolytic mediums prepares the XRD spectra of product: (a) pure water-ethylene glycol (volume ratio 1: 1), (b) pure water.
Fig. 3 is the FESEM figure that in different electrolytic medium, microplasma discharge prepares products therefrom: (a) pure water, (b) pure water-ethylene glycol (volume ratio 1: 1).
Detailed description of the invention
Embodiment
As shown in Figure 1, microplasma reactor adopts glass reactor, high 8.5cm, internal diameter 5.5cm.Anode is copper sheet, long 3cm, wide 1cm, thick 1mm.60mL/min argon injects in stainless steel electrode body until reactor from argon bottle through glass rotameter.Stainless steel electrode is vertically arranged in above reaction solution, electrode outlet side distance solution surface 2mm.Negative electrode is stainless steel tube, long 15cm, diameter 2mm.Stainless steel tube is connected with the earth terminal of DC high-voltage power supply by 10k Ω steady resistance of connecting.Two electrodes keep the distance of 3cm.After starting DC high-voltage power supply, between stainless steel electrode and liquid level, produce microplasma, System forming path.Solution stirring adopts digital display constant temperature blender with magnetic force.
Before reaction, the oxide-film on copper sheet surface is wiped with 400 order sand paper, then clean with dilute hydrochloric acid and remove copper sheet oxide on surface and other impurity, totally with ethanol, deionized water rinsing, dry standby finally.Preparation pure water and pure water-ethylene glycol mixing two kinds of electrolytic medium solution, wherein NaCl, NaOH and NaNO3Concentration respectively 150g/L, 1g/L and 1.3g/L, take 40mL solution and pour reactor into.Being passed into by argon in rustless steel needle tubing, its flow is controlled at 60mL/min by glass rotameter.After device connection is complete, open DC high-voltage power supply, when voltage arrives about 2000V, gas between solution and stainless steel tube is breakdown, produces bright microplasma, immediately regulates voltage and makes discharge stability run, nano cuprous oxide preparation starts, and reacts 20min.After electric discharge terminates, orange product centrifugation is filtered, and use ethanol and deionized water wash for several times according to this, be finally placed in the dry 6h of 60 DEG C of vacuum drying ovens.
The preparation of nano material is produced material impact by electrolytic medium.Therefore, pure water and pure water-ethylene glycol mixing (volume ratio is 1: 1) medium impact (experiment condition: electric current density, 14mA/cm on preparation result are investigated2；Room temperature；Without stirring).Fig. 2 shows that under same experimental conditions, the different electrolytic medium (water and water-ethylene glycol (volume ratio 1: 1)) of microplasma process obtains the XRD spectra (sweep limits 2 θ=10～80 °) of product.For pure water-ethylene glycol medium, it can be seen that five obvious diffraction maximums in Fig. 2 (a), peak position be sequentially located at 2 θ=29.60 °, 36.47 °, 42.38 °, 61.40 °, 73.56 °, its corresponding crystal face respectively (110), (111), (200), (220), (311).The diffraction spectra of this product and Cu in standard diffraction data storehouse2The spectrogram (JCPDS05-667) of O crystal matches.Additionally, figure does not have other assorted peaks occur, illustrate that product purity is significantly high.Therefore, when pure water-ethylene glycol (1: 1) is as electrolytic medium, microplasma can prepare the Cu that purity is higher2O crystal.And for pure water medium, from Fig. 2 (b) it can be seen that except five diffraction maximums mentioned, there is also other diffraction maximums, including the diffraction maximum of CuO and CuCl.Fig. 3 be different solvents as electrolytic medium time microplasma be synthetically derived the awkward silence at a meeting scanning electron microscope (SEM) photograph of product.This it appears that the product morphology that obtains of two media is completely different in figure.From Fig. 3 (a) it can be seen that pure water medium, microplasma prepares nanocrystal different, not of uniform size, for instance nano wire, nanometer sheet, nanosphere etc..By XRD analysis it can be seen that the generation that the phenomenon of this confusion is other impurity such as CuO and CuCl causes.By contrast, for pure water-ethylene glycol (volume ratio 1: 1) medium, the crystal prepared is unified spherical in shape, and particle size range is at 0.2～2 μm (Fig. 3 (b)).Therefore, electrolytic medium just can obtain the Cu of shape identical (spherical) when being pure water-ethylene glycol mixing (volume ratio 1: 1) solution2O micro/nano level granule.
Above-mentioned XRD and FESEM result illustrates that electrolytic medium is very big on the impact of product component and pattern.When pure water-ethylene glycol is as electrolytic medium, it is possible not only to prevent the generation of by-product copper oxide and Cu-lyt., can effectively control again product Cu2The pattern of O.
Claims (2)
1. one kind utilizes the method that microplasma prepares nano cuprous oxide, it is characterised in that the step of the method is as follows: will containing NaCl, NaOH and NaNO3Electrolyte solution pour microplasma reactor into；Open argon bottle, regulate effusion meter and control gas flow, DC high-voltage power supply is opened after steady air current, when voltage arrives about 2000V, the gas between solution and stainless steel tube is breakdown, produces bright microplasma, immediately regulating voltage makes discharge stability run, nano cuprous oxide preparation starts, discharge process reaction 5～20min, completes the preparation of nano cuprous oxide.
2. the device implementing to utilize microplasma to prepare nano cuprous oxide described in claim 1, it is characterised in that the DC high-voltage power supply (1) of include microplasma reactor, powering to microplasma reactor and to the argon bottle (9) of microplasma reactor supply；Microplasma reactor adopts glass reactor (5), solution stirring adopts magnetic stirring apparatus (8), cathode body is capillary stainless steel tube (3), and argon injects in stainless steel electrode body until reactor from argon bottle through glass rotameter；Stainless steel electrode is vertically arranged in above reaction solution, electrode outlet side distance solution surface 2mm；Negative electrode is copper sheet (4)；Copper sheet is connected with the earth terminal of DC high-voltage power supply by series ballast resistance (2)；After starting DC high-voltage power supply, between stainless steel electrode and liquid level, produce microplasma (6), System forming path.
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