CN107119283A - The electrochemical preparation method of mesoporous carbon nanocoils - Google Patents
The electrochemical preparation method of mesoporous carbon nanocoils Download PDFInfo
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- CN107119283A CN107119283A CN201710235768.0A CN201710235768A CN107119283A CN 107119283 A CN107119283 A CN 107119283A CN 201710235768 A CN201710235768 A CN 201710235768A CN 107119283 A CN107119283 A CN 107119283A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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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
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
Abstract
The present invention relates to a kind of preparation method of mesoporous carbon nano-material, category nano-carbon material fabricating technology field.It is characterized in melten salt electriochemistry reduction being integrated with electrochemistry auxiliary etch technology, realizes and directly prepare mesoporous carbon nano-material.Using silicon dioxide powder and carbon dust as initial feed, well mixed silicon/carbon dioxide powder mixture is pressed into porous electrode first.Electrode is assembled as anode using yttria-stabilized zirconia oxygen flow membrane tube, to analyze pure anhydrous CaCl2For molten salt electrolyte, corundum crucible is electrolytic cell.Pass through electrochemistry reduction of fused salts silicon/carbon dioxide powder synthesizing silicon carbide nano wire first.Then again using obtained silicon carbide nanometer line as anode, graphite carbon rod is negative electrode, and mesoporous carbon nano-material is directly prepared using electrochemical etching method.This method can directly be prepared mesoporous carbon nanocoils by cheap carbon dust, and cost is low, technique is simple, its easily controllable product morphology and order.It is expected to provide a brand-new mesoporous carbon nanocoils new synthetic method.
Description
Technical field
The present invention relates to a kind of electrochemical preparation method of mesoporous carbon nano-material, belong to nano-carbon material preparation technology
Technical field.
Background technology
Material is material base and the guide of social technology progress.New material has the superiority not available for traditional material
Energy.Currently, new material industry has penetrated into the every field of national economy, national defense construction and people's lives, to large quantities of high-new
The development of technical industry plays a part of supporting and leading.New carbon has that density is small, intensity big, high temperature resistant, anti-chemistry
A series of excellent characteristics such as rotten candle, highly conductive, high heat conduction, thermal expansion be small, are dual-use new materials, enjoy national governments
With the attention of industrial quarters, its development speed is very surprising, is described as the 4th class industrial materials.
In recent years, porous carbon materials are due to high-specific surface area, good electron conduction, cheap and environment
Friendly the advantages of gas storage with separating, catalyst carrier, sewage purification, especially energy storage and convert etc. field quilt
Extensive use.For the storage of energy, negative pole, lithium-sulfur cell of the porous carbon materials as lithium ion battery or sodium-ion battery
The air electrode of middle sulfur-donor and metal-air battery is reported by increasing researcher.Most of all, mesoporous
Carbon material is considered as most promising electrode material in supercapacitor applications, becomes the research weight of electrode material in recent years
Point.Particularly, the meso-porous carbon material with 1-dimention nano cable architecture has excellent physical and chemical performance, has become at present
Study hotspot.It has very big value in energy storage research, has very in terms of electric chemical super capacitor, fuel cell
Good application prospect.The method of synthesis carbon nanocoils includes arc discharge synthesis, templated deposition, laser ablation and chemical gas at present
Mutually deposit etc..But lacking effective method always, that the carbon nanocoils of synthesis are converted into the carbon material with nanostructured is for example mesoporous
Carbon nanocoils.With the development of nanometer technology, researcher needs to seek a kind of method of new controllable preparation meso-porous carbon material,
So as to prepare the new materials such as mesoporous carbon nanocoils.The present invention is to be directed to this, a brand-new electrochemistry formated of proposition
Mesoporous carbon nanocoils new material new method.
The content of the invention
The present invention be directed to prepare the problem of New Type of Mesoporous carbon material technique is present at present, propose a kind of former by cheap carbon
Expect to change the method for directly preparing New Type of Mesoporous carbon nanocoils material by melten salt electriochemistry.This method can be straight from cheap carbon dust
Connect and be prepared into porous, high-specific surface area, the mesoporous carbon nano-material of high added value.With technological process is simple, preparation efficiency
High, less demanding to original material, with low cost the features such as.
To achieve the above object, silica and carbon dust are converted into carbonization by the synthetic method by electrochemical reduction first
Silicon nanowires, is then converted into mesoporous carbon nano-material by electrochemical etching by silicon carbide nanometer line.A kind of Jie of the invention
The electrochemical preparation method of hole carbon nanocoils, it is characterised in that with procedure below and step：
A, electrochemical reduction prepares silicon carbide nanometer line：Using silicon dioxide powder and carbon dust as initial feed（The silica of selection
It is micron and nano particle material with carbon dust raw material）, according to Mol ratio 1:1, and add 1~10% percentage by weight
Polyvinyl butyral resin or atoleine as binding agent, then ball milling obtains well mixed silicon/carbon dioxide powder and mixed
Compound fine powder material；Well mixed powder is compressed to thin slice under 5~30 MPa pressure, then by thin slice foam nickel screen
Parcel, and it is connected to form electrolysis cathode with wire electrode；By the partial oxidation yttrium stable zirconium oxide base of an end closure（Y2O3-
ZrO2）Load the low-melting-point metal tin or copper of carbon saturation in solid oxygen-ion membrane (som) pipe；Then with wire electrode one end insertion oxygen permeation membrane
Exported in pipe, constitute electrolysis assembling anode；Electrolytic cell is used as using corundum crucible or stainless steel crucible；Calcium chloride base fused salt conduct
Electrolyte；Then above-mentioned silica and carbon dust negative electrode and oxygen flow membrane tube assembling anode are put into electrolytic cell and constitute electrolytic cell；
Electrolytic process temperature control is at 1000~1200 °C；Protection gas is used as by 99.999% high-purity argon gas of purity percent by volume
Body；It is the V of 3.0 V~4.0 to apply voltage between negative electrode and anode；Silica and carbon mix cathode sheets are carried out direct
Reduction synthesis silicon carbide nanometer line；
B, electrochemical etching conversion prepares mesoporous carbon nanocoils：The silicon carbide nanometer line synthesized using in above-mentioned steps a as anode, with
Graphite rod is negative electrode, continues to carry out electrochemical etching conversion in calcium chloride base molten salt system in above-mentioned steps a；With purity volume
Percentage is used as protective gas for 99.999% high-purity argon gas；Temperature control is at 900~1200 °C during electrochemical etching；
Applied voltage is the V of 2.5 V~3.5 between negative electrode and anode；The silicon carbide nanometer line synthesized in above-mentioned steps a is carried out in situ
Electrochemical etching removes silicon formation meso-hole structure, so as to obtain mesoporous carbon nanocoils；And obtain silicon in negative electrode；Gained after being electrolysed
Product is taken out, and low temperature drying after residual fused salt is removed with deionized water soaking flushing and produces mesoporous carbon nano-material.
The principle of the inventive method is：
Electrochemistry electrodeoxidation is integrated with electrochemical etching conversion first, realized directly by silicon/carbon dioxide powder → carbon
It is prepared by the short route of SiClx nano wire → mesoporous carbon nano-material.By being added in silicon dioxide powder after carbon dust mixing directly
The controllable deoxidation of oxygen permeation membrane is carried out, so that synthesizing silicon carbide nano wire first；Then by by the silicon carbide nanometer line of electrosynthesis glyoxal
Product continues as anode, and graphite carbon rod etches conversion to realize silicon carbide nanometer line as negative electrode by electrochemical in-situ
Middle silicon is removed, and forms mesoporous carbon nanocoils.This synthesis technique, i.e., just can be most under a system without other technological process
The preparation by cheap carbon dust to mesoporous carbon nano-material is realized eventually.It is expected to provide a kind of the green of mesoporous carbon nanocoils new material
Color new synthetic method.
The advantage and feature of the inventive method are as described below：
The advantage of the invention is that：It can be changed by common cheap carbon dust by melten salt electriochemistry and directly prepare New Type of Mesoporous
Carbon nanocoils material.The inventive method has with low cost, wide material sources, technique simple and continuous operation, easily controllable, green
The features such as pattern and degree of order pollution-free, that can accurately control product.
Brief description of the drawings
Fig. 1 illustrates for the flow proposed by the present invention for changing directly preparation mesoporous carbon nano-material by melten salt electriochemistry
Figure.
Fig. 2 prepares the electrolyser construction schematic diagram of mesoporous carbon nano-material to be electrochemically converted in the present invention.In figure：1、
2- power circuits are switched, 3- corundum crucibles/stainless steel crucible, 4- sandwich packaging type electrodes, 5- calcium chloride-base fused salt electricity
Xie Zhi, 6- solid oxygen-ion membrane (som) assembling anode, 7- wire electrodes, 8- graphite carbon rod electrodes.
Fig. 3 is the XRD spectra of the mesoporous carbon nanocoils obtained in the embodiment of the present invention one.
Fig. 4 is the SEM shape appearance figures of the mesoporous carbon nanocoils obtained in the embodiment of the present invention one.
Fig. 5 is the N2 adsorption desorption curve figure of the mesoporous carbon nanocoils obtained in the embodiment of the present invention one.
Fig. 6 is the graph of pore diameter distribution of the mesoporous carbon nanocoils obtained in the embodiment of the present invention one.
Fig. 7 is the XRD spectra of the mesoporous carbon nanocoils obtained in the embodiment of the present invention two.
Fig. 8 is the SEM shape appearance figures of the mesoporous carbon nanocoils obtained in the embodiment of the present invention two.
Embodiment
Embodiment 1
Weigh the micron two that ~ 2.0 g are had been added to after the polyvinylbutyral binder and ball milling of percentage by weight 2%
Silica/micrometer carbon powder mixture material fine powder.Wherein, the mol ratio of silica and carbon dust is 1:1.By fine powder material 10
Thin rounded flakes are compressed under the conditions of MPa.The thin slice of compacting is wrapped up with nickel foam and extraction is sandwiched with Fe-Cr-Al wire titanium dioxide is made
Silicon/toner mixture negative electrode.The silicon/carbon dioxide powder mixture negative electrode made modes of emplacement as shown in Figure 2 is positioned over
In molten-salt electrolysis pond.To analyze pure anhydrous CaCl2For molten salt electrolyte；Corundum crucible is reaction vessel, namely electrolytic cell；With height
Pure argon is as protective gas, in sealing resistance furnace Inner electrolysis.Temperature selection is 1000 DEG C, and voltage is 4.0 V, steady with yittrium oxide
Determine zirconium oxide（Y2O3-ZrO2）Oxygen flow membrane tube assembling electrode is anode system, the closure of switch 1, switch 2 is disconnected, by electrolysis 6
Silicon carbide nanometer line is completed after hour and prepares experiment.
Conversion electrode connection mode, the closure of switch 2, switch 1 are disconnected, the carborundum of above-mentioned preparation is received as shown in Figure 2
Rice noodles electrode is as anode, and graphite carbon rod electrode carries out electrochemical etching as negative electrode, continuation in above-mentioned hermetic electrolyte system
Conversion.Temperature selection is 900 DEG C, and voltage is 3.0 V, and the synthesis of mesoporous carbon nanocoils is completed after 12 hours by electrochemical etching
Experiment.After reaction terminates, obtained product is cleaned with deionized water, in atmosphere 100 DEG C of drying to obtain mesoporous carbon nanometers
Line product.The product X RD collection of illustrative plates prepared is as shown in figure 3, the microscopic appearance of product is as shown in figure 4, be typically to receive very much
Rice noodles shape pattern.The nitrogen adsorption desorption curve of product is as shown in figure 5, find that it has the curve of obvious mesoporous material special
Property.Fig. 6 is the graph of pore diameter distribution of the electrolysate obtained in the present embodiment, can significantly find out that the hole size of product mainly collects
In be distributed between 2-4 nm, it was demonstrated that the product hole is main exists in mesoporous form, hence it is demonstrated that synthesis to be mesoporous
Carbon nanocoils material.
Embodiment 2
Weigh the nano-silica that ~ 1.0 g are had been added to after the polyvinylbutyral binder of percentage by weight 10% and ball milling
SiClx/nano-carbon powder mixture material fine powder；Wherein, the mol ratio of silica and carbon dust is 1:1.By fine powder material in 15 MPa
Under the conditions of be compressed to thin rounded flakes.With nickel foam parcel compacting thin slice and sandwich extraction with Fe-Cr-Al wire silica/receive is made
Rice toner mixture negative electrode.The silica made/nano-carbon powder mixture negative electrode modes of emplacement as shown in Figure 2 is placed
In in molten-salt electrolysis pond.To analyze pure anhydrous CaCl2For molten salt electrolyte；Corundum crucible is reaction vessel, namely electrolytic cell；With
High-purity argon gas is as protective gas, in sealing resistance furnace Inner electrolysis reduction.Temperature selection is 1000 DEG C, and voltage is 3.8 V, with
Yttria-stabilized zirconia oxygen flow membrane tube assembling electrode is anode system, and the closure of switch 1, switch 2 are disconnected, small by electrolysis 6
When after complete silicon carbide nanometer line prepare experiment.
Then, electrode connection mode is converted as shown in Figure 2, the closure of switch 2, switch 1 is disconnected, with the carbonization of above-mentioned preparation
Silicon nanowires electrode is as anode, and graphite carbon rod electrode continues to carry out electrochemical etching turn in above-mentioned electrolytic cell as negative electrode
Change.Temperature selection is 1000 DEG C, and voltage is 3.0 V, and the compound experiment of mesoporous carbon nanocoils is completed after being electrolysed 12 hours.
Reaction terminate after, obtained product is cleaned with deionized water, then in atmosphere 100 DEG C be drying to obtain mesoporous carbon nanocoils
Material.The product X RD collection of illustrative plates of preparation is as shown in fig. 7, the microscopic appearance of product is as shown in Figure 8.It can be seen that passing through this method electricity
Chemical preparation for mesoporous carbon nano-material, with the very high degree of order and application prospect.
Claims (1)
1. a kind of electrochemical preparation method of mesoporous carbon nanocoils, it is characterised in that with procedure below and step：
A, electrochemical reduction prepares silicon carbide nanometer line：Using silicon dioxide powder and carbon dust as initial feed（The silica of selection
It is micron and nano particle material with carbon dust raw material）, according to Mol ratio 1:1, and add 1~10% percentage by weight
Polyvinyl butyral resin or atoleine as binding agent, then ball milling obtains well mixed silicon/carbon dioxide powder and mixed
Compound fine powder material, is compressed to thin slice, then by thin slice foam nickel screen by well mixed powder under 5~30 MPa pressure
Parcel, and it is connected to form electrolysis cathode with wire electrode；By the partial oxidation yttrium stable zirconium oxide base of an end closure（Y2O3-
ZrO2）Load the low-melting-point metal tin or copper of carbon saturation in solid oxygen-ion membrane (som) pipe；Then it is described with the insertion of wire electrode one end
In oxygen membrane tube, export constitutes electrolysis assembling anode；Electrolytic cell is used as using corundum crucible or stainless steel crucible；Calcium chloride base fused salt
It is used as electrolyte；Then above-mentioned silica and carbon dust negative electrode and oxygen flow membrane tube assembling anode are put into constitute in electrolytic cell and are electrolysed
Pond, electrolytic process temperature control is at 1000~1200 °C；Guarantor is used as by 99.999% high-purity argon gas of purity percent by volume
Protect gas；It is the V of 3.0 V~4.0 to apply voltage between negative electrode and anode；Silica and carbon mix cathode sheets are carried out
It is reduced directly synthesizing silicon carbide nano wire；
B, electrochemical etching conversion prepares mesoporous carbon nanocoils：The silicon carbide nanometer line synthesized using in above-mentioned steps a as anode, with
Graphite rod is negative electrode, continues to carry out electrochemical etching conversion in calcium chloride base molten salt system in above-mentioned steps a, with purity volume
Percentage is used as protective gas for 99.999% high-purity argon gas；Temperature control is at 900~1200 °C during electrochemical etching；
Applied voltage is the V of 2.5 V~3.5 between negative electrode and anode；The silicon carbide nanometer line synthesized in above-mentioned steps a is carried out in situ
Electrochemical etching removes silicon formation meso-hole structure, so as to obtain mesoporous carbon nanocoils；And obtain silicon in negative electrode；Gained after being electrolysed
Product is taken out, and low temperature drying after residual fused salt is removed with deionized water soaking flushing and produces mesoporous carbon nano-material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110451480A (en) * | 2019-07-31 | 2019-11-15 | 武汉理工大学 | Mesoporous carbon nanocoils and its preparation and application |
| CN110649238A (en) * | 2019-09-27 | 2020-01-03 | 东北大学 | Silicon-based Si-C cathode material and electrochemical synthesis method and application thereof |
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| CN110649238A (en) * | 2019-09-27 | 2020-01-03 | 东北大学 | Silicon-based Si-C cathode material and electrochemical synthesis method and application thereof |
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