CN103708449A - Preparation method of ultra-thin structure carbon plate - Google Patents
Preparation method of ultra-thin structure carbon plate Download PDFInfo
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- CN103708449A CN103708449A CN201410005075.9A CN201410005075A CN103708449A CN 103708449 A CN103708449 A CN 103708449A CN 201410005075 A CN201410005075 A CN 201410005075A CN 103708449 A CN103708449 A CN 103708449A
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Abstract
The invention provides a preparation method of an ultra-thin structure carbon plate and belongs to the technical field of a nanometer material. The preparation method comprises the following steps: carrying out thermal treatment on edible flour in protective atmosphere or vacuum environments, and cooling, thus obtaining the ultra-thin structure carbon plate. The thickness of the prepared ultra-thin structure carbon plate is less than 90nm, and the ultra-thin structure carbon plate is of a flake graphite structure. The preparation method has the advantages that the ultra-thin structure carbon plate product can be obtained by directly carrying out thermal treatment on an industrial commercialization carbon source material in protective atmosphere, raw materials are wide in source, preparation steps are few and simple, the obtained ultra-thin structure carbon plate has excellent morphology and is environmentally-friendly, and the industrial production of the ultra-thin structure carbon plate is facilitated.
Description
Technical field
What the present invention relates to is a kind of method of technical field of nano material, and specifically a kind of thickness is less than the preparation method of the superthin structure carbon plate of 90 nanometers.
Background technology
Carbonaceous material has obtained widely paying close attention to and research because of its excellent thermal property, chemical property and electric property; And wherein carbon plate is especially noticeable as a kind of low-dimensional carbonaceous material of excellence.This is that specific surface area is large, surface is regular, Young's modulus is high, chemical stability is high because ultra-thin carbon plate has, the characteristic of acid-fast alkali-proof, high temperature resistant and lightweight, has extremely widely apply in fields such as matrix material, electrode materials, ultracapacitor, gas sensor, microelectronics.Especially from people such as Novoselov in 2004, delivered and be entitled as " Electric field effect in atomically thin carbon films " (electrical effect of atom level carbon film) (Science306(2004) 666-669) article after, graphene-based material causes the very big enthusiasm of various countries scientific research personnel to the research of low-dimensional carbonaceous material especially as the representative of low-dimensional carbonaceous material.For further enriching the application of low-dimensional carbonaceous material, under the research of graphene-based material drives, the preparation of some non-graphene-based low-dimensional carbonaceous materials also causes people's concern gradually.
The preparation method of report mostly exists the problem that some cannot be avoided at present.As document (carbon49(2001) 237-241) reported a kind of method of preparing amorphous carbon plate, the method is that copper sheet is placed on to spirit lamp flame top, the carbon laydown that utilizes lamp flame incomplete combustion to occur, on substrate copper sheet surface, form certain thickness settled layer, through etching, remove substrate copper sheet and obtain final product carbon plate, although the method is simple, have that product amount is few, efficiency is lower, need etch substrate, and the problem such as volume production difficulty.And document (carbon49(2011) 5117-5123) report a kind of method of preparing carbon-base film, to utilize superlaser to irradiate the polyphenylene Cabbeen film obtaining through spin coating method is carried out to carbonization, thereby obtain a kind of carbon plate product, the product pattern that the method obtains is better, but exist, process reactant toxicity complicated, that relate to is large, cost is high, experimental implementation requires the shortcomings such as high and volume production difficulty.Can find out, although carbon plate material has caused people's concern, the problem that existing preparation method still exists some urgent needs to overcome, as: productive rate is lower, preparation process is complicated, more difficultly realizes commercial scale production etc.Therefore, need to find that a kind of preparation process is convenient, cost is controlled and easily accomplish scale production method.
Through the retrieval of prior art is found, Chinese patent literature CN103011129A, open day 2013-04-03, disclose and a kind ofly take coconut husk and prepare the method for high specific surface area porous graphitization nano carbon plate as raw material, this technology by one, adopt acidic treatment or alkaline purification method to carry out pre-treatment to coconut husk; Two, in solvent, adding the pretreated coconut husk of catalyzer, activator and step 1, is that 50～80 ℃, stirring velocity are to stir 6～8h under 100～350r/min condition in temperature, obtains title complex; Wherein, the mass ratio of coconut husk and catalyzer is 1～5:1, and the mass ratio of coconut husk and activator is 1～5:1; Three, under temperature is the condition of 50 ℃～200 ℃, the title complex that step 2 is obtained solidifies 6～8h, obtains resultant; Four, the speed with 1～15 ℃/min is warming up to 700 ℃～1100 ℃, then the resultant 10min～5h of heat treatment step three under 700 ℃～1100 ℃ conditions, obtain product, wherein heat-treating atmosphere flow is 60～1000mL/min, and heat-treating atmosphere is rare gas element; Five, use the product of pickling process treatment step four, then at 20 ℃～40 ℃, stir 2～6h, being washed with distilled water to washing lotion pH is 7.0 again, in temperature, is finally dry 6～8h under the condition of 80 ℃～120 ℃, obtains high specific surface area porous graphitization nano carbon sheet material.But this technology is carried out pre-treatment, is added catalyzer and activator raw material except needs, and preparation flow is comparatively numerous and diverse, and required time is still longer.
Summary of the invention
The present invention is directed to the described deficiency that prior art exists; a kind of preparation method of superthin structure carbon plate is proposed; directly adopt and can obtain superthin structure carbon plate product to the protective atmosphere thermal treatment of industrial goods carbon source material; raw material sources are extensive; preparation process is few and simple; resulting superthin structure carbon plate pattern is excellent, and environmental friendliness, is beneficial to suitability for industrialized production.。
The present invention is achieved by the following technical solutions:
The present invention relates to a kind of preparation method of superthin structure carbon plate, by edible flour is obtained under protective atmosphere atmosphere or vacuum environment after thermal treatment is also cooling.
Described edible flour refers to the commercially available flours product that wheat-flour is major ingredient of take, and wherein major ingredient refers to: flour quality content surpasses 50%(w/w).
Described protective atmosphere refers to: nitrogen, argon gas, hydrogen or wherein any both or three are in the mixed atmosphere of the gas mixture of any ratio or rare gas element and reducing gas; Also comprise the vacuum-treat condition that does not adopt protective atmosphere.
Described thermal treatment refers to: under protective atmosphere atmosphere or vacuum environment, in enclosed space, in the temperature range of 300-1500 ℃, thermal treatment is more than 30 minutes.
Described enclosed space is realized as carrier by usining high temperature resistant porcelain boat in tube type high-temperature furnace.
Described coolingly refer to that the temperature control carrying out is cooling, naturally cooling progressively under described protective atmosphere atmosphere, artificial accelerating cooling process.
Described temperature control progressively cooling referring at whole system temperature reaches before 150 ℃, and cooling per hour is no more than the temperature control process of cooling progressively of 100 ℃.
Described naturally cooling refers to after thermal treatment completes, and system is by the natural cooling process realizing under the heat exchange condition of carrying out with extraneous physical environment.
Described artificial acceleration is cooling to be referred to after thermal treatment completes, by people for a change the physical environment state outside system (as reduced temperature, increasing speed air flow) carry out the heat exchange of Promotion system and extraneous physical environment, thereby realize the cooling process of acceleration.
The present invention relates to the superthin structure carbon plate that aforesaid method prepares, its thickness is less than 90nm and is flake graphite structure.
The present invention relates to the application of above-mentioned superthin structure carbon plate, by this superthin structure carbon plate for the preparation of sorbing material, lithium ion battery or super capacitor electrode.
Accompanying drawing explanation
Fig. 1 is flour SEM figure in embodiment 1.
Fig. 2 is H2/Ar thermal reduction carbon plate SEM figure.
Fig. 3 is N2 thermal reduction carbon plate SEM figure.
Embodiment
Below embodiments of the invention are elaborated, the present embodiment is implemented take technical solution of the present invention under prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
To the high temperature resistant porcelain boat of common edible flour be housed; put into tube type high-temperature furnace; at H2/Ar(5%/95%) air-discharging after 30 minutes under the atmosphere of gas mixture; start heating; and be warming up to 1100 ℃ and maintain 8h with the temperature rise rate of 10 ℃ of per minutes, and start subsequently naturally cooling and maintain below atmosphere protection state to 100 ℃, stop atmosphere protection; can obtain the carbon plate product of sheet structure, its SEM figure as shown in Figure 2.
The physical chemistry attribute of the product that the present embodiment prepares is: due to the existence of reducing gas H2, the carbonaceous gas that flour is escaped with carbonic acid gas or carbon monoxide form in carbonization restructuring procedure is less, carbon plate output is higher, and product carbonizing degree is higher, and structure is more fine and close.
Due to These characteristics, this product has more using value as lithium ion battery negative material aspect, but is not limited to the application of lithium ion battery electrode material.
To the high temperature resistant porcelain boat of common edible flour be housed; put into tube type high-temperature furnace; under N2 atmosphere, air-discharging is after 30 minutes; start heating; and be warming up to 700 ℃ and maintain 5h with the temperature rise rate of 10 ℃ of per minutes, and start subsequently naturally cooling and maintain below atmosphere protection state to 100 ℃, stop atmosphere protection; can obtain the carbon plate product of sheet structure, its SEM figure is as shown in 3.
The physical chemistry attribute of the product that the present embodiment prepares is: owing to adopting rare gas element N2, the carbonaceous gas that flour is escaped with carbonic acid gas or carbon monoxide form in carbonization restructuring procedure is many when adopting reducing atmosphere to process, therefore, carbon plate output reduces to some extent, its carbon plate structure is comparatively loose, and material structure Hole increases to some extent.
Due to These characteristics, this product has more using value as electrode material for super capacitor aspect, but is not limited to the application of electrode material for super capacitor aspect.
Embodiment 3
To the high temperature resistant porcelain boat of common edible flour be housed; put into tube type high-temperature furnace; under Ar atmosphere, air-discharging is after 30 minutes; start heating; and be warming up to 500 ℃ and maintain 4h with the temperature rise rate of 10 ℃ of per minutes; start subsequently naturally cooling and maintain below atmosphere protection state to 100 ℃, stopping atmosphere protection, can obtain the carbon plate product of sheet structure.
The physical chemistry attribute of the product that the present embodiment prepares is: owing to adopting rare gas element Ar, the carbonaceous gas that flour is escaped with carbonic acid gas or carbon monoxide form in carbonization restructuring procedure is many when adopting reducing atmosphere to process, and thermal treatment temp is lower, therefore, carbon plate structure is comparatively loose, and residual functional group is more.
Due to These characteristics, this product has more using value as sorbing material aspect, but is not limited to the application of sorbing material aspect.
Claims (9)
1. a preparation method for superthin structure carbon plate, is characterized in that, by by edible flour under protective atmosphere atmosphere or vacuum environment, in enclosed space, in the temperature range of 300-1500 ℃ thermal treatment 30 minutes above and cooling after obtain.
2. method according to claim 1, is characterized in that, in described edible flour, wheat-flour mass content surpasses 50%(w/w).
3. method according to claim 1, is characterized in that, described protective atmosphere refers to: nitrogen, argon gas, hydrogen or wherein any both or three are in the mixed atmosphere of the gas mixture of any ratio or rare gas element and reducing gas.
4. method according to claim 1, is characterized in that, described enclosed space is realized as carrier by usining high temperature resistant porcelain boat in tube type high-temperature furnace.
5. method according to claim 1, is characterized in that, described coolingly refers to that the temperature control carrying out is cooling, naturally cooling progressively under described protective atmosphere atmosphere, artificial accelerating cooling process.
6. method according to claim 5, is characterized in that, described temperature control progressively cooling referring at whole system temperature reaches before 150 ℃, and cooling per hour is no more than the temperature control process of cooling progressively of 100 ℃.
7. method according to claim 5, is characterized in that, described naturally cooling refers to after thermal treatment completes, and system is by the natural cooling process realizing under the heat exchange condition of carrying out with extraneous physical environment.
8. the superthin structure carbon plate preparing according to method described in above-mentioned arbitrary claim, is characterized in that, its thickness is less than 90nm and is flake graphite structure.
9. according to an application for the superthin structure carbon plate described in above-mentioned arbitrary claim, it is characterized in that, by this superthin structure carbon plate for the preparation of sorbing material, lithium ion battery or super capacitor electrode.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114409404A (en) * | 2022-02-25 | 2022-04-29 | 温州三锋换向器有限公司 | Production process of carbon sheet for planar carbon commutator |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101289183A (en) * | 2008-06-04 | 2008-10-22 | 天津大学 | Method for preparing starch based active carbon microballoons with high specific surface area |
| CN102317205A (en) * | 2008-12-15 | 2012-01-11 | 康宁股份有限公司 | The absorbent charcoal material that is used for the high-energy-density ultracapacitor |
| CN102712479A (en) * | 2010-01-22 | 2012-10-03 | 康宁股份有限公司 | High-capacitance and low-oxygen porous carbon for edlcs |
| CN102741959A (en) * | 2010-01-22 | 2012-10-17 | 康宁股份有限公司 | Microporous activated carbon for EDLCS |
| CN103011129A (en) * | 2012-12-13 | 2013-04-03 | 黑龙江大学 | Method for preparing high-specific-surface-area porous graphitic nanocarbon plate with coconut shells serving as raw materials |
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2014
- 2014-01-06 CN CN201410005075.9A patent/CN103708449A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101289183A (en) * | 2008-06-04 | 2008-10-22 | 天津大学 | Method for preparing starch based active carbon microballoons with high specific surface area |
| CN102317205A (en) * | 2008-12-15 | 2012-01-11 | 康宁股份有限公司 | The absorbent charcoal material that is used for the high-energy-density ultracapacitor |
| CN102712479A (en) * | 2010-01-22 | 2012-10-03 | 康宁股份有限公司 | High-capacitance and low-oxygen porous carbon for edlcs |
| CN102741959A (en) * | 2010-01-22 | 2012-10-17 | 康宁股份有限公司 | Microporous activated carbon for EDLCS |
| CN103011129A (en) * | 2012-12-13 | 2013-04-03 | 黑龙江大学 | Method for preparing high-specific-surface-area porous graphitic nanocarbon plate with coconut shells serving as raw materials |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114409404A (en) * | 2022-02-25 | 2022-04-29 | 温州三锋换向器有限公司 | Production process of carbon sheet for planar carbon commutator |
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Application publication date: 20140409 |