CN103641101A - Two-dimensional structural carbon nanomaterial and preparation method thereof - Google Patents
Two-dimensional structural carbon nanomaterial and preparation method thereof Download PDFInfo
- Publication number
- CN103641101A CN103641101A CN201310703311.XA CN201310703311A CN103641101A CN 103641101 A CN103641101 A CN 103641101A CN 201310703311 A CN201310703311 A CN 201310703311A CN 103641101 A CN103641101 A CN 103641101A
- Authority
- CN
- China
- Prior art keywords
- preparation
- dimensional
- sodium borohydride
- glucose
- carbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
The invention provides a two-dimensional carbon nanomaterial and a preparation method thereof, and belongs to the technical field of nanomaterials. The preparation method comprises the following steps: adding a mixed solution of glucose and sodium borohydride to a hydrothermal kettle provided with a Teflon inner tank; preparing a mixed solution containing a carbon plate product by the hydrothermal method; washing and separating; and then drying the obtained product to obtain the two-dimensional carbon nanomaterial. According to the preparation method, the mixed solution of sodium borohydride and a low-cost carbon source is directly treated by the hydrothermal method; the two-dimensional structural carbon nanomaterial formed by self-assembling a large number of nano-particles and having the carbon content exceeding 60% can be prepared.
Description
Technical field
What the present invention relates to is a kind of method of technical field of nano material, specifically a kind of two-dirnentional structure carbon nanomaterial and preparation method thereof.
Background technology
From Novoselov in 2004 etc. at < < Science > > (science) (2004, 306, 666-669), delivered the article that is entitled as " Electric field effect in atomically thin carbon films " (electrical effect of atom level carbon film), since preparing grapheme material first, under the drive of the large quantity research of graphene-based material, multiple non-graphene-based two-dimensional material also progresses into people's the visual field, mineral-type two-dimensional material for example, polymer-based two-dimensional material etc.This is mainly due to the block materials compared to them, and in fields such as the conversion of electronics, catalysis, sensing and the energy and storages, its corresponding two-dimensional material has more excellent and unique performance and application potential widely; Especially the huge specific surface area of two-dimensional material is further modified and micro-processing provides more wide space for it.
Through existing pertinent literature retrieval is found, the method for preparing at present two-dimensional material all can adopt the preparation method of " from top to bottom " substantially.The maximum feature of this preparation method needs its bulk material to have laminate structure feature exactly, by some special technique means, lamina block material is dissociated, thereby obtains its two-dimentional secondary structure material.As Guo Shouwu seminar of Shanghai Communications University is published in < < Chemical Communications > > (2010,46, the article that is entitled as " Reduction of graphene oxide via L-ascorbic acid " (vitamins C redox graphene) 1112-1114), wherein reported under the condition of acid with strong oxidizing property lamellar graphite has been oxidized to intercalation, dissociated subsequently and obtain a large amount of individual layer two dimensional oxidation grapheme materials.In addition, the Zhang Hua seminar of Nanyang Technological University utilizes preparation method from top to bottom to prepare a series of inorganic two-dimensional material, the most representative article wherein, as be published in < < AngewandteChemie International Edition > > (2012, 51, the article that is entitled as " An Effective Method for the Fabrication of Few-Layer-Thick Inorganic Nanosheets " (a kind of effective ways of preparing few layer inorganic nano sheet) 9052-9056), reported the mode of utilizing lithium ion cell charging, lithium ion is embedded in lamina block material, ultrasonic dissociating obtains multiple few layer Two-dimensional Inorganic material subsequently.
Although adopt method from top to bottom can successfully prepare multiple two-dirnentional structure nano material, the prerequisite that lamina block material is raw material has still restricted the diversity development of two-dimensional nano material.Therefore,, for breaking away from this restriction, the various countries scientific research personnel strategy of having expected employing " from bottom to top " simultaneously, namely passes through certain reactive force with some molecules or nano particle, enriches the preparation of two-dimensional material.Such as people such as Ikeda, be published in < < AngewandteChemie International Edition > > (2013,52, the article that is entitled as " SupramolecularThiopheneNanosheets " (supramolecule thiophene nanometer sheet) 4845-4848), reported that a kind of multipolymer macromolecular material that utilizes is by the synthetic a kind of supramolecule thiophene nanometer sheet of self-assembly mode, this nanometer sheet is because its abundant functional group in surface has potential application in immobilized fluorescence molecule field.The people such as Zhao are published in < < Journal of the American Chemical Society > > (2013, 135, 1524-1530), be entitled as " Two-Dimensional Mesoporous Carbon Nanosheets and Their Derived GrapheneNanosheets:Synthesis and Efficient Lithium Ion Storage " (2 D mesopore carbon nanosheet and its Graphene derivative: article synthetic and lithium ion storage effectively), reported that a kind of triblock copolymer polymer that utilizes prepares spherical secondary species, by anodic oxidation aluminium formwork, under hydrothermal condition, prepare subsequently a kind of two-dimentional macromolecule membrane, by annealing and template etching, obtain a kind of graphene-based 2 D mesopore carbon nanometer two-dimensional material again, the application of this material in lithium ion battery negative material has extraordinary performance performance.
In the method for preparing two-dimensional material of more than reporting, the problem that all exists some to avoid.Adopt preparation method from top to bottom, be subject to the restriction of this prerequisite of lamina block material; And adopt preparation method from bottom to top, mostly need precursor material (block copolymer macromolecule) that some costs are comparatively expensive and/or by the subsidiary conditions of some templates, thereby the cost that has increased preparation drops into.Therefore, need to find a kind ofly based on preparation method from bottom to top, realize the method that raw material at lower cost is directly prepared two-dimensional nano material simultaneously.
Summary of the invention
The present invention is directed to prior art above shortcomings, propose a kind of two-dirnentional structure carbon nanomaterial and preparation method thereof, by hydrothermal method, directly process sodium borohydride and carbon source material mixed solution cheaply, prepare Two-dimensional Carbon nano material.
The present invention is achieved by the following technical solutions:
The present invention relates to a kind of preparation method of Two-dimensional Carbon nano material, by the mixing solutions of glucose and sodium borohydride being joined in the water heating kettle of being furnished with polytetrafluoroethylliner liner, by hydrothermal method, prepare the mixed solution containing carbon plate product, after cleaning separation, the product obtaining is dried, obtains Two-dimensional Carbon nano material.
In described glucose and the mixing solutions of sodium borohydride: the concentration of glucose is 100mg/mL, the concentration of sodium borohydride is 1-15mg/mL, and solvent is deionized water.This mixing solutions by by glucose and sodium borohydride according to concentration requirement and deionized water blend, through ultrasonic or concussion processing, obtain.
The Heating temperature of described hydrothermal method is 120-200 ℃, and be 2-24h heat-up time.
Described cleaning refers to: with once or secondary deionized water, ethanol, or the mixing solutions of both arbitrary proportions mixes.
Described separation includes but not limited to: standing, centrifugal or suction filtration operates to remove water and/or ethanol.
Described dry including but not limited to: the natural air drying under room temperature condition, vacuum-drying, lyophilize, utilize heating installation the temperature range drying treatment of 35-200 ℃.
Anneal is preferably carried out in described being dried after completing, and is specially:
A) vacuum condition, or
B) inert gas atmosphere, or
C) reducing gas atmosphere, or
D) mixed atmosphere of rare gas element and reducing gas,
In any one, and anneal more than 10 minutes under 100-2000 ℃ of environment.
Described rare gas element includes but not limited to: nitrogen, argon gas;
Described reducing gas includes but not limited to: hydrogen.
The present invention relates to the Two-dimensional Carbon nano material that aforesaid method prepares, the breadth wise dimension of this two-dirnentional structure is below 100 microns, and longitudinal thickness, below 60 nanometers, adopts self-assembly mode to form by nano particle, and carbon content surpasses 60% (w/w).
Technique effect
Compared with prior art, the invention has the advantages that what in preparation process, use is wide material sources, low price and reproducible glucose are carbon source material, by adding as catalysis and the sodium borohydride that plays structure-directing effect as additive, utilize preparation condition gentleness and easy industrialized hydrothermal synthesis method to prepare Two-dimensional Carbon nano material, and can prepare different concns, different heat treatment degree product according to different demands, for the diversity of material, apply precondition is provided.
Accompanying drawing explanation
Fig. 1 is prepared Two-dimensional Carbon nano material field emission scanning electron microscope (FESEM) schematic diagram.
Fig. 2 is prepared Two-dimensional Carbon nano material transmission electron microscope (TEM) schematic diagram.
Fig. 3 is prepared Two-dimensional Carbon nano material atom mechanics microscope (AFM) schematic diagram.
Fig. 4 is field emission scanning electron microscope (FESEM) schematic diagram after prepared Two-dimensional Carbon nano material thermal treatment.
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
The preparation of the present embodiment Two-dimensional Carbon nano material comprises the following steps: at room temperature, take respectively 4 grams of glucose and 0.3 gram of sodium borohydride solids powder, join in 50mL beaker, with deionized water, being mixed with 40mL is solution, through simple ultrasonic or concussion, solution becomes after clear liquid, transfers to 50mL and is furnished with in polytetrafluoroethylliner liner reactor, with iron shell, inner bag is sealed.The reactor that reaction solution is housed is put into the baking oven of Resistant heating, be warming up to 180 ℃, maintain 8 hours under this temperature condition, stop heating, question response still naturally cools to after room temperature, takes out reaction solution, obtains a kind of dark-brown mixed solution; Adopt subsequently the whizzer of 8000 rpms to carry out mixed solution centrifugal, and remove supernatant liquid, retain bottom precipitation; With deionized water, repeatedly wash again centrifugal, till supernatant liquid water white transparency.Finally products therefrom is placed in to vacuum drying oven dry 4 hours, obtains final desciccate and be a kind of Two-dimensional Carbon nano material.
By above-mentioned dry products therefrom; be placed in porcelain boat; put into silica tube, under nitrogen protection, carry out the air displacement of 30 minutes; temperature rise rate with per minute 5 degree is warming up to 900 ℃ subsequently; keep 2 hours, stop heating, under nitrogen atmosphere; naturally cool to room temperature, can obtain the Two-dimensional Carbon nano material after high temperature cabonization.
Embodiment 2
The preparation of the present embodiment Two-dimensional Carbon nano material comprises the following steps: at room temperature, take respectively 4 grams of glucose and 0.4 gram of sodium borohydride solids powder, join in 50mL beaker, with deionized water, being mixed with 40mL is solution, through simple ultrasonic or concussion, solution becomes after clear liquid, transfers to 50mL and is furnished with in polytetrafluoroethylliner liner reactor, with iron shell, inner bag is sealed.The reactor that reaction solution is housed is put into the baking oven of Resistant heating, be warming up to 200 ℃, maintain 20 hours under this temperature condition, stop heating, question response still naturally cools to after room temperature, takes out reaction solution, obtains a kind of dark-brown mixed solution; Adopt subsequently the whizzer of 8000 rpms to carry out mixed solution centrifugal, and remove supernatant liquid, retain bottom precipitation; With deionized water, repeatedly wash again centrifugal, till supernatant liquid water white transparency.Finally products therefrom is placed in to 60 ℃ of loft drier dry 6 hours, obtains final desciccate and be a kind of Two-dimensional Carbon nano material.
By above-mentioned dry products therefrom; be placed in porcelain boat; put into silica tube, under the protection of hydrogen (5%) argon gas (95%) gas mixture, carry out the air displacement of 30 minutes; temperature rise rate with per minute 5 degree is warming up to 600 ℃ subsequently; keep 5 hours, stop heating, under gas mixture atmosphere; naturally cool to room temperature, can obtain the Two-dimensional Carbon nano material after high temperature cabonization.
Embodiment 3
The preparation of the present embodiment Two-dimensional Carbon nano material comprises the following steps: at room temperature, take respectively 4 grams of glucose and 0.2 gram of sodium borohydride solids powder, join in 50mL beaker, with deionized water, being mixed with 40mL is solution, through simple ultrasonic or concussion, solution becomes after clear liquid, transfers to 50mL and is furnished with in polytetrafluoroethylliner liner reactor, with iron shell, inner bag is sealed.The reactor that reaction solution is housed is put into the baking oven of Resistant heating, be warming up to 150 ℃, maintain 24 hours under this temperature condition, stop heating, question response still naturally cools to after room temperature, takes out reaction solution, obtains a kind of dark-brown mixed solution; Adopt subsequently the whizzer of 8000 rpms to carry out mixed solution centrifugal, and remove supernatant liquid, retain bottom precipitation; With deionized water, repeatedly wash again centrifugal, till supernatant liquid water white transparency.Finally products therefrom is placed in to air natural air drying more than 8 hours, obtains final desciccate and be a kind of Two-dimensional Carbon nano material.
By above-mentioned dry products therefrom, be placed in porcelain boat, put into silica tube, after sealing, under the effect of vacuum pump machine, by sealed silica envelope vacuum pumping atmosphere, the temperature rise rate with per minute 5 degree is warming up to 700 ℃ subsequently, keeps 5 hours, stop heating, under vacuum, naturally cool to room temperature, can obtain the Two-dimensional Carbon nano material after high temperature cabonization.
Claims (7)
1. the preparation method of a Two-dimensional Carbon nano material, it is characterized in that, by the mixing solutions of glucose and sodium borohydride being joined in the water heating kettle of being furnished with polytetrafluoroethylliner liner, by hydrothermal method, prepare the mixed solution containing carbon plate product, after cleaning separation, the product obtaining is dried, obtains Two-dimensional Carbon nano material.
2. method according to claim 1, is characterized in that, in described glucose and the mixing solutions of sodium borohydride: the concentration of glucose is 100mg/mL, the concentration of sodium borohydride is 1-15mg/mL, and solvent is deionized water.
3. method according to claim 1, is characterized in that, the Heating temperature of described hydrothermal method is 120-200 ℃, and be 2-24h heat-up time.
4. method according to claim 1, is characterized in that, described cleaning refers to: with once or secondary deionized water, ethanol, or the mixing solutions of both arbitrary proportions mixes.
5. method according to claim 1, is characterized in that, described dry comprising: the natural air drying under room temperature condition, vacuum-drying, lyophilize, utilize heating installation the temperature range drying treatment of 35-200 ℃.
6. method according to claim 1, is characterized in that, after described dry completing, carries out anneal, is specially:
A) vacuum condition, or
B) inert gas atmosphere, or
C) reducing gas atmosphere, or
D) mixed atmosphere of rare gas element and reducing gas,
In any one, and anneal more than 10 minutes under 100-2000 ℃ of environment.
7. a two-dirnentional structure carbon nanomaterial, it is characterized in that, according to method described in above-mentioned arbitrary claim, prepare, the breadth wise dimension of this two-dirnentional structure is below 100 microns, longitudinal thickness is below 60 nanometers, by nano particle, adopt self-assembly mode to form, carbon content surpasses 60% (w/w).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310703311.XA CN103641101A (en) | 2013-12-19 | 2013-12-19 | Two-dimensional structural carbon nanomaterial and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310703311.XA CN103641101A (en) | 2013-12-19 | 2013-12-19 | Two-dimensional structural carbon nanomaterial and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103641101A true CN103641101A (en) | 2014-03-19 |
Family
ID=50246438
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310703311.XA Pending CN103641101A (en) | 2013-12-19 | 2013-12-19 | Two-dimensional structural carbon nanomaterial and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103641101A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104310376A (en) * | 2014-10-10 | 2015-01-28 | 江苏省特种设备安全监督检验研究院无锡分院 | Postprocessing crosslinking method of hydrothermally carbonized spherical particles of biomass carbon source material |
| CN104944405A (en) * | 2014-03-27 | 2015-09-30 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of carbon spheres |
| CN106268739A (en) * | 2016-08-31 | 2017-01-04 | 南昌大学 | A kind of preparation method of C nano material |
| CN109095451A (en) * | 2018-07-23 | 2018-12-28 | 昆明理工大学 | A kind of expired useless medicine vitamin B1The recoverying and utilizing method of injection |
| CN110526228A (en) * | 2019-09-12 | 2019-12-03 | 北京工业大学 | The preparation method of one type petal-shaped carbon nanosheet |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1935638A (en) * | 2005-09-23 | 2007-03-28 | 中国科学技术大学 | Method for preparing carbon nano fiber |
| CN102154694A (en) * | 2011-03-18 | 2011-08-17 | 昆明物理研究所 | Preparation method of hydrogen and oxygen co-doped graphene |
| CN103232035A (en) * | 2013-03-26 | 2013-08-07 | 赵建树 | Nanometer silver-loaded active carbon and preparation method thereof |
-
2013
- 2013-12-19 CN CN201310703311.XA patent/CN103641101A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1935638A (en) * | 2005-09-23 | 2007-03-28 | 中国科学技术大学 | Method for preparing carbon nano fiber |
| CN102154694A (en) * | 2011-03-18 | 2011-08-17 | 昆明物理研究所 | Preparation method of hydrogen and oxygen co-doped graphene |
| CN103232035A (en) * | 2013-03-26 | 2013-08-07 | 赵建树 | Nanometer silver-loaded active carbon and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104944405A (en) * | 2014-03-27 | 2015-09-30 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of carbon spheres |
| CN104310376A (en) * | 2014-10-10 | 2015-01-28 | 江苏省特种设备安全监督检验研究院无锡分院 | Postprocessing crosslinking method of hydrothermally carbonized spherical particles of biomass carbon source material |
| CN106268739A (en) * | 2016-08-31 | 2017-01-04 | 南昌大学 | A kind of preparation method of C nano material |
| CN109095451A (en) * | 2018-07-23 | 2018-12-28 | 昆明理工大学 | A kind of expired useless medicine vitamin B1The recoverying and utilizing method of injection |
| CN110526228A (en) * | 2019-09-12 | 2019-12-03 | 北京工业大学 | The preparation method of one type petal-shaped carbon nanosheet |
| CN110526228B (en) * | 2019-09-12 | 2021-03-30 | 北京工业大学 | Preparation method of petal-like carbon nanosheets |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104916826B (en) | A kind of graphene coated silicium cathode material and preparation method thereof | |
| Jiang et al. | Hierarchically porous N-doped carbon derived from ZIF-8 nanocomposites for electrochemical applications | |
| Wang et al. | Preparation and application of iron oxide/graphene based composites for electrochemical energy storage and energy conversion devices: Current status and perspective | |
| Zhu et al. | A carbon quantum dot decorated RuO 2 network: outstanding supercapacitances under ultrafast charge and discharge | |
| Muraliganth et al. | Facile synthesis of carbon-decorated single-crystalline Fe3O4 nanowires and their application as high performance anode in lithium ion batteries | |
| CN107871617B (en) | Graphene-metal organic frame composite material and preparation method and application | |
| Zhang et al. | ZnO nanowire/reduced graphene oxide nanocomposites for significantly enhanced photocatalytic degradation of Rhodamine 6G | |
| Abulizi et al. | One-step simple sonochemical fabrication and photocatalytic properties of Cu2O–rGO composites | |
| CN109385254B (en) | Graphene elastic polymer phase-change composite material and preparation method thereof | |
| CN106882796B (en) | Preparation method of three-dimensional graphene structure/high-quality graphene | |
| Liu et al. | Multifunctional nitrogen-doped graphene nanoribbon aerogels for superior lithium storage and cell culture | |
| CN106115675B (en) | A kind of method for preparing mesoporous graphene | |
| CN102698774B (en) | Hydrothermal preparation method for single-layer MoS2 and graphene composite nano material | |
| CN101817520B (en) | Method for manufacturing carbon microspheres by using waste macromolecules | |
| Wang et al. | Hydrothermal synthesis and electrochemical performance of NiO microspheres with different nanoscale building blocks | |
| WO2014032399A1 (en) | Method for low-temperature preparation of graphene and of graphene-based composite material | |
| CN103641101A (en) | Two-dimensional structural carbon nanomaterial and preparation method thereof | |
| CN104692368B (en) | A kind of Graphene prepared as raw material with cellulose and preparation method thereof | |
| CN104098089A (en) | Preparation method for doped graphene foams | |
| CN103613093B (en) | A kind of hydrogen reducing prepares the method for Graphene | |
| CN104174422A (en) | High nitrogen doped graphene and fullerene-like molybdenum selenide hollow-ball nanocomposite and preparation method thereof | |
| CN103723705A (en) | Graphene/nano-aluminum compound and preparation method thereof | |
| Lin et al. | Superior performance asymmetric supercapacitors based on flake-like Co/Al hydrotalcite and graphene | |
| CN107240508A (en) | A kind of preparation method of graphene/ferrite nano combination electrode material | |
| CN108054020A (en) | A kind of preparation method and application of nitrogen-doped carbon particle/graphitized carbon nitrogen composite material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140319 |