CN106904593A - The method that hydro-thermal method prepares three-dimensional cohesion carbon ball template - Google Patents
The method that hydro-thermal method prepares three-dimensional cohesion carbon ball template Download PDFInfo
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- CN106904593A CN106904593A CN201710134706.0A CN201710134706A CN106904593A CN 106904593 A CN106904593 A CN 106904593A CN 201710134706 A CN201710134706 A CN 201710134706A CN 106904593 A CN106904593 A CN 106904593A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
The invention discloses a kind of method that hydro-thermal method prepares three-dimensional cohesion carbon ball template, belong to the preparing technical field of nano material.Technical scheme main points are：2g is analyzed into pure glucose to be dissolved in 40mL deionized waters, add 0.3g crystal whisker of gypsum, then the clear transparent solutions obtained after dissolving are transferred in hydrothermal reaction kettle in 190 DEG C of hydro-thermal reaction 12h, naturally cool to room temperature, precipitation is collected by centrifugation, precipitation is washed with deionized water, ethanol respectively, it is the three-dimensional cohesion carbon ball template of 200nm to obtain average grain diameter then at 80 DEG C of drying 12h.The present invention prepares three-dimensional cohesion carbon ball template and compares easy operation than other methods using hydro-thermal method, and with low cost, efficiently solves the problems, such as that simple hydro-thermal method is difficult to obtain three-dimensional coherent structure nano carbon microsphere template by adding flocculating agent.
Description
Technical field
The invention belongs to the preparing technical field of nano material, and in particular to a kind of hydro-thermal method prepares three-dimensional cohesion carbon ball mould
The method of plate.
Background technology
Template is the process that nano structural material is prepared using template i.e. nano-scale reactor.Template substantially can be with
It is divided into two classes, hard template method and soft template method.Hard template method is that precursors material is introduced into hard template duct, after roasting
Nano particle is formed in nano pore, corresponding nano material is obtained after removal hard template, ideally resulting materials can
To keep template used duct pattern, conventional hard template has Woelm Alumina, mesoporous zeolite, MCM-41, porous Si templates
Deng；Soft template rule usually using surfactant molecules aggregate into micelle, reverse micelle, vesica etc. synthesized for template,
Compared with hard template method, soft template method is easier to remove template.In recent years, template and other various method cross developments, shape
Into the new technique method of more conducively practical application.
Graphene oxide composite material due to being used as new type formwork rich in groups such as hydroxyl, epoxy radicals, carboxyls, and based on stone
Black alkene, the composite of graphene oxide are increasingly becoming study hotspot.Two-dimensional graphene material has larger specific surface area, sudden and violent
The more avtive spot of dew, Zhao in 2013 et al. go out super-thin sheet-shaped MnO as templated synthesis using Graphene2；2014
Zhao Yong et al. go out C@MnO with carbon ball as templated synthesis2Material.The three-dimensional structure porous material assembled by two-dimensional material
Electric conductivity with bigger specific surface area and Geng Gao can more effectively extend its application.Due to the table of three-dimensional structure Graphene
Surface properties are improved, and specific surface area increase and active exposed sites increase the favor for making it obtain researcher.Sui etc. makes
Use polyethyleneimine（Polyethylenimine, PEI）It is reactive group bottom, is prepared by easy sol-gal process at room temperature
To dyestuff and CO2There are the three-dimensional graphene oxide-PEI porous materials of preferable suction-operated, great specific surface area Deng gas
（476m2g-1）Its fabulous absorption property is assigned, than single graphene oxide GO（Specific surface area is 31m2g-1）Improved efficiency
A lot.Cao etc. is the compound of skeleton adulteration MOF structures using three-dimensional grapheme, three-dimensional grapheme is obtained after calcination processing and is born
The metal oxide of load, photocatalysis test result show such compound with more excellent performances.
Although the porous graphene three-dimensional framework being self-assembly of significantly improves storage volume, alleviates surface
Power, preferable performance is obtained by the nano structural material prepared by this template, but the system of three-dimensional grapheme template at present
It is standby cumbersome and relatively costly.Cheap more easy-operating hydro-thermal method hardly results in the stronger carbon ball template of cohesion, prepares honest and clean
The carbon ball template of the high-quality 3-D nano, structure of valency is significant in field of nano material preparation, explores hydro-thermal method and prepares
The stronger carbon ball template of cohesion, may advantageously facilitate preparation research and the application of nano structural material.
The content of the invention
Present invention solves the technical problem that there is provided a kind of process is simple and hydro-thermal method with low cost prepare it is three-dimensional solidifying
The method of poly- carbon ball template.
The present invention adopts the following technical scheme that hydro-thermal method prepares three-dimensional cohesion carbon ball template to solve above-mentioned technical problem
Method, it is characterised in that concretely comprise the following steps：2g is analyzed into pure glucose to be dissolved in 40mL deionized waters, 0.3g gypsum is added brilliant
Must, then the clear transparent solutions obtained after dissolving are transferred in hydrothermal reaction kettle in 190 DEG C of hydro-thermal reaction 12h, it is naturally cold
But to room temperature, precipitation is collected by centrifugation, washs precipitation with deionized water, ethanol respectively, average grain diameter is obtained then at 80 DEG C of drying 12h
It is the three-dimensional cohesion carbon ball template of 200nm.
Further preferably, the change of three-dimensional cohesion carbon ball template particle diameter is realized by changing reaction temperature.
The present invention has the advantages that compared with prior art：The present invention prepares cohesion carbon ball template using hydro-thermal method
Easy operation is compared than other methods, it is and with low cost, simple hydro-thermal method is efficiently solved by adding flocculating agent is difficult to
To the problem of three-dimensional coherent structure nano carbon microsphere template.
Brief description of the drawings
Fig. 1 is the XRD spectrum of three-dimensional cohesion carbon ball template obtained in the embodiment of the present invention 2；
Fig. 2 is the SEM figures and TEM figures of three-dimensional carbon ball template obtained in the embodiment of the present invention 1；
Fig. 3 is the SEM figures and TEM figures of three-dimensional cohesion carbon ball template obtained in the embodiment of the present invention 2；
Fig. 4 is that the three-dimensional cohesion carbon ball template obtained by embodiment 2 is obtained three-dimensional honeycomb shape nanostructured MnO2SEM figure.
Specific embodiment
With reference to specific embodiment, the invention will be further described, but does not limit in any form of the invention
Content.
Embodiment 1
2g is analyzed into pure glucose to be dissolved in 40mL deionized waters, then the clear transparent solutions obtained after dissolving is transferred to
In 190 DEG C of hydro-thermal reaction 12h in the hydrothermal reaction kettle of 50mL polytetrafluoroethylliner liners, room temperature is naturally cooled to, it is heavy to be collected by centrifugation
Form sediment, wash precipitation with deionized water, ethanol respectively, the three-dimensional carbon ball mould that average grain diameter is 500nm is obtained then at 80 DEG C of drying 12h
Plate.Fig. 2 is the SEM figures and TEM figures of three-dimensional carbon ball template obtained in the present embodiment, and wherein a schemes for SEM, and b schemes for TEM, can by figure
Know, obtained three-dimensional carbon ball template size more uniform and uniformity is preferable, but connectivity is not strong, and changes reaction temperature
It also is difficult to obtain three-dimensional coherent structure nano carbon microsphere template.
Embodiment 2
2g is analyzed into pure glucose to be dissolved in 40mL deionized waters, add 0.3g crystal whisker of gypsum, then will be obtained after dissolving
Clear transparent solutions are transferred in hydrothermal reaction kettle in 190 DEG C of hydro-thermal reaction 12h, naturally cool to room temperature, and precipitation is collected by centrifugation,
Precipitation is washed with deionized water, ethanol respectively, it is the three-dimensional cohesion carbon ball of 200nm to obtain average grain diameter then at 80 DEG C of drying 12h
Template.Fig. 1 is the XRD spectrum of three-dimensional cohesion carbon ball template obtained in the present embodiment；Fig. 3 is three-dimensional cohesion obtained in the present embodiment
The SEM figures and TEM figures of carbon ball template, wherein a scheme for SEM, and b schemes for TEM, as seen from the figure, obtained three-dimensional cohesion carbon ball template
Size is less uniform, but connectivity is stronger, and the three-dimensional cohesion carbon ball mould of other sizes can be obtained by changing reaction temperature
Plate.
Three-dimensional cohesion carbon ball template and KMnO after embodiment 2 is assembled4The SEM that product is obtained after solution reaction 10h shines
Piece as shown in figure 4, sample is made up of three-dimensional honeycomb shape network structure ordered arrangement as seen from Figure 4, with three-dimensional cohesion used
The duct consistent appearance of carbon ball template, it was demonstrated that prepared three-dimensional cohesion carbon ball template has reached requirement.
Embodiment above describes general principle of the invention, principal character and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, simply original of the invention is illustrated described in above-described embodiment and specification
Reason, under the scope for not departing from the principle of the invention, various changes and modifications of the present invention are possible, and these changes and improvements each fall within
In the scope of protection of the invention.
Claims (2)
1. the method that hydro-thermal method prepares three-dimensional cohesion carbon ball template, it is characterised in that concretely comprise the following steps：2g is analyzed into pure glucose
It is dissolved in 40mL deionized waters, adds 0.3g crystal whisker of gypsum, the clear transparent solutions obtained after dissolving is then transferred to water
In 190 DEG C of hydro-thermal reaction 12h in thermal response kettle, room temperature is naturally cooled to, precipitation is collected by centrifugation, respectively with deionized water, ethanol
Washing precipitation, it is the three-dimensional cohesion carbon ball template of 200nm to obtain average grain diameter then at 80 DEG C of drying 12h.
2. the method that hydro-thermal method according to claim 1 prepares three-dimensional cohesion carbon ball template, it is characterised in that：By changing
Reaction temperature realizes the change of three-dimensional cohesion carbon ball template particle diameter.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107482178A (en) * | 2017-07-06 | 2017-12-15 | 复旦大学 | A kind of hollow TiNb2O7The preparation method of microballoon |
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| CN103043646A (en) * | 2012-12-21 | 2013-04-17 | 浙江大学 | Method for preparing small solid carbon ball and carbon ball prepared thereby |
| CN103183330A (en) * | 2013-04-02 | 2013-07-03 | 中国矿业大学 | Controllable synthesis method for nitrogen and phosphorus co-doped graphitized carbon ball with hollow structure |
| CN103601185A (en) * | 2013-12-05 | 2014-02-26 | 天津工业大学 | Preparation method of spherical porous carbon for super capacitors |
| CN105523551A (en) * | 2016-02-02 | 2016-04-27 | 成都新柯力化工科技有限公司 | Method for preparing graphene nanoplatelets through mechanical stripping and grading |
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2017
- 2017-03-08 CN CN201710134706.0A patent/CN106904593A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043646A (en) * | 2012-12-21 | 2013-04-17 | 浙江大学 | Method for preparing small solid carbon ball and carbon ball prepared thereby |
| CN103183330A (en) * | 2013-04-02 | 2013-07-03 | 中国矿业大学 | Controllable synthesis method for nitrogen and phosphorus co-doped graphitized carbon ball with hollow structure |
| CN103601185A (en) * | 2013-12-05 | 2014-02-26 | 天津工业大学 | Preparation method of spherical porous carbon for super capacitors |
| CN105523551A (en) * | 2016-02-02 | 2016-04-27 | 成都新柯力化工科技有限公司 | Method for preparing graphene nanoplatelets through mechanical stripping and grading |
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| Title |
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| SA LI等: "Design and synthesis of hierarchically porous MnO2/carbon hybrids for high performance electrochemical capacitors", 《JOURNAL OF COLLOID AND INTERFACE SCIENCE》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107482178A (en) * | 2017-07-06 | 2017-12-15 | 复旦大学 | A kind of hollow TiNb2O7The preparation method of microballoon |
| CN107482178B (en) * | 2017-07-06 | 2020-05-12 | 复旦大学 | Hollow TiNb2O7Method for preparing microspheres |
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