CN103908932B - Nano-graphite colloidal sol and preparation method thereof and nano-graphite and preparation method thereof - Google Patents
Nano-graphite colloidal sol and preparation method thereof and nano-graphite and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of nano-graphite colloidal sol and preparation method thereof, wherein, the method includes: in confined conditions, under the electrolytic condition that graphite electrode electrolysis is nano-graphite, in the electrolyte containing volatile component and water soluble surfactant active, it is electrolysed the graphite electrode as anode, obtains nano-graphite colloidal sol, wherein, described volatile component is volatile water-soluble substances and/or the material that can produce volatile water-soluble substances in a heated condition.The invention provides a kind of nano-graphite and preparation method thereof.The nano-graphite collosol stability prepared according to the method for the present invention is good, and the method preparing nano-graphite of the present invention, and step is simple, easily realizes, and without introducing impurity element.
Description
Technical field
The present invention relates to a kind of method preparing nano-graphite colloidal sol, and the preparation nanometer according to the present invention
The nano-graphite colloidal sol that the method for graphite sol prepares, and a kind of method preparing nano-graphite,
And the nano-graphite prepared according to the method preparing nano-graphite of the present invention.
Background technology
The purposes of nano-graphite widely, as may be used for new type chemical fertilizer, battery electrode material, electricity send out
Hot material, magnetic pipe recording material etc..But, when graphite is nanoscale, its specific surface energy is very big,
Having reunites reduces the tendency of specific surface energy, the most easily reunites, and is difficult to disperse, so that tool
There is the preparation of the nano-graphite of polymolecularity and separate the most difficult.
At present, the nano-graphite with polymolecularity mainly uses two kinds of basic skills to prepare: wherein, and one
The method of kind is by forming electric double layer on the surface of nano-particle, making like charges phase between nano-particle
Scold；A kind of method disclosing preparing nano graphite carbon sol with dual graphite electrodes such as CN1378975A, its
Nano-graphite surface is made to form double electrical layers by adding the water soluble compound such as sodium carbonate, sodium chloride,
Thus prepare stable nano-graphite colloidal sol.Although using the method to prepare nano graphite carbon sol can prepare
Stable nano-graphite colloidal sol, but more elementary metal impurities can be introduced, affect the serviceability of product,
And later separation nano-graphite colloidal sol is the most difficult.
Separating stable nano-graphite from nano-graphite colloidal sol, the method commonly used at present has: directly
Spray drying method, natural sedimentation partition method, interpolation alkali metal salt destroy electric double layer equilibrium separation method.Wherein,
Direct spraying seasoning needs to evaporate substantial amounts of moisture, and temperature is it is generally required to higher than 300 DEG C, thus deposit
The defect high in energy consumption, production efficiency is low；Natural sedimentation partition method, due to nano-graphite colloidal sol itself ten
Divide stable, therefore use the method time-consumingly long and be difficult to be kept completely separate；And add alkali metal salt and destroy double electricity
, there is the defect needing to introduce more elementary metal impurities, such as CN102249218A in layer equilibration partition method
Disclose a kind of rapid precipitation and the method for drying nano graphite sol, although the method can rapid precipitation
With drying nano graphite sol, but it introduces more elementary metal impurities in nano-graphite, undoubtedly
Have impact on the performance of nano-graphite.
Also having a small amount of method using coating agent separation preparing nano graphite carbon powder from nano graphite sol, it is
By wrapping up with another kind of material at nano grain surface, make can not contact with each other between nano-particle thus
Reach to separate the purpose of nano-graphite；Prepare as CN1378976A discloses one nano-graphite colloidal sol
The method of carbon powder from nano graphite, it is by adding lignin, oleic acid, receiving in nano-graphite sol system
The coating agents such as rice silicon dioxide stop the contact between nano-particle to be reunited, and are then dried to obtain nano-graphite
Fine powder.Equally, although use the method can isolated carbon powder from nano graphite, but it is also in nanometer
Introduce substantial amounts of impurity on graphite carbon dust, thus affect the performance of nano-graphite.
Summary of the invention
It is an object of the invention to the above-mentioned technological deficiency for overcoming prior art, it is provided that one can quickly be divided
From and the nano-graphite colloidal sol and preparation method thereof of stable performance, and one is substantially free of impurity and performance
Excellent nano-graphite and preparation method thereof.
For achieving the above object, according to the first aspect of the invention, the invention provides one and prepare nanometer
The method of graphite sol, wherein, the method includes:
In confined conditions, under the electrolytic condition that graphite electrode electrolysis is nano-graphite, containing waving
In the electrolyte of the property sent out component and water soluble surfactant active, it is electrolysed the graphite electrode as anode, obtains
Nano-graphite colloidal sol, wherein, described volatile component is volatile water-soluble substances and/or at heating condition
The material of volatile water-soluble substances can be produced down.
According to the second aspect of the invention, the invention provides one to prepare according to the method described in the present invention
The nano-graphite colloidal sol obtained.
According to the third aspect of the invention we, the invention provides a kind of method preparing nano-graphite, wherein,
The method includes: nano-graphite colloidal sol is carried out decompression vacuum pumping operation, then filters, and will be filtrated to get
Solid be dried and obtain nano-graphite；Wherein, described nano-graphite colloidal sol is according to the preparation of the present invention
The method of nano-graphite colloidal sol prepares.
According to the fourth aspect of the invention, the invention provides and a kind of prepare according to the method for the present invention
Nano-graphite.
The method preparing nano-graphite colloidal sol of the present invention, by confined conditions, by graphite electrode
Under the electrolysis electrolytic condition for nano-graphite, at the electricity containing volatile component and water soluble surfactant active
Solve in liquid, be electrolysed the graphite electrode as anode to prepare nano-graphite colloidal sol, wherein, described volatility
Component is volatile water-soluble substances and/or can produce volatile water-soluble substances in a heated condition
Material so that the nano-graphite colloidal sol stable performance and the performance that prepare according to the method for the present invention are excellent
Different, thus it is speculated that reason is: under the airtight condition of the present invention, it is being electrolysed the graphite electrode as anode with system
During standby nano-graphite colloidal sol, as the volatile water-soluble substances of electrolyte of the present invention airtight
Space reaches vapor liquid equilibrium, it is possible to realize the balance and stability of nano-graphite surface adsorption ion, thus
Form stable double electrical layers, so that the nano-graphite colloidal sol stable performance prepared and property
Can be excellent；And if under conditions of prior art, using volatile water-soluble substances as electrolyte electricity
Solve graphite electrode and prepare nano-graphite colloidal sol, owing to volatile water-soluble substances is volatile, take by force by force
Having walked the negative ions on nano-graphite surface, the double charge destroying nano-graphite surface balances, and now
The space steric effect relying solely on surfactant is difficult to keep the stably dispersing of nano-graphite, so that
The nano-graphite colloidal sol unstable properties prepared.
And due to the present invention use volatile water-soluble substances as the main electrolyte of the present invention so that
The nano-graphite colloidal sol that must prepare is follow-up is capable of sharp separation, the most only needs to take out through decompression true
Do-nothing operation, then carries out filtering, being dried can isolated nano-graphite.
The method preparing nano-graphite of the present invention, by using the present invention's to prepare nano-graphite colloidal sol
Method prepares nano-graphite colloidal sol, then described nano-graphite colloidal sol is carried out decompression vacuum pumping operation, so
Rear filtration, is dried the solid being filtrated to get and i.e. can get nano-graphite, so that according to this
The nano-graphite that the bright method preparing nano-graphite prepares is substantially free of any impurity, and performance is excellent
Different.And without additionally adding coating agent, alkali metal salt etc., to carry out nano-graphite molten due to the method for the present invention
The separation of glue so that the method for the present invention is received with preparation compared to the parcel nano-graphite colloidal sol of prior art
The method of meter Shi Mo, and add alkali metal salt and destroy electric double layer equilibrium separation method etc. and prepare nano-graphite
The steps such as method are simple, easily realize, and without introducing impurity element.
Other features and advantages of the present invention will be described in detail in detailed description of the invention part subsequently.
Detailed description of the invention
Hereinafter the detailed description of the invention of the present invention is described in detail.It should be appreciated that this place is retouched
The detailed description of the invention stated is merely to illustrate and explains the present invention, is not limited to the present invention.
Before introducing technical scheme, first introduce and prepare nanometer stone by electrolysis graphite electrode
The principle of ink colloidal sol: in electrolytic process, as the carbon atom in the graphite electrode of anode at the work of electric current
With lower acquisition energy, when the energy obtained exceedes the chemical bond force between carbon atom, and acquisition has shape simultaneously
When becoming nano-scale range carbon microparticle surfaces energy, this part carbon atom is using in the graphite electrode as anode
Pole plate departs from, and forms the graphite granule (i.e. nano-graphite granule) of nano-scale range, is free in electrolysis
In liquid, owing to it has extremely strong Selective adsorption, newborn nano-graphite granule can select absorption electrolysis
Anion in matter makes its negatively charged, according to principle of opposite sex attraction, nonionic can adsorb again just from
Son, thus form double electrical layers at nano-graphite particle surface, if shape in preparing nano-graphite colloidal sol
The double electrical layers become is stable, then can prepare stable nano-graphite colloidal sol.
The invention provides a kind of method preparing nano-graphite colloidal sol, wherein, the method includes: close
Under the conditions of closing, under the electrolytic condition that graphite electrode electrolysis is nano-graphite, containing volatile component
With in the electrolyte of water soluble surfactant active, it is electrolysed the graphite electrode as anode, obtains nano-graphite
Colloidal sol, wherein, described volatile component is volatile water-soluble substances and/or can produce in a heated condition
The material of raw volatile water-soluble substances.
Speculate that the know-why that the present invention uses preceding solution to be capable of the purpose of the present invention is:
In nano-graphite sol system, nano-graphite is due to its minimum particle diameter so that it is have greatly than table
Face energy, therefore has the tendency that absorption is reunited, and the present invention is by using volatility group under conditions of airtight
Divide and surfactant is as electrolyte so that on the one hand under the airtight condition of the present invention, make in electrolysis
For the graphite electrode of anode to prepare nano-graphite colloidal sol during, as electrolyte easy of the present invention
Volatilization water-soluble substances reaches vapor liquid equilibrium at confined space, it is possible to realize nano-graphite surface adsorption
The balance and stability of ion, thus (wherein, nano-graphite surface is formed to form stable double electrical layers
In double electrical layers nexine be negative charge, outer layer be positive charge), so that receiving with like charges
The meter Shi Mo same sex is repelled each other, thus prevents the reunion of nano-graphite granule, and on the other hand surfactant is inhaled
It is attached to nano-graphite surface, is formed sterically hindered, it is also possible to stop the reunion of nano-graphite, above-mentioned two
Under the synergism of the factor of kind so that the nano-graphite colloidal dispersion prepared according to the method for the present invention
Stable.
The method according to the invention, can well realize the present invention according to the preceding solution of the present invention
Purpose, for the present invention, preferably in described electrolyte, on the basis of the gross weight of electrolyte, institute
The content stating water soluble surfactant active is 0.0001-0.001 weight %, preferably 0.0005-0.001 weight
Amount %；The content of described volatile component is 0.1-10 weight %, preferably 1-5 weight %.Aforementioned electricity
Solving in liquid, on the one hand the consumption of surfactant seldom (is at most only 0.001 weight of electrolyte weight
%), therefore, although final described SURFACTANT ADSORPTION is on nano-graphite surface, but its content is basic
Negligible, thus without the serviceability affecting nano-graphite；And on the other hand volatilized by control
Property component and the content of surfactant in aforementioned range so that the nano-graphite that electrolysis obtains is molten
Glue has good stability, therefore, under using the electrolytic condition of electrolyte of aforementioned component, permissible
Improve the stability of the nano-graphite colloidal sol prepared according to the method for the present invention further.
The method according to the invention, optional wider range of the kind of described volatile water-soluble substances, energy
Enough volatile water-soluble substanceses as electrolyte are used equally to the present invention, for the present invention, preferably described
Volatile water-soluble substances is HCl, NH3And CO2In one or more.
The method according to the invention, the described thing that can produce volatile water-soluble substances in a heated condition
Optional wider range of matter, being generally possible to produce in a heated condition can be as the volatile water of electrolyte
The material of soluble substance is used equally to the present invention, for the present invention, preferably described in a heated condition can
The material producing volatile water-soluble substances is carbamide and/or hexamethylene tetraammonia.
The method according to the invention, the purpose using described surfactant is to pass through SURFACTANT ADSORPTION
At newborn nano graphite carbon particle surface, formed sterically hindered, to stop between nano-graphite granule
Reunite and grow.Therefore, it is possible to the surfactant realizing object defined above is used equally to the present invention, for this
Invention, the most described water soluble surfactant active selected from polyvinylpyrrolidone, dodecylbenzene sodium sulfonate,
One or more in sodium lauryl sulphate, cetyl trimethylammonium bromide and Polyethylene Glycol.
The method according to the invention, optional wider range of the kind of the solvent in described electrolyte, existing
The conventional use of solvent as electrolyte of technology is used equally to the present invention, for the present invention, in order to drop
Low cost, the solvent in the most described electrolyte is water.
The method according to the invention, described electrolytic condition can be conventional selection, for the present invention, preferably
Described electrolytic condition includes: temperature be room temperature to 100 DEG C, and negative electrode is inert electrode, such as, can be
One or more in stainless steel electrode, graphite electrode and platinum electrode.Wherein, in foregoing temperature range,
Can carry out selecting temperature according to the kind of described volatile component, such as, be easy when described volatile component
Volatilization water-soluble substances such as HCl, NH3And CO2In one or more time, described temperature is generally room
Temperature is to 60 DEG C, and works as described volatile component for producing volatile water-soluble substances in a heated condition
Material such as carbamide and/or hexamethylene tetraammonia time, described temperature is generally 70-100 DEG C.In aforementioned temperature
It is electrolysed in the range of degree, on the one hand can ensure that the evaporation rate of volatile component, on the other hand can also add
Fast volatile component vapor liquid equilibrium in confined conditions, thus so that according to the method system of the present invention
The standby nano-graphite colloidal sol obtained has preferable stability.
With the method for the invention it is preferred to the method for the present invention also includes: detection nano-graphite collosol concentration,
When nano-graphite collosol concentration is 0.1-5 weight %, stops electrolysis, thus can prepare concentration
Nano-graphite colloidal sol for 0.1-5 weight %.
The invention provides a kind of nano-graphite colloidal sol prepared according to the method for the present invention.According to this
The nano-graphite colloidal sol stable performance for preparing of method of invention and excellent performance, concrete such as,
It is greatly improved compared to the nano-graphite collosol stability prepared according to the method for prior art.
The invention provides a kind of method preparing nano-graphite, wherein, the method includes: to nanometer stone
Ink colloidal sol carries out decompression vacuum pumping operation, then filters, is dried by the solid being filtrated to get and is received
Meter Shi Mo；Wherein, described nano-graphite colloidal sol prepares according to the method described in the present invention.
Owing to the nano-graphite colloidal sol used in the method preparing nano-graphite of the present invention is for according to this
The nano-graphite colloidal sol that bright method prepares (uses volatile water-soluble substances as the master of the present invention
Want electrolyte) so that it only needs to make volatilizable electrolyte a large amount of through decompression vacuum pumping operation
Volatilization (thus destroying the charge balance on nano-graphite surface), then carries out filtering, being dried
To nano-graphite.
And without additionally adding coating agent, alkali metal salt etc., to carry out nano-graphite molten due to the method for the present invention
The separation of glue so that the method for the present invention is received with preparation compared to the parcel nano-graphite colloidal sol of prior art
The method of meter Shi Mo, and add alkali metal salt and destroy electric double layer equilibrium separation method etc. and prepare nano-graphite
The steps such as method are simple, easily realize, and without introducing impurity element.
The invention provides a kind of nano-graphite prepared according to the method for the present invention.
Under preferable case, the particle diameter of the nano-graphite of the present invention is 10-60nm, preferably 15-50nm.
The nano-graphite prepared according to the method preparing nano-graphite of the present invention is substantially free of any
Impurity, excellent performance, concrete such as, compared to the nanometer prepared according to the method for prior art
Graphite, its Particle dispersity is preferable.
The present invention is discussed in detail below by embodiment, but the present invention is not limited to this.
In the present invention, the concentration of nano-graphite colloidal sol uses method of poor quality to be calculated, specific as follows: claim
The nano-graphite colloidal sol taking certain mass is dried, and before and after calculating is dry, nano-graphite colloidal sol is of poor quality, should
Of poor quality be dried before the percentage ratio of quality of nano-graphite colloidal sol be the concentration of nano-graphite colloidal sol
(it is also referred to as the solid content of nano-graphite colloidal sol).
In the present invention, the particle diameter of nano-graphite uses laser particle size analyzer to record.
Embodiment 1
Prepare nano-graphite colloidal sol: 283.93g ammonia (concentration is 28 weight %) and 0.024g are gathered
Vinylpyrrolidone PVP(is purchased from Chengdu Gracia chemical technology company limited, trade mark PVPK30)
Join mix homogeneously in 2795.57g deionized water and obtain electrolyte, pour this electrolyte into electrolyzer
In, with graphite electrode as anode, with stainless steel electrode as negative electrode, then electrolyzer is put into confined space
In, at 50 DEG C, the electrolyte 1h in heating electrolyzer, it is then turn on power supply and is electrolysed, work as inspection
Measure and when the concentration of nano-graphite colloidal sol is 2.6 weight %, stop electrolysis, obtain nano-graphite colloidal sol
NGS-1, in perusal nano-graphite colloidal sol without precipitated nanocrystals graphite (and take out its part as sample,
In confined conditions, after being placed 30 days by sample, precipitation, lamination the most do not occur)；
Prepare nano-graphite: then use vacuum pump that above-mentioned confined space is carried out evacuation process, nanometer
Graphite slowly precipitates, and until nano-graphite colloidal sol in when being significantly layered, closes vacuum pump, filters, will
The solid arrived is dried at 80 DEG C, obtains nano-graphite GP-1(particle diameter between 20-45nm).
Embodiment 2
Prepare nano-graphite colloidal sol: by 40.5g carbamide and 0.018g sodium lauryl sulphate (purchased from Guangdong
Brilliance chemistry Co., Ltd., Factory) join mix homogeneously in 3000g deionized water and obtain electrolyte, should
Electrolyte is poured in electrolyzer, with graphite electrode as anode, with graphite electrode as negative electrode, and then will electrolysis
Pond is put in confined space, at 90 DEG C, and the electrolyte 1h in heating electrolyzer, it is then turn on power supply
It is electrolysed, stops electrolysis when concentration nano-graphite colloidal sol being detected is 0.96 weight %, received
Rice graphite sol NGS-2, (and takes out its portion without precipitated nanocrystals graphite in perusal nano-graphite colloidal sol
Be allocated as sample, in confined conditions, after sample is placed 30 days, the most do not occur precipitation, point
Layer phenomenon)；
Prepare nano-graphite: then use vacuum pump that above-mentioned confined space is carried out evacuation process, nanometer
Graphite slowly precipitates, and until nano-graphite colloidal sol in when being significantly layered, closes vacuum pump, filters, will
The solid arrived is dried at 80 DEG C, obtains nano-graphite GP-2(particle diameter between 15-30nm).
Embodiment 3
Prepare nano-graphite colloidal sol: 0.03g Macrogol 2000 is (purchased from the Guangdong limited public affairs of brilliance laboratory
Department, PEG2000) join mix homogeneously in 3000g deionized water, then pour in electrolyzer, with stone
Electrode ink is anode, with platinum electrode as negative electrode, is then put in confined space by electrolyzer；The most again to
Electrolyzer is passed through the CO of 65.67L2Gas, and at room temperature stand 1h, it is then turn on power supply and carries out
Electrolysis, stops electrolysis, obtains nanometer stone when concentration nano-graphite colloidal sol being detected is 4.3 weight %
Ink colloidal sol NGS-3, in perusal nano-graphite colloidal sol without precipitated nanocrystals graphite (and take out its part work
For sample, after being placed 30 days by sample, precipitation, lamination the most do not occur)；
Prepare nano-graphite: then use vacuum pump that above-mentioned confined space is carried out evacuation process, nanometer
Graphite slowly precipitates, and until nano-graphite colloidal sol in when being significantly layered, closes vacuum pump, filters, will
The solid arrived is dried at 80 DEG C, obtains nano-graphite GP-3, and particle diameter is between 45-50nm.
Embodiment 4
Prepare nano-graphite colloidal sol according to the method for embodiment 2 and prepare nano-graphite, except for the difference that, system
During standby nano-graphite colloidal sol, the consumption of sodium lauryl sulphate is 0.006g, and the consumption of carbamide is
15g, remaining condition is constant, obtains nano-graphite colloidal sol NGS-4, in perusal nano-graphite colloidal sol
Graphite without precipitated nanocrystals (and take out its part as sample, in confined conditions, sample is placed 30
After it, small part precipitation, lamination occur), finally give nano-graphite GP-4(particle diameter at 15-89nm
Between).
Comparative example 1
Prepare nano-graphite colloidal sol according to the method for embodiment 1, except for the difference that, electrolyzer is not put into close
Closing in space and be directly electrolysed, remaining step is the most identical with condition, obtains nano-graphite colloidal sol
NGS-D1, has partly precipitated (and to take out its part as sample, by sample bottom this colloidal sol of perusal
After product are placed 30 days, precipitation and lamination are clearly).
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited to above-mentioned reality
Execute the detail in mode, in the technology concept of the present invention, can be to the technical side of the present invention
Case carries out multiple simple variant, and these simple variant belong to protection scope of the present invention.
It is further to note that each the concrete technology described in above-mentioned detailed description of the invention is special
Levy, in the case of reconcilable, can be combined by any suitable means.
Additionally, combination in any can also be carried out between the various different embodiment of the present invention, as long as its
Without prejudice to the thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. the method preparing nano-graphite colloidal sol, it is characterised in that the method includes:
In confined conditions, under the electrolytic condition that graphite electrode electrolysis is nano-graphite, containing waving
In the electrolyte of the property sent out component and water soluble surfactant active, it is electrolysed the graphite electrode as anode, obtains
Nano-graphite colloidal sol, wherein, described volatile component is volatile water-soluble substances and/or at heating condition
Can produce down the material of volatile water-soluble substances, described volatile water-soluble substances is HCl, NH3
And CO2In one or more, the described thing that can produce volatile water-soluble substances in a heated condition
Matter is carbamide and/or hexamethylene tetraammonia.
Method the most according to claim 1, wherein, in described electrolyte, with electrolyte
On the basis of gross weight, the content of described water soluble surfactant active is 0.0001-0.001 weight %, described
The content of volatile component is 0.1-10 weight %.
Method the most according to claim 2, wherein, in described electrolyte, with electrolyte
On the basis of gross weight, the content of described water soluble surfactant active is 0.0005-0.001 weight %；Described
The content of volatile component is 1-5 weight %.
4. according to the method described in any one in claim 1-3, wherein, described soluble surface
Activating agent is selected from polyvinylpyrrolidone, sodium lauryl sulphate, dodecylbenzene sodium sulfonate, hexadecane
One or more in base trimethylammonium bromide and Polyethylene Glycol.
5. according to the method described in any one in claim 1-3, wherein, in described electrolyte
Solvent is water.
6. according to the method described in any one in claim 1-3, wherein, described electrolytic condition bag
Include: temperature be room temperature to 100 DEG C, and negative electrode is in stainless steel electrode, graphite electrode and platinum electrode
Plant or multiple.
7. according to the method described in any one in claim 1-3, wherein, the method also includes:
Detection nano-graphite collosol concentration, when nano-graphite collosol concentration is 0.1-5 weight %, stops electrolysis.
8. the nano-graphite colloidal sol that in claim 1-7, method described in any one prepares.
9. the method preparing nano-graphite, it is characterised in that the method includes:
Nano-graphite colloidal sol is carried out decompression vacuum pumping operation, then filters, the solid being filtrated to get is entered
Row is dried to obtain nano-graphite；
Wherein, described nano-graphite colloidal sol is prepared according to the method described in any one in claim 1-7
Obtain.
10. the nano-graphite that the method described in claim 9 prepares.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1378975A (en) * | 2002-05-17 | 2002-11-13 | 贵州航天纳米科技有限责任公司 | Process for preparing nano graphite carbon sol with dual graphite electrodes |
| CN1579932A (en) * | 2003-08-12 | 2005-02-16 | 刘键 | Preparation of nano graphite carbon colloidal SOL by pulse electrode process |
| CN101092237A (en) * | 2007-05-29 | 2007-12-26 | 浙江大学 | Method for preparing Nano graphite sol by inputting pulsed dc bias to dual graphite electrodes |
| CN101941694A (en) * | 2010-09-07 | 2011-01-12 | 湘潭大学 | Preparation method of high-dispersivity graphene |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381881A (en) * | 2007-09-05 | 2009-03-11 | 西南交通大学 | Method for preparing hydroxylapatite/chitosan composite coating by pulse electrochemical deposition |
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- 2012-12-31 CN CN201210592129.7A patent/CN103908932B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1378975A (en) * | 2002-05-17 | 2002-11-13 | 贵州航天纳米科技有限责任公司 | Process for preparing nano graphite carbon sol with dual graphite electrodes |
| CN1579932A (en) * | 2003-08-12 | 2005-02-16 | 刘键 | Preparation of nano graphite carbon colloidal SOL by pulse electrode process |
| CN101092237A (en) * | 2007-05-29 | 2007-12-26 | 浙江大学 | Method for preparing Nano graphite sol by inputting pulsed dc bias to dual graphite electrodes |
| CN101941694A (en) * | 2010-09-07 | 2011-01-12 | 湘潭大学 | Preparation method of high-dispersivity graphene |
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