CN103908932A - Nano-graphite sol and its preparation method, nano-graphite and its preparation method - Google Patents
Nano-graphite sol and its preparation method, nano-graphite and its preparation method Download PDFInfo
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- CN103908932A CN103908932A CN201210592129.7A CN201210592129A CN103908932A CN 103908932 A CN103908932 A CN 103908932A CN 201210592129 A CN201210592129 A CN 201210592129A CN 103908932 A CN103908932 A CN 103908932A
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Abstract
The invention provides a nano-graphite sol and a preparation method thereof. The method includes: under an airtight condition, and under the electrolytic conditions of electrolyzing a graphite electrode into nano-graphite, in an electrolyte solution containing volatile component and a water-soluble surfactant, electrolyzing a graphite electrode serving as the anode to obtain the nano-graphite sol. Specifically, the volatile component is an easily volatile water-soluble substance and/or a substance able to generate an easily volatile water-soluble substance under heating. The invention also provides a nano-graphite and its preparation method. The nano-graphite sol prepared according to the method provided by the invention has good stability, and the preparation method of the nano-graphite provided by the invention has the advantages of simple steps, easy implementation, and no need for introduction of impurity elements.
Description
Technical field
The present invention relates to a kind of method of preparing nano-graphite colloidal sol, and the nano-graphite colloidal sol preparing according to the method for preparing nano-graphite colloidal sol of the present invention, and a kind of method of preparing nano-graphite, and the nano-graphite preparing according to the method for preparing nano-graphite of the present invention.
Background technology
The purposes of nano-graphite is very extensive, as can be for new type chemical fertilizer, battery electrode material, electric heating material, magnetic pipe recording material etc.But in the time that graphite is nanoscale, its specific surface energy is very large, having reunites reduces the tendency of specific surface energy, therefore very easily reunites, and is difficult to dispersion, the preparation that makes thus the nano-graphite with polymolecularity with separate very difficult.
At present, the nano-graphite with polymolecularity mainly adopts two kinds of basic skills preparations: wherein, a kind of method is by the surface formation electric double layer at nano particle, and like charges between nano particle is repelled each other; As CN1378975A discloses a kind of method of preparing nano graphite carbon sol with dual graphite electrodes, it,, by adding the water soluble compound such as sodium carbonate, sodium chloride to make nano-graphite surface form double electrical layers, makes stable nano-graphite colloidal sol thus.Can make stable nano-graphite colloidal sol although adopt the method to prepare nano graphite carbon sol, can introduce more metallic element impurity, affect the serviceability of product, and comparatively difficulty of later separation nano-graphite colloidal sol.
The nano-graphite of separating stable from nano-graphite colloidal sol, the method generally using at present has: Direct spraying seasoning, natural sedimentation partition method, the alkali metal salt destruction electric double layer equilibrium separation method of adding.Wherein, Direct spraying seasoning need to be evaporated a large amount of moisture, and temperature generally need to, higher than 300 DEG C, exist the defect that energy consumption is high, production efficiency is low thus; Natural sedimentation partition method, because nano-graphite colloidal sol itself is very stable, therefore adopts the method length consuming time and is difficult to separate completely; Destroy electric double layer equilibrium separation method and add alkali metal salt, existence need to be introduced the defect of more metallic element impurity, as CN102249218A discloses a kind of method of rapid precipitation and drying nano graphite sol, although the method can rapid precipitation and drying nano graphite sol, but it has introduced more metallic element impurity in nano-graphite, affect undoubtedly the performance of nano-graphite.
Also have a small amount of employing coating agent to separate the method for preparing nano graphite carbon powder from nano graphite sol, it is by wrapping up at the another kind of material of nano grain surface, thereby makes can not contact with each other and reach the object that separates nano-graphite between nano particle; As CN1378976A discloses a kind of method with preparing nano graphite carbon powder from nano graphite sol, it stops the contact between nano particle to be reunited by add the coating agents such as lignin, oleic acid, nano silicon in nano-graphite sol system, the then dry nano-graphite fine powder that obtains.Equally, obtain carbon powder from nano graphite although adopt the method to separate, but it has also introduced a large amount of impurity on carbon powder from nano graphite, affects thus the performance of nano-graphite.
Summary of the invention
The object of the invention is the above-mentioned technological deficiency for overcoming prior art, provide a kind of and can separate fast and the nano-graphite colloidal sol of stable performance and preparation method thereof, and a kind of nano-graphite of substantially free from foreign meter and excellent performance and preparation method thereof.
For achieving the above object, according to a first aspect of the invention, the invention provides a kind of method of preparing nano-graphite colloidal sol, wherein, the method comprises:
In confined conditions, under the electrolytic condition that is nano-graphite by graphite electrode electrolysis, in the electrolyte that contains volatile component and water soluble surfactant active, electrolysis is as the graphite electrode of anode, obtain nano-graphite colloidal sol, wherein, described volatile component is volatile water-soluble substances and/or the material that can produce volatile water-soluble substances under heating condition.
According to a second aspect of the invention, the invention provides a kind of nano-graphite colloidal sol preparing according to the method described in the present invention.
According to a third aspect of the invention we, the invention provides a kind of method of preparing nano-graphite, wherein, the method comprises: nano-graphite colloidal sol is carried out to decompression vacuum pumping operation, then filter, the solid that filtration is obtained is dried and obtains nano-graphite; Wherein, described nano-graphite colloidal sol prepares according to the method for preparing nano-graphite colloidal sol of the present invention.
According to a forth aspect of the invention, the invention provides a kind of nano-graphite preparing according to method of the present invention.
The method of preparing nano-graphite colloidal sol of the present invention, by in confined conditions, under the electrolytic condition that is nano-graphite by graphite electrode electrolysis, in the electrolyte that contains volatile component and water soluble surfactant active, electrolysis as the graphite electrode of anode to prepare nano-graphite colloidal sol, wherein, described volatile component is volatile water-soluble substances and/or the material that can produce volatile water-soluble substances under heating condition, make the stable performance of nano-graphite colloidal sol and the excellent performance that prepare according to method of the present invention, infer that reason is: under airtight condition of the present invention, electrolysis as the graphite electrode of anode to prepare in the process of nano-graphite colloidal sol, reach vapor liquid equilibrium as electrolytical volatile water-soluble substances of the present invention at confined space, can realize thus the balance and stability of nano-graphite adsorption ion, thereby form stable double electrical layers, make thus the stable performance of nano-graphite colloidal sol and the excellent performance that prepare, if and under the condition of prior art, use volatile water-soluble substances to prepare nano-graphite colloidal sol as electrolyte electrolysis graphite electrode, because volatile water-soluble substances is volatile, seize by force thus the negative ions on nano-graphite surface, destroy the double charge balance on nano-graphite surface, and the space steric effect that now only relies on surfactant is difficult to keep the stably dispersing of nano-graphite, thereby make the nano-graphite colloidal sol unstable properties preparing.
And because the present invention uses volatile water-soluble substances as main electrolyte of the present invention, thereby make that the nano-graphite colloidal sol for preparing is follow-up can realize quick separation, for example only need through decompression vacuum pumping operation, then filtering, being dried is the separable nano-graphite that obtains.
The method of preparing nano-graphite of the present invention, prepare nano-graphite colloidal sol by adopting the method for preparing nano-graphite colloidal sol of the present invention, then described nano-graphite colloidal sol is carried out to decompression vacuum pumping operation, then filter, the solid that filtration is obtained is dried and can obtains nano-graphite, make thus the nano-graphite preparing according to the method for preparing nano-graphite of the present invention substantially not containing any impurity, and excellent performance.And because method of the present invention is carried out the separation of nano-graphite colloidal sol without extra interpolation coating agent, alkali metal salt etc., make method of the present invention than the parcel nano-graphite colloidal sol of prior art to prepare the method for nano-graphite, and add alkali metal salt and destroy electric double layer equilibrium separation method etc. to prepare the step such as method of nano-graphite simple, easily realize, and without introducing impurity element.
Other features and advantages of the present invention are described in detail the detailed description of the invention part subsequently.
Detailed description of the invention
Below the specific embodiment of the present invention is elaborated.Should be understood that, detailed description of the invention described herein only, for description and interpretation the present invention, is not limited to the present invention.
Before introducing technical scheme of the present invention, paper is prepared the principle of nano-graphite colloidal sol by electrolysis graphite electrode: in electrolytic process, under the effect of electric current, obtain energy as the carbon atom in the graphite electrode of anode, when the energy obtaining exceedes the chemical bonding force between carbon atom, and obtain while thering is the nano-scale range of formation carbon microparticle surface energy simultaneously, this part carbon atom will depart from the graphite electrode pole plate as anode, form the graphite granule (being nano-graphite particle) of nano-scale range, be free in electrolyte, because it has extremely strong Selective adsorption, newborn nano-graphite particle can select the anion in adsorbing electrolyte to make its electronegative property, according to principle of opposite sex attraction, cation can be adsorbed again in anion surface, thereby form double electrical layers at nano-graphite particle surface, if the double electrical layers forming in nano-graphite colloidal sol is stable preparing, can prepare stable nano-graphite colloidal sol.
The invention provides a kind of method of preparing nano-graphite colloidal sol, wherein, the method comprises: in confined conditions, under the electrolytic condition that is nano-graphite by graphite electrode electrolysis, in the electrolyte that contains volatile component and water soluble surfactant active, electrolysis, as the graphite electrode of 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 under heating condition.
Infer that the know-why that the present invention adopts aforementioned techniques scheme can realize object of the present invention is: in nano-graphite sol system, nano-graphite is due to its minimum particle diameter, make it have great specific surface energy, therefore the tendency that has absorption to reunite, and the present invention by using volatile component and surfactant as electrolyte under airtight condition, make on the one hand under airtight condition of the present invention, electrolysis as the graphite electrode of anode to prepare in the process of nano-graphite colloidal sol, reach vapor liquid equilibrium as electrolytical volatile water-soluble substances of the present invention at confined space, can realize thus the balance and stability of nano-graphite adsorption ion, thereby form stable double electrical layers (wherein, in the double electrical layers that nano-graphite surface forms, nexine is negative electrical charge, skin is positive charge), make thus the nano-graphite two like magnetic poles repel each other with like charges, thereby stop the reunion of nano-graphite particle, SURFACTANT ADSORPTION is on nano-graphite surface on the other hand, form sterically hindered, also can stop the reunion of nano-graphite, under the synergy of above-mentioned two kinds of factors, make the nano-graphite colloidal sol stably dispersing preparing according to method of the present invention.
The method according to this invention, can well realize object of the present invention according to aforementioned techniques scheme of the present invention, for the present invention, preferably in described electrolyte, taking the gross weight of electrolyte as benchmark, described water soluble surfactant active's content is 0.0001-0.001 % by weight, is preferably 0.0005-0.001 % by weight; The content of described volatile component is 0.1-10 % by weight, is preferably 1-5 % by weight.In aforementioned electrolyte, seldom (being only 0.001 % by weight of electrolyte weight at most) of the consumption of surfactant on the one hand, therefore, although final described SURFACTANT ADSORPTION is on nano-graphite surface, but its content can be ignored substantially, therefore can not affect the serviceability of nano-graphite; And the content that passes through on the other hand to control volatile component and surfactant is in aforementioned range, can make the nano-graphite colloidal sol that electrolysis obtains there is good stability, therefore, under the electrolytic condition of electrolyte that adopts aforementioned component, can further improve the stability of the nano-graphite colloidal sol preparing according to method of the present invention.
The method according to this invention, optional wider range of the kind of described volatile water-soluble substances, can all can be used for the present invention as electrolytical volatile water-soluble substances, and for the present invention, preferably described volatile water-soluble substances is HCl, NH
3and CO
2in one or more.
The method according to this invention, optional wider range of the described material that can produce volatile water-soluble substances under heating condition, generally can under heating condition, produce and can all can be used for the present invention as the material of electrolytical volatile water-soluble substances, for the present invention, preferably the described material that can produce volatile water-soluble substances under heating condition is urea and/or hexamethylene tetraammonia.
The method according to this invention, the object that adopts described surfactant be by SURFACTANT ADSORPTION at newborn nano graphite carbon particle surface, form sterically hindered, to stop reunion between nano-graphite particle growth.Therefore, the surfactant that can realize aforementioned object all can be used for the present invention, for the present invention, preferred described water soluble surfactant active is selected from one or more in polyvinylpyrrolidone, neopelex, lauryl sodium sulfate, softex kw and polyethylene glycol.
The method according to this invention, optional wider range of the kind of the solvent in described electrolyte, the solvent as electrolyte that the routine of prior art is used all can be used for the present invention, and for the present invention, in order to reduce costs, the solvent in preferred described electrolyte is water.
The method according to this invention, described electrolytic condition can be conventional selection, and for the present invention, preferred described electrolytic condition comprises: temperature is room temperature to 100 DEG C, and negative electrode is inert electrode, for example, can be one or more in stainless steel electrode, graphite electrode and platinum electrode.Wherein, within the scope of aforementioned temperature, can select temperature according to the kind of described volatile component, for example, when described volatile component is that volatile water-soluble substances is as HCl, NH
3and CO
2in one or more time, described temperature is generally room temperature to 60 DEG C, and when described volatile component be the material during as urea and/or hexamethylene tetraammonia that can produce volatile water-soluble substances under heating condition, described temperature is generally 70-100 DEG C.Electrolysis within the scope of aforementioned temperature, can ensure on the one hand the evaporation rate of volatile component, also can accelerate on the other hand volatile component vapor liquid equilibrium in confined conditions, can make thus the nano-graphite colloidal sol preparing according to method of the present invention there is good stability.
The method according to this invention, preferred method of the present invention also comprises: detect nano-graphite collosol concentration, in the time that nano-graphite collosol concentration is 0.1-5 % by weight, stop electrolysis, can prepare thus concentration is the nano-graphite colloidal sol of 0.1-5 % by weight.
The invention provides a kind of nano-graphite colloidal sol preparing according to method of the present invention.The stable performance of nano-graphite colloidal sol and the excellent performance that prepare according to method of the present invention, for example concrete, greatly improve than the nano-graphite collosol stability preparing according to the method for prior art.
The invention provides a kind of method of preparing nano-graphite, wherein, the method comprises: nano-graphite colloidal sol is carried out to decompression vacuum pumping operation, then filter, the solid that filtration is obtained is dried and obtains nano-graphite; Wherein, described nano-graphite colloidal sol prepares according to the method described in the present invention.
Because the nano-graphite colloidal sol using in the method for nano-graphite of preparing of the present invention is the nano-graphite colloidal sol (using volatile water-soluble substances as main electrolyte of the present invention) preparing according to method of the present invention, thereby make it only need through decompression vacuum pumping operation, volatilizable electrolyte to be volatilized the charge balance of nano-graphite surface (thereby destroyed) in a large number, then filter, dryly can obtain nano-graphite.
And because method of the present invention is carried out the separation of nano-graphite colloidal sol without extra interpolation coating agent, alkali metal salt etc., make method of the present invention than the parcel nano-graphite colloidal sol of prior art to prepare the method for nano-graphite, and add alkali metal salt and destroy electric double layer equilibrium separation method etc. to prepare the step such as method of nano-graphite simple, easily realize, and without introducing impurity element.
The invention provides a kind of nano-graphite preparing according to method of the present invention.
Under preferable case, the particle diameter of nano-graphite of the present invention is 10-60nm, is preferably 15-50nm.
The nano-graphite preparing according to the method for preparing nano-graphite of the present invention does not contain any impurity substantially, excellent performance, and for example concrete, than the nano-graphite preparing according to the method for prior art, its Particle dispersity is better.
Introduce in detail the present invention below by embodiment, but the present invention is not limited to this.
In the present invention, the concentration of nano-graphite colloidal sol adopts method of poor quality to calculate, specific as follows: the nano-graphite colloidal sol that takes certain mass is dry, calculate dry before and after nano-graphite colloidal sol of poor quality, this of poor quality and dry before the percentage of quality of nano-graphite colloidal sol be the concentration (it also refers to the solid content of nano-graphite colloidal sol) of nano-graphite colloidal sol.
In the present invention, the particle diameter of nano-graphite adopts laser particle size analyzer to record.
Embodiment 1
Prepare nano-graphite colloidal sol: by 283.93g ammoniacal liquor (concentration is 28 % by weight) and 0.024g polyvinylpyrrolidone PVP(purchased from Chengdu Gracia chemical technology Co., Ltd, trade mark PVPK30) join in 2795.57g deionized water and mix and obtain electrolyte, this electrolyte is poured in electrolytic cell, taking graphite electrode as anode, taking stainless steel electrode as negative electrode, then electrolytic cell is put into confined space, at 50 DEG C, electrolyte 1h in heating electrolytic cell, then switch on power and carry out electrolysis, when detecting that the concentration of nano-graphite colloidal sol stops electrolysis while being 2.6 % by weight, obtain nano-graphite colloidal sol NGS-1, visually observe in nano-graphite colloidal sol and (and take out its part as sample without precipitation nano-graphite, in confined conditions, sample was placed after 30 days, substantially there is not precipitation, lamination),
Prepare nano-graphite: then adopt vavuum pump to vacuumize processing to above-mentioned confined space, nano-graphite slowly precipitates, in the time that nano-graphite colloidal sol is obvious layering, close vavuum pump, filter, the solid obtaining is dried at 80 DEG C, obtain nano-graphite GP-1(particle diameter between 20-45nm).
Embodiment 2
Prepare nano-graphite colloidal sol: 40.5g urea and 0.018g lauryl sodium sulfate (purchased from 1Guanghua Chemical Plant Co., Ltd., Guangdong) are joined in 3000g deionized water and mix and obtain electrolyte, this electrolyte is poured in electrolytic cell, taking graphite electrode as anode, taking graphite electrode as negative electrode, then electrolytic cell is put into confined space, at 90 DEG C, electrolyte 1h in heating electrolytic cell, then switch on power and carry out electrolysis, when detecting that the concentration of nano-graphite colloidal sol stops electrolysis while being 0.96 % by weight, obtain nano-graphite colloidal sol NGS-2, visually observe in nano-graphite colloidal sol and (and take out its part as sample without precipitation nano-graphite, in confined conditions, sample was placed after 30 days, substantially there is not precipitation, lamination),
Prepare nano-graphite: then adopt vavuum pump to vacuumize processing to above-mentioned confined space, nano-graphite slowly precipitates, in the time that nano-graphite colloidal sol is obvious layering, close vavuum pump, filter, the solid obtaining is dried at 80 DEG C, obtain nano-graphite GP-2(particle diameter between 15-30nm).
Embodiment 3
Prepare nano-graphite colloidal sol: 0.03g Macrogol 2000 is (purchased from 1Guanghua Chemical Plant Co., Ltd., Guangdong, PEG2000) join in 3000g deionized water and mix, then pour in electrolytic cell, taking graphite electrode as anode, taking platinum electrode as negative electrode, then electrolytic cell is put into confined space; And then to the CO that passes into 65.67L in electrolytic cell
2gas, and at room temperature leave standstill 1h, then switch on power and carry out electrolysis, when detecting that the concentration of nano-graphite colloidal sol stops electrolysis while being 4.3 % by weight, obtain nano-graphite colloidal sol NGS-3, visually observe in nano-graphite colloidal sol without precipitation nano-graphite (and take out its part as sample, sample was placed after 30 days, substantially do not occur precipitation, lamination);
Prepare nano-graphite: then adopt vavuum pump to vacuumize processing to above-mentioned confined space, nano-graphite slowly precipitates, in the time that nano-graphite colloidal sol is obvious layering, close vavuum pump, filter, the solid obtaining is dried at 80 DEG C, obtain nano-graphite GP-3, particle diameter is between 45-50nm.
Embodiment 4
Prepare nano-graphite colloidal sol and prepare nano-graphite according to the method for embodiment 2, different is, prepare in the process of nano-graphite colloidal sol, the consumption of lauryl sodium sulfate is 0.006g, the consumption of urea is 15g, all the other conditions are constant, obtain nano-graphite colloidal sol NGS-4, visually observe in nano-graphite colloidal sol and (and take out its part as sample without precipitation nano-graphite, in confined conditions, sample was placed after 30 days, is occurred small part precipitation, lamination), finally obtain nano-graphite GP-4(particle diameter between 15-89nm).
Comparative example 1
Prepare nano-graphite colloidal sol according to the method for embodiment 1, different is, electrolytic cell is not put into confined space and directly carried out electrolysis, all the other steps and condition are all identical, obtain nano-graphite colloidal sol NGS-D1, visually observe this colloidal sol bottom and have partly precipitated (and take out its part as sample, sample was placed after 30 days, precipitation and lamination are very obvious).
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition each the concrete technical characterictic described in above-mentioned detailed description of the invention, in reconcilable situation, can combine by any suitable mode.
In addition, between various embodiment of the present invention, also can be combined, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (11)
1. a method of preparing nano-graphite colloidal sol, is characterized in that, the method comprises:
In confined conditions, under the electrolytic condition that is nano-graphite by graphite electrode electrolysis, in the electrolyte that contains volatile component and water soluble surfactant active, electrolysis is as the graphite electrode of anode, obtain nano-graphite colloidal sol, wherein, described volatile component is volatile water-soluble substances and/or the material that can produce volatile water-soluble substances under heating condition.
2. method according to claim 1, wherein, in described electrolyte, taking the gross weight of electrolyte as benchmark, described water soluble surfactant active's content is 0.0001-0.001 % by weight, the content of described volatile component is 0.1-10 % by weight.
3. method according to claim 2, wherein, in described electrolyte, taking the gross weight of electrolyte as benchmark, described water soluble surfactant active's content is 0.0005-0.001 % by weight; The content of described volatile component is 1-5 % by weight.
4. according to the method described in any one in claim 1-3, wherein, described volatile water-soluble substances is HCl, NH
3and CO
2in one or more, the described material that can produce volatile water-soluble substances under heating condition is urea and/or hexamethylene tetraammonia.
5. according to the method described in any one in claim 1-3, wherein, described water soluble surfactant active is selected from one or more in polyvinylpyrrolidone, lauryl sodium sulfate, neopelex, softex kw and polyethylene glycol.
6. according to the method described in any one in claim 1-3, wherein, the solvent in described electrolyte is water.
7. according to the method described in any one in claim 1-3, wherein, described electrolytic condition comprises: temperature is room temperature to 100 DEG C, and negative electrode is one or more in stainless steel electrode, graphite electrode and platinum electrode.
8. according to the method described in any one in claim 1-3, wherein, the method also comprises: detect nano-graphite collosol concentration, in the time that nano-graphite collosol concentration is 0.1-5 % by weight, stop electrolysis.
9. the nano-graphite colloidal sol that in claim 1-8, the method described in any one prepares.
10. a method of preparing nano-graphite, is characterized in that, the method comprises:
Nano-graphite colloidal sol is carried out to decompression vacuum pumping operation, then filter, the solid that filtration is obtained is dried and obtains nano-graphite;
Wherein, described nano-graphite colloidal sol prepares according to the method described in any one in claim 1-8.
The nano-graphite that 11. methods claimed in claim 10 prepare.
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Citations (5)
| 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 |
| 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 |
| CN101941694A (en) * | 2010-09-07 | 2011-01-12 | 湘潭大学 | Preparation method of high-dispersivity graphene |
-
2012
- 2012-12-31 CN CN201210592129.7A patent/CN103908932B/en active Active
Patent Citations (5)
| 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 |
| 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 |
| CN101941694A (en) * | 2010-09-07 | 2011-01-12 | 湘潭大学 | Preparation method of high-dispersivity graphene |
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