CN101250714A - Composite electrode and method for preparing high purity polyaniline nanometer line - Google Patents
Composite electrode and method for preparing high purity polyaniline nanometer line Download PDFInfo
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- CN101250714A CN101250714A CNA2008100525220A CN200810052522A CN101250714A CN 101250714 A CN101250714 A CN 101250714A CN A2008100525220 A CNA2008100525220 A CN A2008100525220A CN 200810052522 A CN200810052522 A CN 200810052522A CN 101250714 A CN101250714 A CN 101250714A
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Abstract
The invention discloses a composite electrode which prepares polyaniline nano-wires with high purity and a method for preparing the composite electrode, which belongs to the technique for preparing polyaniline nano-wire materials. A substrate of the composite electrode is stainless steel, titanium, nickel, cobalt, aluminum, iron, copper, graphite or glassy carbon, and thin film of polysulfone, polyether sulfone, polyimide or polyether imide is compounded on the substrate. The method for preparing the composite electrode comprises following steps: dissolving the polysulfone, the polyether sulfone, the polyimide or the polyether imide in N, N-dimethylacetamide, N, N-dimethylformamide, N-methyl pyrrolidone, dimethyl sulfoxide or m-cresol, preparing even and transparent casting solution, coating the casting solution on the surface of a substrate electrode, then, rapidly dipping the electrode in coagulation bath to finish phase inversion, and obtaining the composite electrode. The method of the invention has the advantages that the composite electrode is used as a working electrode to prepare the polyaniline nano-wires, which solves the problem that polyaniline particles exist in the polyaniline nano-wires and increases the purity of the polyaniline nano-wires.
Description
Technical field
The present invention relates to a kind of combined electrode and preparation method who prepares high purity polyaniline nanometer line, belong to the technology of preparation polyaniline nano wire material.
Background technology
Polyaniline has the protonic acid doping behavior that raw material is easy to get, synthetic method is simple, unique, good electrochemistry and optical property, structure diversity and good advantages such as environmental stability.These excellent characteristics make polyaniline be subjected to paying close attention to widely in the application in fields such as transmitter, driver, electromagnetic shielding, anti-static coating, anti-corrosion of metal, gas separation membrane, capacitor with super capacity and opto-electronic device, are considered to one of conductive polymers that is hopeful to be applied in practice most.In recent years, polyaniline nano-line is owing to the physicochemical property with big specific surface area and excellence cause investigator's very big concern.Aniline is easy to form nano wire at the polymerization initial stage, along with polymeric often obtains granular product.Therefore, just must control the process of aniline polymerization or the space of control aniline polymerization for obtaining polyaniline nano-line.At present, the technology of Chang Yong preparation polyaniline nano-line comprises chemical polymerization (template and non-template method) and electrochemical polymerization method.The advantage of template polymerization method is that the productive rate of product when the template of using is suitable is higher, and shortcoming is that product purity step low, that obtain pure nano wire is numerous and diverse.When using non-template method (interfacial polymerization and short mix method), the purity height of the polyaniline nano-line that obtains, the diameter of nano wire and length controlled, but productive rate is low.Electrochemical polymerization method productive rate height, environmental friendliness, but in polymerization process, at first form one deck polyaniline particle at electrode surface easily, make the purity of the polyaniline nano-line that obtains not high.Therefore the new technology of developing a kind of electrochemical preparation high purity polyaniline nanometer line is very necessary.
Summary of the invention
The object of the present invention is to provide a kind of combined electrode and preparation method who prepares high purity polyaniline nanometer line, described combined electrode is used to prepare polyaniline nano-line, nano wire purity height, and described combined electrode preparation process is simple.
The present invention is realized by following technical proposals: a kind of combined electrode for preparing high purity polyaniline nanometer line, this combined electrode is a matrix with stainless steel, titanium, nickel, cobalt, aluminium, iron, copper, graphite or vitreous carbon, it is characterized in that composite thickness is the film of polysulfones, polyethersulfone, polyimide or the polyetherimide of 5～150 μ m on the surface of matrix.
The preparation method of above-mentioned combined electrode is characterized in that comprising following process:
According to quality percentage composition 3～30% polysulfones, polyethersulfone, polyimide or polyetherimide are dissolved in N,N-dimethylacetamide, N, in dinethylformamide, N-Methyl pyrrolidone, dimethyl sulfoxide (DMSO) or the meta-cresol, are mixed with the homogeneous transparent film-casting liquid.Film-casting liquid evenly is coated in stainless steel, titanium, nickel, cobalt, aluminium, iron, copper, graphite or vitreous carbon surface after standing and defoaming, it is immersed in rapidly finishes inversion of phases in the precipitation bath afterwards, obtains combined electrode.
The invention has the advantages that prepared combined electrode is used to prepare polyaniline nano-line, nano wire purity height, diameter are 30～300nm, and length is 500nm～5 μ m, and this method for preparing composite electrode process is simple.
Description of drawings
Fig. 1 is the stereoscan photograph of the prepared polyaniline nano-line of the combined electrode that makes with the embodiment of the invention 2.
Fig. 2 is the stereoscan photograph of the prepared polyaniline nano-line of the combined electrode that makes with the embodiment of the invention 18.
The scanning electricity border photo of the product that Fig. 3 obtains when preparing polyaniline nano-line with stainless steel electrode.
By Fig. 1 and Fig. 2 finding, adopt combination electrode of the present invention to prepare polyaniline nano-line, there is not the polyaniline particle, poly-Aniline nano line purity height. And as seen from Figure 3, adopt to have polyaniline in the polyaniline nano-line of stainless steel electrode preparation Grain.
Embodiment
Embodiment 1.
The polysulfones of 0.629g is dissolved in the N,N-dimethylacetamide of 6mL, obtains containing the N,N-dimethylacetamide solution of 10% polysulfones.At the stainless steel electrode surface coatings, the control thickness of liquid film is 5 μ m then.The stainless steel electrode that will scribble the N,N-dimethylacetamide solution of polysulfones afterwards rapidly is immersed in the precipitation bath (water) finishes inversion of phases, obtains polysulfones/stainless steel double composite electrode.With polysulfones/stainless steel double composite electrode is working electrode, is counter electrode with another sheet stainless steel, is under the condition of 1.5cm, with 0.25molL in spacing
-1Aniline and 1.00molL
-1Sulfuric acid is electrolytic solution, uses 1.80V bath voltage electrolytic polymerization 40min to obtain the product polyaniline nano-line, and polyaniline nano-line purity is 100%.
Embodiment 2.
The polysulfones of 1.415g is dissolved in the N,N-dimethylacetamide of 6mL, obtains containing the N,N-dimethylacetamide solution of 20% polysulfones.At the stainless steel electrode surface coatings, the control thickness of liquid film is 100 μ m then.The stainless steel electrode that will scribble the N,N-dimethylacetamide solution of polysulfones afterwards rapidly is immersed in the precipitation bath (water) finishes inversion of phases, obtains polysulfones/stainless steel double composite electrode.With polysulfones/stainless steel double composite electrode is working electrode, is counter electrode with another sheet stainless steel, is under the condition of 1.5cm, with 0.25molL in spacing
-1Aniline and 1.00molL
-1Sulfuric acid is electrolytic solution, uses 1.80V bath voltage electrolytic polymerization 40min to obtain the product polyaniline nano-line, and polyaniline nano-line purity is 100%.
Embodiment 3.
The polysulfones of 2.425g is dissolved in the N,N-dimethylacetamide of 6mL, obtains containing the N,N-dimethylacetamide solution of 30% polysulfones.At the stainless steel electrode surface coatings, the control thickness of liquid film is 150 μ m then.The stainless steel electrode that will scribble the N,N-dimethylacetamide solution of polysulfones afterwards rapidly is immersed in the precipitation bath (water) finishes inversion of phases, obtains polysulfones/stainless steel double composite electrode.With polysulfones/stainless steel double composite electrode is working electrode, is counter electrode with another sheet stainless steel, is under the condition of 1.5cm, with 0.25molL in spacing
-1Aniline and 1.00molL
-1Sulfuric acid is electrolytic solution, uses 1.80V bath voltage electrolytic polymerization 40min to obtain the product polyaniline nano-line, and polyaniline nano-line purity is 100%.
Embodiment 4.
The polysulfones of 0.192g is dissolved in the meta-cresol of 6mL, obtains containing the m-cresol solution of 3% polysulfones.At the stainless steel electrode surface coatings, the control thickness of liquid film is 100 μ m then.The stainless steel electrode that will scribble the m-cresol solution of polysulfones afterwards rapidly is immersed in the precipitation bath (water) finishes inversion of phases, obtains polysulfones/stainless steel double composite electrode.With polysulfones/stainless steel double composite electrode is working electrode, is counter electrode with another sheet stainless steel, is under the condition of 1.5cm, with 0.25molL in spacing
-1Aniline and 1.00molL
-1Sulfuric acid is electrolytic solution, uses 1.80V bath voltage electrolytic polymerization 40min to obtain the product polyaniline nano-line, and polyaniline nano-line purity is 100%.
Embodiment 5.
The polysulfones of 0.300g is dissolved in the N of 6mL, in the dinethylformamide, obtains containing the N of 5% polysulfones, dinethylformamide solution.At the stainless steel electrode surface coatings, the control thickness of liquid film is 100 μ m then.To scribble the N of polysulfones afterwards rapidly, the stainless steel electrode of dinethylformamide solution is immersed in the precipitation bath (water) and finishes inversion of phases, obtains polysulfones/stainless steel double composite electrode.With polysulfones/stainless steel double composite electrode is working electrode, is counter electrode with another sheet stainless steel, is under the condition of 1.5cm, with 0.25molL in spacing
-1Aniline and 1.00molL
-1Sulfuric acid is electrolytic solution, uses 1.80V bath voltage electrolytic polymerization 40min to obtain the product polyaniline nano-line, and polyaniline nano-line purity is 100%.
Embodiment 6.
The polysulfones of 0.731g is dissolved in the dimethyl sulfoxide (DMSO) of 6mL, obtains containing the dimethyl sulphoxide solution of 10% polysulfones.At the stainless steel electrode surface coatings, the control thickness of liquid film is 100 μ m then.The stainless steel electrode that will scribble the dimethyl sulphoxide solution of polysulfones afterwards rapidly is immersed in the precipitation bath (water) finishes inversion of phases, obtains polysulfones/stainless steel double composite electrode.With polysulfones/stainless steel double composite electrode is working electrode, is counter electrode with another sheet stainless steel, is under the condition of 1.5cm, with 0.25molL in spacing
-1Aniline and 1.00molL
-1Sulfuric acid is electrolytic solution, uses 1.80V bath voltage electrolytic polymerization 40min to obtain the product polyaniline nano-line, and polyaniline nano-line purity is 100%.
Embodiment 7.
The polysulfones of 1.086g is dissolved in the N-Methyl pyrrolidone of 6mL, obtains containing the N-Methyl pyrrolidone solution of 15% polysulfones.At the stainless steel electrode surface coatings, the control thickness of liquid film is 100 μ m then.The stainless steel electrode that will scribble the N-Methyl pyrrolidone solution of polysulfones afterwards rapidly is immersed in the precipitation bath (water) finishes inversion of phases, obtains polysulfones/stainless steel double composite electrode.With polysulfones/stainless steel double composite electrode is working electrode, is counter electrode with another sheet stainless steel, is under the condition of 1.5cm, with 0.25molL in spacing
-1Aniline and 1.00molL
-1Sulfuric acid is electrolytic solution, uses 1.80V bath voltage electrolytic polymerization 40min to obtain the product polyaniline nano-line, and polyaniline nano-line purity is 100%.
Embodiment 8.
The polyethersulfone of 0.629g is dissolved in the N,N-dimethylacetamide of 6mL, obtains containing the N,N-dimethylacetamide solution of 10% polyethersulfone.At the stainless steel electrode surface coatings, the control thickness of liquid film is 100 μ m then.The stainless steel electrode that will scribble the N,N-dimethylacetamide solution of polyethersulfone afterwards rapidly is immersed in the precipitation bath (water) finishes inversion of phases, obtains polyethersulfone/stainless steel double composite electrode.With polyethersulfone/stainless steel double composite electrode is working electrode, is counter electrode with another sheet stainless steel, is under the condition of 1.5cm, with 0.25molL in spacing
-1Aniline and 1.00molL
-1Sulfuric acid is electrolytic solution, uses 1.80V bath voltage electrolytic polymerization 40min to obtain the product polyaniline nano-line, and polyaniline nano-line purity is 100%.
Embodiment 9.
The polyimide of 0.629g is dissolved in the N,N-dimethylacetamide of 6mL, obtains containing the N,N-dimethylacetamide solution of 10% polyimide.At the stainless steel electrode surface coatings, the control thickness of liquid film is 100 μ m then.The stainless steel electrode that will scribble the N,N-dimethylacetamide solution of polyimide afterwards rapidly is immersed in the precipitation bath (water) finishes inversion of phases, obtains polyimide/stainless steel double composite electrode.With polyimide/stainless steel double composite electrode is working electrode, is counter electrode with another sheet stainless steel, is under the condition of 1.5cm, with 0.25molL in spacing
-1Aniline and 1.00molL
-1Sulfuric acid is electrolytic solution, uses 1.80V bath voltage electrolytic polymerization 40min to obtain the product polyaniline nano-line, and polyaniline nano-line purity is 100%.
Embodiment 10.
The polyetherimide of 0.629g is dissolved in the N,N-dimethylacetamide of 6mL, obtains containing the N,N-dimethylacetamide solution of 10% polyetherimide.At the stainless steel electrode surface coatings, the control thickness of liquid film is 100 μ m then.The stainless steel electrode that will scribble the N,N-dimethylacetamide solution of polyetherimide afterwards rapidly is immersed in the precipitation bath (water) finishes inversion of phases, obtains polyetherimide/stainless steel double composite electrode.With polyetherimide/stainless steel double composite electrode is working electrode, is counter electrode with another sheet stainless steel, is under the condition of 1.5cm, with 0.25molL in spacing
-1Aniline and 1.00molL
-1Sulfuric acid is electrolytic solution, uses 1.80V bath voltage electrolytic polymerization 40min to obtain the product polyaniline nano-line, and polyaniline nano-line purity is 100%.
Embodiment 11.
The polysulfones of 0.629g is dissolved in the N,N-dimethylacetamide of 6mL, obtains containing the N,N-dimethylacetamide solution of 10% polysulfones.Film at the titanium electrode surface then, the control thickness of liquid film is 100 μ m.The titanium electrode that will scribble the N,N-dimethylacetamide solution of polysulfones afterwards rapidly is immersed in the precipitation bath (water) finishes inversion of phases, obtains polysulfones/titanium combined electrode.With polysulfones/titanium combined electrode is working electrode, is counter electrode with another sheet stainless steel, is under the condition of 1.5cm, with 0.25molL in spacing
-1Aniline and 1.00molL
-1Sulfuric acid is electrolytic solution, uses 1.80V bath voltage electrolytic polymerization 40min to obtain the product polyaniline nano-line, and polyaniline nano-line purity is 100%.
Embodiment 12.
The polysulfones of 0.629g is dissolved in the N,N-dimethylacetamide of 6mL, obtains containing the N,N-dimethylacetamide solution of 10% polysulfones.At the nickel electrode surface coatings, the control thickness of liquid film is 100 μ m then.The nickel electrode that will scribble the N,N-dimethylacetamide solution of polysulfones afterwards rapidly is immersed in the precipitation bath (water) finishes inversion of phases, obtains polysulfones/nickel combined electrode.With polysulfones/nickel combined electrode is working electrode, is counter electrode with another sheet stainless steel, is under the condition of 1.5cm, with 0.25molL in spacing
-1Aniline and 1.00molL
-1Sulfuric acid is electrolytic solution, uses 1.80V bath voltage electrolytic polymerization 40min to obtain the product polyaniline nano-line, and polyaniline nano-line purity is 100%.
Embodiment 13.
The polysulfones of 0.629g is dissolved in the N,N-dimethylacetamide of 6mL, obtains containing the N,N-dimethylacetamide solution of 10% polysulfones.At the cobalt electrode surface coatings, the control thickness of liquid film is 100 μ m then.The cobalt electrode that will scribble the N,N-dimethylacetamide solution of polysulfones afterwards rapidly is immersed in the precipitation bath (water) finishes inversion of phases, obtains polysulfones/cobalt combined electrode.With polysulfones/cobalt combined electrode is working electrode, is counter electrode with another sheet stainless steel, is under the condition of 1.5cm, with 0.25molL in spacing
-1Aniline and 1.00molL
-1Sulfuric acid is electrolytic solution, uses 1.80V bath voltage electrolytic polymerization 40min to obtain the product polyaniline nano-line, and polyaniline nano-line purity is 100%.
Embodiment 14.
The polysulfones of 0.629g is dissolved in the N,N-dimethylacetamide of 6mL, obtains containing the N,N-dimethylacetamide solution of 10% polysulfones.Film at the aluminium electrode surface then, the control thickness of liquid film is 100 μ m.The aluminium electrode that will scribble the N,N-dimethylacetamide solution of polysulfones afterwards rapidly is immersed in the precipitation bath (water) finishes inversion of phases, obtains polysulfones/aluminium combined electrode.With polysulfones/aluminium combined electrode is working electrode, is counter electrode with another sheet stainless steel, is under the condition of 1.5cm, with 0.25molL in spacing
-1Aniline and 1.00molL
-1Sulfuric acid is electrolytic solution, uses 1.80V bath voltage electrolytic polymerization 40min to obtain the product polyaniline nano-line, and polyaniline nano-line purity is 100%.
Embodiment 15.
The polysulfones of 0.629g is dissolved in the N,N-dimethylacetamide of 6mL, obtains containing the N,N-dimethylacetamide solution of 10% polysulfones.At ferroelectric utmost point surface coatings, the control thickness of liquid film is 100 μ m then.The ferroelectric utmost point that will scribble the N,N-dimethylacetamide solution of polysulfones afterwards rapidly is immersed in the precipitation bath (water) finishes inversion of phases, obtains polysulfones/iron combined electrode.With polysulfones/iron combined electrode is working electrode, is counter electrode with another sheet stainless steel, is under the condition of 1.5cm, with 0.25molL in spacing
-1Aniline and 1.00molL
-1Sulfuric acid is electrolytic solution, uses 1.80V bath voltage electrolytic polymerization 40min to obtain the product polyaniline nano-line, and polyaniline nano-line purity is 100%.
Embodiment 16.
The polysulfones of 0.629g is dissolved in the N,N-dimethylacetamide of 6mL, obtains containing the N,N-dimethylacetamide solution of 10% polysulfones.At the copper electrode surface coatings, the control thickness of liquid film is 100 μ m then.The copper electrode that will scribble the N,N-dimethylacetamide solution of polysulfones afterwards rapidly is immersed in the precipitation bath (water) finishes inversion of phases, obtains polysulfones/copper combined electrode.With polysulfones/copper combined electrode is working electrode, is counter electrode with another sheet stainless steel, is under the condition of 1.5cm, with 0.25molL in spacing
-1Aniline and 1.00molL
-1Sulfuric acid is electrolytic solution, uses 1.80V bath voltage electrolytic polymerization 40min to obtain the product polyaniline nano-line, and polyaniline nano-line purity is 100%.
Embodiment 17.
The polysulfones of 0.629g is dissolved in the N,N-dimethylacetamide of 6mL, obtains containing the N,N-dimethylacetamide solution of 10% polysulfones.Film at graphite electrode surface then, the control thickness of liquid film is 100 μ m.The Graphite Electrodes that will scribble the N,N-dimethylacetamide solution of polysulfones afterwards rapidly is immersed in the precipitation bath (water) finishes inversion of phases, obtains polysulfones/graphite combined electrode.With polysulfones/graphite combined electrode is working electrode, is counter electrode with another sheet stainless steel, is under the condition of 1.5cm, with 0.25molL in spacing
-1Aniline and 1.00molL
-1Sulfuric acid is electrolytic solution, uses 1.80V bath voltage electrolytic polymerization 40min to obtain the product polyaniline nano-line, and polyaniline nano-line purity is 100%.
Embodiment 18.
The polysulfones of 0.629g is dissolved in the N,N-dimethylacetamide of 6mL, obtains containing the N,N-dimethylacetamide solution of 10% polysulfones.At the glassy carbon electrode surface coatings, the control thickness of liquid film is 100 μ m then.The glassy carbon electrode that will scribble the N,N-dimethylacetamide solution of polysulfones afterwards rapidly is immersed in the precipitation bath (water) finishes inversion of phases, obtains polysulfones/vitreous carbon combined electrode.With polysulfones/vitreous carbon combined electrode is working electrode, is counter electrode with another sheet stainless steel, is under the condition of 1.5cm, with 0.25molL in spacing
-1Aniline and 1.00molL
-1Sulfuric acid is electrolytic solution, uses 1.80V bath voltage electrolytic polymerization 40min to obtain the product polyaniline nano-line, and polyaniline nano-line purity is 100%.
Claims (2)
1. combined electrode for preparing high purity polyaniline nanometer line, this combined electrode is a matrix with stainless steel, titanium, nickel, cobalt, aluminium, iron, copper, graphite or vitreous carbon, it is characterized in that composite thickness is the film of polysulfones, polyethersulfone, polyimide or the polyetherimide of 5～150 μ m on the surface of matrix.
2. preparation method by the combined electrode of the described preparation high purity polyaniline nanometer line of claim 1, it is characterized in that comprising following process: according to quality percentage composition 3～30% with polysulfones, polyethersulfone, polyimide or polyetherimide are dissolved in N, the N-N,N-DIMETHYLACETAMIDE, N, dinethylformamide, N-Methyl pyrrolidone, in dimethyl sulfoxide (DMSO) or the meta-cresol, be mixed with the homogeneous transparent film-casting liquid, film-casting liquid is after standing and defoaming, evenly be coated in stainless steel, titanium, nickel, cobalt, aluminium, iron, copper, graphite or vitreous carbon surface, afterwards it is immersed in rapidly and finishes inversion of phases in the precipitation bath, obtain preparing the combined electrode of high purity polyaniline nanometer line.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101859731A (en) * | 2010-05-07 | 2010-10-13 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for manufacturing nano-wire piezoelectric device |
| CN101673831B (en) * | 2008-09-11 | 2011-09-21 | 元智大学 | Composite proton exchange membrane of acidic nanofiber/alkaline high polymer and preparation method thereof |
| CN102575007A (en) * | 2009-09-24 | 2012-07-11 | 塔塔钢铁荷兰科技有限责任公司 | Method of preparing a polyetherimide coating on a metallic substrate |
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| CN107833654A (en) * | 2017-11-07 | 2018-03-23 | 贵州电网有限责任公司 | A kind of corrosion-resistant compound ground wire of soft graphite for reducing pole tower ground resistance and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101673831B (en) * | 2008-09-11 | 2011-09-21 | 元智大学 | Composite proton exchange membrane of acidic nanofiber/alkaline high polymer and preparation method thereof |
| CN102575007A (en) * | 2009-09-24 | 2012-07-11 | 塔塔钢铁荷兰科技有限责任公司 | Method of preparing a polyetherimide coating on a metallic substrate |
| CN101859731A (en) * | 2010-05-07 | 2010-10-13 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for manufacturing nano-wire piezoelectric device |
| CN101859731B (en) * | 2010-05-07 | 2012-08-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for manufacturing nano-wire piezoelectric device |
| CN104928713A (en) * | 2015-06-17 | 2015-09-23 | 上海交通大学 | Preparation method and application of nickel-based hydrogen production electrode coated with conducting polymers |
| CN107833654A (en) * | 2017-11-07 | 2018-03-23 | 贵州电网有限责任公司 | A kind of corrosion-resistant compound ground wire of soft graphite for reducing pole tower ground resistance and preparation method thereof |
| CN107833654B (en) * | 2017-11-07 | 2020-07-28 | 贵州电网有限责任公司 | Flexible graphite composite grounding wire with corrosion resistance and reduced tower grounding resistance and preparation method thereof |
| CN110144611A (en) * | 2019-06-10 | 2019-08-20 | 河北工业大学 | A kind of Mg alloy surface corrosion-proof wear composite coating and preparation method thereof |
| CN110144611B (en) * | 2019-06-10 | 2021-10-22 | 河北工业大学 | Magnesium alloy surface corrosion-resistant wear-resistant composite coating and preparation method thereof |
| CN112993247A (en) * | 2019-12-13 | 2021-06-18 | 中国科学院大连化学物理研究所 | High-surface-capacity self-supporting hard carbon cathode and preparation and application thereof |
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| CN100595337C (en) | 2010-03-24 |
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