CN111439934A - Preparation method of porous graphene-glass composite electrode - Google Patents
Preparation method of porous graphene-glass composite electrode Download PDFInfo
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- CN111439934A CN111439934A CN202010186844.5A CN202010186844A CN111439934A CN 111439934 A CN111439934 A CN 111439934A CN 202010186844 A CN202010186844 A CN 202010186844A CN 111439934 A CN111439934 A CN 111439934A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
- C03C14/004—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of particles or flakes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C11/00—Multi-cellular glass ; Porous or hollow glass or glass particles
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2214/00—Nature of the non-vitreous component
- C03C2214/04—Particles; Flakes
Abstract
The invention provides a preparation method of a porous graphene-glass composite electrode, which comprises the following steps: putting powder obtained by uniformly mixing graphene powder and glass powder into a mold, pressing the powder into a block-shaped blank under a pressure condition to form a graphene-glass block-shaped intermediate product, wherein the mass mixing ratio of the graphene powder to the glass powder is 1: 0.1-1: 20; transferring the graphene-glass block intermediate product to a vacuum or high-temperature box furnace with protective atmosphere to calcine at a specified temperature; and naturally cooling to room temperature after sintering, and taking out to obtain the porous graphene-glass composite electrode material. Compare in traditional three-dimensional graphene materials and rely on the adhesive force of low contact condition inter-lamellar van der waals's power, micro-nano glass powder forms stronger adhesion with graphite alkene under the molten condition, can form fixed effect through fusing between the adjacent glass powder simultaneously, and glass powder only attaches a part graphite alkene surface, and other interfaces can participate in electrochemical reaction.
Description
Technical Field
The invention relates to the technical field of electrode preparation, in particular to a preparation method of a porous graphene-glass composite electrode.
Background
The electrochemical technology for treating wastewater is an important component of the advanced oxidation technology, a large amount of hydroxyl free radicals can be generated through technical routes such as electro-Fenton, electro-catalytic oxidation and the like, the hydroxyl free radicals are far higher than those generated by the traditional ozone direct oxidation, selectivity hardly exists, most organic matters can be reacted, and therefore the effect of degrading the organic matters is stable when the electrochemical technology is used for treating wastewater, and the electrochemical technology is an important development direction of the current advanced oxidation technology.
In electrocatalytic oxidation technology, since hydroxyl radicals are highly active and have short lifetimes, the reaction is usually concentrated near the electrodes, which places demands on the active surface area of the catalyst. In general, the higher the active surface area of the electrode, the greater the number of hydroxyl radicals that can be generated per unit time, and the higher the efficiency of catalytic degradation of organic matter. Whereas in electro-Fenton technology, a high active area cathode material is capable of reducing O2Generate more H2O2And thus there is also a pressing need for high active surface area electrode materials.
Currently, commonly used electrodes include metal electrodes, metal oxide electrodes, and carbon material electrodes. The carbon material electrode is paid attention by technicians because of its good chemical stability and low price. The carbon felt and the foam carbon material are more researched materials, the specific surface area of the carbon felt is relatively small, the preparation process of the foam carbon is complex, and the cost is high. Therefore, there is still a need to develop more porous carbon material electrodes which are easy to be applied industrially.
Graphene attracts much research interest because of its geometric specific surface area of 2600m 2/g. At present, much research and development work is carried out on porous graphene materials, including three-dimensional graphene, three-dimensional graphene composite materials and the like, but the problems of limited mechanical strength, easiness in powder removal and the like exist generally. Min Yongbo et al propose a hydrothermal binding template method to prepare a three-dimensional porous graphene material, but the graphene interlayer binding force in the material is weak, and the material is mainly maintained to be shaped by virtue of van der Waals force between graphene interlayers, so that the graphene material is easy to wear and shed powder in practical application. Therefore, a new method for processing porous graphene materials is required to be developed to obtain a high-strength and high-surface-area graphene electrode material.
Disclosure of Invention
The invention provides a preparation method of a porous graphene-glass composite electrode, which is simple in process, easy for industrial production and strong in binding force.
A preparation method of a porous graphene-glass composite electrode comprises the following steps:
A. putting powder obtained by uniformly mixing graphene powder and glass powder into a mold, pressing the powder into a block-shaped blank under a pressure condition to form a graphene-glass block-shaped intermediate product, wherein the mass mixing ratio of the graphene powder to the glass powder is 1: 0.1-1: 20;
B. transferring the graphene-glass block intermediate product to a vacuum or high-temperature box furnace with protective atmosphere to calcine at a specified temperature;
C. and naturally cooling to room temperature after sintering, and taking out to obtain the porous graphene-glass composite electrode material.
Further, the mass mixing ratio of the graphene powder to the glass powder is 1: 0.5-1: 5.
Further, the graphene powder is laminated in 1-20 layers, and the carbon content is more than 80%.
Further, the number of the graphene powder sheet layers is 1-10, and the carbon content is more than 90%.
Further, the pressure of the pressure forming in the die is 0.1MPa-5 MPa.
Further, the temperature of the high-temperature chamber furnace is 500-1000 ℃.
Further, the glass powder refers to common glass, potassium glass or borate glass, and the size of the glass powder is within the range of 100nm-30 um.
Further, the glass powder is low-softening-point lead-free glass with the size of 500nm-5 um.
By adopting the technical scheme of the invention, the invention has the following technical effects:
compare in traditional three-dimensional graphene materials and rely on the adhesive force of low contact condition inter-lamellar van der waals's power, micro-nano glass powder forms stronger adhesion with graphite alkene under the molten condition, can form fixed effect through fusing between the adjacent glass powder simultaneously, and glass powder only attaches a part graphite alkene surface, and other interfaces can participate in electrochemical reaction. The prepared electrode can be used as a basic electrode for electrocatalytic oxidation, a cathode electrode for electro-Fenton process and electrochemical reduction, has the advantages of high active area, corrosion resistance, good stability and the like, and can improve the degradation efficiency of treating pollutants by an electrochemical method, wherein the distance between conducting strips is in the micron and submicron level.
Drawings
Fig. 1 is a schematic view of a preparation process of a graphene-glass porous material.
Fig. 2 is a graph of electrode-based CV cycles.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The basic preparation process of the invention is as shown in fig. 1, mixing graphene powder and glass powder uniformly according to a certain proportion, putting the mixed powder into a mould, pressing into a block-shaped blank under a certain pressure, transferring the graphene-glass block-shaped intermediate product into a vacuum or high-temperature box furnace with protective atmosphere, calcining at a specified temperature, naturally cooling to room temperature after sintering, and taking out to obtain the porous graphene-glass composite electrode material. Compare in traditional three-dimensional graphene materials and rely on the adhesive force of low contact condition inter-lamellar van der waals's power, micro-nano glass powder forms stronger adhesion with graphite alkene under the molten condition, can form fixed effect through fusing between the adjacent glass powder simultaneously, and glass powder only attaches a part graphite alkene surface, and other interfaces can participate in electrochemical reaction.
The first embodiment is as follows:
10 g of graphene (provided by Oncung novel carbon material Hezhou Co., Ltd.) stripped by a physical method, wherein the number of layers is 1-10, D90 is 30 mu m, and the carbon content is 95%; 20 g of ordinary glass powder with 12500 meshes is adopted. Pouring the two powders into a vacuum mixer, mixing for 30 minutes, and discharging. Pouring the mixed powder into a cylindrical mold with the diameter of 10cm for three times, maintaining the pressure at 0.8MPa for 30 minutes, and taking out the composite board. Placing the mixture in a high-temperature sintering furnace, heating to 620 ℃ at a speed of 10 ℃/min under the protection of nitrogen, preserving heat for 1.5h, cooling to room temperature, and taking out. And (3) carrying out frosting treatment on the surface of the composite plate, removing the surface layer, and finally obtaining the graphene-glass composite electrode with a smooth surface. The porosity of the electrode was found to be 75.4% by the impregnation method, and the specific surface area of the material was found to be 36.5m2/g by the methylene blue adsorption method. The conductivity of the electrode material tested by the two-electrode method is 1380S/m. The electrode is used as a working electrode, Ag/AgCl is used as a reference electrode, a platinum sheet is used as a counter electrode, and a Cyclic Voltammetry (CV) is performed in a 1M sodium sulfate solution by a three-electrode method, and the effect is shown in figure 2, which shows that the material has a typical surface double-capacitor structure and a higher active area.
The second embodiment:
20 g of graphene (provided by Oncung novel carbon material Hezhou Co., Ltd.) peeled by a physical method, wherein the number of layers is 1-10, the D90 is 50um, and the carbon content is 85%; 4 g of 3000-mesh common glass powder is adopted. Pouring the two powders into a vacuum mixer, mixing for 30 minutes, and discharging. Pouring the mixed powder into a cylindrical mold with the diameter of 10cm in three times, maintaining the pressure at 0.2MPa for 30 minutes, and then taking out the composite sheet. Placing the mixture in a high-temperature sintering furnace, heating to 650 ℃ at a speed of 10 ℃/min under the protection of nitrogen, preserving heat for 2h, cooling to room temperature, and taking out. And (3) carrying out frosting treatment on the surface of the composite plate, removing the surface layer, and finally obtaining the graphene-glass composite electrode with a smooth surface. The porosity of the electrode was 81.5% by the impregnation method, and the specific surface area of the material measured by the methylene blue adsorption method was 48.5m 2/g. The conductivity of the electrode material tested by the two-electrode method is 3520S/m.
The third embodiment is as follows:
3 g of graphene (provided by Oncung novel carbon material Hezhou Co., Ltd.) stripped by a physical method, wherein the number of layers is 1-10, D90 is 50um, and the carbon content is 97%; 30 g of 5000-mesh common glass powder is adopted. Pouring the two powders into a vacuum mixer, mixing for 30 minutes, and discharging. The mixed powder was poured into a cylindrical mold having a diameter of 10cm in three times, and pressure was maintained at 5MPa for 30 minutes, and then the composite sheet was taken out. And (3) placing the mixture in a high-temperature sintering furnace, heating to 620 ℃ at a speed of 10 ℃/min under the protection of nitrogen, preserving heat for 2 hours, cooling to room temperature, and taking out. And (3) carrying out frosting treatment on the surface of the composite plate, removing the surface layer, and finally obtaining the graphene-glass composite electrode with a smooth surface. The porosity of the electrode was found to be 54.4% by the impregnation method, and the specific surface area of the material was found to be 9.6m2/g by the methylene blue adsorption method. The conductivity of the electrode material tested by the two-electrode method was 50.3S/m.
The fourth embodiment is as follows:
the method comprises the steps of adopting 8 g of graphene stripped by a physical method (provided by Naxing, a novel carbon material, Hezhou limited company), 1-10 layers of sheets of graphene, 30 mu M of D90 and 95 percent of carbon, adopting 18 g of 10000-mesh common glass powder, pouring the two kinds of powder into a vacuum mixer, mixing for 30 minutes, then adding 2 g of 3mm short-cut carbon fiber powder, mixing for 3 minutes, pouring the mixed powder into a cylindrical mold with the diameter of 10cm for three times, keeping the pressure for 30 minutes under the pressure of 1MPa, taking out a composite plate, placing the composite plate into a high-temperature sintering furnace, heating to 650 ℃ at the temperature of 10 ℃/min under the protection of nitrogen, keeping the temperature for 1 hour, cooling to room temperature, taking out the composite plate, carrying out frosting treatment on the surface of the composite plate, removing the surface layer, finally obtaining a graphene-glass composite electrode with carbon fibers with a flat surface, measuring the porosity of the electrode by an immersion method, using phenol as a simulated pollutant, carrying out electro-Fenton degradation experiment by adopting phenol as an electrode plate, wherein the electrode plate has a good effect, the following experiment, the concentration of 8 g of an initial power supply, a direct current of Na 3, a sample is used as an Fe6M 3/3, a sample cell, a sample, a pH value of an air flow rate of an electrolyte is used as an initial power supply, a sample is used for removing cell, a sample, a direct current of an electrolyte is used for removing cell, a sample cell is used for removing process of 10 mg, a.
The porosity of the porous graphene-glass composite material prepared by the invention is 50-85%, the specific surface area of the porous graphene-glass composite material is 10-100m2/g when the methylene blue adsorption method is used for testing, the conductivity of the porous graphene-glass composite material is 100S/m-5000S/m when the two-electrode method is used for testing, and the performances can be regulated and controlled by changing indexes such as raw materials of graphene powder, mass ratio of the graphene powder to glass powder, molding pressure and the like.
It should be understood that the parameters in the examples should not be construed as limiting the present invention, and should be construed as the protection scope of the present application as long as the method of the present invention is used to achieve the purpose of the present invention.
The mass mixing ratio of the graphene powder to the glass powder is 1: 0.1-1: within 20, preferably 1: 0.5-1: within 5. Including but not limited to the following parameters:
the graphene powder refers to a graphene-based material with 1-20 layers, a carbon content higher than 80%, an oxygen content not more than 20%, and a sheet diameter size of 1-500 um, wherein the number of layers is preferably 1-10, the carbon content is preferably > 90%, the oxygen content is preferably < 10%, and the sheet diameter is preferably 5-50 um. In addition, other carbon materials such as carbon fiber can be introduced as the composite material in the preparation process.
The glass powder refers to common glass (Na)2SiO3、CaSiO3、Na2O∙CaO∙6SiO2) Potassium glass (K)2O、CaO、SiO2) Borate glass (SiO)2、B2O3) Etc., the size distribution is in the range of 100nm-30um, the low softening point lead-free glass is preferred, and the size is preferably 500nm-5 um.
The pressure of the powder in the die for compression molding is within the range of 0.1MPa to 5MPa, preferably 0.3 MPa to 2 MPa.
The calcination temperature of the intermediate product is above the softening point temperature of the glass, typically 500-1000 deg.C, preferably 600-800 deg.C.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A preparation method of a porous graphene-glass composite electrode is characterized by comprising the following steps:
A. putting powder obtained by uniformly mixing graphene powder and glass powder into a mold, pressing the powder into a block-shaped blank under a pressure condition to form a graphene-glass block-shaped intermediate product, wherein the mass mixing ratio of the graphene powder to the glass powder is 1: 0.1-1: 20;
B. transferring the graphene-glass block intermediate product to a vacuum or high-temperature box furnace with protective atmosphere to calcine at a specified temperature;
C. and naturally cooling to room temperature after sintering, and taking out to obtain the porous graphene-glass composite electrode material.
2. The method for preparing the porous graphene-glass composite electrode according to claim 1, wherein the mass mixing ratio of the graphene powder to the glass powder is 1: 0.5-1: 5.
3. the method for preparing a porous graphene-glass composite electrode according to claim 1, wherein the graphene powder is layered in 1-20 layers and has a carbon content of more than 80%.
4. The method for preparing a porous graphene-glass composite electrode according to claim 1, wherein the number of graphene powder sheets is 1-10, and the carbon content is greater than 90%.
5. The method for preparing a porous graphene-glass composite electrode according to claim 1, wherein the pressure of the pressure molding in the mold is 0.1MPa-5 MPa.
6. The method of claim 1, wherein the temperature of the high-temperature chamber furnace is 500-1000 ℃.
7. The method for preparing a porous graphene-glass composite electrode according to claim 1, wherein the glass powder refers to common glass, potassium glass or borate glass, and the size is in the range of 100nm to 30 um.
8. The method for preparing the porous graphene-glass composite electrode according to claim 1, wherein the glass powder is low-softening-point lead-free glass with a size of 500nm-5 um.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3492197A (en) * | 1965-03-22 | 1970-01-27 | Dow Chemical Co | Novel compressed cohered graphite structures and method of preparing same |
| CN104829138A (en) * | 2015-04-22 | 2015-08-12 | 同济大学 | Carbon nanotube or graphene doped borate glass bracket and preparation method thereof |
| CN107611416A (en) * | 2017-08-15 | 2018-01-19 | 武汉科技大学 | A kind of Si-C composite material, its preparation method and application |
| CN108840328A (en) * | 2018-08-20 | 2018-11-20 | 苏州宏久航空防热材料科技有限公司 | A kind of preparation method of graphene modified glass piece |
-
2020
- 2020-03-17 CN CN202010186844.5A patent/CN111439934A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3492197A (en) * | 1965-03-22 | 1970-01-27 | Dow Chemical Co | Novel compressed cohered graphite structures and method of preparing same |
| CN104829138A (en) * | 2015-04-22 | 2015-08-12 | 同济大学 | Carbon nanotube or graphene doped borate glass bracket and preparation method thereof |
| CN107611416A (en) * | 2017-08-15 | 2018-01-19 | 武汉科技大学 | A kind of Si-C composite material, its preparation method and application |
| CN108840328A (en) * | 2018-08-20 | 2018-11-20 | 苏州宏久航空防热材料科技有限公司 | A kind of preparation method of graphene modified glass piece |
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Application publication date: 20200724 |