CN113416070A - Ti4O7Method for preparing ceramic electrode - Google Patents

Ti4O7Method for preparing ceramic electrode Download PDF

Info

Publication number
CN113416070A
CN113416070A CN202110647847.9A CN202110647847A CN113416070A CN 113416070 A CN113416070 A CN 113416070A CN 202110647847 A CN202110647847 A CN 202110647847A CN 113416070 A CN113416070 A CN 113416070A
Authority
CN
China
Prior art keywords
ceramic electrode
titanium dioxide
preparation
substrate sheet
ceramic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202110647847.9A
Other languages
Chinese (zh)
Other versions
CN113416070B (en
Inventor
马红超
蒋泽琦
李文峰
付颖寰
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dalian Polytechnic University
Original Assignee
Dalian Polytechnic University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dalian Polytechnic University filed Critical Dalian Polytechnic University
Priority to CN202110647847.9A priority Critical patent/CN113416070B/en
Publication of CN113416070A publication Critical patent/CN113416070A/en
Application granted granted Critical
Publication of CN113416070B publication Critical patent/CN113416070B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/46Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104Devices therefor; Their operating or servicing
    • C02F1/46109Electrodes
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/467Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
    • C02F1/4672Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104Devices therefor; Their operating or servicing
    • C02F1/46109Electrodes
    • C02F2001/46133Electrodes characterised by the material
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/308Dyes; Colorants; Fluorescent agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/02Specific form of oxidant
    • C02F2305/023Reactive oxygen species, singlet oxygen, OH radical
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54Particle size related information
    • C04B2235/5418Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562Heating rate
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567Treatment time
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658Atmosphere during thermal treatment
    • C04B2235/6582Hydrogen containing atmosphere

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Hydrology & Water Resources (AREA)
  • Structural Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)
  • Hybrid Cells (AREA)
  • Catalysts (AREA)

Abstract

The present invention provides a Ti4O7The preparation method of the ceramic electrode comprises the following steps: s1 precursor anatase type TiO2Preparing a substrate sheet; s2 at H2Reducing at high temperature in atmosphere to obtain Ti4O7A ceramic electrode. Ti prepared by the method of the invention4O7Stable performance, high purityThe surface has no titanium oxide passivation layer, the reaction activity is high, the absorption effect in a visible light spectrum region is strong, the degradation rate of reactive brilliant blue KN-R of refractory organic pollutants under visible light reaches 75.28%, and the method is simple to operate, shortens the production period, reduces the production cost and is easy for large-scale preparation.

Description

Ti4O7Method for preparing ceramic electrode
Technical Field
The invention relates to the field of conductive materials, in particular to Ti4O7A method for preparing a ceramic electrode.
Background
In recent years, with social development, environmental pollution is more serious, and particularly, pollution to water bodies damages the ecological environment and even influences the production and life of people. Therefore, people pay more and more attention to solving the problem of water pollution. Ti4O7The ceramic electrode has TinO2n-1The titanium suboxide with the chemical general formula has unique physical, chemical and electrochemical properties, including excellent conductivity, wherein the conductivity is 1500S/cm and is far higher than that of graphite; strong chemical stability and strong acid and alkali resistance; has wide forbidden band width which can reach more than 3.0V, and has wide practical prospect in the field of degrading organic wastewater.
In the prior art, the titanium dioxide block material is mainly prepared by mixing titanium dioxide powder and metal titanium powder, and then reacting and sintering the mixture. Titanium suboxide is formed by the abstraction of a certain amount of oxygen from titanium dioxide by metallic titanium to form oxygen defects, the finer the original reactant particle size, the more uniform the fraction, and the faster the reaction rate. Titanium dioxide can be prepared into superfine powder by various methods, and because titanium metal is easy to react with oxygen when being prepared into fine powder, the superfine titanium powder is difficult to obtain, the time for preparing the block material in the prior art is as long as more than three days. Other methods for preparing titanium suboxide block materials, such as titanium hydride, require the addition of other auxiliary materials, so that the production process is complex, and the production cost is increased.
Disclosure of Invention
The invention provides a Ti4O7The preparation method of the ceramic electrode aims to solve the problems that in the prior art, other auxiliary materials are required to be added, the preparation is difficult and long, the production process is complex, and the production cost is high.
In order to achieve the above object, the present invention provides a Ti4O7The preparation method of the ceramic electrode comprises the following steps:
s1: fully mixing titanium dioxide and a binder uniformly according to the proportion of 8:2, grinding, and pressing to obtain a precursor substrate sheet;
s2: preparing the precursor substrate sheet in step S1, at H2And N2Heating to 1000-1150 ℃ at a heating rate of 5-10 ℃/min under an atmosphere, calcining for 3-5 h, and cooling to room temperature to obtain Ti4O7A ceramic electrode.
Preferably, the binder in step S1 includes polypropylene powder and polyvinyl butyral mixed in a ratio of 1: 1.
Preferably, the particle size of the powder after bonding and mixing is 5-10 μm.
Preferably, the titanium dioxide is in anatase form in step S1.
Preferably, the titanium dioxide particle size is 1-2 μm.
Preferably, said H in step S22And N2The volume ratio of (A) to (B) is 1-2: 1.
Preferably, the pressing pressure in step S1 is 50 to 100 MPa.
Preferably, the precursor substrate sheet comprises a square, a triangle, a rectangle, or a rectangle.
The invention has the beneficial effects that:
(1)Ti4O7is TinO2n-1The material with the best conductivity has a plurality of excellent properties such as sharp photoresponse capability, stronger acid corrosion resistance and better electrochemical stability, and the invention adopts the method of introducing H2The conductive ceramic electrode obtained by the thermal reduction technology is Ti4O7The surface of the product prepared by the method has no titanium oxide passivation layer, the reaction activity is higher, and the catalytic efficiency is 3 times of that of the common titanium dioxide anode material under the same experimental condition;
(2) ti prepared by the invention4O7The surface has a large amount of pores, compared with the same volume of non-porous and less-porous Ti in the prior art4O7The material has larger surface area, has larger contact area with degraded wastewater, is beneficial to the generation of OOH, OH and O, and has effect on organic pollutionThe water has stronger degradation effect compared with the Ti prepared by the prior art4O7The degradation rate of the conductive material to the dye wastewater is improved by about 12%;
(3) because the metallic titanium is relatively active and is easy to react with oxygen, the superfine titanium powder is difficult to obtain, so the time for preparing the block material in the prior art is more than three days; the invention has simple manufacturing process, reduces the cost and greatly shortens the Ti content4O7And (3) manufacturing period of the conductive ceramic electrode.
Drawings
FIG. 1 is a macroscopic view of the surface of a substrate sheet of anatase titanium dioxide precursor;
FIG. 2 is an XRD diffractogram of anatase titanium dioxide;
FIG. 3 is Ti4O7Macroscopic view of the surface of the ceramic electrode;
FIG. 4 is Ti4O7Scanning Electron Microscope (SEM) images of the ceramic electrode surface;
FIG. 5 is an enlarged view of a portion of FIG. 4;
FIG. 6 is Ti4O7(XRD) pattern of ceramic electrode;
FIG. 7 is Ti4O7The ceramic electrode is used as an anode material to degrade an active brilliant blue KN-R effect picture.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
In the following examples, unless otherwise specified, the experimental methods used were all conventional methods, the titanium dioxide powder used in the present invention was purchased from Shanghai chemical reagent company, China medicine (group), and the binder used was purchased from Meclin chemical reagent company, Inc.
Ti4O7A method for preparing a ceramic electrode, the method comprising the steps of:
s1: mixing titanium dioxide powder and a binder by using an agate mortar, fully grinding the powder according to the proportion of 8:2, uniformly mixing, putting the mixture into a mould, and pressing under the pressure of 50-100MPa to obtain the precursor substrate sheet.
The titanium dioxide powder is anatase type, and the particle size of the mixed powder is 1-2 mu m; the particle size of the mixed powder of the binder is 5-10 mu m.
The components of the binder are 1:1 Polypropylene Powder (PP) and polyvinyl butyral (PVB).
S2: and S1, the precursor substrate sheet is obtained, the precursor substrate sheet is arranged in a ceramic boat in an overhead mode, the ceramic boat is arranged in a tube furnace, and the tube furnace is closed. Introduction of H2And N2Discharging air from the mixed gas with the volume ratio of 1-2:1 for 20min, heating to 1000 ℃ at the heating rate of 10 ℃/min, calcining for 4h, and cooling to room temperature after heat preservation to obtain Ti4O7A ceramic electrode.
The precursor substrate sheet comprises a square, a triangle, a rectangle and a square.
Example 1
Ti4O7A method for preparing a ceramic electrode, the method comprising the steps of:
s1: and (3) fully and uniformly mixing titanium dioxide powder and binder powder according to the proportion of 8:2 by using an agate mortar, grinding, putting the mixture into a die, and pressing under the pressure of 60MPa to obtain the precursor substrate sheet. As shown in figure 1, the macroscopic view of the surface of the anatase titanium dioxide precursor substrate sheet is obtained by putting the mixture into a mold for pressing. FIG. 2 is a (XRD) diagram of anatase titanium dioxide, from which it can be seen that the peaks of the XRD curves of the samples correspond to PDF standard cards of anatase titanium dioxide, which can prove that the starting material used is anatase titanium dioxide.
The titanium dioxide powder is anatase type, and the particle size is 2 mu m; the powder particle size of the binder was 10 μm.
The components of the binder are 1:1 Polypropylene Powder (PP) and polyvinyl butyral (PVB).
S2: and S1, placing the precursor substrate sheet prepared in the step S1 in an overhead manner in a ceramic boat, placing the ceramic boat in a tube furnace, heating the ceramic boat to 1000 ℃ in the air at a heating rate of 10 ℃/min, calcining the ceramic boat for 4h, and cooling the ceramic boat to room temperature after heat preservation to obtain the titanium dioxide electrode. Placing the precursor substrate sheet on the ceramic boat in an overhead mannerIn the middle, the ceramic boat is placed in a tube furnace, and the tube furnace is closed. Introduction of H2And N2Discharging air from the mixed gas with the volume ratio of 1:1 for 20min, heating to 1000 ℃ at the heating rate of 10 ℃/min, calcining for 4h, cooling to room temperature after heat preservation to obtain Ti4O7A ceramic electrode. FIG. 3 shows Ti4O7Macroscopic view of the surface of the ceramic electrode. FIGS. 4 to 5 are each Ti4O7Scanning Electron Microscope (SEM) image of the surface of the ceramic electrode, from which Ti can be seen4O7The surface of the ceramic electrode has a large number of pores, has larger surface area compared with a material without pores and with less pores in the same volume, and has larger contact area with degraded wastewater, namely, more reaction sites in the same volume. FIG. 6 is Ti4O7(XRD) pattern of ceramic electrode, from which the peaks of XRD curve of sample and Ti can be seen4O7Corresponding to the PDF standard card, the material produced according to the experimental process can be proved to be Ti4O7
In this embodiment, the precursor substrate sheet is circular square, but is not limited to circular, and specifically includes square, triangle, and rectangle.
Example 2
Ti prepared in example 14O7Experiments of using the ceramic electrode and the titanium dioxide electrode as anode materials to degrade active brilliant blue KN-R:
the experimental device, namely the photocatalytic activity testing device, is composed of a light source, a magnetic stirrer, a photocatalytic reactor and a photocatalytic adjustable direct current stabilized power supply. The light source is a 175W xenon lamp, and is inserted into the photocatalytic reactor to ensure that light rays can directly irradiate on the working electrode; the magnetic stirrer is used for ensuring that the dye concentration is kept in a relatively uniform state; the photocatalytic reactor is a quartz backflow cooling sleeve, and the quartz material is adopted to ensure that ultraviolet light can effectively pass through the sleeve. And during the whole reaction period, continuously introducing condensed water into the sleeve to ensure that the temperature of the whole reaction system is within a certain range.
250mL of reactive brilliant blue KN-R solution with the concentration of 60mg/L is prepared, and 3.55g of anhydrousSodium sulfate (Na)2SO4) And as a supporting electrolyte, pouring the prepared reactive brilliant blue KN-R solution into a photocatalytic reactor to serve as a simulated dye. Ti prepared in example 14O7And (3) taking a ceramic electrode as a reaction anode, taking a platinum sheet as a reaction cathode, inserting the platinum sheet into the reactor, placing the platinum sheet in parallel, then opening condensed water and the stirrer, and taking 3mL of reactor liquid as a No. 1 sample by using a 5mL liquid transfer gun after the solution is completely mixed. The dark reaction is carried out for 30min without turning on the light source, so that the dye and the catalyst reach an adsorption-desorption equilibrium state. After the dark reaction was completed, 3mL of the reactor liquid was taken as sample # 2 by using a 5mL pipette. And turning on a light source to start the photoelectrocatalysis reaction, wherein the photoelectrocatalysis reaction lasts for 120 min. During the whole photoreaction process, 3mL of reactor liquid was taken out by a 5mL pipette at 20min intervals, and the reactor liquid was sequentially sequenced into a 3# sample and a 4# sample, … … 7# sample.
After the experiment, the absorbance of all samples at 592nm was measured with a UV759 ultraviolet spectrophotometer (Shanghai apparatus electric analyzer Co., Ltd.), the degradation rate of active brilliant blue KN-R was calculated according to formula 1, and the experimental results are shown in FIG. 7, which shows that the catalytic efficiency is 3 times that of white titanium dioxide as an anode material under the same experimental conditions.
D=(A0-At)/A0100% of formula 1
In the formula:
d-degradation rate,%;
A0-initial absorbance of reactive brilliant blue KN-R solution;
Atthe absorbance of the reactive brilliant blue KN-R at the time of degradation t.
Ti4O7The ceramic electrode is used as an anode material, and after the dark reaction stage is finished, the result shows that the ceramic electrode has no catalytic degradation effect on the active brilliant blue KN-R. In the photoreaction stage, the photocatalytic time is prolonged at any time, the degradation efficiency of the reactive brilliant blue KN-R is gradually improved, and after the reaction is finished, the degradation rate of the reactive brilliant blue KN-R reaches 75.28%. This is because Ti is used in photoelectric conversion4O7The valence band electrons of the ceramic electrode can be excited to the conduction band to form electrons and holes, and O adsorbed on the surface of the valence band electrons2And H2O interaction, generationThe free radical with strong oxidative decomposition capability is formed and used as an electrode material to efficiently catalyze and degrade the active brilliant blue KN-R.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.

Claims (8)

1. Ti4O7The preparation method of the ceramic electrode is characterized by comprising the following steps of:
s1: fully mixing titanium dioxide and a binder uniformly according to the proportion of 8:2, grinding, and pressing to obtain a precursor substrate sheet;
s2: preparing the precursor substrate sheet in step S1, at H2And N2Heating to 1000-1150 ℃ at a heating rate of 5-10 ℃/min under an atmosphere, calcining for 3-5 h, and cooling to room temperature to obtain Ti4O7A ceramic electrode.
2. The Ti of claim 14O7The method for preparing the ceramic electrode is characterized in that the binder in the step S1 comprises polypropylene powder and polyvinyl butyral which are mixed according to a ratio of 1: 1.
3. The Ti of claim 24O7The preparation method of the ceramic electrode is characterized in that the particle size of the powder after bonding and mixing is 5-10 mu m.
4. The Ti of claim 14O7The method for producing a ceramic electrode, wherein the titanium dioxide is in anatase form in step S1.
5. The Ti of claim 44O7The preparation method of the ceramic electrode is characterized in that the granularity of the titanium dioxide is 1-2 mu m.
6. The Ti of claim 14O7The method for producing a ceramic electrode, wherein H is the same as H in step S22And N2The volume ratio of (A) to (B) is 1-2: 1.
7. The Ti of claim 14O7The method for manufacturing a ceramic electrode is characterized in that the pressing pressure in step S1 is 50-100 MPa.
8. The Ti of claim 14O7The preparation method of the ceramic electrode is characterized in that the precursor substrate sheet comprises a square shape, a triangular shape, a rectangular shape and a round square shape.
CN202110647847.9A 2021-06-10 2021-06-10 Ti 4 O 7 Method for preparing ceramic electrode Active CN113416070B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110647847.9A CN113416070B (en) 2021-06-10 2021-06-10 Ti 4 O 7 Method for preparing ceramic electrode

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110647847.9A CN113416070B (en) 2021-06-10 2021-06-10 Ti 4 O 7 Method for preparing ceramic electrode

Publications (2)

Publication Number Publication Date
CN113416070A true CN113416070A (en) 2021-09-21
CN113416070B CN113416070B (en) 2022-11-25

Family

ID=77788375

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110647847.9A Active CN113416070B (en) 2021-06-10 2021-06-10 Ti 4 O 7 Method for preparing ceramic electrode

Country Status (1)

Country Link
CN (1) CN113416070B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115947614A (en) * 2022-06-09 2023-04-11 松山湖材料实验室 Titanium suboxide ceramic electrode, preparation method and application thereof and electrical equipment

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104016673A (en) * 2014-05-28 2014-09-03 长沙沃瑞新材料科技有限公司 Preparation technology for titanium-suboxide conductive ceramic electrode
CN106277042A (en) * 2016-08-29 2017-01-04 湖南科莱新材料有限公司 One prepares Ti4o7method
JP2017043521A (en) * 2015-08-28 2017-03-02 国立大学法人弘前大学 Ti4O7 PRODUCTION METHOD
WO2017043449A1 (en) * 2015-09-07 2017-03-16 国立大学法人東京大学 Titanium oxide agglomerate, method for producing titanium oxide agglomerate, titanium oxide powder, titanium oxide molded body, battery electrode catalyst, battery electrode conductive material, and microwave and millimeter wave dieletric
CN111847597A (en) * 2020-06-12 2020-10-30 武汉尚源新能环境有限公司 Preparation method and application of three-dimensional electrode material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104016673A (en) * 2014-05-28 2014-09-03 长沙沃瑞新材料科技有限公司 Preparation technology for titanium-suboxide conductive ceramic electrode
JP2017043521A (en) * 2015-08-28 2017-03-02 国立大学法人弘前大学 Ti4O7 PRODUCTION METHOD
WO2017043449A1 (en) * 2015-09-07 2017-03-16 国立大学法人東京大学 Titanium oxide agglomerate, method for producing titanium oxide agglomerate, titanium oxide powder, titanium oxide molded body, battery electrode catalyst, battery electrode conductive material, and microwave and millimeter wave dieletric
CN106277042A (en) * 2016-08-29 2017-01-04 湖南科莱新材料有限公司 One prepares Ti4o7method
CN111847597A (en) * 2020-06-12 2020-10-30 武汉尚源新能环境有限公司 Preparation method and application of three-dimensional electrode material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
田嫚等: "Zr还原法制备高纯度Ti_4O_7及其电催化处理2,4-二氨基甲苯废水", 《功能材料》 *
陈芳等: "陶瓷负载TiO_2光催化降解印染废水的研究", 《上海化工》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115947614A (en) * 2022-06-09 2023-04-11 松山湖材料实验室 Titanium suboxide ceramic electrode, preparation method and application thereof and electrical equipment
CN115947614B (en) * 2022-06-09 2024-05-03 松山湖材料实验室 Titanium dioxide ceramic electrode, preparation method and application thereof, and electric equipment

Also Published As

Publication number Publication date
CN113416070B (en) 2022-11-25

Similar Documents

Publication Publication Date Title
CN108736028B (en) Porous nitrogen-doped carbon-loaded cobalt nano material, preparation method and application thereof
Xu et al. Electrochemical synthesis of ammonia using a cell with a Nafion membrane and SmFe 0.7 Cu 0.3− x Ni x O 3 (x= 0− 0.3) cathode at atmospheric pressure and lower temperature
CN101549895B (en) Preparation method of carbon aerogel loaded titanium dioxide electrodes and application thereof
CN109590006B (en) Preparation method of triazine/heptazine homone heterojunction carbon nitride photocatalyst
CN111346642B (en) High-dispersion metal nanoparticle/biomass carbon composite electrode material and preparation method and application thereof
CN107195908B (en) A kind of foamed material composite cathode of microorganism electrolysis cell and preparation method thereof
CN108940255A (en) A kind of zinc oxide catalysis material and the preparation method and application thereof
CN109292827A (en) A kind of hollow caged ferroferric oxide nano granules and preparation method thereof
CN113416070B (en) Ti 4 O 7 Method for preparing ceramic electrode
CN104628031A (en) Preparation method of one-dimensional auto-doped titanium dioxide nanometer material and obtained product
CN111206259A (en) Preparation method of novel carbon black air diffusion cathode sheet capable of efficiently and stably producing hydrogen peroxide
CN113526623A (en) Preparation method of manganese oxide nano electrode and application of manganese oxide nano electrode in tetracycline hydrochloride wastewater treatment
CN114784303B (en) Preparation and application of rare earth-based organic framework anode material modified by copper polyphenol supermolecular network interface
CN106169632A (en) Visible light photocatalysis fuel cell based on membrane electrode and preparation method thereof
CN115947614B (en) Titanium dioxide ceramic electrode, preparation method and application thereof, and electric equipment
CN111952606A (en) Fe/HKUST-1 catalyst, and preparation method and application thereof
CN108821394B (en) Preparation method of iron (II) molybdate/graphene oxide catalytic electrode
CN111215070A (en) Preparation method of iron oxide photoelectric catalyst with exposed high-activity surface
CN114849689B (en) Heterojunction type composite photocatalytic material and preparation method thereof
CN114210315B (en) Preparation and application of rare earth erbium modified pollen carbon composite photocatalyst
CN107973367B (en) Fe-doped coated TiO2Process for degrading wastewater by using photocatalyst
CN109133259A (en) A method of utilizing light anode activation sulfuric acid salt treatment waste water and by-product hydrogen
CN108686644B (en) Scale-like Bi-based visible-light-driven photocatalyst, preparation method and application thereof
CN112973732A (en) In2O3/Zn0.8Cd0.2Preparation method of S photocatalytic nano reactor
CN105712446A (en) Preparation method of electrocatalytic anode material for treating ammonia-nitrogen wastewater

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant