CN113416070B - Ti 4 O 7 Method for preparing ceramic electrode - Google Patents
Ti 4 O 7 Method for preparing ceramic electrode Download PDFInfo
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Abstract
The present invention provides a Ti 4 O 7 The preparation method of the ceramic electrode comprises the following steps: s1, precursor anatase type TiO 2 Preparing a substrate sheet; s2 in H 2 Reducing at high temperature in atmosphere to obtain Ti 4 O 7 A ceramic electrode. Ti prepared by the method of the invention 4 O 7 The method has the advantages of stable performance, high purity, no titanium oxide passivation layer on the surface, high reaction activity, stronger absorption effect in a visible light spectrum region, and 75.28 percent of degradation rate of active brilliant blue KN-R of the organic pollutant which is difficult to degrade under visible light, is simple to operate, shortens the production period, reduces the production cost, and is easy for large-scale preparation.
Description
Technical Field
The invention relates to the field of conductive materials, in particular to Ti 4 O 7 A 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. Ti 4 O 7 The ceramic electrode has Ti n O 2n-1 The titanium suboxide with the chemical general formula has unique physical, chemical and electrochemical properties, including excellent conductivity of 1500S/cm and high conductivityOn 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 ultrafine powder by various methods, and because titanium metal is easy to react with oxygen when prepared into fine powder and is difficult to obtain ultrafine titanium powder, the time for preparing block materials in the prior art can be 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 Ti 4 O 7 The 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 Ti 4 O 7 The 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;
s2: the precursor base sheet prepared in the step S1 is subjected to a treatment in the presence of hydrogen 2 And N 2 Heating to 1000-1150 ℃ at a heating rate of 5-10 ℃/min under the atmosphere, calcining for 3-5 h, and cooling to room temperature to obtain Ti 4 O 7 A ceramic electrode.
Preferably, the binder in step S1 comprises polypropylene powder and polyvinyl butyral mixed in a ratio of 1.
Preferably, the particle size of the powder after bonding and mixing is 5-10 μm.
Preferably, the titanium dioxide in step S1 is in anatase form.
Preferably, the titanium dioxide particle size is 1-2 μm.
Preferably, said H in step S2 2 And N 2 The volume ratio of (A) to (B) is 1-2.
Preferably, the pressing pressure in step S1 is 50 to 100MPa.
Preferably, the precursor substrate sheet comprises a square, a triangle, a rectangle, or a rectangle.
The invention has the beneficial effects that:
(1)Ti 4 O 7 is Ti n O 2n－1 The material with the best middle conductivity has a plurality of excellent properties such as sharp photoresponse capability, stronger acid corrosion resistance and better electrochemical stability, and H is introduced into the material 2 The conductive ceramic electrode obtained by the thermal reduction technology is Ti 4 O 7 The 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 invention 4 O 7 The surface has a large amount of pores, compared with the same volume of non-porous and less-porous Ti in the prior art 4 O 7 The material has larger surface area, larger contact area with degraded wastewater, is beneficial to the generation of OOH, OH and O, has stronger degradation effect on organic sewage, and is compared with Ti prepared by the prior art 4 O 7 The 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 content 4 O 7 And (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 Ti 4 O 7 Macroscopic view of the surface of the ceramic electrode;
FIG. 4 is Ti 4 O 7 Scanning Electron Microscope (SEM) images of the ceramic electrode surfaces;
FIG. 5 is an enlarged view of a portion of FIG. 4;
FIG. 6 is Ti 4 O 7 (XRD) pattern of ceramic electrode;
FIG. 7 is Ti 4 O 7 The 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.
Ti 4 O 7 A method for preparing a ceramic electrode, the method comprising the steps of:
s1: and (3) mixing titanium dioxide powder and the binder by using an agate mortar, fully grinding the powder according to the proportion of 8.
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.
S2: and (3) preparing a precursor substrate sheet in the step (S1), placing the precursor substrate sheet in a ceramic boat in an overhead manner, placing the ceramic boat in a tube furnace, and closing the tube furnace. Introduction of H 2 And N 2 Discharging air for 20min from mixed gas with the volume ratio of 1-2 and 1, heating to 1000 ℃ at the heating rate of 10 ℃/min, calcining for 4h, and cooling to room temperature after heat preservation to obtain Ti 4 O 7 A ceramic electrode.
The precursor substrate sheet comprises a square, a triangle, a rectangle and a square.
Example 1
Ti 4 O 7 A 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. 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 granularity is 2 mu m; the powder particle size of the binder was 10 μm.
The components of the binder are 1.
S2: and (2) 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. And (3) placing the precursor substrate sheet in a ceramic boat in an overhead manner, placing the ceramic boat in a tube furnace, and closing the tube furnace. Introduction of H 2 And N 2 Discharging air from mixed gas with volume ratio of 1 4 O 7 A ceramic electrode. FIG. 3 shows Ti 4 O 7 Macroscopic view of the surface of the ceramic electrode. FIGS. 4 to 5 are Ti 4 O 7 Scanning Electron Microscope (SEM) image of the surface of the ceramic electrode, from which Ti can be seen 4 O 7 The ceramic electrode surface has a large amount of pores, has larger surface area compared with the same volume of non-porous and less-porous material, has larger contact area with degraded wastewater, and means that the ceramic electrode surface has more opposite pores under the same volumeThe stress site. FIG. 6 is Ti 4 O 7 (XRD) pattern of ceramic electrode, from which the peaks of XRD curve of sample and Ti can be seen 4 O 7 Corresponding to the PDF standard card, the material produced according to the experimental process can be proved to be Ti 4 O 7 。
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 1 4 O 7 Experiments 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 four parts, namely a light source, a magnetic stirrer, a photocatalytic reactor and a photocatalytic adjustable direct current stabilized voltage 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, and ensuring the temperature of the whole reaction system within a certain range.
250mL of reactive brilliant blue KN-R solution with the concentration of 60mg/L is prepared, and 3.55g of anhydrous sodium sulfate (Na) is added into the solution 2 SO 4 ) 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 1 4 O 7 And (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. Dark reaction is carried out for 30min without turning on a 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 120min. During the whole photoreaction process, the material is used for every 20min for 5mThe L pipette gun takes 3mL of reactor liquid and sorts the reactor liquid into 3# sample, 4# sample \8230: \8230and7 # sample in sequence.
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＝(A 0 -A t )/A 0 *100% of formula 1
In the formula:
d-degradation rate,%;
A 0 -initial absorbance of reactive brilliant blue KN-R solution;
A t the absorbance of the reactive brilliant blue KN-R at the time of degradation t.
Ti 4 O 7 The 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 percent. This is because Ti is used in photoelectric conversion 4 O 7 The 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 electrons 2 And H 2 And (4) generating free radicals with strong oxidative decomposition capacity by the interaction of O, and efficiently catalyzing and degrading the active brilliant blue KN-R by using the free radicals as electrode materials.
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 (7)
1. Ti 4 O 7 The 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: the precursor base sheet prepared in the step S1 is subjected to a treatment in the presence of hydrogen 2 And N 2 Heating to 1000-1150 ℃ at a heating rate of 5-10 ℃/min under the atmosphere, calcining for 3-5h, and cooling to room temperature to obtain Ti 4 O 7 A ceramic electrode;
the adhesive in the step S1 comprises polypropylene powder and polyvinyl butyral which are mixed according to the ratio of 1: 1.
2. The Ti of claim 1 4 O 7 The 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.
3. The Ti of claim 1 4 O 7 The method for producing a ceramic electrode is characterized in that the titanium dioxide in step S1 is in anatase form.
4. The Ti of claim 1 4 O 7 The preparation method of the ceramic electrode is characterized in that the granularity of the titanium dioxide is 1-2 mu m.
5. The Ti of claim 1 4 O 7 The method for preparing the ceramic electrode is characterized in that H is used in the step S2 2 And N 2 The volume ratio of (A) to (B) is 1-2:1.
6. The Ti of claim 1 4 O 7 The preparation method of the ceramic electrode is characterized in that the pressing pressure in the step S1 is 50-100MPa.
7. The Ti of claim 1 4 O 7 The preparation method of the ceramic electrode is characterized in that the precursor substrate sheet comprises a square shape, a triangular shape and a rectangular shape.
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| 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 |
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