CN115084555B - Carbon-coated flower-like titanium oxide/titanium dioxide heterostructure supported ruthenium catalyst and preparation and application thereof - Google Patents
Carbon-coated flower-like titanium oxide/titanium dioxide heterostructure supported ruthenium catalyst and preparation and application thereof Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9041—Metals or alloys
- H01M4/905—Metals or alloys specially used in fuel cell operating at high temperature, e.g. SOFC
- H01M4/9058—Metals or alloys specially used in fuel cell operating at high temperature, e.g. SOFC of noble metals or noble-metal based alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8663—Selection of inactive substances as ingredients for catalytic active masses, e.g. binders, fillers
- H01M4/8673—Electrically conductive fillers
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention provides a titanium oxide/titanium dioxide heterostructure nanoflower for preparing carbon-coated supported ruthenium nano particles, a preparation method thereof and application thereof in hydrogen oxidation reaction of fuel cells, which is characterized in that glacial acetic acid and n-butyl titanate are subjected to hydrothermal reaction to generate TiO 2 Roasting the nanoflower precursor in argon atmosphere and ammonia atmosphere to obtain TiO/TiO 2 Heterostructure nanoflower, loading ruthenium trichloride on the surface of the heterostructure nanoflower, and polymerizing Dopamine (DA) into polydopamine in situ and coating TiO/TiO containing ruthenium trichloride on the surface of the polydopamine 2 The surface of the heterostructure nanoflower is subjected to hydrogen/argon reduction heat treatment to obtain the carbon-coated ruthenium nanoparticle-loaded titanium oxide/titanium dioxide heterostructure nanoflower Ru-TiO/TiO 2 @ NC. Ru-TiO/TiO obtained by the invention 2 The nano flower of the @ NC heterostructure has good conductivity, high stability and good catalytic activity and stability for the hydrogen oxidation reaction of the fuel cell. The preparation method has simple preparation process, easy scale-up production and good application prospect.
Description
Technical Field
The invention relates to a carbon-coated flower-shaped titanium oxide/titanium dioxide heterostructure supported ruthenium and a preparation method thereof, and application thereof in a fuel cell, and belongs to the technical field of new energy materials.
Background
The fuel cell directly converts chemical energy into electric energy through electrochemical reaction, has high energy conversion efficiency and environment-friendly property, and has wide development prospect. In recent years, attention has been paid to alkaline anion-exchange membrane fuel cells (AEMFCs) because their operating environments are alkaline, which makes possible the use of non-platinum catalysts, as compared to acidic proton-exchange membrane fuel cells (PEMFCs). However, the catalytic activity and stability of non-platinum catalysts to anodic oxidation (HOR) in alkaline media are both to be improved. In the aspect of catalytic activity, the performance of the non-platinum catalyst still cannot be compared with that of platinum, especially, the anode HOR dynamics is 2 to 3 orders of magnitude slower than that of the anode HOR dynamics under the alkaline condition, and the improvement of the catalytic activity of the non-platinum catalyst is important; in terms of catalyst stability, non-platinum metal active components are susceptible to electrochemical oxidation at the HOR potential to deactivate; in addition, the traditional fuel cell catalysts all adopt high specific surface active carbon as a carrier, so that the dispersity of active components is improved while ensuring good conductivity; however, under the condition that the active carbon carrier causes reverse polarity of the battery when the fuel battery is started or stopped or the load is changed, electrochemical oxidation corrosion can occur due to the too high potential of the anode, and the loaded metal active substances are further caused to fall off and agglomerate. Therefore, the development of a non-carbon support and catalyst with high activity, high stability and high specific surface area is critical to the development of fuel cells.
TiO 2 Good stability, is a carrier commonly used in thermocatalysis, but TiO 2 Poor conductivity and low specific surface area, severely limiting its application as a fuel cell catalyst support. When used as an electrocatalyst support, it is generally mixed with a conductive agent such as activated carbon, graphene, or the like, thereby improving the conductivity thereof. To improve TiO 2 The specific surface area of the material is improved by morphology regulation, such as preparing the material into a two-dimensional array or a three-dimensional lamellar structure. For example, the literature (Nature Catalysis,2020,3,454-462) reports a sea urchin-like TiO 2 Preparation method as electrocatalyst carrier for improving TiO 2 To the conductivity of the Ru/TiO to be prepared 2 Catalyst and conductive agent nitrogen doped graphene are mixed, and Ru/TiO is improved by means of graphene 2 Exhibits good HOR electrocatalytic activity and stability. However, the catalyst and the conductive agent are physically mixedThe mode is difficult to improve TiO 2 The conductivity of the body; in addition, tiO 2 Lower specific surface areas also make it difficult to support more catalytically active components, resulting in a catalytic activity that does not meet the application requirements. To solve this problem, patent (publication No. CN 112968181A) discloses an in-situ coating of high specific surface area TiO with a carbon layer 2 Strategy of nanoflower, tiO 2 The nano flower structure can improve the surface area of the nano flower structure, and the carbon layer is coated to enable TiO 2 The conductivity of the composite is improved, so that after the Pt nano catalyst is loaded, the carbon coats the TiO 2 The nanoflower supported Pt catalyst shows good catalytic activity and stability to oxygen reduction reaction. However, despite the TiO prepared by this method 2 Surface conductivity is improved by the carbon layer, but TiO 2 The conductivity of the bulk is not improved, and electrons are in TiO 2 The bulk phase transmission is difficult, and the conduction of electrons in bulk phase and interface is affected, so that the electrode reaction efficiency is affected.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a carbon-coated flower-shaped titanium oxide/titanium dioxide heterostructure with high conductivity, high activity and high stability and a preparation method thereof.
In order to achieve the above purpose, the invention is realized by adopting the following specific scheme:
(1) Dissolving n-butyl titanate in glacial acetic acid according to a certain proportion, and uniformly stirring to obtain a milky solution; heating the mixed solution to 100-180 ℃ in a hydrothermal kettle, preserving heat for 6-24 hours, centrifuging and washing the obtained product after the hydrothermal kettle is naturally cooled, and finally drying the product to obtain the titanium dioxide nanoflower precursor (p-TiO) 2 )；
Preferably, the volume ratio of the n-butyl titanate to the glacial acetic acid is 1:10-1:100.
(2) The flower-shaped titanium dioxide precursor obtained in the step (1) is treated in argon atmosphere at the temperature of 1-5 ℃ for min -1 Heating to 450 ℃ and preserving heat for 0.5-3 hours, and then heating to 1-5 ℃ for min under ammonia atmosphere -1 Heating upPreserving heat for 0.1-4 hr at 600-800 deg.C, naturally cooling to obtain titanium oxide/titanium dioxide nanoflower powder (TiO/TiO) 2 )；
(3) TiO/TiO obtained in the step (2) 2 Adding nanoflower into ethanol, ultrasonically forming suspension, adding ruthenium trichloride aqueous solution, stirring at room temperature for 1-8 hr, filtering and drying to obtain ruthenium precursor-loaded titanium oxide/titanium dioxide nanoflower powder (Ru-TiO/TiO) 2 )；
(4) Adding the titanium oxide/titanium dioxide nanoflower powder loaded with the ruthenium precursor obtained in the step (3) into a tris (hydroxymethyl) aminomethane-buffer solution (pH: 8.5) solution, performing ultrasonic treatment to form a suspension, adding a dopamine hydrochloride solution into the suspension under stirring, stirring at room temperature to polymerize dopamine and coat the surface of the titanium oxide/titanium dioxide nanoflower, and finally performing centrifugal washing and drying on the suspension to obtain polydopamine-coated ruthenium-loaded titanium oxide/titanium dioxide nanoflower;
(5) The sample obtained in the step (4) is treated in H 2 Heating to 350-700 ℃ in Ar atmosphere, and preserving heat for 0.5-6 hours to obtain the titanium oxide/titanium dioxide nanoflower (Ru-TiO/TiO) coated with the azacarbon and loaded with ruthenium nano particles 2 -NC)；
Preferably, H 2 The Ar atmosphere contains 1-5% hydrogen.
Compared with the prior art, the invention has the following advantages and effects:
compared with titanium dioxide, the flower-shaped titanium oxide/titanium dioxide heterostructure electrocatalyst carrier has good conductivity, and is an excellent electrocatalyst carrier. The carrier has good electrocatalytic activity and stability to the hydrogen oxidation reaction after loading Ru nano particles. The preparation method is simple in preparation process, suitable for large-scale production and has obvious application prospect.
Description of the drawings:
FIG. 1A scanning electron microscope picture of a sample prepared in example 1.
FIG. 2 is an X-ray diffraction pattern of the samples prepared in comparative example 1, example 1 and example 2.
Fig. 3 a transmission electron micrograph of the sample prepared in example 2.
Fig. 4 electrochemical impedance spectra of the samples prepared in comparative example 2 and example 2.
Fig. 5 is a linear scan curve of the sample vs HOR prepared in comparative example 2 and example 2.
FIG. 6 is a plot of the chronoamperometric current of the samples prepared in comparative example 2 and example 2 versus HOR.
The specific embodiment is as follows:
the invention is further illustrated below in connection with specific examples. It is also to be understood that the following examples are given solely for the purpose of illustration and are not to be construed as limitations upon the scope of the invention, since numerous insubstantial modifications and variations will now occur to those skilled in the art in light of the foregoing disclosure. The specific process parameters and the like described below are also merely examples of suitable ranges, i.e., one skilled in the art can make a suitable selection from the description herein and are not intended to be limited to the specific values described below.
Comparative example 1
2ml of n-butyl titanate is dissolved in 60ml of glacial acetic acid and stirred uniformly to obtain a milky white solution; heating the mixed solution to 140 ℃ in a hydrothermal kettle, and preserving heat for 12 hours; after the hydrothermal kettle is naturally cooled, centrifugally washing the obtained product with deionized water, and finally drying the product to obtain a white flower-like titanium dioxide precursor p-TiO 2 . Then the p-TiO is treated in air atmosphere 2 At 2 ℃ for min -1 Heating to 500 ℃ and preserving the temperature for 3 hours to obtain flower-like titanium dioxide powder (TiO) 2 )。
Comparative example 2
90mg of the flower-like titanium dioxide powder obtained in comparative example 1 was added to 30ml of ethanol and sonicated to form a suspension, and 2.72ml of an aqueous solution of ruthenium trichloride (Ru concentration: 3.67mg ml) was further added -1 ) Stirred at room temperature for 5 hours. Then rotary evaporating to remove the solvent to obtain the flower-shaped titanium dioxide Ru-TiO carrying ruthenium 2 And (3) powder. 90mg of dried Ru-TiO 2 The powder was added to 30ml of tris buffer (pH 8.5),uniformly dispersing by ultrasonic wave, then adding 90mg of dopamine hydrochloride, and stirring for 48 hours at room temperature. And then centrifugally washing and drying the obtained product to obtain the polydopamine-coated ruthenium-loaded flower-shaped titanium dioxide. Then at H 2 In Ar atmosphere at 5℃ for min -1 Heating to 500 ℃ at a heating rate and preserving heat for 2 hours to obtain the flower-shaped titanium dioxide Ru-TiO of the carbon-coated supported ruthenium nano particles 2 @NC。
Example 1
2ml of n-butyl titanate is dissolved in 60ml of glacial acetic acid and stirred uniformly to obtain a milky white solution; heating the mixed solution to 140 ℃ in a hydrothermal kettle, and preserving heat for 12 hours; after the hydrothermal kettle is naturally cooled, centrifugally washing the obtained product with deionized water, and finally drying the product to obtain a white flower-like titanium dioxide precursor p-TiO 2 . And then the titanium dioxide precursor p-TiO 2 Placing in a porcelain boat, placing in a tube furnace at one side close to the outlet gas, and firstly placing p-TiO in argon atmosphere 2 At 5 ℃ for min -1 Heating to 450 ℃ at a heating rate of 0.25 hours, and converting the atmosphere into ammonia gas at 3 ℃ for min -1 Heating to 800 ℃ at a heating rate of (2) and preserving heat for 2 hours, and naturally cooling to obtain flower-like titanium oxide/titanium dioxide powder (TiO/TiO) 2 )。
As can be seen from the scanning electron microscope photograph of the sample prepared in example 1 of fig. 1, the sample prepared in example 1 has a spherical nano flower structure. As can be seen from the X-ray diffraction patterns shown in FIG. 2, the X-ray diffraction patterns of comparative example 1 and example 1 are significantly different, the three strong peaks appear in comparative example 1 at diffraction angles of 25.28, 37.80 and 48.05 degrees, and the sample is anatase phase TiO as can be seen from the comparative X-ray diffraction pattern standard card 2 (JCPFD 21-1272); example 1 diffraction peaks appear at 37.33, 43.36 and 62.96 degrees diffraction angles, except at 25.28, 37.80 and 48.05 degrees diffraction angles, which corresponds to cubic phase TiO (JCPDF 08-0117) as seen from comparison with X-ray standard cards. As can be seen from this, the sample prepared in example 1 contains TiO 2 And TiO.
Example 2
Weighing the flower-like TiO/TiO obtained in example 1 2 90mg of powder is added into 30ml of ethanol, and the mixture is superA suspension was formed by shaking, and 2.72ml of an aqueous solution of ruthenium trichloride (Ru concentration: 3.67mg ml) was added -1 ) Stirred at room temperature for 5h. Then rotary evaporating to remove the solvent to obtain the flower-like titanium oxide/titanium dioxide Ru-TiO/TiO of the load ruthenium 2 And (3) powder. Then 90mg of dried Ru-TiO/TiO is taken 2 The powder was added to 30ml of tris buffer (pH 8.5) and dispersed by sonication, followed by the addition of 90mg of dopamine hydrochloride and stirring at room temperature for 48 hours. Then centrifugally washing and drying the mixture to obtain the polydopamine coated Ru-TiO/TiO 2 . Then in H2/Ar atmosphere at 5 ℃ for min -1 Heating to 500 ℃ at a heating rate, preserving heat for 2 hours, naturally cooling to obtain the carbon-coated ruthenium-loaded titanium oxide/titanium dioxide nanoflower Ru-TiO/TiO 2 @NC。
As can be seen from the high-power transmission electron micrograph of the sample obtained in example 2 in fig. 3, the substance having a lattice spacing of 0.209nm contained in the sample corresponds to the TiO (200) crystal face; substances adjacent thereto having a lattice spacing of 0.352nm correspond to TiO 2 (002) crystal plane; in addition, there are nanoparticles having a lattice spacing of 0.214nm, corresponding to Ru (002) crystal planes. By combining the X-ray diffraction pattern of example 2 in FIG. 2, it was confirmed that TiO/TiO was formed in the sample obtained in example 2 2 Heterostructures with Ru nanoparticles loaded on their surface.
Effect example 1
Samples obtained in comparative example 2 and example 2 were used as catalysts, coated on the surface of a glassy carbon electrode, used as working electrodes, graphite rods and mercury/mercury oxide electrodes were used as counter electrodes and reference electrodes, and 1M aqueous potassium hydroxide solution was used as electrolyte, and electrochemical impedance spectra of the samples were tested in a three-electrode system, and the results are shown in fig. 4. After fitting, the charge transport resistances of comparative example 2 and example 2 were 35.23 ohms and 16.54 ohms, respectively, and it can be seen that the example 2 sample was due to TiO/TiO 2 The formation of the heterostructure significantly reduces the charge transport resistance during the electrochemical reaction, thereby facilitating the electrocatalytic reaction.
Effect example 2
The samples obtained in comparative example 2 and example 2 were respectivelyThe catalyst is coated on the surface of a glassy carbon electrode, and is used as a working electrode, a graphite rod and a mercury/mercury oxide electrode are used as a counter electrode and a reference electrode, a hydrogen saturated 0.1M potassium hydroxide aqueous solution is used as an electrolyte, and the catalytic activity of a sample on hydrogen oxidation reaction is tested in a three-electrode system. The test conditions were: the electrolyte is 0.1M potassium hydroxide saturated by hydrogen, the rotating speed of the electrode is 2500rpm, and the sweeping speed is high: 10mV s -1 . As shown in FIG. 5, the HOR currents at 100mV VS.RHE for the samples obtained in comparative example 2 and example 2 were 2.46 and 0.24mA cm, respectively -2 Indicating that compared with Ru-TiO 2 NC, ru-TiO/TiO obtained in example 2 2 The catalytic activity of @ NC to HOR is obviously improved.
Effect example 3
The samples obtained in comparative example 2 and example 2 were coated on the surface of a glassy carbon electrode as a working electrode, a graphite rod and a mercury/mercury oxide electrode as a counter electrode and a reference electrode, and a hydrogen-saturated 0.1M aqueous potassium hydroxide solution as an electrolyte, respectively, and the catalytic activity of the samples on hydrogen oxidation reaction was tested in a three-electrode system. The catalytic stability of the samples of comparative example 2 and example 2 to HOR was tested separately in a three electrode system using chronoamperometry. The test conditions were: the electrolyte is hydrogen saturated 0.1M KOH, the rotating speed of the electrode is 400rpm, and the potential is set to be 0.1V RHE The test time was 3600 seconds. As shown in FIG. 6, ru-TiO/TiO is obtained in example 2 2 Both the activity and the stability of @ NC are obviously better than those of Ru-TiO obtained in comparative example 2 2 At NC and after testing, 68.7% of the initial current density was maintained, no significant decay occurred, indicating Ru-TiO/TiO 2 NC is a catalyst with good stability.
Claims (4)
1. The preparation method of the carbon-coated titanium oxide/titanium dioxide heterostructure nanoflower supported ruthenium nano catalyst is characterized by comprising the following steps of:
(1) Glacial acetic acid and n-butyl titanate generate flower-like TiO through hydrothermal reaction 2 A precursor;
(2) The flower-like TiO obtained in the step (1) is prepared 2 Precursor bodyFirstly, in argon atmosphere, heating to 450 ℃ from room temperature and preserving heat for a certain time, then in ammonia atmosphere, heating to 600-800 ℃ and preserving heat for a certain time, cooling to obtain titanium oxide/titanium dioxide TiO/TiO 2 Heterostructure nanoflower;
(3) TiO/TiO obtained in the step (2) 2 Uniformly mixing the nanoflower and the ruthenium trichloride solution, and drying to obtain a complex Ru-TiO/TiO loaded with metal salt ions 2 A nanoflower powder;
(4) Ru-TiO/TiO obtained in the step (3) 2 Adding nanometer flower powder and Dopamine (DA) into tris (hydroxymethyl) aminomethane-buffer solution to make polydopamine coated Ru-TiO/TiO 2 A nanoflower;
(5) Coating the polydopamine coated Ru-TiO/TiO obtained in the step (4) 2 Nanoflower H 2 Performing heat treatment in Ar atmosphere to obtain carbon-coated Ru nanoparticle-loaded titanium oxide/titanium dioxide heterostructure nanoflower Ru-TiO/TiO 2 @NC。
2. The method according to claim 1, wherein the TiO/TiO in the step (2) 2 The heterostructure nanoflower is made of flower-like TiO 2 The precursor is firstly heated to 450 ℃ in the argon atmosphere and kept for 0.5 to 3 hours, and then is treated for 1 to 5 ℃ for min in the ammonia atmosphere -1 Heating to 600-800 ℃ and preserving heat for 0.5-4 hours, and naturally cooling to obtain the product.
3. The catalyst according to claim 1, which is flower-like TiO/TiO 2 Heterostructure, surface loaded with Ru nanoparticles.
4. Use of the catalyst obtained by the preparation method according to claim 1 in a fuel cell hydrogen oxidation reaction.
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