CN113388846A - Au @ Pt/CNT catalyst and preparation method and application thereof - Google Patents
Au @ Pt/CNT catalyst and preparation method and application thereof Download PDFInfo
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- CN113388846A CN113388846A CN202110657057.9A CN202110657057A CN113388846A CN 113388846 A CN113388846 A CN 113388846A CN 202110657057 A CN202110657057 A CN 202110657057A CN 113388846 A CN113388846 A CN 113388846A
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Abstract
The invention relates to the technical field of catalysts, and particularly relates to an Au @ Pt/CNT catalyst as well as a preparation method and application thereof. The invention discloses an Au @ Pt/CNT catalyst, which comprises: a carbon nanotube CNT and Au @ Pt alloy nanoparticles supported on the carbon nanotube CNT; the Au @ Pt alloy nanoparticles are of a core-shell structure, wherein a shell layer is Au, and a core layer is Pt. The noble metal shell layer of the Au @ Pt alloy nanoparticles with the core-shell structure is beneficial to realizing the high utilization efficiency of the catalyst; the addition of the carbon nano tube greatly improves the specific surface area of the catalyst and increases the number of active sites. According to experimental data, the Au @ Pt/CNT catalyst provided by the invention has good hydrogen evolution performance in an alkaline solution, and the Au @ Pt/CNT catalyst is irradiated by visible light at 10mA cm‑2The overpotential of (A) was up to 19mV, 25mV higher than commercial Pt/C.
Description
Technical Field
The invention relates to the technical field of catalysts, and particularly relates to an Au @ Pt/CNT catalyst as well as a preparation method and application thereof.
Background
Currently, Pt catalysts have good Hydrogen Evolution Reaction (HER) performance on the cathode side of a fuel cell, but the catalytic activity is reduced due to poisoning of the Pt catalyst by intermediate products (such as CO and-OH) generated during the reaction. And the alkaline HER activity of the Pt catalyst is obviously lower than that of the Pt catalyst under an acidic condition.
Disclosure of Invention
In view of the above, the invention provides an Au @ Pt/CNT catalyst, and a preparation method and application thereof.
The specific technical scheme is as follows:
the invention provides an Au @ Pt/CNT catalyst, which comprises: a carbon nanotube CNT and Au @ Pt alloy nanoparticles supported on the carbon nanotube CNT;
the Au @ Pt alloy nanoparticles are of a core-shell structure, wherein a shell layer is Au, and a core layer is Pt.
In the invention, the particle size of the Au @ Pt alloy nano particles is 5-30 nm.
In the invention, the thickness of the shell layer is 10-30 nm, preferably 20nm, and the particle size of the core layer is 5-20nm, preferably 10 nm.
In the present invention, the carbon nanotube CNT is a multi-walled carbon nanotube;
the wall width of the multi-wall carbon nano tube is 15-20nm, and the length of the multi-wall carbon nano tube is 5-6 mu m.
In the invention, the mass contents of Au, Pt and carbon nanotube CNT in the Au @ Pt/CNT catalyst are respectively 5-10%, 10-15% and 75-85%, preferably 7.86%, 13.02% and 79.12%.
The invention also provides a preparation method of the Au @ Pt/CNT catalyst, which comprises the following steps:
step 1: mixing a surfactant solution and a gold source solution, then adding a carbon nano tube, and then adding a first reducing agent for reaction;
step 2: and (3) adding a platinum source solution into the product obtained in the step (1), and adding a second reducing agent for reaction to obtain the Au @ Pt/CNT catalyst.
In the invention, in the step 1, the gold source forms an Au core through reduction reaction, and in the step 2, the platinum source forms a shell layer through reduction reaction.
The step 1 of the invention specifically comprises the following steps: uniformly mixing the gold source solution and the surface active solution, adding the carbon nano tube, carrying out ultrasonic treatment, and then dropwise adding a first reducing agent to react under the ice bath condition;
the gold source is HAuCl4·3H2O、NaAuCl4·2H2O、KAuCl4·2H2O and Au2Cl6One or more than two of the above;
the concentration of the gold source solution is 0.05-0.2 mol/L, preferably 0.1 mol/L;
the surfactant is one or more than two of cetyl trimethyl ammonium bromide, cetyl trimethyl ammonium chloride, sodium dodecyl benzene sulfonate and sodium dodecyl sulfate;
the mass ratio of the surfactant to the gold source is 5: 1-10: 1, preferably 7: 1;
the speed of ultrasonic treatment is 5000-10000 r/min, preferably 9000 r/min, and the time is 3-10 min, preferably 6 min;
the first reducing agent is sodium borohydride or potassium borohydride;
the mass ratio of the first reducing agent to the gold source is 1: 15-1: 5, preferably 1: 10;
the dropping rate of the first reducing agent is 1 drop/second;
the reaction temperature is 0-10 ℃, preferably 5 ℃, and the reaction time is 20-60 minutes, preferably 40 minutes.
In step 2 of the invention, the platinum source is H2PtCl6·6H2O and/or Pt (acac)2；
The concentration of the platinum source solution is 0.05-0.2 mol/L, preferably 0.1 mol/L;
the second reducing agent is one or more than two of L-ascorbic acid, sodium citrate and glucose; the sodium citrate in the second reducing agent can also be used as a surfactant.
The mass ratio of the second reducing agent to the platinum source is 1: 15-1: 5, and preferably 1: 9;
the reaction temperature is 90-110 ℃, the preferable temperature is 100 ℃, and the reaction time is 2-8 h, and the preferable time is 3.5 h.
In the invention, the mass ratio of the gold source to the platinum source to the carbon nanotube is 2:1: 3-1: 1:2, preferably 2:3: 5.
The reaction solvent in step 1 and step 2 of the invention is deionized water.
The invention also provides the application of the Au @ Pt/CNT catalyst or the Au @ Pt/CNT catalyst prepared by the preparation method in hydrogen evolution reaction.
In the present invention, the Au @ Pt/CNT catalyst is used in a PEM hydrogen fuel cell.
The application of the Au @ Pt/CNT catalyst in the hydrogen evolution reaction comprises the following steps:
dropwise adding the catalyst ink on a glassy carbon electrode polished by alumina powder to serve as a working electrode, taking graphite as a counter electrode and an Ag/AgCl electrode as a reference electrode, constructing a three-electrode system, and carrying out electrocatalytic reaction in an alkaline solution to precipitate hydrogen.
In the invention, in the electrocatalytic reaction process, a light source is preferably adopted to irradiate the working electrode, the light source is preferably a xenon lamp,the optical density is preferably 10.8-89.9 mW cm-2。
In the present invention, the alkaline solution is preferably a potassium hydroxide solution; the concentration of the alkaline solution is 1-2M, and 1M is preferred; the voltage of the electrocatalytic reaction is-0.7V to-1.5V, and the time of the electrocatalytic reaction is 3-10 minutes, preferably 6 minutes.
The preparation steps of the catalyst ink are as follows: the Au @ Pt/CNT catalyst was dispersed in a mixed solution of isopropanol, deionized water and Nafion.
In the invention, in the mixed solution, the volume ratio of isopropanol, deionized water and Nafion is 490: 490: 20; the concentration of the Au @ Pt/CNT catalyst in the mixed solution is 5-10 mg/mL, and preferably 5 mg/mL.
According to the technical scheme, the invention has the following advantages:
the invention provides an Au @ Pt/CNT catalyst, which comprises: a carbon nanotube CNT and Au @ Pt alloy nanoparticles supported on the carbon nanotube CNT; the Au @ Pt alloy nanoparticles are of a core-shell structure, wherein a shell layer is Au, and a core layer is Pt. The noble metal shell layer of the Au @ Pt alloy nanoparticles with the core-shell structure is beneficial to realizing the high utilization efficiency of the catalyst; the addition of the carbon nano tube greatly improves the specific surface area of the catalyst and increases the number of active sites. According to experimental data, the Au @ Pt/CNT catalyst provided by the invention has good hydrogen evolution performance in an alkaline solution, and the Au @ Pt/CNT catalyst is irradiated by visible light at 10mA cm-2The overpotential of (A) was up to 19mV, 25mV higher than commercial Pt/C.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
FIG. 1 is a transmission electron micrograph of an Au @ Pt/CNT catalyst prepared in example 1 of the present invention;
FIG. 2 is an X-ray photoelectron spectrum of the Au @ Pt/CNT catalyst of example 1 of the present invention;
FIG. 3 is an X-ray diffraction pattern of the Au @ Pt/CNT catalyst prepared in example 1 of the present invention;
FIG. 4 is an EDX linear scan element distribution plot of the Au @ Pt/CNT catalyst prepared in example 1 of the present invention;
FIG. 5 is a plot of linear sweep voltammograms of the Au @ Pt/CNT catalyst and commercial Pt/C prepared in example 1 of the present invention under different optical densities of visible light;
FIG. 6 is a linear sweep voltammogram of the Au @ Pt/CNT catalyst prepared in example 2 of the present invention;
FIG. 7 is a linear sweep voltammogram of the Au @ Pt/CNT catalyst prepared in example 3 of the present invention;
FIG. 8 is a graph of Au @ Pt obtained in comparative example 1 of the present invention0.5Linear sweep voltammograms of the CNT catalyst under different optical densities of visible light;
FIG. 9 is a graph of Au @ Pt obtained in comparative example 1 of the present invention0.5Linear sweep voltammogram of CNT catalyst under different wavelength illumination;
FIG. 10 is a linear sweep voltammogram of the Au @ Pt/CNT catalyst of comparative example 2 of the present invention;
FIG. 11 is a linear sweep voltammogram of the Au @ Pt/CNT catalyst of comparative example 3 of the present invention.
Detailed Description
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it should be apparent that the embodiments described below are only a part of the embodiments of the present invention, and not all 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.
Example 1
This example is the preparation of an Au @ Pt/CNT catalyst
1. 30mL of distilled water was added to a 100mL volumetric flask, and 4mL of cetyltrimethylammonium bromide CTAB at a concentration of 0.1mol/L and a total molar amount of 5.3 x 10 were further added-5mol of HAuCl4·3H2O (530. mu.L, concentration 0.1mol/L) solution, and mixing well. 103mg of multi-walled carbon nanotubes (CNT, wall width 15-20nm, length 5-6 μm) were added and sonicated for 1h (sonication rate 9000 revolutions/min). Slowly dripping 2mL of NaBH with the concentration of 0.06mol/L under ice bath4And (5) reacting for 40 min.
2. Adding the total mole number of 7.95 x 10-5mol of H2PtCl6·6H2O (620. mu.L, concentration 0.1mol/L) solution, 4mL of sodium citrate with concentration 0.2mol/L and 5mL of L-ascorbic acid solution with concentration 0.03mol/L were added and the mixture was maintained at 100 ℃ for 3.5 hours. The product was centrifuged at 9000 rpm for 6 minutes to give the product, washed with ethanol and deionized water, and then dried in a 60 ℃ dry box overnight to give the Au @ Pt/CNT catalyst.
FIG. 1 is a transmission electron microscope image of the Au @ Pt/CNT catalyst prepared in this example, wherein the stripes are multiwall carbon nanotubes, and the particles are Au @ Pt alloy nanoparticles with a particle size of 5-30 nm. As can be seen from the figure, the Au @ Pt nanoparticles are randomly dispersed on the multi-walled carbon nanotubes.
FIG. 2 is a full spectrum of X-ray photoelectron spectrum of Au @ Pt/CNT catalyst prepared in this example, and it can be seen from the figure that the catalyst contains five elements of Au, Pt, C and O, indicating that the precursor is reduced and the target catalyst is successfully prepared.
FIG. 3 shows the X-ray diffraction pattern of the Au @ Pt/CNT catalyst prepared in this example, and it can be seen from the figure that the Au @ Pt/CNT catalyst has a significant crystal form and good crystallinity. The mass contents of Au, Pt and carbon nano tube CNT in the Au @ Pt/CNT catalyst are respectively 7.86%, 13.02% and 79.12%.
FIG. 4 is an EDX linear scan element distribution plot of the Au @ Pt/CNT catalyst made in example 1 of this invention. It can be seen that the Au and Pt elements in the Au @ Pt/CNT catalyst are uniformly distributed, Au is mainly and intensively distributed in the middle of the Au @ Pt nano particles, and Pt is distributed on the surface layer of the Au @ Pt nano particles. The thickness of the shell layer is 20nm, and the particle size of the core layer is 10 nm.
Example 2
This example is the preparation of an Au @ Pt/CNT catalyst
This example differs from example 1 in that: the amount of carbon nanotubes used was different: the amount of carbon nanotubes used was 50 mg.
Example 3
Example 3 differs from example 1 in that: the Pt source adopts Pt (acac)2Replacement of H2PtCl6·6H2O。
Comparative example 1
In this example, Au @ Pt0.5Preparation of/CNT
This example differs from example 1 in that: the amount of Pt source added varied: h2PtCl6·6H2The amount of O added was 0.0265 mmol.
Comparative example 2
This comparative example is the preparation of an Au @ Pt/CNT catalyst
This example differs from example 1 in that: the amount of the aqueous reaction solvent solution was varied: the amount of distilled water used in step 1 was 60 ml.
Comparative example 3
Comparative example 2 differs from example 1 in that: the surfactant adopts CTAC to replace CTAB.
Test examples
HER performance was tested using a standard three-electrode system on an electrochemical workstation model CHI-750E and in 1M KOH solution. Graphite rods and Ag/AgCl (3M KCl) electrodes were used as counter and reference electrodes, respectively.
The glassy carbon electrode was polished with alumina and then sonicated continuously in 0.1M sulfuric acid, deionized water and ethanol for 10 min. The non-speckle electrode is then irradiated with ultraviolet light from a UV-BZD250-S light source to remove any organic contamination.
The catalyst ink was prepared as follows: first, 5mg of catalyst was dispersed in 1mL of a mixed solution of ethanol, deionized water and Nafion (0.5 wt.%), and sonication was performed for 1 minute to prepare a catalyst ink containing 5mg of catalyst, 490 μ L of ethanol, and 490 μ L of deionized water per 1mL of the catalyst ink. Then 10. mu.L of the suspension10 μ L of commercial Pt/C was respectively dropped into an L-type glassy carbon electrode (GCE, surface area of 0.125 cm) polished with alumina powder2) And naturally drying at room temperature. In a 1M KOH solution first between-0.7 and-1.5V (vs. Ag/AgCl) at 10mV s-1Is activated by cyclic voltammetric scanning (CV) followed by linear voltammetric (LSV) measurement. Example 1 and comparative example 1 the surface of a glassy carbon electrode (optical density of 10.8mW cm) was irradiated with a xenon lamp (CEL-HXF300) during the test-2、29.6mW cm-2、40.1mW cm-2、89.9mW cm-2) And the wavelength of the emitted light is changed by adding different kinds of filters (the wavelengths adopt 410nm, 450nm, 485nm, 530nm, 550nm, 565nm, 590nm and 705nm respectively). The potential measured for Ag/AgCl was converted to a potential relative to the Reversible Hydrogen Electrode (RHE) according to the equation E (vs. RHE) ═ E (vs. Ag/AgCl) +0.197V +0.059 pH.
FIG. 5 is a plot of linear sweep voltammograms of the Au @ Pt/CNT catalyst prepared in example 1 and commercial Pt/C under different optical densities of visible light. Under the condition of no illumination, the current density is 10mA cm-2When the overpotential of Au @ Pt/CNT is 37mV and the overpotential of commercial Pt/C is 44mV, the overpotential of Au @ Pt/CNT is obviously reduced along with the increase of optical density after illumination, and the lowest overpotential reaches 19 mV.
FIG. 6 is a linear sweep voltammogram of the Au @ Pt/CNT catalyst prepared in example 2 of the present invention. As shown in the figure, at a current density of 10mA cm-2The overpotential of Au @ Pt/CNT was 37 mV.
FIG. 7 is a linear sweep voltammogram of the Au @ Pt/CNT catalyst prepared in example 3 of the present invention. As shown in the figure, at a current density of 10mA cm-2The overpotential of Au @ Pt/CNT was 34 mV.
FIG. 8 is the Au @ Pt composition prepared in comparative example 10.5Linear sweep voltammogram of the/CNT catalyst under different optical density visible light. As shown, the current density was 10mA cm in the absence of light-2When, Au @ Pt0.5The overpotential of the/CNT was 58mV, the commercial Pt/C was 44mV, and after light irradiation, Au @ Pt0.5The overpotential of the/CNT is obviously reduced along with the increase of optical density, and the lowest overpotential reaches 46mV, it is clear from the figure that the content of Pt in the catalyst is reduced, and the influence trend of visible light illumination on HER overpotential is not changed.
FIG. 9 is the Au @ Pt prepared in comparative example 10.5Linear sweep voltammogram of the/CNT catalyst under different wavelengths of light. As shown, the current density was 10mA cm in the absence of light-2When, Au @ Pt0.5The overpotential of the/CNT is 58mV, the commercial Pt/C is 44mV, and after illumination of different wavelengths, the overpotential of the hydrogen evolution reaction is not changed remarkably and is respectively larger than the visible illumination density of 89.9mW cm-2The overpotential of time.
FIG. 10 is a linear sweep voltammogram of the Au @ Pt/CNT catalyst of comparative example 2 of the present invention. As shown in the figure, at a current density of 10mA cm-2The overpotential of Au @ Pt/CNT was 47 mV.
FIG. 11 is a linear sweep voltammogram of the Au @ Pt/CNT catalyst of comparative example 3 of the present invention. As shown in the figure, at a current density of 10mA cm-2The overpotential of Au @ Pt/CNT was 53 mV.
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. An Au @ Pt/CNT catalyst, comprising: a carbon nanotube CNT and Au @ Pt alloy nanoparticles supported on the carbon nanotube CNT;
the Au @ Pt alloy nanoparticles are of a core-shell structure, wherein a shell layer is Au, and a core layer is Pt.
2. The Au @ Pt/CNT catalyst of claim 1, wherein the Au @ Pt alloy nanoparticles have a particle size of 5-30 nm.
3. The Au @ Pt/CNT catalyst of claim 1, wherein the shell layer has a thickness of 10 to 30nm and the core layer has a particle size of 5 to 20 nm.
4. The Au @ Pt/CNT catalyst of claim 1, wherein the carbon nanotube CNT is a multi-walled carbon nanotube;
the wall width of the multi-wall carbon nano tube is 15-20nm, and the length of the multi-wall carbon nano tube is 5-6 mu m.
5. The Au @ Pt/CNT catalyst of claim 1, wherein the Au @ Pt/CNT catalyst comprises 5-10%, 10-15%, and 75-85% by mass of Au, Pt, and CNT, respectively.
6. A preparation method of an Au @ Pt/CNT catalyst is characterized by comprising the following steps:
step 1: mixing a surfactant solution and a gold source solution, then adding a carbon nano tube, and then adding a first reducing agent for reaction;
step 2: and (3) adding a platinum source solution into the product obtained in the step (1), and adding a second reducing agent for reaction to obtain the Au @ Pt/CNT catalyst.
7. The method according to claim 6, wherein the gold source is HAuCl4·3H2O、NaAuCl4·2H2O、KAuCl4·2H2O and Au2Cl6One or more than two of the above;
the platinum source is H2PtCl6·6H2O and/or Pt (acac)2。
8. The production method according to claim 6, wherein the first reducing agent is sodium borohydride or potassium borohydride;
the second reducing agent is one or more than two of L-ascorbic acid, sodium citrate and glucose;
the surfactant is one or more than two of cetyl trimethyl ammonium bromide, cetyl trimethyl ammonium chloride, sodium dodecyl benzene sulfonate and sodium dodecyl sulfate.
9. The preparation method according to claim 6, wherein the mass ratio of the surfactant to the gold source is 5:1 to 10: 1;
the mass ratio of the first reducing agent to the gold source is 1: 15-1: 5;
the mass ratio of the second reducing agent to the platinum source is 1: 15-1: 5;
the mass ratio of the gold source to the platinum source to the carbon nano tube is 2:1: 3-1: 1: 2.
10. Use of the Au @ Pt/CNT catalyst of any one of claims 1 to 5 or the Au @ Pt/CNT catalyst prepared by the preparation method of any one of claims 6 to 9 in a hydrogen evolution reaction.
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| CN102500365A (en) * | 2011-10-19 | 2012-06-20 | 华南理工大学 | Preparation method of catalyst with core-shell structure for low-temperature fuel cell |
| CN102723504A (en) * | 2012-05-09 | 2012-10-10 | 北京化工大学 | Multi-wall carbon nano-tube carried core-shell silver-platinum cathode catalyst and preparation method |
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| CN112864407A (en) * | 2021-01-12 | 2021-05-28 | 邵阳学院 | Ordered Pt-Au/C composite catalyst, preparation method thereof and application thereof in fuel cell |
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| CN102500365A (en) * | 2011-10-19 | 2012-06-20 | 华南理工大学 | Preparation method of catalyst with core-shell structure for low-temperature fuel cell |
| CN102723504A (en) * | 2012-05-09 | 2012-10-10 | 北京化工大学 | Multi-wall carbon nano-tube carried core-shell silver-platinum cathode catalyst and preparation method |
| CN110350204A (en) * | 2019-07-10 | 2019-10-18 | 广东工业大学 | It is the fuel-cell catalyst and the preparation method and application thereof of shell by core, platinum of gold nano cluster |
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| SUNG-FU HUNG ET AL: "Synergistic Effect of a Well-Defined Au@Pt Core-Shell Nanostructure toward Photocatalytic Hydrogen Generation: Interface Engineering to Improve Schottky Barrierand Hydrogen-Evolved Kinetics", 《CHEMCOMM》 * |
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