Method for preparing nano platinum/titanium dioxide nanotube electrode by pulse electrodeposition

A technology of pulse electrodeposition and titanium dioxide, applied in the direction of electrolytic coating, surface reaction electrolytic coating, coating, etc., can solve the problems of low current density, uneven deposition layer, high recombination rate of photogenerated carriers, and achieve Pt nanoparticles The effect of small size, excellent photocatalytic performance, and wide application prospects

Inactive Publication Date: 2011-11-23
BEIJING UNIV OF TECH
0 Cites 21 Cited by

AI-Extracted Technical Summary

Problems solved by technology

It also has certain defects: (1) The recombination rate of photogenerated carriers is high, and the efficiency of photocatalytic reaction is low
(2) Pure TiO 2 Nanotube arrays are wide-bandgap semiconductors, which are generally only excited by ultraviolet light and have no response in the visible region, so they have low utilization of sunlight (about 5%), which limits their applications.
(3) TiO 2 The barrier layer between the nanotube array and t...
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Abstract

The invention relates to a method for preparing a nano platinum/titanium dioxide nanotube electrode by pulse electrodeposition, belonging to the technical field of photoelectric catalysis. The existing Pt-TiO2/Ti nanotube electrodes are mostly prepared by a direct-current electrodeposition method, and have the defects of low current density, serious hydrogen evolution reaction and nonuniform surface deposit platinum. The preparation method of the Pt-TiO2/Ti nanotube electrode comprises the following steps: preparing a titanium dioxide nanotube array, which is regularly arranged and perpendicularly oriented, on a titanium sheet by an anodic oxidation method, and depositing Pt on the titanium dioxide nanotubes in a chloroplatinic acid/sulfuric acid solution by a pulse electrodeposition method to obtain the required electrode. No surfactant is needed in the deposition process, so the technique is simple, and the Pt nanoparticles are fine and have large specific area and excellent photoelectric catalysis property. The nano platinum/titanium dioxide nanotube electrode prepared by the method provided by the invention is applicable to the fields of fuel batteries, pollution treatment, catalysts and the like.

Application Domain

Technology Topic

Anodic oxidationPlatanic acid +15

Image

  • Method for preparing nano platinum/titanium dioxide nanotube electrode by pulse electrodeposition
  • Method for preparing nano platinum/titanium dioxide nanotube electrode by pulse electrodeposition
  • Method for preparing nano platinum/titanium dioxide nanotube electrode by pulse electrodeposition

Examples

  • Experimental program(3)

Example

[0022] Example 1. After surface treatment of 1.5mm*1.5mm TA1 titanium sheet, put 1g/L NH 4 HF 2 , 50g/LH 2 The ethylene glycol solution of O was anodized at a constant pressure of 10V and a temperature of 20°C for 1 hour, with constant mechanical stirring during the period. TiO 2 After the nanotubes are rinsed, they are put into an electrolyte containing 1.0~4.0mM chloroplatinic acid+0.5M sulfuric acid, and the pulse current density at the cathode is -70mA/cm 2 , The anode pulse current density is 70mA/cm 2 , The cathode pulse conduction time is 10ms, the anode pulse conduction time is 1ms, the turn-off time is 1s, and the electrodeposition time is 15min, that is, the electrode is prepared. The test of the prepared electrode to catalyze methanol is: put the electrode in 0.5M H 2 SO 4 +0.5M CH 3 In OH solution, the reference electrode is a saturated calomel electrode, the counter electrode is a platinum electrode, and the working electrode is Pt-TiO 2 /Ti nanotube electrode. Before the measurement, high-purity nitrogen was introduced into the solution to remove the oxygen dissolved in the solution, and the measurement was performed under the protection of a high-purity nitrogen stream. The scanning speed of cyclic voltammetry was 50mV/s. The measured CV curve is as figure 2.

Example

[0023] Example 2: After surface treatment of 1.5mm*1.5mm TA1 titanium sheet, put 5g/L NH 4 HF 2 , 200g/LH 2 The ethylene glycol solution of O was anodized at a constant pressure of 60V and a temperature of 30°C for 6 hours, during which time it was continuously stirred mechanically. TiO 2 After the nanotubes are rinsed, they are put into the electrolyte of 1.0~4.0mM chloroplatinic acid+0.5M sulfuric acid, and the pulse current density at the cathode is -10mA/cm 2 , The anode pulse current density is 10mA/cm 2 , The cathode pulse conduction time is 2ms, the anode pulse conduction time is 1ms, the turn-off time is 1s, and the electrodeposition time is 5min, that is, the electrode is prepared. The test of the prepared electrode to catalyze methanol is: put the electrode into 0.5MH 2 SO 4 +0.5M CH 3 In OH solution, the reference electrode is a saturated calomel electrode, the counter electrode is a platinum electrode, and the working electrode is Pt-TiO 2 /Ti nanotube electrode. Before the measurement, high-purity nitrogen was introduced into the solution to remove the oxygen dissolved in the solution, and the measurement was performed under the protection of a high-purity nitrogen stream. The scanning speed of cyclic voltammetry was 50mV/s. The measured CV curve is as image 3.

Example

[0024] Example 3: After surface treatment of 1.5mm*1.5mm TA1 titanium sheet, put 3g/L NH 4 HF 2 , 100g/LH 2 The ethylene glycol solution of O was anodized at a constant pressure of 30V and a temperature of 10°C for 2h, with constant mechanical stirring during the period. TiO 2 After the nanotubes are rinsed, they are put into the electrolyte of 1.0~4.0mM chloroplatinic acid+0.5M sulfuric acid, and the pulse current density at the cathode is -50mA/cm 2 , The anode pulse current density is 50mA/cm 2 , The cathode pulse conduction time is 6ms, the anode pulse conduction time is 1ms, the turn-off time is 1s, and the electrodeposition time is 25min, that is, the electrode is prepared. The test of the prepared electrode to catalyze methanol is: put the electrode in 0.5M H 2 SO 4 +0.5M CH 3 In OH solution, the reference electrode is a saturated calomel electrode, the counter electrode is a platinum electrode, and the working electrode is Pt-TiO 2 Nanotube electrode. Before the measurement, high-purity nitrogen was introduced into the solution to remove the oxygen dissolved in the solution, and the measurement was performed under the protection of a high-purity nitrogen stream. The scanning speed of cyclic voltammetry was 50mV/s. The measured CV curve is as Figure 4.
[0025] Example 4. In specific example 3, the pulse waveform becomes: cathode pulse current density is -90mA/cm 2 , The anode pulse current density is 90mA/cm 2 , The cathode pulse on time is 8ms, the anode pulse on time is 1ms, the off time is 1s, and the electrodeposition time is 15min. The measured CV curve is as Figure 5.
[0026] Example 5. After surface treatment of 1.5mm*1.5mm TA1 titanium sheet, put 3g/L NH 4 HF 2 , 100g/LH 2 The ethylene glycol solution of O was anodized at a constant pressure of 30V and a temperature of 10°C for 2h, with constant mechanical stirring during the period. TiO 2 After the nanotubes are rinsed, they are put into an electrolyte containing 1.0~4.0mM chloroplatinic acid+0.5M sulfuric acid, and the pulse current density at the cathode is -70mA/cm 2 , The anode pulse current density is 70mA/cm 2 , The cathode pulse conduction time is 10ms, the anode pulse conduction time is 1ms, the turn-off time is 1s, and the electrodeposition time is 15min, that is, the electrode is prepared. The test of the prepared electrode to catalyze methanol is: put the electrode in 0.5M H 2 SO 4 +0.5M CH 3 In OH solution, the reference electrode is a saturated calomel electrode, the counter electrode is a platinum electrode, and the working electrode is Pt-TiO 2 /Ti nanotube electrode. Before the measurement, high-purity nitrogen was introduced into the solution to remove the oxygen dissolved in the solution, and the measurement was performed under the protection of a high-purity nitrogen stream. The scanning speed of cyclic voltammetry was 50mV/s. The measured CV curve is as Image 6.
[0027] Table 1 Pulse waveform parameters of different preparation conditions (Examples 1-5)
[0028]
[0029] Figure 8 This is the XRD pattern of the nano-platinum/titanium dioxide nanotube electrode prepared in specific example 3 of the present invention. In the figure, 2θ of 39.861°, 46.440°, and 67.661° are the diffraction peaks of nano-Pt particles. It shows that the load is nano-Pt particles, and from the XRD diagram, it can be calculated that the particle size of the nano-Pt particles is about 11nm, indicating that the particles are fine.
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
Particle size11.0nm
tensileMPa
Particle sizePa
strength10

Description & Claims & Application Information

We can also present the details of the Description, Claims and Application information to help users get a comprehensive understanding of the technical details of the patent, such as background art, summary of invention, brief description of drawings, description of embodiments, and other original content. On the other hand, users can also determine the specific scope of protection of the technology through the list of claims; as well as understand the changes in the life cycle of the technology with the presentation of the patent timeline. Login to view more.
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Similar technology patents

Classification and recommendation of technical efficacy words

Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products