Preparation method of ruthenium@ruthenium dioxide core-shell nanospheres containing tensile strain for acidic oxygen production electrocatalyst

An electrocatalyst, tensile strain technology, applied in the direction of catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, chemical instruments and methods, etc., to achieve the effects of easy control, convenient operation, and increased intrinsic activity

Active Publication Date: 2020-04-28
TIANJIN UNIV
6 Cites 3 Cited by

AI-Extracted Technical Summary

Problems solved by technology

[0005] In view of the fact that there is no way to adjust Ru without introducing heteroatoms 4+ The electronic structure of the active site and then the problem of modifying the ruthenium dioxide-based catalyst,...
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Abstract

The invention relates to a preparation method of ruthenium@ruthenium dioxide core-shell nanospheres containing tensile strain for an acidic oxygen production electrocatalyst. Ruthenium dioxide powderis placed in ultrapure water to be subjected to ultrasonic dispersion to obtain turbid liquid without sediment; the turbid liquid is continuously stirred at room temperature, and the turbid liquid isirradiated by using nanosecond parallel pulse laser to obtain a black solution; the black solution is placed in a refrigerator to be frozen into a solid, then the frozen solid is placed in a freeze dryer to be freeze-dried, and the ruthenium@ruthenium dioxide core-shell nanospheres containing strain are obtained. According to the prepared sample, the overpotential at 10 mA cm <-2 > is only 191 mVand is reduced by 100 mV or above compared with commercial ruthenium dioxide, and the ruthenium@ruthenium dioxide core-shell nanospheres are a ruthenium-based catalyst which is optimal in performanceat present and does not introduce other atoms. The preparation method is simple in process, convenient to operate and easy to control, and a useful way is provided for designing and synthesizing an efficient electrocatalyst.

Application Domain

Catalyst activation/preparationMetal/metal-oxides/metal-hydroxide catalysts +1

Technology Topic

Ruthenium dioxideFreeze dry +8

Image

  • Preparation method of ruthenium@ruthenium dioxide core-shell nanospheres containing tensile strain for acidic oxygen production electrocatalyst
  • Preparation method of ruthenium@ruthenium dioxide core-shell nanospheres containing tensile strain for acidic oxygen production electrocatalyst
  • Preparation method of ruthenium@ruthenium dioxide core-shell nanospheres containing tensile strain for acidic oxygen production electrocatalyst

Examples

  • Experimental program(4)

Example Embodiment

[0026] Example 1:
[0027] (1) Place the commercial ruthenium dioxide powder in ultrapure water and ultrasonically disperse it to a suspension without precipitation at a concentration of 1.0 mg/mL;
[0028] (2) The suspension prepared in step (1) was continuously stirred at room temperature at a stirring speed of 400 rpm, and irradiated with nanosecond parallel pulse laser for 20 minutes, and the laser energy was 518mJ , Get a black solution;
[0029] (3) Put the black solution obtained in step (2) into a freezer at -4°C and freeze it into a solid, then place the frozen solid in a freeze dryer and freeze-dry it at -50°C and 50Pa to obtain a strain-containing Ruthenium@Ruthenium dioxide core-shell nanospheres.
[0030] The process device diagram for preparing strained ruthenium@ruthenium dioxide core-shell nanospheres by nanosecond laser irradiation figure 1 Shown, with RuO 2 The water dispersion container is placed on a magnetic stirrer and irradiated with pulsed laser parallel light.
[0031] Strained ruthenium@ruthenium dioxide core-shell nanospheres (Ru@RuO) prepared by nanosecond parallel pulse laser (20min, 518mJ) irradiation 2 -L) morphology and phase characterization such as figure 2 Shown. figure 2 (a) XRD pattern description Ru@RuO 2 -L is by RuO 2 It is composed of two phases with Ru and has good crystallinity. figure 2 (b) It shows that the size of the nanospheres obtained after laser irradiation is uniform, and the statistical distribution of the particle size in the illustration shows that the size of the nanospheres is smaller, about 21.7nm. figure 2 (c) and (d) are Ru@RuO 2 -L and RuO 2 -C's high magnification transmission electron microscope image, clearly showing Ru@RuO 2 -L core-shell structure, the shell thickness is 2-3nm, and the lattice of the shell corresponds to RuO 2 (PDF#88-0322) (110) crystal plane, the lattice spacing is 0.338nm, greater than figure 2 (d) Medium RuO 2 The 0.318nm of -C(110) crystal plane shows that in RuO 2 The presence of tensile strain in the shell.
[0032] To Ru@RuO 2 -L strain and Ru valence state characterization such as image 3 Shown. by image 3 (a) R space spectrum, RuO 2 -C in The peak at is attributed to the Ru-O bond, and Ru@RuO 2 The length of the Ru-O bond in -L is slightly extended to Show in Ru@RuO 2 -L sample, Ru-O bond stretched by 6%, namely RuO 2 There is 6% tensile strain in the shell; image 3 (b) Show, and RuO 2 -C compared to Ru@RuO 2 -L of Ru 4+ The peak of is shifted to higher binding energy; image 3 (c) Show, and RuO 2 -C compared to Ru@RuO 2 -L of M 2 , M 3 Peak shift to higher energy loss, XPS and EELS results together explain Ru@RuO 2 -L in Ru 4+ The site charge density decreases and Ru is produced X+ (4 <5).
[0033] Ru@RuO 2 -L’s acidic electrocatalytic oxygen production performance Figure 4 Shown. 10mAcm -2 The over-potential is 191mV, which is better than RuO 2 -C reduced by more than 100 mV, with a lower Tafel slope (48.90mV dec -1 ) And smaller interface transfer resistance. At the same time, the area specific activity and mass specific activity are significantly improved, and the mass specific activity is better than RuO 2 -C increased by 18 times.

Example Embodiment

[0034] Example 2:
[0035] (1) The commercial ruthenium dioxide powder is placed in ultrapure water and ultrasonically dispersed at a concentration of 0.5 mg/mL to a suspension without precipitation.
[0036] (2) The suspension prepared in step (1) was continuously stirred at room temperature at a stirring speed of 500 rpm, and irradiated with nanosecond parallel pulse laser for 60 minutes, and the laser energy was 185mJ , Get a black solution;
[0037] (3) Place the black solution obtained in step (2) in a refrigerator at -20°C and freeze it into a solid, and then place the frozen solid in a freeze dryer, and lyophilize at -10°C and 20Pa to obtain a strain-containing Ruthenium@Ruthenium dioxide core-shell nanospheres.

Example Embodiment

[0038] Example 3:
[0039] (1) The commercial ruthenium dioxide powder is placed in ultrapure water and ultrasonically dispersed at a concentration of 0.5 mg/mL to a suspension without precipitation.
[0040] (2) The suspension prepared in step (1) was continuously stirred at room temperature at a stirring speed of 300 rpm, and irradiated with nanosecond parallel pulse laser for 10 minutes, and the laser energy was 409mJ , Get a black solution;
[0041] (3) Put the black solution obtained in step (2) into a freezer at -10°C and freeze it into a solid, then place the frozen solid in a freeze dryer and lyophilize at -20°C and 40Pa to obtain a strain containing Ruthenium@Ruthenium dioxide core-shell nanospheres.

PUM

PropertyMeasurementUnit
Thickness2.0 ~ 3.0nm

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