CN116024606B - Preparation of Ru-Cu amorphous nanomaterial rich in defects - Google Patents
Preparation of Ru-Cu amorphous nanomaterial rich in defects Download PDFInfo
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Abstract
The invention relates to a preparation method of a Ru-Cu amorphous nano material (a-Ru-Cu) rich in defects, which is characterized in that metal Ru salt and Cu are used 2 O is a precursor, and the alpha-Ru-Cu nano material is prepared by ion exchange and annealing, and the method is simple and controllable, is easy to implement and has high-efficiency alkaline seawater electrocatalytic oxygen evolution reaction activity.
Description
Technical Field
The invention relates to a preparation method of a Ru-Cu amorphous nano material rich in defects and application of the Ru-Cu amorphous nano material in electrocatalytic seawater decomposition, belonging to the field of material preparation.
Background
The development of hydrogen energy economy provides important guarantee for accelerating green transformation of the pushing energy and realizing important strategy of 'carbon reaching peak, carbon neutralization' double-carbon targets. In the field of hydrogen production by water electrolysis in a plurality of hydrogen sources, the method can realize green sustainable pollution-free hydrogen production, and is honored as one of the most promising hydrogen production modes. However, almost all systems currently use fresh water resources as electrolytes, which undoubtedly exacerbates the problem of fresh water resource shortage. Seawater is one of the most abundant resources on earth (96.5% of the earth's water resources are occupied), and seawater electrolysis is attracting wide attention as a sustainable green method for large-scale production of hydrogen. However, the problems of low activity, insufficient durability and the like are caused by electrode reaction and corrosion caused by complex components of seawater, and the practical feasibility is seriously challenged. Therefore, the preparation of the high-activity electrocatalyst is the key for realizing high-efficiency seawater electrocatalytic decomposition and hydrogen production energy efficiency.
At present, noble metal catalysts such as Ir and Ru are still the most effective catalysts, and compared with Ir-based materials, ru has the price which is only one tenth of that of the Ir-based materials, and is favored by researchers. Researchers designed to synthesize a large number of Ru-based nanomaterials with different types, however, most reported nanomaterials are crystalline structures, and although crystalline materials have simplicity in terms of characterization, crystalline nanomaterials can only perform surface catalysis, limiting their applicability. Amorphous nanomaterial electrocatalysts have attracted extensive research attention due to their catalytic properties over crystalline catalysts under a number of conditions. The catalyst has remarkable advantages in the aspects of catalytic performance, electron transfer and corrosion resistance, and becomes an ideal choice of high-activity and long-service-life electrocatalyst. Amorphous nanomaterials often have abundant defects, the presence of which can optimize the electronic structure of the relevant sites, thus enhancing the catalytic activity, and the catalyst is advantageous for achieving dynamic surface reconstruction and optimizing the surface state, and in addition, the amorphous nanomaterials are easier to self-heal due to disordered atomic arrangement, so that the amorphous electrocatalyst generally has better catalytic activity and corrosion resistance.
Therefore, based on the analysis, the amorphous nano material is constructed, and has important practical significance for improving the conductivity of the Ru-based nano material and improving the intrinsic activity of active sites, thereby enhancing the electrocatalytic performance of the material.
Disclosure of Invention
The invention aims to provide a preparation method of an amorphous Ru-Cu nano material and application of an alkaline seawater oxygen evolution reaction thereof.
Based on the above objects, the technical scheme of the invention is as follows:
(1) (1) preparation of self-sacrifice templates: cuprous oxide (Cu) 2 O) is used as a self-sacrifice template, and the synthesis steps are as follows: cupric chloride dihydrate (CuCl) 2 ·2H 2 O,0.1-1 g) is dissolved in 20mL deionized water; then 0.1-1g sodium hydroxide (NaOH) is dissolved in 20mL deionized water, and then the solution is transferred to Cu in turn 2+ In the solution, stirring and reacting for 5min. 0.1-2g of ascorbic acid (C) 6 H 8 O 6 ) Dissolving in 10mL deionized water, transferring to the solution, stirring for 30min, washing with deionized water and ethanol three times, centrifuging, and vacuum drying.
(2) Preparation of amorphous Ru-Cu nanomaterial: 10-100mg Cu 2 O and 10-100mg of ruthenium trichloride (RuCl) 3 ·xH 2 O) dispersing in deionized water of 50 mL; then 0.1-2g sodium thiosulfate (Na) 2 S 2 O 3 ) Dissolved in 10mL deionized water and transferred to the above solution, stirred for 1-30min, centrifuged and dried. Then, the obtained powder was placed in a tube furnace at 3℃for min under an atmosphere of air -1 The temperature is raised to 400-900 ℃ and the reaction is carried out for 2h. The resulting product was designated as a-Ru-Cu.
(2) Seawater of the a-Ru-Cu nano material in 1M KOH is subjected to oxygen evolution reaction test to reach 10mA cm -2 At a current density of only 320mV of overpotential is required
The invention has the following advantages:
by metal Ru salt and Cu 2 O is a precursor, and the alpha-Ru-Cu nano material is prepared by ion exchange and annealing, and the method is simple, controllable and easy to implement, and the method isHas high-efficiency electrocatalytic activity.
Drawings
Fig. 1: cu is obtained in example 1 2 X-ray powder diffraction pattern of O material, precursor with excellent crystal phase corresponding to Cu 2 O。
Fig. 2: the X-ray powder diffraction pattern of the a-Ru-Cu material obtained in example 1, and a-Ru-Cu prepared by a series of means such as high-temperature annealing, etc., exhibit amorphous characteristics.
Fig. 3: cu is obtained in example 1 2 Transmission electron microscopy of O material, cu prepared 2 The nano-size of the O material is 50-100nm, which is far lower than the reported similar size.
Fig. 4: a transmission electron micrograph of the a-Ru-Cu material obtained in example 1 still shows lower nano-dimensions.
Fig. 5: the electrochemical linear scanning pattern of the a-Ru-Cu material is obtained in the example 1, seawater of the a-Ru-Cu nano material in 1M KOH is subjected to oxygen evolution reaction test, and the oxygen evolution reaction reaches 10mA cm -2 Only 320mV of overpotential is required at the current density of (c).
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
0.681g of CuCl 2 ·2H 2 O is dissolved in 20mL deionized water; then 0.96g NaOH was dissolved in 20mL deionized water, and then this solution was transferred to Cu described above in succession 2+ In the solution, stirring and reacting for 5min. Dissolving 1.41g of ascorbic acid in 10mL of deionized water, transferring to the solution, continuously stirring for 30min, washing with deionized water and ethanol for three times, centrifuging, and vacuum drying to obtain Cu 2 O。50mg Cu 2 O and 63mg RuCl 3 ·xH 2 O is dispersed in 50mL of deionized water; 1.42g of Na 2 S 2 O 3 Dissolved in 10mL deionized water and transferred to the above solution, stirred for 15min, centrifuged and dried. Then, the obtained powder was placed in a tube furnace under an atmosphere of air to3℃min -1 The reaction was carried out for 2 hours at a rate of 500 ℃. The resulting product was designated as a-Ru-Cu.
Example 2
0.681g of CuCl 2 ·2H 2 O is dissolved in 20mL deionized water; then 0.96g NaOH was dissolved in 20mL deionized water, and then this solution was transferred to Cu described above in succession 2+ In the solution, stirring and reacting for 5min. Dissolving 1.41g of ascorbic acid in 10mL of deionized water, transferring to the solution, continuously stirring for 30min, washing with deionized water and ethanol for three times, centrifuging, and vacuum drying to obtain Cu 2 O。50mg Cu 2 O and 63mg RuCl 3 ·xH 2 O is dispersed in 50mL of deionized water; 1.42g of Na 2 S 2 O 3 Dissolved in 10mL deionized water and transferred to the above solution, stirred for 10min, centrifuged and dried. Then, the obtained powder was placed in a tube furnace at 3℃for min under an atmosphere of air -1 The reaction was carried out for 2 hours at a rate of 500 ℃. The resulting product was designated as a-Ru-Cu.
Example 3
0.681g of CuCl 2 ·2H 2 O is dissolved in 20mL deionized water; then 0.96g NaOH was dissolved in 20mL deionized water, and then this solution was transferred to Cu described above in succession 2+ In the solution, stirring and reacting for 5min. Dissolving 1.41g of ascorbic acid in 10mL of deionized water, transferring to the solution, continuously stirring for 30min, washing with deionized water and ethanol for three times, centrifuging, and vacuum drying to obtain Cu 2 O。50mg Cu 2 O and 63mg RuCl 3 ·xH 2 O is dispersed in 50mL of deionized water; 1.42g of Na 2 S 2 O 3 Dissolved in 10mL deionized water and transferred to the above solution, stirred for 15min, centrifuged and dried. Then, the obtained powder was placed in a tube furnace at 3℃for min under an atmosphere of air -1 The reaction was carried out for 2 hours at a rate of 600 ℃. The resulting product was designated as a-Ru-Cu.
Example 4
0.681g of CuCl 2 ·2H 2 O is dissolved in 20The method comprises the steps of (1) adding deionized water into mL; then 0.96g NaOH was dissolved in 20mL deionized water, and then this solution was transferred to Cu described above in succession 2+ In the solution, stirring and reacting for 5min. Dissolving 1.41g of ascorbic acid in 10mL of deionized water, transferring to the solution, continuously stirring for 30min, washing with deionized water and ethanol for three times, centrifuging, and vacuum drying to obtain Cu 2 O。50mg Cu 2 O and 50mg RuCl 3 ·xH 2 O is dispersed in 50mL of deionized water; 1.42g of Na 2 S 2 O 3 Dissolved in 10mL deionized water and transferred to the above solution, stirred for 15min, centrifuged and dried. Then, the obtained powder was placed in a tube furnace at 3℃for min under an atmosphere of air -1 The reaction was carried out for 2 hours at a rate of 500 ℃. The resulting product was designated as a-Ru-Cu.
Example 5
0.681g of CuCl 2 ·2H 2 O is dissolved in 20mL deionized water; then 0.96g NaOH was dissolved in 20mL deionized water, and then this solution was transferred to Cu described above in succession 2+ In the solution, stirring and reacting for 5min. Dissolving 1.41g of ascorbic acid in 10mL of deionized water, transferring to the solution, continuously stirring for 30min, washing with deionized water and ethanol for three times, centrifuging, and vacuum drying to obtain Cu 2 O。50mg Cu 2 O and 50mg RuCl 3 ·xH 2 O is dispersed in 50mL of deionized water; 1.42g of Na 2 S 2 O 3 Dissolved in 10mL deionized water and transferred to the above solution, stirred for 20min, centrifuged and dried. Then, the obtained powder was placed in a tube furnace at 3℃for min under an atmosphere of air -1 The reaction was carried out for 2 hours at a rate of 500 ℃. The resulting product was designated as a-Ru-Cu.
Claims (2)
1. The preparation method of the Ru-Cu amorphous nanomaterial rich in defects is characterized by comprising the following steps of:
(1) preparation of self-sacrifice templates: cuprous oxide (Cu) 2 O) is used as a self-sacrifice template, and the synthesis steps are as follows: cupric chloride dihydrate (CuCl) 2 •2H 2 O,0.1-1 g) is dissolved in 20mL deionized water; then 0.1-1g sodium hydroxide (NaOH) is dissolved in 20mL deionized water, and then the solution is transferred to Cu in turn 2+ Stirring and reacting for 5min in the solution; 0.1-2g of ascorbic acid (C) 6 H 8 O 6 ) Dissolving in 10mL deionized water, transferring to the above solution, stirring for 30min, washing with deionized water and ethanol for three times, centrifuging, and vacuum drying to obtain Cu 2 O nanometer size is 50-100nm;
(2) preparation of amorphous Ru-Cu nanomaterial: 10-100mg Cu 2 O and 10-100mg of ruthenium trichloride (RuCl) 3 •xH 2 O) dispersing in deionized water of 50 mL; then 0.1-2g sodium thiosulfate (Na) 2 S 2 O 3 ) Dissolving in 10mL deionized water, transferring to the above solution, stirring for 1-30min, centrifuging, and drying; then, the obtained powder was placed in a tube furnace at 3℃for min under an atmosphere of air -1 The reaction was carried out for 2 hours at a rate of 500℃to give the product designated a-Ru-Cu.
2. Use of a defect-rich Ru-Cu amorphous nanomaterial prepared by the method of claim 1, wherein: the application refers to that the Ru-Cu amorphous nano material rich in defects is used as an anode catalyst to be applied to electrocatalytic seawater decomposition in an alkaline environment.
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