US-12618165-B1 - Electrode and method of preparation thereof

Abstract

An electrode which includes nanoparticles of a carbon-doped tin oxide of formula C—SnO 2-x where x=is from 0.001 to 0.1, having surface oxygen vacancies. The electrode includes a fluorine-doped tin oxide substrate. A film of the nanoparticles is present on at least one surface of the fluorine-doped tin oxide substrate. The surface oxygen vacancies correspond to an O 1s peak shift of 0.5-2 eV in the X-ray photoelectron spectroscopy (XPS) for C—SnO 2-x compared to C—SnO 2 without surface oxygen vacancies.

Inventors

• Maged Naji Yahya Shaddad

Assignees

• PRINCE SATTAM BIN ABDULAZIZ UNIVERSITY

Dates

Publication Date

20260505

Application Date

20250822

Claims (5)

1. 1 . An electrode, comprising: nanoparticles of a carbon-doped tin oxide of formula C—SnO 2-x wherein x=is from 0.001 to 0.1, having surface oxygen vacancies, a fluorine-doped tin oxide substrate, wherein a film of the nanoparticles is present on at least one surface of the fluorine-doped tin oxide substrate, wherein the surface oxygen vacancies correspond to a O 1s peak shift of 0.5-2 eV in the X-ray photoelectron spectroscopy (XPS) for C—SnO 2-x compared to C—SnO 2 without surface oxygen vacancies.
2. 2 . The electrode of claim 1 , wherein the nanoparticles have a surface oxygen vacancy density of 0.5-2 oxygen vacancies per square nanometer (Ovs nm −2 ).
3. 3 . The electrode of claim 1 , wherein the nanoparticles have a textured and pitted surface morphology.
4. 4 . The electrode of claim 1 , wherein the nanoparticles have an average diameter of 1-5 nm.
5. 5 . The electrode of claim 1 , having a hydrogen peroxide detection sensitivity of 22-5 μA μM −1 cm −2 .

Description

BACKGROUND Technical Field The present disclosure relates to an electrode, more particularly, the present disclosure pertains to a method of preparation thereof and its use for the electrochemical production and detection of hydrogen peroxide. Description of Related Art The ‘background’ description provided herein is for the purpose of generally presenting the context of the disclosure. The work of the presently named inventors, to the extent it is described in this background section, as well as aspects of the description which may not otherwise qualify as prior art at the time of filing, are neither expressly nor impliedly admitted as prior art against the present invention. Hydrogen peroxide is a versatile oxidant widely employed across industries such as chemical synthesis, healthcare, water treatment, and renewable energy due to its clean decomposition and strong oxidizing ability. The predominant production method-using the anthraquinone process-utilizes hazardous solvents, demands high energy, and poses safety concerns during transportation and storage. Electrochemical production of hydrogen peroxide via the two-electron oxygen reduction reaction (ORR) provides a promising alternative, enabling on-site generation at lower potentials while minimizing explosion hazards. Achieving high selectivity toward hydrogen peroxide over water depends on tuning catalyst properties to favor the two-electron pathway by enhancing intermediate adsorption and preserving the oxygen-oxygen bond. Tin oxide is a promising, inexpensive electrocatalyst for ORR, yet its current performance falls short. Accordingly, an object of the present disclosure is directed to an electrocatalyst configured to selectively promote the two-electron oxygen reduction reaction for efficient in situ hydrogen peroxide generation, thereby overcoming the limitations of the prior art. SUMMARY In an exemplary embodiment, an electrode is described. The electrode includes nanoparticles of a carbon-doped tin oxide of formula C—SnO2-x where x=is from 0.001 to 0.1, having surface oxygen vacancies. The electrode includes a fluorine-doped tin oxide substrate. A film of the nanoparticles is present on at least one surface of the fluorine-doped tin oxide substrate. The surface oxygen vacancies correspond to a O 1s peak shift of 0.5-2 eV in the X-ray photoelectron spectroscopy (XPS) for C—SnO2-x compared to C—SnO2 without surface oxygen vacancies. In some embodiments, the nanoparticles have an average diameter of 1-5 nm. In some embodiments, the nanoparticles have a hydrogen peroxide detection sensitivity of 2-5 μA μM−1 cm−2. In some embodiments, the electrode is crystalline. In some embodiments, a method of generating hydrogen peroxide is described. The method includes applying an electrical potential to an electrolytic cell including the electrode an anode and an electrolytic solution, to form the hydrogen peroxide. In some embodiments, the electrolytic solution includes water, a base and dissolved oxygen. In some embodiments, the base is KOH. In some embodiments, the concentration of base is 1 M. In another exemplary embodiment, a method of detecting hydrogen peroxide at a concentration of 1 μM to 20 μM in an alkaline solution is described. The method includes immersing the electrode into an electrolytic cell containing the alkaline solution. The method includes applying an electrical potential to the electrolytic cell and recording a peak current. The method includes determining a concentration of the H2O2 in the alkaline solution. In some embodiments, the alkaline solution is an aqueous solution of KOH. In some embodiments, the concentration of KOH is 1 M. In some embodiments, the peak current density is directly proportional to the concentration of H2O2 in the alkaline solution. In some embodiments, the electrical potential is 0.4-0.9 V vs. SCE. In yet another exemplary embodiment, a method of making the electrode is described. The method includes autoclaving a mixture including a tin salt, a sugar and water to form a reaction product. The method includes vacuum heat treating the reaction product to form the nanoparticles. The method includes coating a surface of a fluorine-doped tin oxide substrate with the nanoparticles. In some embodiments, the tin salt is tin chloride. In some embodiments, the concentration of the tin salt is 10-30 mM. In some embodiments, the sugar is sucrose. In some embodiments, the concentration of the sugar is 0-4 M. In some embodiments, the autoclaving is at a temperature of 80-100° C. In some embodiments, the vacuum heat treating is at a temperature of 300-400° C. The foregoing general description of the illustrative embodiments and the following detailed description thereof are merely exemplary aspects of the teachings of this disclosure, and are not restrictive. BRIEF DESCRIPTION OF THE DRAWINGS A more complete appreciation of this disclosure and many of the attendant advantages thereof will be readily obtained as the same