Fabrication of hard bound mesoporous silica stabilized Cu(I) electrocatalyst for 4-nitrophenol sensor via alcothermal strategy

Muthukumar, Thennila; Shenbagapushpam, Muthumanickam; Madasamy, Siva Bharathy; Paulpandian, Muthu Mareeswaran; Selvakumar, Kodirajan

doi:10.1016/j.jelechem.2019.113792

Cited by 9 publications

(9 citation statements)

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“…Although it is quite difficult to discriminate between Cu(I) and Cu(0) based on XPS spectra due to their nearly identical binding energy value, the spin−orbit coupling constant value (≤19.8 eV) indicates the formation of Cu(I) in Cu-TEPTS@SBA-15. 52 The Cu 2p XPS spectrum of the CuMS catalyst exhibited four peaks at 932.9, 934.8, 952.7, and 954.9 eV. The peaks at 932.9 and 952.7 eV are due to Cu(I) 2p 3/2 and Cu(I) 2p 1/2 , respectively.…”

Section: ■ Results and Discussionmentioning

confidence: 95%

“…The survey spectrum of Cu-TEPTS@SBA-15 and CuMS (Figure S3) reveals the presence of silicon (102.5 and 154.0 eV), oxygen (532.9 eV), and copper (932.9 and 952.7 eV). Figure a depicts the high-resolution calibrated XPS peak for Cu 2p of Cu-TEPTS@SBA-15, which consists of two peaks at 932.9 and 952.7 eV, which appear for Cu 2p 3/2 and Cu 2p 1/2 , respectively . The absence of strong satellite peaks indicates the presence of Cu(I) or Cu(0) species.…”

Section: Resultsmentioning

confidence: 99%

“…The absence of strong satellite peaks indicates the presence of Cu(I) or Cu(0) species. Although it is quite difficult to discriminate between Cu(I) and Cu(0) based on XPS spectra due to their nearly identical binding energy value, the spin–orbit coupling constant value (≤19.8 eV) indicates the formation of Cu(I) in Cu-TEPTS@SBA-15 . The Cu 2p XPS spectrum of the CuMS catalyst exhibited four peaks at 932.9, 934.8, 952.7, and 954.9 eV.…”

Section: Resultsmentioning

confidence: 99%

“…Figure 3a depicts the high-resolution calibrated XPS peak for Cu 2p of Cu-TEPTS@SBA-15, which consists of two peaks at 932.9 and 952.7 eV, which appear for Cu 2p 3/2 and Cu 2p 1/2 , respectively. 52 The absence of strong satellite peaks indicates the presence of Cu(I) or Cu(0) species. Although it is quite difficult to discriminate between Cu(I) and Cu(0) based on XPS spectra due to their nearly identical binding energy value, the spin−orbit coupling constant value (≤19.8 eV) indicates the formation of Cu(I) in Cu-TEPTS@SBA-15.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…Among the mesoporous silica family of materials, SBA-15 with 2D hexagonally arranged ordered mesoporous silica has attracted special attention over the years due to their high internal surface area, large pore volume, ease of surface functionalization, and high hydrothermal stability . Functionalized SBA-15 materials are largely employed as catalyst supports through hosting metal ions/metallic nanoparticles. , Though transition-metal-grafted SBA-15 materials are widely utilized as heterogeneous catalysts for several organic transformations, − only a few transition-metal-grafted functionalized SBA-15 materials are reported for colorimetric − and electrochemical sensing of toxic pollutants. − The first-row transition-metal immobilization over the surface of SBA-15 is generally achieved through post-synthetic wet impregnation or organic functionalization. These post-synthetic modifications often lead to reduced surface area and pore blockage.…”

Section: Introductionmentioning

confidence: 99%

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Copper Immobilized over 2D Hexagonal SBA-15 for Electrochemical and Colorimetric Sulfite Sensing

et al. 2023

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Sulfite (SO 3 2−) is considered a highly toxic anion for living organisms. Herein, we report the synthesis of copper immobilized over a 2D hexagonally ordered mesoporous silica material CuMS as an electrochemical and colorimetric dual-technique-based sensing platform for sulfite detection. The immobilization of copper on silica was achieved through the bis[3-(triethoxysilyl)propyl]tetrasulfide (TEPTS) ligand. Morphological and physical properties of the material were confirmed by several characterization techniques, including scanning electron microscopy, transmission electron microscopy, X-ray diffraction, N 2 sorption, and X-ray photoelectron spectroscopy. The CuMS material retained mesoporosity with a narrow pore size distribution (D ≈ 5.4 nm) and a high Brunauer−Emmett−Teller surface area of 682 m 2 g −1 after the immobilization of copper. The prepared catalyst shows promising electrocatalytic activity toward sulfite oxidation. A linear variation in the peak current was obtained for SO 3 2− oxidation in the 0.2−15 mM range with a high sensitivity of 62.08 μA cm −2 , under optimum experimental conditions. The limit of detection (LOD) was found to be 1.14 nM. CuMS also shows excellent activity toward colorimetric detection of sulfite anions with an LOD of 0.4 nM. The proposed sensor shows high selectivity toward the sulfite anion, even in the presence of common interferents. The detection of sulfite in white wine with excellent recovery demonstrates the practical applicability of this sensor.

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Section: ■ Results and Discussionmentioning

confidence: 95%

Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: ■ Results and Discussionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Copper Immobilized over 2D Hexagonal SBA-15 for Electrochemical and Colorimetric Sulfite Sensing

et al. 2023

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Heterogeneous Cu(I)‐SBA‐15 Mediated Catalytic Reduction of Substituted Nitroarenes

Muthukumar¹,

Shenbagapushpam²,

Sivabharathy³

et al. 2020

ChemistrySelect

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A strategy for heterogeneous copper(I) mesoporous silica [Cu (I)-SBA-15] mediated catalytic reduction has been developed for the reduction of various nitroarenes in excellent yields. In addition to alcothermal strategy, other strategies have been attempted for the preparation of Cu(I) substituted mesoporous silica, however, the desired oxidation state is obtained only through alcothermal strategy. The crystalline phases and oxidation state of synthesized materials were characterized by XRD and XPS measurements and tested for catalytic reduction of nitroarenes. Among the tested materials, the best catalytic reduction of nitroarenes with an excellent substrate scope and good catalytic reusability was established by Cu(I)-SBA-15 material. The reduction kinetics and the controlled experimental studies reveal that the reaction proceeds through pseudofirst-order kinetics and nitrosobenzene intermediate pathway.

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Silicon nanoparticles: a new and enhanced operational material for nitrophenol sensing

Wahab

Ahmad

Alam

2020

J Mater Sci: Mater Electron

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Fabrication of hard bound mesoporous silica stabilized Cu(I) electrocatalyst for 4-nitrophenol sensor via alcothermal strategy

Cited by 9 publications

References 50 publications

Copper Immobilized over 2D Hexagonal SBA-15 for Electrochemical and Colorimetric Sulfite Sensing

Copper Immobilized over 2D Hexagonal SBA-15 for Electrochemical and Colorimetric Sulfite Sensing

Heterogeneous Cu(I)‐SBA‐15 Mediated Catalytic Reduction of Substituted Nitroarenes

Silicon nanoparticles: a new and enhanced operational material for nitrophenol sensing

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