{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,9,14]],"date-time":"2026-09-14T00:02:45Z","timestamp":1789344165940,"version":"build-2803163510"},"reference-count":32,"publisher":"MDPI AG","issue":"2","license":[{"start":{"date-parts":[[2026,2,16]],"date-time":"2026-02-16T00:00:00Z","timestamp":1771200000000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"funder":[{"name":"OPPO Guangdong Mobile Telecommunications Co., Ltd","award":["99901230708"],"award-info":[{"award-number":["99901230708"]}]}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Micromachines"],"abstract":"<jats:p>Enzyme-free flexible glucose sensors hold great promise in the field of wearable health monitoring. However, their performance is limited by the balance between the catalytic interface activity and stability. This paper reports a strategy for interface gradient roughening of screen-printed carbon electrodes (SPCE) via controllable electrochemical exfoliation (EE). It systematically reveals the inherent relationships among the degree of EE treatment, electrode morphology, surface chemistry, and electrochemical performance. On this basis, the deposition of gold nanoparticles (AuNPs) with high density and uniform distribution is achieved, and a high-performance flexible enzyme-free glucose sensor is constructed. The study finds that EE treatment can significantly increase the true surface area of the electrode and introduce abundant oxygen-containing functional groups, thus effectively reducing the charge transfer resistance. Nevertheless, excessive exfoliation leads to the degradation of the conductive network, indicating the existence of a critical \u201cperformance window\u201d. The EE-SPCE optimized with 150 cycles has both a high active area and good electrical conductivity, providing an ideal deposition substrate for AuNPs, increasing their distribution density by approximately 158% and reducing the average particle size to 125 nm. The fabricated AuNPs\/EE-SPCE sensor exhibits excellent performance in glucose detection: it has a high sensitivity of 550.766 \u03bcA\u00b7mM\u22121\u00b7cm\u22122 in the range of 0.1\u20133 mM, a detection limit of 0.0998 mM, a wide linear range, excellent selectivity, long-term stability, and good mechanical flexibility. This research not only develops an efficient and scalable method for constructing flexible sensing interfaces but also clarifies the trade-off relationship among \u201croughening\u2013conductivity\u2013catalytic performance\u201d at the mechanistic level, providing an important theoretical basis and a general strategy for rationally designing high-performance flexible electrochemical devices.<\/jats:p>","DOI":"10.3390\/mi17020251","type":"journal-article","created":{"date-parts":[[2026,2,16]],"date-time":"2026-02-16T11:11:28Z","timestamp":1771240288000},"page":"251","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["Construction of Highly Active Interfaces on Screen-Printed Carbon Electrodes via Controllable Electrochemical Exfoliation for High-Performance Flexible Enzyme-Free Glucose Sensing"],"prefix":"10.3390","volume":"17","author":[{"given":"Wenjing","family":"Xue","sequence":"first","affiliation":[{"name":"Key Laboratory of Wide Band-Gap Semiconductor Materials and Devices, School of Microelectronics, Xidian University, Xi\u2019an 710071, China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ziyan","family":"Chen","sequence":"additional","affiliation":[{"name":"Key Laboratory of Wide Band-Gap Semiconductor Materials and Devices, School of Microelectronics, Xidian University, Xi\u2019an 710071, China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xiao","family":"Peng","sequence":"additional","affiliation":[{"name":"OPPO Guangdong Mobile Communications Co., Ltd., Chang\u2019an Town, Dongguan 523860, China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0008-8703-9325","authenticated-orcid":false,"given":"Haocheng","family":"Yin","sequence":"additional","affiliation":[{"name":"Guangzhou Institute of Technology, Xidian University, Guangzhou 510555, China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yimeng","family":"Zhang","sequence":"additional","affiliation":[{"name":"Key Laboratory of Wide Band-Gap Semiconductor Materials and Devices, School of Microelectronics, Xidian University, Xi\u2019an 710071, China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yuming","family":"Zhang","sequence":"additional","affiliation":[{"name":"Key Laboratory of Wide Band-Gap Semiconductor Materials and Devices, School of Microelectronics, Xidian University, Xi\u2019an 710071, China"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"1968","published-online":{"date-parts":[[2026,2,16]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"689","DOI":"10.1007\/s00604-013-1098-0","article-title":"Advances in enzyme-free electrochemical sensors for hydrogen peroxide, glucose, and uric acid","volume":"181","author":"Chen","year":"2014","journal-title":"Microchim. Acta"},{"key":"ref_2","doi-asserted-by":"crossref","first-page":"14553","DOI":"10.1039\/D0CC05650B","article-title":"Electrochemical non-enzymatic glucose sensors: Recent progress and perspectives","volume":"56","author":"Wei","year":"2020","journal-title":"Chem. Commun."},{"key":"ref_3","doi-asserted-by":"crossref","first-page":"310","DOI":"10.1016\/j.jcis.2020.09.051","article-title":"Facile preparation of Ni nanoparticle embedded on mesoporous carbon nanorods for non-enzymatic glucose detection","volume":"583","author":"Jia","year":"2021","journal-title":"J. Colloid Interface Sci."},{"key":"ref_4","doi-asserted-by":"crossref","first-page":"17","DOI":"10.1016\/j.scriptamat.2011.03.025","article-title":"Nanoporous gold for enzyme-free electrochemical glucose sensors","volume":"65","author":"Chen","year":"2011","journal-title":"Scr. Mater."},{"key":"ref_5","doi-asserted-by":"crossref","first-page":"161","DOI":"10.1007\/s00604-012-0923-1","article-title":"Non-enzymatic electrochemical sensing of glucose","volume":"180","author":"Wang","year":"2013","journal-title":"Microchim. Acta"},{"key":"ref_6","doi-asserted-by":"crossref","first-page":"126","DOI":"10.1016\/j.electacta.2013.10.168","article-title":"Enzyme-free sensing of hydrogen peroxide and glucose at a CuS nanoflowers modified glassy carbon electrode","volume":"115","author":"Yang","year":"2014","journal-title":"Electrochim. Acta"},{"key":"ref_7","doi-asserted-by":"crossref","first-page":"144009","DOI":"10.1016\/j.electacta.2024.144009","article-title":"Enzyme-free glucose sensor based on electrodeposition of multi-walled carbon nanotubes and Zn-based metal framework-modified gold electrode at low potential","volume":"483","author":"Xue","year":"2024","journal-title":"Electrochim. Acta"},{"key":"ref_8","doi-asserted-by":"crossref","first-page":"45","DOI":"10.1016\/j.bios.2019.03.064","article-title":"Enzyme-free glucose sensor based on layer-by-layer electrodeposition of multilayer films of multi-walled carbon nanotubes and Cu-based metal framework modified glassy carbon electrode","volume":"135","author":"Wu","year":"2019","journal-title":"Biosens. Bioelectron."},{"key":"ref_9","doi-asserted-by":"crossref","first-page":"134498","DOI":"10.1016\/j.snb.2023.134498","article-title":"Construction of a portable enzyme-free electrochemical glucose detection system based on the synergistic interaction of Cu-MOF and PtNPs","volume":"395","author":"Chen","year":"2023","journal-title":"Sens. Actuators B Chem."},{"key":"ref_10","doi-asserted-by":"crossref","first-page":"123587","DOI":"10.1016\/j.talanta.2022.123587","article-title":"The nickel phosphate rods derived from Ni-MOF with enhanced electrochemical activity for non-enzymatic glucose sensing","volume":"247","author":"Xiao","year":"2022","journal-title":"Talanta"},{"key":"ref_11","doi-asserted-by":"crossref","first-page":"394","DOI":"10.1021\/ac504300n","article-title":"Tattoo-based noninvasive glucose monitoring: A proof-of-concept study","volume":"87","author":"Bandodkar","year":"2015","journal-title":"Anal. Chem."},{"key":"ref_12","doi-asserted-by":"crossref","first-page":"2209","DOI":"10.1021\/acssuschemeng.2c05438","article-title":"Flexible, bifunctional sensing platform made with biodegradable mats for detecting glucose in urine","volume":"11","author":"Gomes","year":"2023","journal-title":"ACS Sustain. Chem. Eng."},{"key":"ref_13","doi-asserted-by":"crossref","first-page":"113078","DOI":"10.1016\/j.bios.2021.113078","article-title":"Integration of interstitial fluid extraction and glucose detection in one device for wearable non-invasive blood glucose sensors","volume":"179","author":"Yao","year":"2021","journal-title":"Biosens. Bioelectron."},{"key":"ref_14","doi-asserted-by":"crossref","unstructured":"Zhang, S., Wang, M., Wang, X., Song, J., and Yang, X. (2024). Electrocatalysis in MOF films for flexible electrochemical sensing: A comprehensive review. Biosensors, 14.","DOI":"10.20944\/preprints202408.1169.v1"},{"key":"ref_15","doi-asserted-by":"crossref","first-page":"471","DOI":"10.1016\/j.snb.2008.05.028","article-title":"Enzyme-free glucose sensor based on a three-dimensional gold film electrode","volume":"134","author":"Bai","year":"2008","journal-title":"Sens. Actuators B Chem."},{"key":"ref_16","doi-asserted-by":"crossref","unstructured":"Cardoso, A.R.A., Barquinha, P.M.C., and Sales, M.G.F. (2025). Enzyme-Free Monitoring of Glucose Using Molecularly Imprinted Polymers and Gold Nanoparticles. Biosensors, 15.","DOI":"10.3390\/bios15080537"},{"key":"ref_17","doi-asserted-by":"crossref","first-page":"524","DOI":"10.1016\/j.apsusc.2013.10.064","article-title":"Gold nanoparticles directly modified glassy carbon electrode for non-enzymatic detection of glucose","volume":"288","author":"Chang","year":"2014","journal-title":"Appl. Surf. Sci."},{"key":"ref_18","doi-asserted-by":"crossref","first-page":"168","DOI":"10.1002\/elan.202100281","article-title":"Electrochemical biosensors based on micro-fabricated devices for point-of-care testing: A review","volume":"34","author":"Zhang","year":"2022","journal-title":"Electroanalysis"},{"key":"ref_19","doi-asserted-by":"crossref","unstructured":"Costa-Rama, E., and Fern\u00e1ndez-Abedul, M.T. (2021). Paper-based screen-printed electrodes: A new generation of low-cost electroanalytical platforms. Biosensors, 11.","DOI":"10.3390\/bios11020051"},{"key":"ref_20","doi-asserted-by":"crossref","unstructured":"Lin, J., Chen, Y., Liu, X., Jiang, H., and Wang, X. (2025). Engineered Intelligent Electrochemical Biosensors for Portable Point-of-Care Diagnostics. Chemosensors, 13.","DOI":"10.3390\/chemosensors13040146"},{"key":"ref_21","doi-asserted-by":"crossref","first-page":"1399","DOI":"10.1039\/b102934g","article-title":"Effect of pre-treatment on the surface and electrochemical properties of screen-printed carbon paste electrodes","volume":"126","author":"Cui","year":"2001","journal-title":"Analyst"},{"key":"ref_22","doi-asserted-by":"crossref","first-page":"297","DOI":"10.1016\/j.aca.2007.02.006","article-title":"Enhanced electrochemical performance at screen-printed carbon electrodes by a new pretreating procedure","volume":"588","author":"Wei","year":"2007","journal-title":"Anal. Chim. Acta"},{"key":"ref_23","doi-asserted-by":"crossref","first-page":"4937","DOI":"10.1016\/j.electacta.2009.04.006","article-title":"Enhancement of electrochemical properties of screen-printed carbon electrodes by oxygen plasma treatment","volume":"54","author":"Wang","year":"2009","journal-title":"Electrochim. Acta"},{"key":"ref_24","doi-asserted-by":"crossref","unstructured":"Haroon, N., and Stine, K.J. (2025). Surface Modification of Screen-Printed Carbon Electrodes. Coatings, 15.","DOI":"10.3390\/coatings15101182"},{"key":"ref_25","doi-asserted-by":"crossref","first-page":"4684","DOI":"10.1002\/adfm.201203686","article-title":"The exfoliation of graphene in liquids by electrochemical, chemical, and sonication-assisted techniques: A nanoscale study","volume":"23","author":"Xia","year":"2013","journal-title":"Adv. Funct. Mater."},{"key":"ref_26","doi-asserted-by":"crossref","first-page":"e202218080","DOI":"10.1002\/ange.202218080","article-title":"Electrochemical Nano-Roughening of Gold Microstructured Electrodes for Enhanced Sensing in Biofluids","volume":"135","author":"Saem","year":"2023","journal-title":"Angew. Chem."},{"key":"ref_27","doi-asserted-by":"crossref","first-page":"037510","DOI":"10.1149\/1945-7111\/ac5ad5","article-title":"A Study of the effect of electrochemical roughening of platinum on the sensitivity and selectivity of glutamate biosensors","volume":"169","author":"Tan","year":"2022","journal-title":"J. Electrochem. Soc."},{"key":"ref_28","doi-asserted-by":"crossref","first-page":"12185","DOI":"10.1021\/acs.analchem.7b02830","article-title":"High surface area electrodes generated via electrochemical roughening improve the signaling of electrochemical aptamer-based biosensors","volume":"89","author":"Scida","year":"2017","journal-title":"Anal. Chem."},{"key":"ref_29","doi-asserted-by":"crossref","first-page":"96","DOI":"10.1016\/j.talanta.2013.02.022","article-title":"Bienzymatic glucose biosensor based on direct electrochemistry of cytochrome c on gold nanoparticles\/polyaniline nanospheres composite","volume":"110","author":"Xiang","year":"2013","journal-title":"Talanta"},{"key":"ref_30","doi-asserted-by":"crossref","first-page":"23","DOI":"10.1016\/j.snb.2011.04.057","article-title":"A novel glucose biosensor based on direct electrochemistry of glucose oxidase incorporated in biomediated gold nanoparticles\u2013carbon nanotubes composite film","volume":"158","author":"Zhang","year":"2011","journal-title":"Sens. Actuators B Chem."},{"key":"ref_31","doi-asserted-by":"crossref","first-page":"1937","DOI":"10.1002\/elan.200603607","article-title":"Gold nanoparticles in nonenzymatic electrochemical detection of sugars","volume":"18","author":"Kurniawan","year":"2006","journal-title":"Electroanalysis"},{"key":"ref_32","doi-asserted-by":"crossref","first-page":"177796","DOI":"10.1016\/j.jallcom.2024.177796","article-title":"Electrochemical non-enzymatic glucose sensors based on CuO nanostructures","volume":"1010","author":"Yang","year":"2024","journal-title":"J. Alloys Compd."}],"container-title":["Micromachines"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/www.mdpi.com\/2072-666X\/17\/2\/251\/pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2026,2,16]],"date-time":"2026-02-16T11:35:09Z","timestamp":1771241709000},"score":1,"resource":{"primary":{"URL":"https:\/\/www.mdpi.com\/2072-666X\/17\/2\/251"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2026,2,16]]},"references-count":32,"journal-issue":{"issue":"2","published-online":{"date-parts":[[2026,2]]}},"alternative-id":["mi17020251"],"URL":"https:\/\/doi.org\/10.3390\/mi17020251","relation":{},"ISSN":["2072-666X"],"issn-type":[{"value":"2072-666X","type":"electronic"}],"subject":[],"published":{"date-parts":[[2026,2,16]]}}}