Preparation of NiCo-LDH/AuRu and Its Non-Enzymatic Glucose Sensing Performance AITranslate

［1］Saha T，Del Caño R，Mahato K，De La Paz E，Chen C R，Ding S C，Yin L，Wang J. Wearable electrochemical glucose sensors in diabetes management：a comprehensive review［J］.Chemical Reviews，2023，123（12）：7854.

［2］Zhong S J，Chen K Y，Wang S L，Manshaii F，Jing N，Wang K D，Liu S C，Zhou Y L. Metal-based nanowires in electrical biosensing［J］.Rare Metals，2024，43（12）：6233.

［3］Adeel M，Rahman M M，Caligiuri I，Canzonieri V，Rizzolio F，Daniele S. Recent advances of electrochemical and optical enzyme-free glucose sensors operating at physiological conditions［J］.Biosensors and Bioelectronics，2020，165：112331.

［4］李江，李作鹏，罗宿星，丁志明，白云峰，樊佩，武美霞，郭永. 基于柔性MXenes/石墨烯纤维直接电沉积NiS构建非酶葡萄糖传感器［J］.分析试验室，2023，42（6）：800.

J Li，Z P Li，S X Luo，Z M Ding，Y F Bai，P Fan，M X Wu，Y Guo. Non-enzymatic glucose sensor based on flexible MXenes/graphene-fiber with directly electrodeposited by NiS［J］.Chinese Journal of Analysis Laboratory，2023，42（6）：800.

［5］Zhang S，Zhao W J，Zeng J Y，He Z T，Wang X，Zhu Z H，Hu R Q，Liu C，Wang Q Q. Wearable non-invasive glucose sensors based on metallic nanomaterials［J］.Materials Today Bio，2023，20：100638.

［6］李静静，梁宽，张泽娜，张海麒，奚红霞，段崇雄. 纳米尺度多级孔金属-有机骨架材料应用研究进展［J］.稀有金属，2023，47（7）：1013.

J J Li，K Liang，Z N Zhang，H Q Zhang，H X Xi，C X Duan. Recent advances in application of nanoscale hierarchically porous metal-organic frameworks［J］.Chinese Journal of Rare Metals，2023，47（7）：1013.

［7］孔军，李蓉，刘勇，许立信，叶明富，万超. 金属催化剂催化水合肼分解制氢的研究进展［J］.稀有金属，2024，341（8）：1177.

J Kong，R Li，Y Liu，L X Xu，M F Ye，C Wang. Research progress of hydrogen production from hydrous hydrazine decomposition catalyzed by metal catalysts［J］.Chinese Journal of Rare Metals，2024，341（8）：1177.

［8］屠海令，赵鸿滨，魏峰，张青竹，樊彦艳，杜军. 新型传感材料与器件研究进展［J］.稀有金属，2019，43（1）：1.

H L Tu，H B Zhao，F Wei，Q Z Zhang，Y Y Fan，J Du. Research progress in advanced sensing materials and related devices［J］.Chinese Journal of Rare Metals，2019，43（1）：1.

［9］王步祥，舒庆. 单原子电催化析氢催化剂的研究进展［J］.有色金属科学与工程，2022，13（5）：92.

B X Wang，Q Shu. Research progress in single-atomic electrocatalytic hydrogen evelution reaction catalyst［J］.Nonferrous Metals Science and Engineering，2022，13（5）：92.

［10］Zhong S J，Lu B H，Wang D C，Arianpour B，Wang S L，Han H Y，Yin J Y，Bao H，Liu Y N，Wen Z，Zhou Y L. Passive isothermal flexible sensor enabled by smart thermal-regulating aerogels［J］.Advanced Materials，2025，37（8）：2415386.

［11］Mousty C，Farhat H. Recent advances in layered double hydroxides‐based electrochemical sensors：insight in transition metal contribution［J］.Electroanalysis，2023，35（7）：e202200527.

［12］沈思齐，王广铄，鄢非非，袁涛. 金属有机框架结构材料衍生的过渡金属单原子催化剂应用于氧还原电催化的研究进展［J］.稀有金属，2023，47（1）：28.

S Q Shen，G S Wang，F F Yan，T Yan. Research progress in MOF derived transition metal single atomic catalysts for oxygen reduction reaction［J］.Chinese Journal of Rare Metals，2023，47（1）：28.

［13］Qin B L，Pan Z J，Ye S R，Shen G Z，Liu Z，Yang W J，Liang P，He X. Interface engineering of NiCo LDH and 2D materials for advanced non-invasive glucose sensors［J］.Journal of Alloys and Compounds，2025，1010：177231.

［14］Wang X D，Zheng Y Y，Yuan J H，Shen J F，Hu J G，Wang A J，Wu L J，Niu L. Three-dimensional NiCo layered double hydroxide nanosheets array on carbon cloth，facile preparation and its application in highly sensitive enzymeless glucose detection［J］.Electrochimica Acta，2017，224：628.

［15］宋晓文，张恩磊，陈娇娇，徐睿，张本贵，王国胜. 钴铜层状双金属氢氧化物合成及其催化还原对硝基苯酚性能 的研究［J］.铜业工程，2024，（4）：22.

X W Song，E L Zhang，J J Chen，R Xu，B G Zhang，G S Wang. Synthesis of cobalt-copper layered double hydroxides and their catalytic reduction of 4-nitrophenol［J］.Copper Engineering，2024，（4）：22.

［16］Tang S，Yao Y，Chen T Y，Kong D Z，Shen W，Lee H K. Recent advances in the application of layered double hydroxides in analytical chemistry：a review［J］.Analytica Chimica Acta，2020，1103：32.

［17］文超举，刘春影，舒佳玉，陆婧，王欢，董强，徐星星. 纯钛表面氧化石墨烯涂层的制备及生物学性能研究［J］.有色金属工程，2024，14（2）：1.

C J Wen，C Y Liu，J Y Shu，Q Lu，H Wang，Q Dong，X X Xu. Preparation and biological properties of graphene oxide coating on pure titanium surface［J］.Nonferrous Metals Engineering，2024，14（2）：1.

［18］Fu S，Fan G L，Yang L，Li F. Non-enzymatic glucose sensor based on Au nanoparticles decorated ternary Ni-Al layered double hydroxide/single-walled carbon nanotubes/graphene nanocomposite［J］.Electrochimica Acta，2015，152：146.

［19］Zhou Y L，Wang Y N，Qiu S C，Zhao W，Wang S L，Bao H，Qu Y P，Wen Z. Microscopic response mechanism of epsilon-negative and epsilon-near-zero metacomposites［J］.Research，2025，8：0556.

［20］Zhuge Y F，Fan G L，Lin Y J，Yang L，Li F. A hybrid composite of hydroxyapatite and Ca-Al layered double hydroxide supported Au nanoparticles for highly efficient base-free aerobic oxidation of glucose［J］.Dalton Trans.，2019，48（25）：9161.

［21］Shen M，Li W，Chen L，Chen Yu X，Ren S B，Han D M. NiCo-LDH nanoflake arrays-supported Au nanoparticles on copper foam as a highly sensitive electrochemical non-enzymatic glucose sensor［J］.Analytica Chimica Acta，2021，1177：338787.

［22］丁成，蔚志红，巩春龙，乔瞻，张谷平. 黄金纳米复合材料工业化生产工艺设计及应用［J］.黄金，2023，44（5）：32.

C Ding，Z H Yu，C L Gong，Z Qiao，G P Zhang. Design and application of industrial production process for nano-gold composite materials［J］.GOLD，2023，44（5）：32.

［23］Wu Q B，Liang J W，Xiao M J，Long C，Li L，Zeng Z H，Mavrič A，Zheng X，Zhu J，Liang H W，Liu H F，Valant M，Wang W，Lv Z X，Li J，Cui C H. Non-covalent ligand-oxide interaction promotes oxygen evolution［J］.Nature Communications，2023，14（1）：997.

［24］Zhao Z T，Sun Y J，Song J X，Li Y J，Xie Y，Cui H，Gong W P，Hu J，Chen Y. Highly sensitive nonenzymetic glucose sensing based on multicomponent hierarchical NiCo-LDH/CCCH/CuF nanostructures［J］.Sensors and Actuators B：Chemical，2021，326：128811.

［25］Li M H，Fang L，Zhou H，Wu F，Lu Y，Luo H J，Zhang Y X，Hu B S. Three-dimensional porous MXene/NiCo-LDH composite for high performance non-enzymatic glucose sensor［J］.Applied Surface Science，2019，495：143554.

［26］Asadian E，Shahrokhian S，Iraji Z A. Highly sensitive nonenzymetic glucose sensing platform based on MOF-derived NiCo LDH nanosheets/graphene nanoribbons composite［J］.Journal of Electroanalytical Chemistry，2018，808：114.

［27］Shishegari N，Sabahi A，Manteghi F，Ghaffarinejad A，Tehrani Z. Non-enzymatic sensor based on nitrogen-doped graphene modified with Pd nano-particles and NiAl layered double hydroxide for glucose determination in blood［J］.Journal of Electroanalytical Chemistry，2020，871：114285.

［28］Lu Y，Jiang B，Fang L，Fan S Y，Wu F，Hu B S，Meng F M. Highly sensitive nonenzymatic glucose sensor based on 3D ultrathin nife layered double hydroxide nanosheets［J］.Electroanalysis，2017，29（7）：1755.

［29］Kang L Q，He D P，Bie L L，Jiang P. Nanoporous cobalt oxide nanowires for non-enzymatic electrochemical glucose detection［J］.Sensors and Actuators B：Chemical，2015，220：888.

Basic Information:

DOI：10.13373/j.cnki.cjrm.XY25030024

Chinese Library Classification Number:O657

Citation Information:

The global health crisis triggered by diabetes has accelerated the advancement of blood glucose monitoring technologies，prioritising non-invasive methodologies and sub-millimolar precision through demand-driven innovation. Enzyme-free glucose sensors，which directly oxidize glucose via electrocatalytic materials，have emerged as research hotspots due to their rapid response，exceptional stability，and cost-effectiveness. To address critical bottlenecks including the trade-off between sensitivity and detection range，mutual constraints between catalytic activity and electron transfer efficiency，and the inverse relationship between mass transport rate and structural stability，current research on electrocatalytic materials for enzyme-free glucose sensors has evolved from single-component optimization to multi-scale collaborative design. Nickel-cobalt layered double hydroxides （NiCo-LDH） have attracted significant attention in enzyme-free glucose sensing due to their unique 2D layered structure，tunable Ni²⁺/Ni³⁺ and Co²⁺/Co³⁺ redox couples，and high specific surface area. Their interlayer anion-exchange capability enables dynamic regulation of reaction microenvironments，while the bimetallic synergy reduces glucose oxidation activation energy，achieving a sensitivity of 1.55 mA· （mmol·L^-1）^-1·cm^-2 within 0.001~6 mmol·L^-1 range. However，inherent limitations including low intrinsic conductivity （<10^-3 S·cm^-1）and nanosheet stacking-induced mass transfer resistance restrict their wide-concentration detection capability. Although noble metal nanoparticle-modified 3D metal foam-supported NiCo-LDH structures have shown improved electron transfer and mass diffusion，challenges persist in controlling nanoparticle dispersion uniformity and preventing detachment during electrochemical cycling. To address these challenges，we proposed a porous AuRu alloy with high conductivity and 3D interconnected channels to simultaneously enhance electron transfer and glucose diffusion in NiCo-LDH-based sensors. The corrosion-resistant AuRu matrix （Ru doping enhanced passivation in acidic/alkaline media）ensured electrode durability. A hierarchical NiCo-LDH/AuRu/Au-SPE architecture was constructed through hydrogen bubble template-assisted AuRu deposition on commercial screen-printed Au electrodes，followed by NiCo-LDH electrodeposition. Field emission scanning electron microscope （FE-SEM） confirmed retention of the porous AuRu framework after NiCo-LDH integration. X-ray photoelectron spectroscopy （XPS）analysis verified successful formation of hydroxylated Ni²⁺/Ni³⁺ and Co²⁺/Co³⁺ species in the heterostructure. Systematic optimization revealed optimal performance at Ni/Co molar ratio=3∶2 with 300 s deposition time，achieving dual linear ranges （0.005~0.9 mmol·L^-1 and 0.9~11 mmol·L^-1）with sensitivities of 2.73 and 2.36 mA· （mmol·L^-1）^-1·cm^-2，respectively. The sensor demonstrated remarkable Cl^- poisoning resistance and anti-interference capability，attributed to synergistic interfacial electron coupling and hierarchical mass transport channels. These results confirmed that rational interface engineering and structural design effectively overcame the conductivity-catalytic activity trade-off in NiCo-LDH-based enzyme-free glucose sensors.