Hybrid Metal Organic Frameworks Research Articles

MOF-on-MOF Growth: Inducing Naturally Nonpreferred MOFs and Atypical MOF Growth.

ConspectusOverflowing metal-organic frameworks (MOFs) have been synthesized from a wide range of metal and organic components for specific purposes and intellectual curiosity. Each MOF has unique chemical and structural characteristics directed by the incorporated components, metal ions (or clusters), organic linkers, and their intrinsic coordination interactions. These incorporated components and structural characteristics are two pivotal factors influencing MOFs' fundamental properties and subsequent applications. Therefore, selecting the appropriate metal and organic components, considering their innate chemical and structural properties, is crucial to endow the final MOFs with the desired properties. Ultimately, producing MOFs with a desired structure using ideal components is the best approach to achieving the best MOFs tailored for specific purposes with desired properties. However, achieving MOFs with the intended structure from chosen components remains underdeveloped. In many cases, the resulting MOF structure is governed by the thermodynamically and/or kinetically preferred configuration (refers to a naturally preferred structure) of the chosen components and given reaction conditions. Additionally, producing hybrid MOFs with complex components, structures, and morphologies presents a great opportunity to obtain special MOFs with advanced properties and functions. In this Account, we outline our group's efforts over the past few years to develop naturally nonpreferred MOFs through the induced MOF-on-MOF growth process and atypical hybrid MOFs via nonstandard MOF-on-MOF growth. First, we highlight the prime strategy for producing naturally nonpreferred MOFs based on template-induced MOF-on-MOF growth. In this section, we discuss the two basic growth behaviors, isotropic and anisotropic growth of naturally nonpreferred MOFs, determined by the degree of matching between the cell lattices of the two MOFs. Second, we introduce the MOF farming concept for the productive cultivation and effective harvesting of naturally nonpreferred MOFs made by MOF-on-MOF growth. Here we discuss the importance of selecting the ideal MOF template for productive growth and developing an efficient method for harvesting cultivated MOFs. Next, we describe atypical anisotropic MOF-on-MOF growths between two MOFs with mismatched cell lattices. In this section, we introduce tip-to-middle MOF-on-MOF growth involving self-structural adjustment of the secondary MOF, logical inference of unidentified MOF structures based on MOF-on-MOF growth behavior and morphological features, and MOF-on-MOF growth accompanied by etching and transformation of the template. Finally, we discuss the perspectives and challenges of MOF-on-MOF growth and the synthesis of naturally nonpreferred MOFs. We hope that this Account offers valuable insights into the rational design and development of MOFs with desired structural and compositional characteristics, leading to the creation of ideal MOFs.

Perovskite/cobalt-based metal-organic framework hybrid promotes hydrogen production from oilfield wastewater electrolysis

Hydrogen has been recognized as a new green energy source. However, in regions where fresh water is scarce, research on the use of complex water systems, such as seawater and oilfield wastewater, to produce hydrogen by electrolysis instead of fresh water has become a pressing issue. In this paper, a low-cost and easy-to-synthesized hybrid catalyst composed of perovskite oxide SrCo0.7Fe0.3O3-δ (SCF) and cobalt-based metal-organic framework (Co-MOF) were synthesized using a simple and feasible in-situ coprecipitation method and exhibited excellent hydrogen evolution reaction (HER) activity in oilfield wastewater. The improvement of activity can be attributed to the synergistic effect between the two materials, which have more concentration of oxygen vacancies and more HER active sites due to Co ion migration. This work provides a practical approach to enhance HER activity in complex water systems by constructing spatial composite structures.

A sensitive electrochemical aptasensor based on MOF-74(Mg)/GO for impedimetric detection of ultra-trace streptomycin

Metal–organic frameworks (MOFs), as a class of functional porous materials, have gained extensive attention for constructing excellent electrochemical aptasensors. To overcome the insufficient conductivity of MOF materials, various conductive materials are gradually applied to assemble with MOFs. At present, the construction of sensitive MOF hybrid material-based electrochemical aptasensor is still significant importance. In this work, a hybrid material, namely MOF-74(Mg)/GO, is successfully synthesized by the in situ assembly of MOF-74(Mg) and graphene oxide (GO). The as-synthesized composite possesses the advantages of MOF-74(Mg) and GO, resulting in the fabricated electrochemical aptasensor with excellent detection performance toward ultra-trace streptomycin via electrochemical impedance spectroscopy.

Molecular sieves hybrid metal–organic framework for efficient simultaneously capturing carbon dioxide and collecting water from air

Water scarcity and climate change associated with global warming are two common challenges facing humankind. The simultaneous removal of water and carbon dioxide (CO2) from the air has become a popular candidate strategy to address these challenges. In this paper, molecular sieve@MOF composites were synthesized in-situ for the first time by adding ZSM-5 and HZSM-5 during the preparation of Mg/DOBDC. A comprehensive review of the air capture CO2 and water harvesting properties of the novel composites was also presented. Primarily, the effects of molecular sieve category and ratio on the composite were systematically investigated. Subsequently, the crystal structure, morphological composition and textural properties of the composites were characterized. Finally, CO2/H2O co-adsorption performance, adsorption and desorption cycle stability and adsorption mechanism were investigated. The results demonstrated that the metal nodes of Mg/DOBDC interacted with the molecular sieve surface functional groups to increase the metal active sites and porosity. The obtained 0.5HZSM-5@Mg/DOBDC MOF showed the maximum CO2 uptake of 15.90 mmol/g (0.1 MPa, 25 °C), which was 3.66 times the amount of Mg/DOBDC.

Sulfidation and reassembly strategy enables yolk-shell metal sulfide/alloy nanoparticles @carbon with efficient electromagnetic wave absorption

Constructing hybrid metal-organic frameworks (MOFs) demonstrates significant potential to improve electromagnetic wave (EMW) absorption performance by leveraging synergistic effects between composition and structure, addressing challenges in tuning electromagnetic parameters of single-composition MOFs. This study proposes a sophisticated strategy involving sulfidation-interface growth-reassembly: sulfide nanoparticles form by sulfidating the core (CoFe-MIL-88A), and then ZIF-67 guests grow and reassemble on the sulfided host MOF, resulting in a layered EMW absorption material. The composite material integrates synergistic effects, which include high conductive loss and defect/interface/dipole polarization induced by N and S atom doping. The CFSNC composite material outperforms previously published values, achieving a minimum reflection loss (RLmin) of −65.96 dB and an effective absorption bandwidth (EAB) of 6.15 GHz with a thickness of merely 2 mm. Simulation calculations of the real far-field radar cross-section (RCS) further validate its practical application potential. This work introduces novel ideas and methods for designing and preparing high-performance EMW absorption materials, offering both theoretical insights and practical applications.

Integrating sodium cholate-modified MOF hybrid lipase and solubilization of hydrophobic candidates into a step for liganding fishing lipase inhibitors from Nelumbinis Folium

Enzyme immobilization by metal organic frameworks (MOFs) is an efficient way for screening active constituents in natural products. However, the enzyme’s biocatalysis activity is usually decreased due to unfavorable conformational changes during the immobilization process. In this study, sodium cholate was firstly used as the modifier for zeolitic imidazolate framework-8 (ZIF-8) immobilized lipase to increase both the stability and activity. More importantly, with the help of solubilization of sodium cholate, a total of 3 flavonoids and 6 alkaloids candidate compounds were fished out. Their structures were identified and the enzyme inhibitory activities were verified. In addition, the binding information between the candidate compound and the enzyme was displayed by molecular docking. This study provides valuable information for the improvement of immobilized enzyme activity and functional active ingredients in complicated medicinal plant extracts.

Nanosize Controllable Two‐Dimensional (Cu–S)n Metal–Organic Framework Hybrid With Reduced Graphene Oxide by In Situ Microwave and Hydrothermal Synthesis for Electrochemical Neurotransmitter Detection

ABSTRACTWe present a groundbreaking technique for controllably synthesizing nanosized semiconductive two‐dimensional (2D) (Cu–S)n metal–organic framework (MOF)/graphene nanocomposites for electrochemical sensing of neurotransmitter 2‐phenethylamine (PEA). The (Cu–S)n MOF size is controlled by graphene oxide proportions, enhancing electrocatalytic activity. The modified electrode exhibits a surface area increase from 0.0639 to 0.1906 cm2 and impressive limit of detection (0.0156 and 0.004 μM) within linear ranges of 15–200 μM and 1–10 μM, offering exceptional selectivity, reproducibility, and repeatability for biosensing.

A ternary heterostructure aptasensor based on metal-organic framework and polydopamine nanoparticles for fluorescent detection of sulfamethazine

Residue of sulfamethazine (SMZ), a typical short-acting drug to prevent bacterial infections, in food is a threat to human health. A ternary heterogeneous metal-organic framework hybrid (Zn/Fe-MOF@PDANSs) of Zn-TCPP-MOF, MIL-101 (Fe) and polydopamine nanoparticles (PDANSs) was proposed to establish an aptasensor for the sensitive and selective detection of SMZ. In this sensor, Zn-TCPP-MOF and FAM emitted fluorescence at 609 nm and 523 nm, respectively, and the fluorescence of FAM-ssDNA could be quenched when it was adsorbed on the surface of MOF hybrid. In the presence of SMZ, the fluorescence of FAM-ssDNA recovered due to the dropping from MOF hybrid, while the fluorescence of MOF hybrid remained. With this strategy, a wide concentration range and high sensitivity of SMZ were detection. And the ternary Zn/Fe-MOF@PDANSs sensor exhibited more excellent performance than binary Zn/Fe-MOF aptasensor. In addition, the sensor showed pleasurable selectivity, and was utilized for SMZ determination in authentic chicken and pork samples, implying the fascinating potential in practical application.

Metal-Organic-Frameworks Based Mixed-Matrix Membranes for CO2 Separation: An Applicable-Conceptual Approach.

A promising class of porous crystalline materials, metal-organic frameworks (MOFs), have recently emerged as a potential material in fabricating mixed matrix membranes (MMMs) for gas separation applications. Their unique chemistry and structural versatility offer substantial advantages over conventional fillers. This review gives an in-depth exploration of MOF chemistry, focusing on strategies to manipulate their adsorption behavior to enhance separation properties. We scrutinize the impact of various MOF-based MMM components, including polymer matrix, MOFs fillers and polymer/filler interface, on the overall gas separation performance. This involves a detailed analysis of key parameters associated with MMM preparation. Additionally, we offer a comprehensive overview of the determining factors in MOF-based MMM development for gas separation, including MOF structure, synthesis, and chemistry. Moreover, the most advances in modification strategies of MOF for CO2 separation, such as a wide variety of hybrid MOFs will be outlined, which opens the door to an improved CO2 separation process. Finally, the gas transport mechanisms of MMMs are thoroughly discussed to understand the factors affecting the gas permeation through the polymer matrix, MOFs and interface between them.

Achieving a balance between permeability and selectivity in a ZIF-8-matrix nanocomposite membrane for desalination

Hybrid metal–organic framework (MOF)-polymer membranes are promising for addressing the permeability-selectivity tradeoff in membrane applications. The key challenges for achieving high-efficiency separation performance have been identified as increasing the MOF loading while maintaining interfacial compatibility with polymeric matrices. Herein, a novel design of ZIF-8 matrix nanocomposite membrane, with ZIF-8 nanoparticles (NPs) serving as the main matrix, was prepared by functionalizing the external surface of zeolitic imidazolate framework-8 (ZIF-8) NPs with polyethyleneimine and subsequent crosslinking into the selective layer using trimesoyl chloride as a crosslinking agent via confined interfacial polymerization. The content of ZIF-8 NPs in the selective layer was up to about 70 wt%, resulting in superior permeability (＞ 43.6 LMH bar−1) for desalination due to the large number of transport channels, which was several folds as compared to most of the reported membranes. Meanwhile, a reasonably high Na2SO4 rejection (∼95.1 %) was maintained as the polyamide fragments formed during interfacial polymerization, which filled defects among the ZIF-8 NPs. Overall, such strategy paves the way for the design of efficient MOF-based membranes for balancing between permeability and selectivity in desalination.

Cyclodextrin-metal-organic framework (CD-MOF)/ organic-inorganic hybrid composite as a potential material for drug delivery devices

Metal-organic frameworks (MOFs) constitute a distinctive class of materials composed of metal ions or clusters intricately linked by organic ligands. Among MOFs, γ-cyclodextrin- based MOFs (γ-CD-MOFs) have attracted significant attention for their potential in edible, non toxic, and renewable applications. This study introduces a facile and environmentally friendly method for synthesizing γ-CD-MOFs, integrated with a ureasyl-polyether film to develop a cutaneous patch exhibiting a unique release profile. This system's physicochemical properties, encapsulation, and release kinetics were rigorously evaluated using Ibuprofen as a model anti-inflammatory drug. The resulting films, integrated with γ-CD-MOFs, exhibited an impressive encapsulation efficiency exceeding 80 %, and a controlled release effect. Notably, the system demonstrated superior ability in sustaining Ibuprofen release, indicating a synergistic combination of multiple mechanisms, including drug diffusion and erosion of metal-organic frameworks. The comprehensive findings underscore the potential of these systems as effective topical drug-delivery platforms, meeting the stringent criteria of releasing less than 10 % of the payload within 12 h. This study emphasizes the crucial role of rational MOF and organic-inorganic hybrid selection, shedding light on the intricate interplay of chemical parameters among MOF, polymer, and drug, which significantly influence drug adsorption and release dynamics. The outcomes presented herein contribute to advancing our understanding of MOF-based drug delivery systems and highlight their promising future applications in pharmaceutical research.

Modified metal–organic frameworks for sonophotocatalytic elimination of wastewater pollutants

In recent decades, people have witnessed a rapid development of society, accompanied by the increase sharply of numerous organic/inorganic contaminants from industrial effluents. The high toxicity of pollutants has led to long‐term risk to human health. To connect with environment‐friendly green chemistry and sustainable development, photocatalysis technology has emerged. Metal–organic framework (MOF)‐based photocatalysts performed high efficiency for the elimination of wastewater pollutants. Nevertheless, the large band gap energy and high recombination rate of photogenerated electron–hole pair decrease the catalytic efficiency. Sonochemistry is regarded as a safe, highly efficient, clean, and eco‐friendly technology, which has aroused a lot of interest in the treatment of wastewater. The cavitation effect induced by ultrasonic waves promotes the generation of additional active radicals. The ultrasonic oscillation facilitates cleaning the surface of catalysts, dispersing catalyst particles, and increasing proton transport. Therefore, photocatalysis coupling with ultrasonic waves, known as sonophotocatalysis (SPC), is a promising means for enhancing the overall performance of wastewater treatments. This review discusses the recent advancements of hybrid MOF‐based photocatalysts driving the wastewater treatments in SPC system. The catalytic performance of hybrid MOF is discussed in the SPC process. The inner properties of phases in hybrid MOF such as the location of redox potential and transfer direction of electrons and energy after hybridization are elucidated. Additionally, the review discusses the existing challenges and obstacles of MOF‐based SPC system and proposes feasible improvements to meet the future requirements of practical applications.

Nanoscale CdS enwrapped zeolite-like Zn-MOF nanocomposite for advanced energy storage systems

With reference to the promising characteristics of metal–organic frameworks (MOFs) and the contributions of nanoparticles (NPs) to their electrochemical activities, the hybrid MOF built with metal sulphides has garnered a lot of attention, primarily as electrode materials in energy storage devices. The polyhedral-shaped CdS enwrapped zeolitic imidazolate framework-8 (ZIF-8) nanocomposites have been prepared by in-situ chemical synthesis. The electrochemical performance was evaluated in 6 M KOH electrolyte, achieving a specific capacitance of 1063.48 Fg−1 at 5 mV/s. The nanocomposite electrode material exhibits good cyclic stability, with 82.32 % (6 M KOH) and 85.91 % (redox additive electrolyte) capacity retention after 6000 cycles at 5 A/g. The energy and power density of the asymmetric supercapacitor were found to be 2.81 Wh/kg and 1785.71 W/kg, respectively.

Metal-organic framework/MXene nanohybrid composites as an emerging electrochemical sensing platform for food safety and biomedical monitoring: From synthesis to application

Metal-organic frameworks (MOFs) are created through the self-assembly process of metal ions or clusters with organic linkers. These materials have attracted important interest owing to their advantageous features, comprising abundant pore structures, ultrahigh porosity, and well-exposed active sites. However, some traditional MOFs have limitations in terms of low stability and conductivity. Despite significant endeavors to enhance the stability of MOF materials, limited advancement has prompted researchers to concentrate on the development of hybrid materials. MXenes, a group of 2D transition-metal compounds comprising nitrides, carbides, and carbonitrides, are recognized for their diverse composition and their ability to form various buildings with rich surface chemistry. The hybridization of MOFs with functional MXene layered could be advantageous if the host structure offers suitable interactions to enhance and stabilize the desired features. Current research has concentrated on incorporating MXenes and MOFs to generate nanohybrid materials with boosted electrochemical features, thus broadening the scope for new applications. This review explores potential design approaches for MXene@MOF nanohybrids, the tunable characteristics of the resulting hybrids, and their use in electrochemical sensing platforms for food safety and biomedical monitoring. Finally, the authors discuss the challenges and future opportunities of MOF@MXene-derived nanocomposites.

Microwave-Enabled Fast Preparation of a Metal-Organic Framework Hybrid Membrane for Filtration-Enhanced Simultaneous Separation and Detection of Aflatoxin B1.

Mycotoxin contamination in food and the environment seriously harms human health. Sensitive and timely detection of mycotoxins is crucial. Here, we report a dual-functional hybrid membrane with absorptivity and responsiveness for fluorescent-quantitative detection of mycotoxin aflatoxin B1 (AFB1). A biomineralization-inspired and microwave-accelerated fabrication method was established to prepare a hybrid membrane with a metal-organic framework (MOF) loaded in high density. The MOF presented high efficiency in capturing AFB1 and showed fluorescence intensity alteration simultaneously, enabling a dual adsorption-response mode. Deriving from the inherent porous structure of the hybrid membrane and the absorptive/responsive ability of the loaded MOF, a filtration-enhanced detection mode was elaborated to provide a 1.67-fold signal increase compared with the conventional soaking method. Therefore, the hybrid membrane exhibited a rapid response time of 10 min and a low detection limit of 0.757 ng mL-1, superior to most analogues in rapidity and sensitivity. The hybrid membrane also presented superior specificity, reproducibility, and anti-interference ability and even performed well in extreme environments such as strong acid or alkaline, satisfying the practical requirements for facile and in-field detection. Therefore, the membrane had strong applicability in chicken feed samples, with a detection recovery between 70.6% and 101%. The hybrid membrane should have significant prospects in the rapid and in-field inspection of mycotoxins for agriculture and food.

Assembly of Amorphizing Porous Bimetallic Metal‐Organic Frameworks Spheres with Zn─O─Fe Cluster and Coordination Deficiency via Ligand Competition for Efficient Electro‐Fenton Catalysis

AbstractElectro‐Fenton process stands out as a highly promising approach for generating reactive oxygen‐containing radicals to address the escalating issue of environmental pollution. However, the long‐term goal of application necessitates ongoing pursuit of high‐quality catalysts with both sufficient activity and stability. Herein, a general route is reported for large‐scale synthesis of amorphizing porous bimetallic metal‐organic framework (MOF) spheres with Zn─O─Fe structure and coordination deficiency through facile and low‐cost synthesis of ligand competition. Assisted by a coordination modulator, deprotonation of terephthalic acid is accelerated and rapid synthesis of amorphous bimetallic MOF spheres is successfully achieved at room temperature. As inactive metal Zn is introduced into metal clusters of MOFs, the cycling efficiency of Fe3+/Fe2+ is improved and a secondary building unit of Zn─O─Fe is constructed, greatly accelerating electron conduction rate. Compared to crystalline spindle cMIL‐88B(Fe2Zn) by traditional solvothermal route, amorphous aMIL‐88B(Fe2Zn) has a unique spherical porous structure with larger surface area, higher conductivity, and more exposed active sites. Endowed with unique textural and surface chemistry, aMIL‐88B(Fe2Zn) exhibits superior catalytic activity in the degradation of refractory organic pollutants. The progress offers a feasible way to rational design of iron‐based hybrid MOF materials with tunable structures and enhance properties for various applications.

Graphene conductance modulation through controlled molecular release in a hybrid coordination polymer/graphene field-effect transistor

Coordination polymers, including metal-organic frameworks (MOFs), present a wide range of functionalities ranging from sensing to energy storage. Despite this, many coordination polymers are typically insulating which prevents their implementation into nanoscale electronic devices. Besides, the hybridization of MOFs with other conducting materials, like graphene, is rather unexplored. Here we introduce the grafting of a soft non-porous coordination polymer, the 1·2CH3CN, on a single-layer graphene to form a hybrid 1·2CH3CN/graphene field effect transistor. Electron transport measurements show that the sharp structural transformations in 1·2CH3CN, triggered at two specific temperatures, are detected in graphene as two sharp increments in the electrical current. Gate spectroscopy measurements show that the origin of the electrical modulation is an abrupt p-doping due to the sudden release of acetonitrile right at the structural transition temperatures. Reciprocally, the sensitivity of graphene to external perturbations allows to detect additional transformations in the coordination polymer not observed in direct transport measurements across crystals. Finally, the results have been reproduced in in-situ grown 1·2CH3CN nanoscale films on CVDG FETs. This simple method optimizes the contact area between graphene and 1·2CH3CN and facilitates the integration of coordination polymers with van der Waals materials and electronic devices. Further, a selective doping at specific temperatures could be obtained by modifying the nature of the interstitial molecule in 1.

Universal Strategy for Metal-Organic Framework Growth: From Cascading-Functional Films to MOF-on-MOFs.

Transformation of metal-organic framework (MOF) particles into thin films is urgently needed for the persistent development of well-applicable devices, and recently emerging functional-integrated hybrid frameworks. Although some flexible polymers and exclusive modification approaches have been proposed, the additive-free and widely applicable strategy has not been reported, hampering the deep investigation of the structure-performance relationship. A universal strategy for the in situ growth of large-area and continuous MOF films with controllable microstructures is introduced, through the modification of multi-scale and multi-structure substrates with poly(4-vinylpyridine) as the anchor to capture metal ions via Coulomb attraction. Based on the clarified structure-adsorption-separation mechanisms, the customized devices fabricated by in situ growth can achieve highly selective adsorption and excellently synergetic separation of various industrially relevant isomers. In addition, this strategy is also feasible for the construction of MOF-on-MOFs with varied lattice parameters. This strategy is easy to implement and will be widely applicable to the surface growth of diverse MOFs on desired substrates, and provides a new concept for developing hybrid MOFs integrating with customized functionalities.

In-situ construction of Ti3C2TX/Ni-HHTP heterostructure as anode for lithium-ion batteries

Pursuing anode materials with high specific capacity and long cycle stability is critical for advanced lithium-ion batteries (LIBs). Metal-organic frameworks (MOFs) with high specific surface area, regular pore channels, and multiple active sites are promising anode materials for LIBs. However, the poor electronic conductivity limits their application in LIBs. Thus, introducing some conducting materials is necessary. MXene, known for its excellent electronic conductivity in electrochemical energy storage systems, is an ideal candidate. Herein, a heterostructure composite material (Ti3C2TX/Ni-HHTP) that combines the advantages of both MOFs and MXene has been synthesized via an in-situ growth method, the composite exhibits regular pore channels, enhanced electronic conductivity, and excellent stability. When it is used as an anode material in LIBs, the composite presents satisfying rate performance and cycling stability. The initial discharge capacity of the Ti3C2TX/Ni-HHTP electrode exhibits 424.4 mA h g−1 at 0.5 A g−1 and remains at 390.2 mA h g−1 after 800 cycles with a capacity retention rate of 92.0%. This design strategy provides valuable insights into constructing MOF hybrid materials with enhanced electronic conductivity for various electrochemical applications.

Enhanced simultaneous voltammetric detection of dopamine and uric acid using Au@Ni‐metal–organic framework‐modified electrode

A novel conductive Ni‐based metal–organic framework (MOF) decorated with Au nanoparticles (AuNPs; Au@Ni‐MOF) was developed and used as a drop‐cast thin‐film electrode to individually and simultaneously quantify dopamine (DA) and uric acid (UA). The Ni‐MOF composite was synthesized using an in situ growth strategy involving the growth of [Ni3(BTC)2(H2O)6]n (BTC = 1,3,5‐benzenetricarboxylate) with coordinatively unsaturated Ni (II) sites. The Ni‐MOF powder was then mixed with a AuNP solution to produce a Au@Ni‐MOF hybrid material. The synthesized Au@Ni‐MOF hybrid material was employed as a surface modifier for a screen‐printed carbon electrode, and its efficacy for the detection of DA and UA was assessed using differential pulse voltammetry (DPV) and cyclic voltammetry. The developed sensor exhibited remarkable sensitivity, achieving low detection limits of approximately 0.027 and 0.028 μM (S/N = 3) in the simultaneous quantification of DA and UA, respectively. The sensor exhibited an extensive linear range of 0.5 μM to 1 mM, coupled with excellent sensitivities for DA and UA of 1.43 and 1.35 μA μM−1 cm−2, respectively. Furthermore, the sensor performance in human serum and urine samples was successfully validated using DPV, which revealed outstanding recovery rates of 93.8–105.0% with a minimal relative standard deviation below 3%. Moreover, the synthesized Au@Ni‐MOF composite exhibited exceptional dispersion stability, high sensitivity, and remarkable selectivity, which were attributed to the well‐arranged combination of AuNPs and Ni‐MOFs, enabling its use in non‐enzymatic sensing applications targeting DA and UA.