
The intrinsic physical anisotropy of low-symmetry materials makes them highly promising candidates for polarization-sensitive devices. However, their practical application remains constrained by the scarcity of single materials that can combine low symmetry with high performance. Here, we report a novel low-symmetry [Bi2CuO3]SO4 crystal with an insulating nature, designed to enable symmetry control over conventional high-performance semiconductors. We achieve controllable growth of layered [Bi2CuO3]SO4 nanosheets via a gradient-mass-transfer-assisted chemical vapor deposition method, with thicknesses down to 1.43 nm. Alternating [Bi2CuO3]2+ cationic layers and SO4 2- anionic layers, coupled with disparate ionic radii of Bi3+ and Cu2+, endow the [Bi2CuO3]SO4 material with low structural symmetry, resulting in pronounced in-plane optical anisotropy. Upon integration with high-symmetry MoS2, [Bi2CuO3]SO4 induces interfacial symmetry breaking, driven by strong interfacial coupling and substantial charge redistribution. Notably, by fabricating devices along different crystallographic orientations of [Bi2CuO3]SO4, tunable polarization ratios are exhibited, reaching a maximum of 5.44 along the a-axis and a minimum of 1.57 along the b-axis. This work establishes a reliable strategy for obtaining heterostructures with low symmetry and tunable anisotropy, advancing next-generation directional optoelectronic devices.
Electrocatalytic nitrate reduction reaction (NO3RR) to ammonia has been regarded as a sustainable strategy for industrial wastewater denitrification and fertilizer manufacturing toward green nitrogen circulation. However, complex pH conditions of practical nitrate wastewater result in poor catalyst universality, severely hindering their long-term deployment. Furthermore, the underlying reaction mechanisms in different pH scenarios remain ambiguous, obstructing the rational design of pH-universal electrocatalysts. Here we propose a crystal phase engineering approach to enhance the NO3RR performance in complex pH scenarios. The as-designed unconventional face-centered cubic (fcc) RuW nanoflowers exhibit excellent ammonia Faradaic efficiency (FE) above 91.0% over a wide pH range of 1-14, with the largest yield rate of 40.1 mg h-1 mgcat -1. Mechanism studies indicate that fcc RuW nanoflowers adaptively steer reaction pathways toward diverse pH environments. Based on the long-term durability test at an industrial-level current density of 300 mA cm-2 for 200 h in flow reactors, techno-economic analysis with the optimized process further demonstrates promising application potential. This study not only provides a fundamental insight into the pH-dependent mechanisms of nitrate electroreduction, but also offers a robust catalyst design approach toward complex practical conditions.
Inverted perovskite solar cells (PSCs) possess great potential for improving efficiency and operating stability, but parasitic charge recombination at the interfaces still limits their performance. As additives and surface treatment agents, ammonium ligands have been reported to form either two/three-dimensional (2D/3D) heterojunctions or passivation layers. In this work, we first conduct a comprehensive, large language model (LLM)-enabled literature mining to systematically enumerate ligand molecules reported over the past decade, through which we identify a pronounced knowledge gap concerning thiazole-based ligands. Then, in a comparative case study, perovskite films are treated with two thiazole- and thiophen-based ligands, which are small rigid aromatic heterocycles with similar molecular conformation. Thiophen-2-ylmethanamine hydrochloride (TPMA) induces 2D phase formation within 3D perovskite films. In comparison, 1,3-thiazol-2-ylmethanamine hydrochloride (TMA), with enhanced charge-transfer interactions associated with the S ions on the aromatic rings, demonstrates a stronger defect passivation capability. Overall, the TMA-based counterpart exhibits lower defect density, extended carrier lifetime, and a more favorable band offset. With the thiazole-based ligand, the resulting inverted PSC achieves an efficiency of 26.81% (certified 26.43%) and retains 96.4% of its initial performance after 1000 h tracking under continuous illumination at the maximum power point.
Electrically-driven hydrogels are crosslinked, charged polymer networks that can deform in an electric field, prompted by osmotic pressure changes. To date, such actuators generally suffer from sluggish response time, with equilibrium actuation times ranging from minutes to hours in aqueous electrolytes, and lack sophisticated design, due to established manufacturing protocols. Herein, these limitations are overcome through the fabrication of polyelectrolyte hydrogel microstructures via two-photon polymerization (2PP). This approach allows for the realization of microscale electrically-driven actuators exhibiting fast actuation (∼200 ms equilibrium time). The work highlights three photoresist formulations for poly(anionic) and poly(cationic) hydrogel networks and their fabrication via 2PP to produce micro-electro-actuators with sub-micron features. The electrically-driven actuation performance is investigated by varying the hydrogel composition, actuator geometry, along with electric field strength and direction, and local environment (pH and electrolyte concentration) during actuation. It was determined that micro-cantilevers of 80 × 20 × 10 µm3 reached equilibrium bending of up to 44.9 ± 7.8°, in ∼ 200 ms, in response to electric fields of 6 V mm-1. This pioneering work marks the first integration of 2PP with electrically actuated gelatin-based hydrogels, showcasing micro-electro-actuators with rapid and programmable 4D motion.
The complementary structural tunability of polymers of intrinsic microporosity (PIMs) and metal-organic frameworks (MOFs) redefines the design space for engineering precise transport channels in mixed-matrix membranes (MMMs). Herein, we present that trace-oxygen-mediated thermal reorganization (TOTR) of PIM-1 micropores enables MOF-dominated gas transport in MMMs without requiring high filler loading. Spectroscopic analyses and molecular simulations reveal trace-oxygen-mediated radical processes that induce the PIM-1 backbone rearrangement, together with triazine crosslinking and partial π-conjugation extension, resulting in a contracted and homogenized ultramicropore distribution. Meanwhile, the dual-interface design establishes a covalently coupled MOF-polymer interface, where the interfacial carboxylated PIM-1 (cPIM-1) layer co-reorganizes with the polymer matrix to form an integrated microporous environment with suppressed defects and enhanced mechanical robustness. This coupled pore-and-interface regulation integrates PIM-1 ultramicropores and MOF micropores into pore-matched transport channels, enabling effective expression of MOF sieving capability at an ultralow filler loading of 2 wt.%. The resulting MMMs deliver approximately threefold enhancement in CO2/CH4 and CO2/N2 selectivity compared with PIM-1 membranes, while maintaining high CO2 permeability and improved resistance to physical aging and plasticization. This study may broaden the design concepts for advanced MMMs toward challenging molecular separations.
The diagnosis of bacterial infections remains slow because many existing methods rely on enrichment steps such as nucleic acid amplification or growth culture. RNA-cleaving DNAzymes offer a promising route to accelerate bacterial diagnosis because they can be selected and programmed to specifically recognize disease-causing bacteria and generate reporter DNA strands for signal readout. However, integrating DNAzymes into biosensors capable of analyzing complex biological matrices remains challenging, as matrix-associated interferents can destabilize DNAzymes, suppress catalytic activity, and compromise signal detection. Here, we integrate redox RNA-cleaving DNAzymes housed on antifouling magnetic beads with a lab-in-a-tube platform that incorporates hierarchically structured sensing electrodes within a tubular flow cell for enrichment-free detection of Clostridioides difficile in stool samples. The combination of antifouling magnetic beads and fluidic replenishment of DNA reporters across the hierarchical electrodes reduces nonspecific binding and enhances reporter capture efficiency, achieving a limit of detection as low as 1.3 × 102 CFU mL-1 in buffer. Using an optimized stool-processing procedure, the sensor enabled detection of C. difficile infection in 38 human stool samples, demonstrating 94.7% concordance with the current gold-standard polymerase chain reaction method. These results demonstrate a promising platform for enrichment-free, point-of-care diagnosis of infectious diseases in clinic settings.
Negative differential resistance (NDR), a counterintuitive transport phenomenon in which current decreases with increasing voltage, challenges conventional transistor-centric computing paradigms based on monotonic electronic transport and opens new opportunities for beyond-Boolean computing. Here, we present a comprehensive and concept-driven review of NDR devices spanning memristor-based, diode-type, and transistor-based platforms. We establish a unified framework that links diverse NDR mechanisms, including resonant tunneling, electrothermal feedback, defect dynamics, and ferroelectric polarization, through their shared nonmonotonic transport characteristics. Beyond device-level classification, we further propose NDR as a physical foundation for functionally compressed computing, in which circuit functionalities traditionally implemented using multiple transistors and feedback networks can be partially embedded into the intrinsic nonlinear response of a single NDR device or compact device unit. We further compare representative NDR technologies using common performance metrics and analyze the key challenges that currently limit large-scale deployment, including variability, CMOS compatibility, compact modeling, and the distinction between intrinsic NDR behavior and measurement-induced artifacts. Finally, we discuss future opportunities in materials-by-design, heterogeneous and 3D integration, physics-informed modeling, and closed-loop intelligent systems. By connecting nonmonotonic transport physics with circuit and system-level functionality, NDR electronics offers a promising route toward compact and energy-efficient computing architectures in the post-Moore era.
Renewable-electricity-driven electrocatalysis is difficult to maintain under steady-state operation because of the intermittent, variable, and stochastic nature of renewable power. This challenge is particularly critical for selective electrocatalytic hydrogenation (ECH), such as phenol-to-cyclohexanone conversion in acidic media, where fluctuating operation can induce transient accumulation of active hydrogen intermediates, compromising product selectivity and energy efficiency. In this study, we develop a dynamic active-hydrogen-buffering interface strategy to construct fluctuation-resistant electrocatalysts using the short-chain surfactant butyltrimethylammonium bromide (BTAB). Under simulated power fluctuations in a flow cell, the BTAB-modified catalyst maintains near-steady-state performance, achieving 90.1% cyclohexanone selectivity and 83.6% Faradaic efficiency (FE), and outperforms the unmodified system by 1.69-fold in cyclohexanone FE under more drastic fluctuations. Mechanistic studies reveal that the BTAB layer weakens the interfacial hydrogen-bond network and attenuates Grotthuss-type proton relay, thereby regulating proton flux and buffering active hydrogen accumulation during current fluctuations. This suppresses competing hydrogen evolution and overhydrogenation to cyclohexanol while preserving phenol hydrogenation kinetics. Combined with techno-economic analysis, this work establishes active-hydrogen buffering as an interfacial strategy for maintaining selective electrosynthesis under dynamic operating conditions.
Nickel-based layered cathodes are promising candidates for high-performance, high-energy lithium-ion batteries, yet their high-voltage application is jointly limited by synthesis-inherited structural defects and an unstable lattice oxygen framework. Here, we show that both limitations can be overcome by decoupled synthesis pathway (DSP) via La/Nb oxalate functionalization of the Ni0.6Co0.1Mn0.3(OH)2 precursor. Unlike the conventional coupled synthesis pathway (CSP) where precursor dehydration and Li2CO3 decomposition overlap in temperature, the DSP introduces a low‑temperature decomposition of La/Nb oxalates at 200°C, which effectively avoids localized contact between the precursor and Li2CO3 and shifts Li2CO3-related reactions to high temperatures. This allows sequential precursor dehydroxylation, rock‑salt (RS) intermediate formation, and layered‑phase transformation over a broad temperature window. The resulting LiNi0.6Co0.1Mn0.3O2 cathode with La/Nb functionalization (NCM-LN) features a uniform surface LaNiO3 perovskite heterostructure and a Nb‑doped layered bulk with suppressed RS and spinel defects. Consequently, under 4.5 V operation (vs. Li+/Li), NCM-LN exhibits homogeneous Li+ (de)intercalation, and a stabilized oxygen framework. In graphite||NCM-LN full cells, NCM-LN retains 80.1% of its capacity after 2000 cycles at 1C, substantially outperforming the pristine cathode. This decoupling strategy is broadly effective across various Ni‑based systems, providing a generalizable route toward high‑energy, long‑life cathode materials.
Light, temperature, and humidity are critical external factors triggering phase separation in wide-bandgap (WBG) perovskite solar cells (PSCs). Conventional passivators only achieve static and short-term defect passivation and cannot address the continuously generated dynamic defects and ion migration during device operation. In this work, 1,3,3-trimethylindolino-6-bromobenzopyrylospiropyran (TBS) was introduced into the perovskite bulk. This molecule isomerized into the ring-opened O-TBS structure with abundant active sites under light, heat, and humidity stimuli, thereby enabling on-demand passivation of the device under various environments, ultimately achieving a synergistic balance between static passivation of pristine defects and dynamic repair of newly formed defects. Meanwhile, as a built-in dipole, O-TBS can accelerate carrier extraction and separation, and inhibit phase separation by optimizing the phase structure at the initial stage of nucleation and crystallization. Based on this strategy, a photoelectric conversion efficiency (PCE) of 23.83% was achieved in PSCs with a bandgap of 1.67 eV. Unencapsulated devices retained 91% of their initial efficiency after 1000 h of maximum power point tracking (MPPT) under AM 1.5G illumination, and maintained 88% and 87% of their efficiency after continuous testing for 1000 h at 85°C and 60% humidity, respectively, significantly enhancing the optoelectronic performance and long-term stability of the devices.
Bismuth ferrite (BiFeO3) thin films possess large ferroelectric polarization and antiferromagnetic order, yet their magnetoelectric coupling is limited by weak intrinsic magnetization. Here, a multiferroic morphotropic phase boundary (MPB) is demonstrated wherein the crystal structure, polarization, and magnetic order simultaneously evolve across a chemically induced phase boundary in strain-engineered (1-x)BiFeO3-(x)BaTiO3 thin films. Between 0.1 < x < 0.2, the crystal structure evolves from a monoclinic phase to a newly stabilized tetragonal phase through an intermediate mixed-phase region. This structural transition is accompanied by concurrent changes in magnetic order, resulting in dramatically enhanced functional responses as compared with those of BiFeO3. Specifically, films with x = 0.2 exhibit larger electromechanical strains (≈ 0.3%, about three-times larger than BiFeO3) and a significantly enhanced magnetoelectric-coupling coefficient (αME ≈ 416 mV cm-1 Oe-1, nearly 1000- and 19-times larger than bulk and thin-film BiFeO3, respectively). These enhancements diminish beyond the MPB (x > 0.2) and arise from polarization rotation and evolving spin configurations driven by the near degeneracy of competing ferroic states at the multiferroic MPB. These results establish a rare multiferroic MPB where both the polar and magnetic order evolve simultaneously, providing a promising strategy for designing materials with strongly coupled ferroic order parameters.
ABSTRACT The intrinsic physical anisotropy of low‐symmetry materials makes them highly promising candidates for polarization‐sensitive devices. However, their practical application remains constrained by the scarcity of single materials that can combine low symmetry with high performance. Here, we report a novel low‐symmetry [Bi 2 CuO 3 ]SO 4 crystal with an insulating nature, designed to enable symmetry control over conventional high‐performance semiconductors. We achieve controllable growth of layered [Bi 2 CuO 3 ]SO 4 nanosheets via a gradient‐mass‐transfer‐assisted chemical vapor deposition method, with thicknesses down to 1.43 nm. Alternating [Bi 2 CuO 3 ] 2+ cationic layers and SO 4 2− anionic layers, coupled with disparate ionic radii of Bi 3+ and Cu 2+ , endow the [Bi 2 CuO 3 ]SO 4 material with low structural symmetry, resulting in pronounced in‐plane optical anisotropy. Upon integration with high‐symmetry MoS 2 , [Bi 2 CuO 3 ]SO 4 induces interfacial symmetry breaking, driven by strong interfacial coupling and substantial charge redistribution. Notably, by fabricating devices along different crystallographic orientations of [Bi 2 CuO 3 ]SO 4 , tunable polarization ratios are exhibited, reaching a maximum of 5.44 along the a ‐axis and a minimum of 1.57 along the b ‐axis. This work establishes a reliable strategy for obtaining heterostructures with low symmetry and tunable anisotropy, advancing next‐generation directional optoelectronic devices.
The practical application of composite solid-state sodium metal batteries is critically limited by poor organic-inorganic compatibility, causing particle agglomeration, high interfacial resistance, and dendrite growth. Here, a covalent surface grafting strategy constructs a multifunctional interlayer covalently anchored on Na3Zr2Si2PO12, featuring a cross‑linked siloxane network and terminal ─NH2 groups. Covalent anchorage transforms inert particle surfaces into dispersible units, while ─NH2 groups anchor TFSI- and confine residual solvent via hydrogen bonding and Lewis acid‑base interactions. This dual regulation decouples ion transport from side reactions, yielding a high Na+ transference number (0.58) and a stable, NaF‑rich, thin solid‑electrolyte interphase (SEI). The optimized electrolyte enables symmetric cells with exceptional cycling stability and high critical current density (CCD). Full cells achieve fast‑charging (92 mAh g-1 at 15 C) and ultralong cycle life (76.4% retention after 7000 cycles at 10 C). A flexible pouch cell retains 97% capacity after 150 cycles. This work establishes that precise molecular‑level interfacial design, rather than simple physical blending, is key to high‑performance, dendrite‑resistant solid‑state sodium batteries.
Two intrinsically flexible conjugated polymers, PBT-90 and PFBT-90, were designed and synthesized via aldol polycondensation. Both polymers incorporate a novel double-flexible-node unit, 5,5'-bis(1,1,2,2-tetrafluoro-2-(thiophen-2-yl)ethyl)-2,2'-bithiophene, which can reduce brittleness and enhance recoverability in both bulk polymers and processed films. Both polymers displayed n-type charge transport in transistors fabricated on a polyethylene terephthalate substrate, achieving high electron mobilities (µe) of 3.85 and 4.56 cm2 V-1 s-1 for PBT-90 and PFBT-90, respectively, only slightly inferior to 5.44 and 6.37 cm2 V-1 s-1 of their fully conjugated analogues, PBT-100 and PFBT-100. Utilizing a self-developed PET/CYTOP/AlOx three-layer thin film transfer process, combined with orthogonal solvent design and interlayer protection strategies, we fabricated high-performance stretchable transistors. The PFBT-90-based devices exhibited a record-high µe of 3.51 cm2 V-1 s-1 in the pristine state. Under 100% strain, they retained a µe > 2.86 cm2 V-1 s-1 (>80% retention). The remarkable device performance originates from its suitable frontier molecular orbitals structure, low backbone glass transition temperature, and well-balanced finitely conjugated backbone, where rigid conjugated segments ensure highly efficient charge carrier transport and flexible nonconjugated segments dissipate stress. Our findings offer a pivotal molecular design strategy and a versatile fabrication process for advanced stretchable organic electronics.
Aniline is a critical chemical feedstock for dyes, pharmaceuticals, and polymers, but its synthesis via nitroarene hydrogenation demands harsh conditions, precious metal catalysts, and incurs a substantial environmental footprint. Solar-driven catalysis offers a sustainable alternative, but suffer from limited efficiency. Photothermal catalysis simultaneously utilize photothermal energy and charge carriers to overcome the reaction kinetics barriers, and has become a promising strategy. Here, we show that an Fe-aminoterephthalate MOF (NM-101) enables photothermal catalytic aniline synthesis with exceptional efficiency by synergistically coupling thermal energy and charge carrier activation. Under sunlight irradiation, NM-101 achieves an aniline production rate of 303.13 mmol·g-1·h-1 with 100% selectivity and a turnover frequency (TOF) of 226.2 h-1, surpassing all reported nonnoble metal photo(thermal)catalysts. Mechanistic studies reveal a direct hydrodeoxygenation pathway for the aniline production. In this process, photons not only provide thermal energy to drive the reaction but also generate carriers to participate in the reaction and reduce the activation barrier. When immobilized on 3D Al2O3 foam, NM-101 operates for 180 h and produces 42.2 g of aniline with a turnover number of 8470. This synergistic thermal and carriers overcomes kinetic bottlenecks in photocatalytic aniline production, demonstrating the feasibility and scalability of chemical synthesis using solar energy.
Lithium-ion batteries (LIBs) are central to the global energy transition, dominating the markets for electric vehicles and grid-scale renewable energy storage. However, as LIBs are pushed toward their theoretical energy density limits to meet ever-escalating performance demands, they are confronted with challenges to their intrinsic operational safety and long-term cycling stability. In recent years, protonic species within LIBs have been increasingly recognized as critical drivers of accelerated cell degradation and premature failure. In this contribution, we first recapitulate the diverse sources and generation pathways of protonic species, with a particular emphasis on the chemical and electrochemical oxidation of state-of-the-art carbonate-based electrolytes. Subsequently, we elucidate the proton-mediated failure network and associated self-amplifying proton-regeneration cycle, including electrolyte degradation and proton-driven parasitic interfacial side reactions at both the anode- and cathode-electrolyte interphases. Furthermore, we highlight critical advancements in in situ/operando characterization techniques for elucidating the sources and degradation mechanisms of protonic species, and propose a mitigation framework centered on proton source suppression and proton scavenging strategies. Finally, we pinpoint unresolved challenges and outline prospective research directions in this field. This contribution establishes critical connections between fundamental proton chemistry and failure modes, which will provide key strategic guidelines toward durable and safe high-energy-density LIBs.
The discovery of ferroelectric ScAlN sparked a search for new polar wurtzite alloys; however, incorporating transition metals remains a formidable challenge. Here, we demonstrate the synthesis of wurtzite-phase NbAlN, a polar transition-metal nitride alloy that is highly compatible with GaN-based heterostructures. Despite the strong metallic character of elemental Nb, we achieved coherent epitaxial NbAlN films that preserve the wurtzite crystal structure and metal polarity of the underlying GaN, as directly visualized by annular bright-field scanning transmission electron microscopy. Nb incorporation induces a monotonic lattice expansion and produces coherent Nb-enriched nanoscale regions that are accommodated within the continuous wurtzite framework. Functionally, NbAlN barriers induce a substantial enhancement in the two-dimensional electron gas density at the AlN/GaN heterointerface, consistent with polarization-related carrier modulation by the metal-polar NbAlN barrier. This study demonstrates that d-electron transition metals can be integrated into polar nitride systems without compromising their functional asymmetry, making NbAlN a promising building block for polar nitride heterostructures and carrier-density-engineered GaN electronics.
All-inorganic CsPbI3 perovskite solar cells are promising for durable photovoltaics owing to their superior resistance to thermal decomposition and halide segregation compared with hybrid counterparts. However, their photovoltaic performance remains hampered by poor crystalline quality arising from heterogeneous intermediate-phase evolution and nonuniform crystallization kinetics. Herein, an intermediate-phase homogenization strategy is developed to fabricate uniform CsPbI3 films, wherein calcium ascorbate regulates the intermediate phases through synergistic interactions with perovskite components-including electrostatic interactions, hydrogen bonding, and coordination bonding. This modulation approach effectively suppresses the formation of Cs4PbI6 intermediates and redirects the intermediate from a heterogeneous Cs4PbI6/DMAPbI3 mixture toward a predominant CsxDMA1-xPbI3(Asc) intermediate, yielding high-quality CsPbI3 films with improved structural and energetic homogeneity, as well as enhanced stability. The modified p-i-n CsPbI3 solar cells achieve a champion power conversion efficiency of 22.08%, among the highest reported for inverted CsPbI3 devices. Unencapsulated devices retain 97% of their initial efficiency after 1000 h of maximum power point tracking under 1 sun illumination at 40 ± 5°C in N2 and 94% after aging at 85°C for 500 h in N2. This work demonstrates the effectiveness of suppressing crystallization-kinetic heterogeneity for homogeneous perovskite films, offering a general strategy for rationally fabricating high-performance thin-film optoelectronic devices.
2D perovskites exhibit remarkable features such as strong X-ray absorption, high resistivity, and low ion migration, endowing them with high competitiveness in X-ray detection. Although numerous 2D perovskites (RP, DJ, and ACI phases) have drawn substantial attention, their widespread application is still restricted by excessively large interlayer spacing and limited structural stability. In this study, an aromatic diamine 2AMPY (2-aminomethylpyridine) is designed to enhance structural rigidity and reduce interlayer spacing of the 2D perovskites by modulating the tailored hydrogen bonding interactions and the embedding depth of organic cations within the inorganic octahedral frameworks. Moreover, high quality centimeter-sized 2D perovskites (2AMPY)PbX4 (X = Cl, Br, I) single crystals (SCs) are successfully grown via a solution method. Among them, (2AMPY)PbBr4 SCs display the shortest interlayer spacing and therefore the highest carrier mobility-lifetime product. As a result, detectors fabricated using these SCs achieve high sensitivity (13306 µC Gy-1 cm-2), ultralow detection limit (1.69 nGy s-1), superior stability, and high-resolution x-ray imaging. These detectors exhibit superior performance among the reported 2D perovskite X-ray detectors. In conclusion, this work establishes a new strategy for constructing novel 2D perovskite using aromatic diammonium cations, providing a promising solution for the development of X-ray detection technology.
In vitro models of the human neuromuscular system recapitulate key features of neuromuscular connectivity and are increasingly used to study disease mechanisms. However, activity-dependent adaptation and the contribution of endothelial cells (ECs) remain incompletely represented in vitro. Here, we establish a bottom-up, microchip-based method that supports motor innervation of three-dimensional (3D) human muscle and permits local or bath application of defined chemical stimuli. The same architecture also supports endothelial ingrowth, producing myobundles with concurrent neural and endothelial integration. Repeated local L-glutamate stimulation induced structural, metabolic, and transcriptional changes associated with activity-dependent muscle adaptation, whereas high-glucose exposure produced a distinct, largely opposing response. Addition of ECs further altered calcium dynamics in motor neurons (MNs) and innervated muscle fibers. This modular method enables controlled investigation of responses to neural, metabolic, and endothelial cues in engineered human neuromuscular system.